Daily Activities, Diet and Resource Use at Neolithic Çatalhöyük: Microstratigraphic and biomolecular evidence from middens 9781407307947, 9781407337869

Table of contents :
Cover Page
Title Page
Copyright
Abstract
Acknowledgements
INTRODUCTION
THE CASE STUDY AND SAMPLING STRATEGY
CHAPTER 3: METHODS ANDINSTRUMENTATION
4: THIN SECTION MICROMORPHOLOGY
5: PHYTOLITH ANALYSIS
6: SPECTROSCOPY AND SEM-EDX
7: BIOMOLECULAR ANALYSIS OF ORGANIC RESIDUES
8: DISCUSSION
References

Citation preview

BAR S2232 2011 SHILLITO DAILY ACTIVITIES, DIET AND RESOURCE USE AT NEOLITHIC ÇATALHÖYÜK

B A R Shillito 2232 cover.indd 1

Daily Activities, Diet and Resource Use at Neolithic Çatalhöyük Microstratigraphic and biomolecular evidence from middens

Lisa-Marie Shillito

BAR International Series 2232 2011

20/05/2011 14:24:29

Daily Activities, Diet and Resource Use at Neolithic Çatalhöyük Microstratigraphic and biomolecular evidence from middens

Lisa-Marie Shillito

BAR International Series 2232 2011

ISBN 9781407307947 paperback ISBN 9781407337869 e-format DOI https://doi.org/10.30861/9781407307947 A catalogue record for this book is available from the British Library

BAR

PUBLISHING

Abstract This research examines formation processes of middens and the associated activities at the site of Çatalhöyük, Turkey. Using this site as a case study, this research has wider significance for understanding the Neolithic of the region and for the study of middens in general. Middens are a unique deposit in that they contain traces of activities that may not be found in cleaner contexts such as floors, and contain materials such as ash, animal dung, phytoliths and coprolites which can inform on plant resource use, diet and subsistence strategies at a high temporal resolution. In this research thin section micromorphology is used, combined with phytolith analysis of individual layers, to examine both the composition and associations of finely stratified midden deposits in situ. Additional analyses of mineral components using FT-IR and SEM-EDX has been carried out, along with biomolecular analysis of organic residues in coprolites by GC-MS, to further characterise material that is difficult to analyse by thin section alone. This integrated analysis contributes to the understanding of midden formation processes and activities, as well as environment, agriculture, plant resource use, diet and fuel use. This analysis has developed a new method for classifying complex midden deposits based on their micro-inclusions and micro-structure, and has identified key deposits such as hackberry pericarps in coprolites, which can potentially be used as seasonal “markers”. Examination of midden deposits has provided direct evidence for the use of dung as fuel through the presence of faecal spherulites and reed phytoliths in fuel ash layers, and FT-IR analysis of material embedded in ash indicates clay deposits which could be linked to large open-air firing of pottery. This has wider significance for understanding early pyrotechnology during the Neolithic, and the widespread use of wetland resources i.e. reeds. The dominance of reed phytoliths in the midden assemblage supports the idea of a local wetland environment during the Neolithic. However, thin section observations indicate that phytolith taphonomy at the site is currently poorly understood, and that phytolith size is not a reliable indicator of the growing environment. The samples analysed were found to contain surprisingly few cereals, which also raises questions about the taphonomy of the non-charred cereal remains, and the role of crop growing in the economy. Analysis of coprolites, a frequent deposit in middens, has indicated the presence of lithocholic acid and coprostanol which indicate a human origin for much of this material. This has raised interesting questions on the idea of cleanliness, and has allowed further analysis of diet through observing phytoliths and other inclusions, such as bone, embedded in coprolites, both in situ in thin section, and through examination of extracted phytoliths.

i

Acknowledgements The site map and plans in Chapter 2 were kindly provided by the Çatalhöyük project. Thankyou to Ian Hodder for allowing me to carry out my research at the site and thankyou to Shahina Farid and all the excavators for their time and help with this research. I am grateful to the NERC LSMSF for the two grants which allowed the work in Chapter 7 to be carried out (LSMSF_Bristol_005; LSMSBRIS015_10/06), and the CCLRC for a Project Facility Grant for aspects of the work in Chapter 6. Thank you especially to Ian Bull for training in the analysis of coprolites and invaluable help in analysing and interpreting the results, and providing very helpful comments. Thank you to John Jack and Karen Gutteridge for extensive and invaluable help in thin section preparation. Arlene Rosen and Emma Jenkins for training in phytolith analysis and discussions of my results, Minolas Pantos and James Nicholson for help in SRS analysis at Daresbury. Thank you to my supervisors Matthew Almond and Wendy Matthews, and also to Joanne Wiles, Andrew Keyne, Tom Jefferies and Aleks Pluskowski for their friendship, support, and many essential coffee breaks.

ii

Abstract Acknowledgements

i ii

CONTENTS

iii

List of Figures List of Tables List of acronyms

vii x xi

1. INTRODUCTION

1

Midden formation processes and daily activity

1

People and environment – resource use and seasonality Environment Seasonality Resource use – fuel and fire Resource use – craft activities

2 2 2 3 4

Origins of agriculture and diet

4

Methods of enquiry Midden formation processes Thin section micromorphology Resource use, seasonality and diet. Phytolith analysis Spectroscopic techniques in archaeology Organic Residue Analysis

6 6 6 7 8 9 11

Integration of analytical techniques

13

Summary of analytical techniques used in this research

13

Specific research questions and hypotheses

14

Summary

15

2. THE CASE STUDY AND SAMPLING STRATEGY

16

The Case Study: Çatalhöyük, Turkey The organisation of excavation at Çatalhöyük Geology and soils and climate of the region Dating sequence at Çatalhöyük

16 17 18 19

Field work and sampling strategy South Area 4040 Area TP Area

20 21 22 25

Comparison of microanalysis data and field data

25

Summary of the case study and sampling

25

3. METHODS AND INSTRUMENTATION

26

Introduction

26

Laboratory sub-sampling for secondary analyses

26

iii

Thin section methodology Stage 1: resin impregnation Stage 2: slice cutting and temporary mounting Stage 3: grinding and polishing face Stage 4: permanent mounting Stage 6: hand finishing and coverslipping Analysis by optical microscopy

26 26 26 27 27 27 27

Phytolith methodology Stage 1: Carbonate removal Stage 2: Clay removal Stage 3: Organic matter removal Stage 4: Removal of non phytolith mineral material Stage 5: Weighing and mounting extracted phytolith material Quantifying phytoliths and interpretation of results

27 28 28 28 28 28 28

Fourier Transform Infra Red Spectroscopy (FT-IR)

29

Scanning Electron Microscopy and Energy Dispersive X ray analysis

29

Coprolite residue extraction method Stage 1: Soxhlet extraction Stage 2: Saponification Stage 3: Water removal Stage 4: Aminopropyl SPE extraction Stage 5: Neutral fraction processing Stage 6: Acid fraction processing

29 29 29 29 30 30 30

GC and GC-MS Instrumentation

30

GC-MS conditions

31

Summary of techniques used in this research

31

4. THIN SECTION MICROMORPHOLOGY

32

Introduction

32

Hypotheses to be tested Results Midden microscale inclusions Major inclusions – plant material Major inclusions – ash Major inclusions – coprolitic material Classification of coprolite types Major inclusions – mineral and rock material Major inclusions – burnt and unburnt aggregates Major inclusions – burnt and unburnt bone

32 32 34 34 41 41 41 42 42 42

Midden microstructure

43

Classification of Midden Deposit types

43

Post depositional and preservation features of middens

43

Summary of midden inclusions and microstructure

44

Microstratigraphy overview and discussion of integrated results by area South Area, Midden 1 (Levels VIII/VII) and Midden 2 (Level VI) South Area Macroscale Midden 1

44 44 44

iv

South Area Macroscale Midden 2 South Area Microscale of Midden 1 South Area Microscale of Midden 2 4040 area – Middens 3, 4 (Levels III, IV, V), 5 (Levels VI, VII) and 6 (Levels VI/V) Midden 3, 4 and 5 Macroscale analysis Midden 6 Macroscale analysis Midden 3, 4 and 5 Microscale analysis Midden 6 Microscale analysis Microscale postdepositional processes in 4040 middens TP Area – Midden 7 (Levels III – 0) Midden 7 Macroscale analysis Midden 7 Microscale analysis Post depositional processes observed at the microscale in Midden 7

44 45 45 46 46 46 47 48 48 48 59 50 50

Summary of micromorphology results

50

5. PHYTOLITH ANALYSIS

53

Introduction Previous phytolith research Advantages of the integrated approach Phytolith terminology Hypotheses related to phytolith analysis of middens Methods Results Major Phytolith types identified in midden deposits Single cell phytoliths identified Multi cell phytoliths identified Amorphous single cell phytoliths from dicotyledonous species Phytolith assemblages of high resolution sequences in middens South Area South area summary of assemblage 4040 Area 4040 area summary of assemblages TP Area Phytoliths from coprolites Phytoliths from repeated burning and ash layers

53 53 54 54 54 55 55 56 56 56 57 57 57 58 64 64 65 67 69

Discussion The assemblage based approach Classification of phytolith assemblage types Comparison with contextual observations in thin section Variations in phytolith types Discussion of results from the South Area Variable to consistent ratio Discussion of results from the 4040 Area Variations in phytolith types Discussion of results from the TP Area Variations in phytolith types Discussion of phytoliths from coprolites Variations in phytolith types Dietary implications of coprolite phytolith content Discussion of results from repeated burning and ash layers Variations in phytolith types General observations from phytolith analysis of middens Taphonomic considerations Consideration of phytolith types Seasonality Contributions to the study of fuel use

70 70 70 71 71 72 72 72 72 72 73 74 74 75 76 76 77 77 77 78 78

v

Conclusions from phytolith analysis

79

Further work on phytoliths

79

6. SPECTROSCOPY AND SEM-EDX ANALYSIS

80

Introduction

80

Reference materials FT-IR of reference materials Calcite, apatite and aragonite Quartz and opaline silica Clay minerals SEM-EDX of reference materials

81 81 82 82 82 83

Results Analysis of coprolites and other samples which potentially contain organic residues FT-IR of coprolites SEM-EDX studies of coprolites Analysis of phytoliths FT-IR of phytoliths SEM-EDX of phytoliths Analysis of other midden components of interest FT-IR and XRD of mineral nodules identified as gypsum FT-IR and XRD of Hackberry samples FT-IR of clay/aggregate samples found within ash layer and experimental clay burning FT-IR of sub sample sequence from thin section blocks 8932, 11016 and sequence of ashes from 12524 Sequence 8932 Sequence 11016 Sequence 12524

83 83 83 84 85 85 85 85 85 85 87 88

Discussion and summary Analysis of coprolites Analysis of phytoliths Analysis of hackberries and gypsum nodules Analysis of micromorphology sub-sample sequences Conclusions

90 90 91 91 91 92

7. BIOMOLECULAR ANALYSIS OF ORGANIC RESIDUES

93

Introduction Current methods of identifying faecal material and problems Advantages of biomolecular analysis Sterols and bile acids Previous studies using sterols and bile acids as faecal biomarkers Hypotheses and aims of this investigation

93 93 93 94 95 97

Sample selection and methods

97

Results Analysis of sterols Bile acids

98 98 99

Discussion Samples containing faecal residues Samples containing non-faecal residues Samples containing no residues Identification of coprolitic deposits in the field Identification of coprolites in burials

101 101 102 102 102 102

vi

89 89 90

Identification of coprolites in middens and open areas Identification of coprolitic material from middens in thin section Implications of faecal residues for the interpretation of midden formation processes and human activity

102 103 103

Conclusions Further work

105 105

8. DISCUSSION

106

Introduction

106

Midden formation processes and activities identified Identification of midden deposits from thin section analysis and macro scale observation Phytolith variations in deposits Midden accumulation rates Activities identified from thin section and phytolith analyses Activities identified Activities not identified Summary of midden formation processes and activities

106 106 107 108 108 108 110 110

People and environment - Resource use and seasonality Environment Seasonality and cyclicity of activities Identification of “seasonal” indicators in midden layers Cycles in midden formation processes and possible seasonality Problems in determining seasonality

110 110 111 111 112 113

Resource use – fuel, fire and craft activity Ash and the use of plant resources as fuel - Contribution to questions of fuel use Craft activity

113 114 115

Origins of agriculture and diet Phytolith evidence for cereal consumption in midden deposits Evidence for diet from coprolites Organic residue analysis of coprolites Phytolith analysis of coprolites from spot sampling and thin section analysis Dietary evidence from other inclusions in coprolites

115 115 116 116 117 118

Methodological developments Screening of coprolites for GC-MS using FT-IR

118 118

The importance of specific context for phytolith analysis Micromorphology and integrated microanalysis

119 119

Limitations and Future work CONCLUSIONS

119 120

References

122

List of Figures Figure 1.1: Figure 1.2: Figure 1.3: Figure 1.4: Figure 1.5: Figure 1.6: Figure 1.7:

Multiple fine layers in Midden 1 in the South Area. Burning dung fuel in the reconstructed oven in the experimental house. Photograph to illustrate the dimensions of a single midden (Midden 2, South Area). Phytolith basketry impression from unit 3228, Building 5, in the North Area (left), and matting impression from unit 10406, Building 42, in the South Area (right). The symmetric stretches of the free carbonate (CO32-) or silicate (SiO44-) ions. Faecal spherulites in thin section at x100 (above) and x200 (below). An individual spherulite is circled in red. Structure of 5β-coprostanol (a) and lithocholic acid (b).

vii

1 3 4 5 10 11 11

Figure 1.8:

Coprolite material in thin section, showing pseudomorphic voids and a fish tooth. The coprolite is suggested as human (Matthews al. 1996).

Figure 2.1: Figure 2.2: Figure 2.3: Figure 2.4: Figure 2.5: Figure 2.5:

Map showing the location of Çatalhöyük in Turkey. Site plan of Çatalhöyük showing the different excavation areas Map showing the geomorphology of Central Anatolia (Kuzucuoğlu 2002). Dates of Çatalhöyük levels (from Cessford et al. 2005). Section drawing of Midden 1, South Area, Unit 1668, East face. Section drawing of the South Area Midden 2, West and North faces 2006, showing positions of thin section block samples and organic residue samples (marked with crosses).2.2.2 4040 Area 4040 area, Midden 6, West face detail. Wide angle photograph to include whole section. Photograph from the Çatalhöyük Image Collection database at http://sac.stanford.edu/res/sites/Catalhoyuk/ Plan of buildings in the South Area. Plan of buildings around Space 280, showing location of Midden 3, 4, 5 and 6 Details of features around Space 287 TP area section, Midden 7. Sample collection procedure. Equipment set up for the addition of epoxy resin under vacuum to micromorphology samples. Diagrammatic summary of the GC-MS extraction method utilised in this work (after Bull, pers. comm.) Stacked bulliform phytoliths from Phragmites in extensive layer of articulated reed and grass phytoliths. PPL. Midden 6, 13103 S26. Calcitic plant ash with (a) typical rhombohedral crystals (Canti 2003) PPL. Midden 6, sample 13103 S26. Type 1 coprolite showing amorphous yellow organic material with bone and charred plant inclusions (a) overlain by a linear bone fragment (b) and burnt plant material (c). Midden 7, sample 8932 S7. Longitudinal section, stacked bulliform phytoliths from Phragmites PPL. Midden 7, 8932 S3. Transverse section of burnt wood charcoal showing tissue structure PPL. Fragment of volcanic rock observed in Midden 2, South Area, sample 12519 S9. Type 3a coprolite showing black spots which indicate possible microbial activity. Midden 3, sample base of 11016 S2. Type 3b. Like 3a but with more visible phytolith inclusions. Midden 2, sampling 12558 S2. Coarse reddish brown plant tempered aggregate with pseudomorphic voids (a) indicating building material, possibly mudbrick or oven plaster. Aggregate type 1. Midden 3, 11016 S2. Brown type aggregate with abundant charred plant inclusions (black flecks). Finely grained with fewer coarse mineral inclusions. Aggregate type 2. Midden 7, sample 8932 S7. Silty calcitic grey aggregate with shell or ostracod inclusions and pseudomorphic voids, indicating building plaster. Partially burnt bone PPL. Midden 7, sample 7867 S2. Calcareous aggregate with large rounded and sub rounded mineral inclusions. Showing modern root material (a) and bioturbation from root channels PPL. Midden 3, sample 11016 S2. Figure 4.14 under XPL showing the root channel filled with gypsum crystals. These also act to disaggregate the material. calcareous spherulites in XPL from ash layer indicating dung ash Calcitic ash layer of 13103 S25 in PPL showing phytolith inclusions Type 1 coprolite from 3922.10 room deposit, identified as human by GC-MS, showing phytolith inclusions and pseudomorphic voids. Large articulated Phragmites stem fragment (a) partially embedded and partially exposed within a void PPL. Midden 6, sample 13103 S26 Articulated possible Phragmites (a). The stomatal cells are only just visible. Thin sections are 30 µm thick, but phytoliths are only 3-5 µm thick so are easily obscured by other material PPL. Midden 6, sample 13103 s26. Small Phragmites stem fragment embedded in a mix of ashy and organic material (a). This illustrates the difficulty of seeing phytoliths in thin section PPL. Midden 7, 8932 S3. Brown stained stem phytoliths (a) and charred black Phragmites phytoliths (b) PPL. Midden 2, sample 12558 S2. Articulated grass and reed stems in mixed ash layer. PPL. Midden 6, 13103 S25. Type 2 coprolite with phytolith inclusions (a) PPL. Midden 7, sample 8932 S7. Photograph of Midden 1, Units 1668. For section drawing see Chapter 2, Figure 2.12. Photograph of Midden 3 in the 4040 area, units 11016 and 11017. Space 232. Photograph of Midden 4, unit 10711, room fill midden deposit. Photograph of Midden 5, unit 7931, room fill midden material between walls. Midden 6, 4040 Area. Photograph of Midden 7 Units 8932 and 7867 TP area. Arrow points to a particularly dense concentration of gypsum nodules. Photograph of Midden 2 showing the cut that separates the two phases of midden deposition. Graph illustrating the relationship between size and abundance of charred plant material in thin section. Numbers refer to deposit type categories in Table 4.4 Graph illustrating the relationship between size and abundance of phytolith material in thin section. Numbers refer to deposit type categories in Table 4.4. Thin section sample 13103 S20 from Midden 6 showing (a) non burnt aggregates from large building demolition debris with (b) pre depositional layering in one aggregate fragment, and (c) partial pre depositional burning in another fragment Weight percent phytoliths per gram of sediment for block 1668 sequence, Midden 1. Percentage contribution of each phytolith type to the overall phytolith assemblage in block 1668, Midden 1 (single cells). Microscope photographs of the major phytolith types present in the samples. Starting top left and reading downwards: 1. Rugulose spheroid 2. Keystone bulliform 3. Smooth long cell 4. Crenate 5. Trichome 6. Rondel (tower type) 7. Amorphous phytoliths from wood 8. Smooth long cell, bulliform and dendritic long cell 9. Wild grass husk 10. Saddle 11. Phragmites leaf 12. Reference of Setaria italica showing hairs/trichomes and bilobes 13. Cyperaceae multi cell 14. Celtis type. 15. Conjoined wheat husk Extracted Phragmites multi cell phytolith. Midden 7, 8932 S7 /05 (observed in thin section as yellowish amorphous fine fabric with ashy grey areas). Extracted sedge multi cell, Midden 7, 8932 S7/ 08 (sub sample observed in thin section as mixed charred plants and Phragmites and grass leaf/stem cells, Midden 7, 8932 S7/08 (observed in thin section as mixed charred plants)

Fiigure 2.6: Figure 2.7: Figure 2.8: Figure 2.9: Figure 2.10: Figure 2.11: Figure 3.1: Figure 3.2: Figure 4.1: Figure 4.2: Figure 4.3: Figure 4.4: Figure 4.5: Figure 4.6: Figure 4.7: Figure 4.8: Figure 4.9: Figure 4.10: Figure 4.11: Figure 4.12: Figure 4.13: Figure 4.14: Figure 4.15: Figure 4.16: Figure 4.17 Figure 4.18: Figure 4.19: Figure 4.20: Figure 4.21: Figure 4.22: Figure 4.23: Figure 4.24: Figure 4.25: Figure 4.26: Figure 4.27: Figure 4.27: Figure 4.28: Figure 4.29: Figure 4.30: Figure 4.31: Figure 4.32: Figure 4.33: Figure 5.1: Figure 5.2: Figure 5.3:

Figure 5.4: Figure 5.5: Figure 5.6:

viii

11

16 17 19 19 20 21 21 22 22 22 24 24 27 30 36 36 36 36 36 36 37 37 37 37 37 37 38 38 38 38 38 38 39 39 39 39 39 39 40 40 40 40 40 40 40 41 41 49 59 60 63

64 64 64

Figure 5.7: Figure 5.8: Figure 5.9: Figure 5.10: Figure 5.11: Figure 5.12: Figure 5.13: Figure 5.14: Figure 5.15: Figure 5.16: Figure 5.17:

Phragmites stem, Midden 7, 8932 S7/11 (observed in thin section as containing large bone and charcoal fragments, underneath ashy layer). Extracted husk phytolith and dendritic long cells from coprolite sample 12519 S7, South Area Midden 2. Extracted grass and reed stem cells from ash layer 12524 S15, South Area Midden 2. Organic material with articulated stem cells. Midden 2, 12558 S2. Husk phytolith in mixed deposit. Midden 7, 8932 S7. Articulated stem with hair cells in phytolith/charcoal layer. Midden 2, 12558 S2. Phragmites multi cell within ash deposit. Midden 2, 12558 S2. Phragmites stacked bulliforms in partially mixed ashy/organic layer, Midden 7, 8932 S9. 8932 S7 partially charred reeds and grasses 13103 S29 Phragmites stem showing bulliforms and wave Wheat husks from in situ decay sample 12519 S9

64 64 64 64 65 65 65 65 65 65

Figure 5.18: Figure 5.19: Figure 5.20: Figure 5.21: Figure 5.22: Figure 5.23: Figure 5.24: Figure 5.25: Figure 5.26:

In situ decay of plants in 13193 S26, showing long cells and rondels In situ decay of reeds in 13103 S26 showing stacked bulliforms Percentage contribution of each phytolith type to the overall phytolith assemblage in block 1668 Midden 1 (multi cells). Graph showing the weight percent of phytoliths from the 11017 sequence, Midden 3. Percentage of each phytolith type of the total assemblage for the 11017 sequence, Midden 3 (single cells). Percentage of each phytolith type of the total assemblage for the 11017 sequence, Midden 3 (multi cells). Weight percentage of phytoliths in the 8932 sequence, Midden 7 (2 thin section blocks). Microscope photograph of phytoliths from sample 13103 S24, Midden 6. Graph showing the weight percent phytoliths per gram of sediment for coprolite samples.

65 65 60 67 67 67 67 69 69

Figure 5.27

Stacked chart showing the relative percentages that each phytolith type contributes to the overall assemblage in coprolite samples (single cells). Stacked chart showing the relative percentages that each phytolith type contributes to the overall assemblage in coprolite samples (multi cells). Graph showing the weight percent phytoliths per gram of sediment for the ash sequence (Midden 2, Unit 12524). A photograph of this ash sequence can be seen in Chapter 6, Figure 6.45. Graph showing the relative percentage of each phytolith type in the burning/ash sequence (Midden 2, Unit 12524) from the South Area (single cells). Graph showing the relative percentage of each phytolith type in the burning/ash sequence (Midden 2, Unit 12524) from the South Area (multi cells). Graph showing the floral:stem ratio for phytoliths from 1668 S12, Midden 1. Comparing the n/gm of dendritic and husk phytoliths from 1668 S12, Midden 1. Graph comparing the mutli cell : single cell ratio for the phytoliths from the 1668 samples, Midden 1. Graph showing the variable: consistent ratio for phytoliths from the 1668 samples, Midden 1. Graph comparing the numbers per gram of dendritic long cells and smooth long cells for the 11017 sequence, Midden 3. Graph comparing the ratio of floral: stem phytoliths for the 11017 sequence, Midden 3. Graph comparing the numbers per gram of dendritic long cells and husks for the 11017 sequence, Midden 3. Graph comparing the numbers of phytoliths per gram of different husk types in the two samples from 11017 containing wheat husks. Graph comparing the multi cell: single cell ratio for the 11017 sequence, Midden 3. Graph comparing the variable: consistent ratio for the 11017 sequence, Midden 3. Comparison of C3 and C4 phytolith types from the 11017 sequence, Midden 3. Graph comparing the n/gm of dendritic long cells and husk phytoliths for 8932 sequences, Midden 7 Graph showing the floral: stem ratio for phytoliths from the 8932 sequences, Midden 7. Chart showing variations in the type of short cells in coprolite samples. Graph showing variations in the numbers of smooth and dendritic long cells in the coprolite samples. Variations in the numbers of dendritic long cells and husks in the coprolite samples. Variations in the multi cell: single cell ratio in the coprolite samples. Graph showing the floral: stem ratio in the coprolite samples. Graph showing the variable: consistent ratio in the coprolite samples. Graph comparing the numbers per gram of dendritic long cells and smooth long cells for ash sequence (12524, Midden 2). Graph showing the floral: stem ratio for the ash sequence (12524, Midden 2). Graph comparing the numbers per gram of dendritic long cells and husks for ash sequence (12524, Midden 2). Graph showing the multi cell: single cell ratio for the ash sequence (12524, Midden 2). Graph showing the variable: consistent ratio for the ash sequence, Midden 2. highly silicified wheat husk with c. 120 conjoined cells from 12519 12519 wheat husks in thin section showing layers of husks possibly from crop processing Graph showing variations in the number of amorphous dicotyledonous phytoliths per gram in all the samples sequences studied. Tetrahedral SiO44- unit (left) and octahedral AlO69- (right). FT-IR spectra of reference kaolinit and montmorillonite Reference spectra of opal and quartz SEM photograph of keystone bulliform phytolith. South Area, Midden 1, 1668/02. SEM photograph of grass stem cells SEM photograph of Phragmites leaf SEM-EDX for 13103 s24. Hackberries in coprolite deposit FT-IR spectrum of gypsum nodule FT-IR spectra of hackberry and reference calcite and aragonite XRD for hackberry Orange aggregate material embedded within large ash layer, unit 12524, Midden 2, South Area. Repeated burning and ash layers in the South Area FT-IR spectra of the 12524 ash sequence

69

Figure 5.28: Figure 5.29: Figure 5.30: Figure 5.31: Figure 5.32: Figure 5.33: Figure 5.34: Figure 5.35: Figure 5.36: Figure 5.37: Figure 5.38: Figure 5.39: Figure 5.40: Figure 5.41: Figure 5.42: Figure 5.43: Figure 5.44: Figure 5.45: Figure 5.46: Figure 5.47: Figure 5.48: Figure 5.49: Figure 5.50: Figure 5.51: Figure 5.52: Figure 5.53: Figure 5.54: Figure 5.55: Figure 5.56: Figure 5.57: Figure 5.58: Figure 6.1: Figure 6.2: Figure 6.3: Figure 6.4: Figure 6.5: Figure 6.6: Figure 6.7: Figure 6.8: Figure 6.9: Figure 6.10: Figure 6.11: Figure 6.12: Figure 6.13: Figure 6.14:

ix

64

69 71 72 72 74 74 74 74 75 75 75 76 76 76 76 76 77 77 77 77 77 78 78 78 79 79 79 79 80 80 81 85 85 86 87 87 87 87 89 89 89 90 90 91 92

Figure 6.15: Figure 7.1:

Figure 7.2: Figure 7.3: Figure 7.4:

Figure 7.5: Figure 7.6: Figure 7.7: Figure 7.8: Figure 7.9: Figure 7.10: Figure 7.11: Figure 7.12: Figure 7.13: Figure 7.14: Figure 7.15: Figure 7.16: Figure 7.17: Figure 7.18: Figure 8.1: Figure 8.2: Figure 8.3: Figure 8.4: Figure 8.5: Figure 8.6: Figure 8.7: Figure 8.8: Figure 8.9: Figure 8.10: Figure 8.11: Figure 8.12: Figure 8.13: Figure 8.14: Figure 8.15: Figure 8.16: Figure 8.17: Figure 8.18: Figure 8.19:

FT-IR spectra of experimentally heated clay Structures of major lipid and bile acid biomarkers detected. 1. Coprostanol 2. Epicoprostanol 3. 5β-campestanol 4. 5βepicampestanol 5. 5β-stigmastanol 6. 5β-epistigmastanol 7. Cholesterol 8. 5β-cholestanol 9. Campestanol 10. Sitosterol 11. Hyodeoxycholic acid 12. Deoxycholic acid 13. Lithocholic acid 14. Chenodeoxycholic acid 15. Hyocholic acid. Data from Bull et al. (1999). The route of formation and deposition of 5b-sterols and 5a-stanols formed from cholesterol, campesterol and sitosterol (from Bull et al. 1999). A summary of the criteria used to determine the source of faecal material using multiple biomarkers, redrawn from Bull et al. 2002. GC trace for sample 15 (2754 S2) showing structures of major biomarkers that determine the order of elution. Shaded peaks indicate the first biomarker in each homologous series. 1: coprostanol 2: cholesterol 3: 5α-cholestanol 4: 5β-campestanol 5: 5β-stigmastanol 6: 5α-campestanol 7: sitosterol 8: 5α-stigmastanol. Figure courtesy of Dr Ian Bull, University of Bristol. Ratios for sample set A. Ratios for sample set B. GC trace for sample 11 (8932 S3/09) 1. coprostanol 2. epicoprostanol 3. cholesterol 4. 5α-cholestanol 5. 5β-campestanol 6. 5β-epicampestanol 7. 5β-stigmastanol 8. 5β-epistigmastanol 9. sitosterol 10. 5α-stigmastanol. GC Trace for sample 18 (2754 S4) 1. coprostanol 2. epicoprostanol 3. cholesterol 4. 5α-cholestanol 5. 5β-campestanol 6. 5βepicampestanol 7. 5β-stigmastanol 8. 5β-epistigmastanol 9. sitosterol 10. 5α-stigmastanol. GC trace for sample 4 (1494 S6) 1. coprostanol 2. epicoprostanol 3. cholesterol 4. 5β-stigmastanol 5. 5β-epistigmastanol 6. sitosterol 7. 5α-stigmastanol. GC trace from sample 3 (12519 S7) 1. coprostanol 2. epicoprostanol 3. cholesterol 4. 5α-cholestanol 5. 5β-campestanol 6. 5βepicampestanol 7. 5β-stigmastanol 8. 5β-epistigmastanol 9. sitosterol 10. 5α-stigmastanol. GC trace for sample 7 (13103 S27) 1. coprostanol 2. epicoprostanol 3. cholesterol 4. 5α-cholestanol 5. 5β-campestanol 6. 5βepicampestanol 7. 5β-stigmastanol 8. 5β-epistigmastanol 9. sitosterol 10. 5α-stigmastanol. GC trace for sample 11(8932 S3/09) showing the presence of LC and DOC bile acids. HC is the internal standard. GC trace for sample 18 (2754 S4) showing the presence of LC and DOC bile acids. HC is the internal standard. GC trace for sample 4 (1494 S6) showing the presence of LC and DOC bile acids. HC is the internal standard. GC trace for sample 3 (12519 S7) showing the presence of LC and DOC bile acids. HC internal standard not shown. GC trace for sample 7 (13103 S27) showing the presence of LC and DOC bile acids. HC is the internal standard. Block 8932 S3 (Midden 7, TP Area) and organic residue samples 8932 S3/05, 09 and 13. Microscope photographs show the appearance of the coprolites under PPL at x10 magnification. 05 and 09 are human, 13 is human mixed with other organic residues. Block 13103 S26 (Midden 6, 4040 Area) showing location organic residue sample 13103 S27, identified as human. Microscope photographs show the appearance of the coprolite under PPL at x10 (above) and x20 (below) magnification. Aggregate in sample 13103 S29 at x4 magnification, showing pseudomorphic voids from decayed plant material (aggregate type 4). From Midden 6 in the 4040 Area. Possible activities at Çatalhöyük and how materials may be deposited within middens. A seasonal schedule of activities showing changing environmental conditions and suggested population conditions (Fairbairn et al. 2005a). Midden 2 (South Area), hackberries in north face in fine layering above large ash layer. Samples with increased ratios of dendritic to smooth phytoliths. Midden deposit sequences. Polyhedral phytolith in 1542. Polyhedral phytolith in 1542. An example of a cluster of hackberries in the field, Midden 2, South Area. Single cell phytoliths in 1542, South Area, Midden 1. Husk and dendritic phytoliths from 4477, Midden 1, South Area. Husk and dendritic phytoliths from 4477, Midden 1, South Area. Short cells phytoliths in coprolite samples. Long cell phytoliths in coprolite samples. Coprolite with embedded phytoliths in sample 12558 S2, Midden 2, South Area. Coprolite with embedded phytoliths in sample 12558 S2, Midden 2, South Area. Bone fragment embedded in coprolite sample 12558 S2, Midden 2, South Area. Bone fragment (b) embedded in coprolite sample 8932 S3/05, Midden 7, TP Area. Phytoliths (a) and bone fragments (b) embedded in coprolite, sample 8932 S3/09, Midden 7, TP Area.

93 97

97 98 100

101 102 102 103 103 103 103 103 103 104 104 104 108 108 340 344 352 354 356 361 372 372 373 373 374 375 375 376 376 377 378 378 379

List of Tables Table 1.1: Table 2.1: Table 2.2: Table 3.1: Table 3.3: Table 3.4: Table 3.5: Table 4.1: Table 4.2: Table 4.3: Table 5.1: Table 5.2: Table 5.3: Table 5.4: Table 5.5: Table 5.6:

Summary of analytical techniques used in this research and rationale for their selection Summary of the Çatalhöyük excavation areas. Summary of micromorphology samples. Summary of stages in thin section methodology Summary of the stages in phytolith sample preparation. Summary of the stages in the residue extraction method Summary of techniques used and research rationale. Area and level of samples studied (see Chapter 2 for an explanation of area, space and level). Summary of midden inclusion types. Summary of midden deposit type classifications. Common phytolith names used in this thesis and the official ICPN terminology (ICPN terms Madella et al. 2005). Summary of phytolith samples analysed and associated thin section blocks Summary of phytolith types encountered and their relative frequencies. A list of common Gramineae/Poaceae from archaeological literature and some important characteristics. Number of phytoliths per gram (n/gm) for 1668 samples, Midden 1. Phytolith numbers per gram for the 11017 sequence, Midden 3.

x

15 17 23 26 27 29 31 33 34 51 175 177 178 183 190 194

Table 5.7: Table 5.8: Table 5.9: Table 5.10: Table 6.1: Table 6.2: Table 6.3: Table 6.4: Table 6.5: Table 6.6: Table 6.7: Table 7.1: Table 7.2: Table 7.3: Table 7.4: Table 7.5: Table 8.1: Table 8.2:

Numbers of phytolith per gram for the coprolite samples. Numbers of phytoliths per gram for the ash sequence (12524, Midden 2). Correlations between selected phytolith data sets. Phytolith assemblage types and possible associated activities. Summary of samples whose spectra are presented. The coprolite samples were also analysed by GC-MS, details are given in Chapter 7, Table 7.3. Summary of coprolite samples analysed with SEM-EDX. Summary of phytolith samples analysed by SEM-EDX.

200 203 205 206 84

Reference data for sterols showing molecular weight and characteristic fragment ions present in the mass spectra of the methyl ester – trimethylsilyl ether derivatives. Data from Bull et al. (1999, 2002). Reference data for bile acids. Data from Elhmmali et al. (1997). Summary of samples selected for organic residue analysis. Summary of bile acids present in the samples analysed. Summary of ratios and which species these indicate for both sample sets. Summary of possible activity types expected and observed at Çatalhöyük, related micromorphological features, and deposit types identified in the samples studied which show these features. Expected seasonal indictors (W. Matthews n.d. after Fairbairn et al. 2005a and Hodder ed. 2005).

99

Acronyms SEM-EDX FT-IR IR GC GC-MS AAS SRS XRD CCLRC NERC LSMSF RETF

Scanning Electron Microscopy – Energy Gispersive X-Ray Analysis Fourier Transform Infra Red Spectroscopy Infra Red Gas Chromatography Gas Chromatography Mass Spectrometry Atomic Absorption Spectroscopy Synctrotron Radiation Source X-Ray Diffraction Council for the Central Laboratory of the Research Councils Natural Environment Research Council Life Sciences Mass Spectrometry Facility University of Reading Research Endowment Trust Fund

xi

240

99 99 105 106 345 355

xii

of information, for example in understanding discard practises (Martin and Russell 2000), they are excavated in large units which do not represent actual units of deposition. Specialist research on animal bone assemblages and plant macro remains from middens are routinely limited to these large units, which represent multiple discard events. The research conducted aims to examine the information from individual layers in middens to complement and expand upon what has been learnt from other methods of enquiry at the site. In order to study midden formation processes, a number of techniques have been selected, to study middens from the macro to micro scale. In this introduction a critical review is given of previous research on the research questions relating to environment, diet and resource use, and how the present research aims to extend and build upon this. Following this an overview is given of the research methods selected, and how these have previously been employed in archaeology, discussing how they will be integrated and employed in the present research.

INTRODUCTION The Neolithic of the Near East is a subject of archaeological research which has worldwide significance, being of key importance to substantive issues including the development of human interactions with the environment, and the origins and development of agricultural practices and animal domestication. Çatalhöyük, the case study which is examined here, is a key site in the understanding of the development of early society in the region, and is of importance both for Turkish and global heritage. Since the initial excavations here in the 1960s (Mellaart 1967), it has become recognised as an internationally significant site, one of the first “towns” in the world. Initially of interest due to the exceptional wall paintings and wall art, it has become key in our understanding of the origins of agriculture and settlements. Central questions of the research at Çatalhöyük include the origin of the site and socio economic development and variation, including reasons for the adoption and intensification of agriculture, the beginnings of ceramic use, and its relationships with other sites in the region (Hodder 2006).

Midden formation processes and daily activity Middens are traditionally defined as archaeological refuse deposits (Schiffer 1987). The study of midden formation processes enables us to infer cultural and natural events that create the archaeological assemblage. The study of midden formation process is important, as middens are a rich but often underutilised source of information, containing a wide range of important deposits relating to activities such as food processing, cooking, diet and discard (Hodder 1996). In turn these deposits can be interpreted to understand broader issues such as human and environment relationships. It has been noted that at Çatalhöyük, as at many tell sites, there are few archaeological remains to be found on the floors within buildings that can help us understand what those rooms were used for, as the larger artefactual remains of activities are carried or swept away (Rosen 1989, Hodder and Cessford 2004). The microstratigraphy of these buildings has been created by human activity, and thus can be interpreted to give us information on human behaviour (Matthews 2005). The midden deposits are equally as important, but so far have been studied in much less detail than other contexts at the site, despite them being, as Hodder and Cessford (2004 p. 29) describe, “the end product of very careful regulation of daily practises inside the house”. As such they are important sources of information on short and longer term sequences of activities, and fundamental to linking the themes of seasonality and cyclicity with resource use, agriculture and diet.

A particular issue of debate is the traditional assumption that the Neolithic of the Near East is a crucial transition between two starkly contrasting human cultures i.e. nomadic hunter gatherers versus settled agriculturalists (Barker 2006). Current research at Çatalhöyük, under the direction of Professor Ian Hodder since 1992 is beginning to suggest that the traditional model is flawed and that the gathering of wild resources was still important at Çatalhöyük. The extent of reliance on each of these sources however, is debated, with some arguing for agricultural production as a key component of the food economy (e.g. Fairbairn 2005), and others placing a more equal importance of wild food resources (Atalay and Hastorf 2006). This research aims to contribute to our understanding of the Neolithic in the Near East through examining midden formation processes at Çatalhöyük, which can help identify sequences of domestic and craft activities, such as, food processing, preparation and consumption, fuel use, and basketry and lithic production. These activities are closely linked to questions of food procurement and production, diet and resource use. Questions of diet include wild versus domesticated resources, the consumption of plant versus animal products, and possible temporal or seasonal variations in the exploitation of these, based on availability or preference. Questions of resource use include types of fuel and their links to domestic and craft activities.

At Çatalhöyük, midden research has been focused on evidence from components and artefacts such as: animal bones as indicators of animal management strategies, domestication and food (Russell and Martin 2005); charred plant macroremains and charcoal as indicators of fuel use, crop use and other food (Fairbairn et al 2002, Asouti and Austin 2005); and artefacts such as lithic debris (Carter et al. 2006, Carter et al. 2008) and pottery recovered during excavation and flotation. Questions

These questions are approached in this research through examining midden formation processes, and subsequently, human activities. Whilst the floors of buildings and primary deposits are often very clean (Matthews 2005), middens are a major source of domestic residues, containing a rich range of sediments and bioarchaeological and micro-artefactual remains. Although middens are recognised as an important source 1

arising from this previous research include the relative importance of cereals and wild plants, the change in fuel use from mixed wood types to a predominance of oak, and changing technological strategies.

with other material, it will be possible to distinguish between multiple possible sources, for example plants deriving from animal dung or coprolites by studying spherulites, fine fabric and contents, or fuel by examination of phytoliths in different type of ash, or food processing. The use of these resources for specific activities can be examined through the association with other depositional components such as craft debris, for example phytolith ash with pottery. This provides firmer evidence and a better distinction between the deposits than using a single technique.

The units of study for this previous research have been the excavation units. Thus these midden components have been separated from their associations, as well as having several depositional units combined. This creates an artificial sequence of deposition in which these components are interpreted, and blurs any cyclical or seasonal patterns, giving instead longer trends over the lifespan of the midden. In addition, charred plant macro remains and charcoal only represent plant remains which have been subjected to low temperature burning (Boardman and Jones 1990).

Environment A detailed review of the paleoenvironment of the Konya plain at the time of Çatalhöyük’s occupation, and questions relating to this, is provided when discussing the nature of the site in Chapter 2. In studying human activity and possible seasonal or cyclical patterns in activity, a consideration must be given to the environment affecting these activities. In particular the study of phytoliths in context will contribute to the debates of dryland versus wetland habitat exploitation, including proximity to the site and for cereal cultivation (Roberts and Rosen 2009; below and Chapter 4 for a detailed discussion of this debate). Experimental phytolith work in Israel suggests plants growing under wetland conditions in alluvial soils produce larger multicell phytoliths due to increased availability of silica (Rosen and Weiner 1994), so it would be expected that cereals being grown in the marshy environment adjacent to the site would have large multicell phytoliths. In addition, phytolith analysis provides evidence for wetland species such as Phragmites that may not be represented in the charred plant record, which is recognised to contain only a certain portion of the plants that may have been present on site (Van der Venn 2006). Previous research at Çatalhöyük suggests cereals were cultivated on drylands, based on scarcity of large multi-cell husks (Rosen 2005), but does not consider taphonomic processes that impact multicell phytolith size and articulation. By considering phytoliths within their precise depositional context using thin section analysis, such problems can be better understood.

There has been little consideration of the importance of the deposits themselves as data sources, and the importance of examining individual layers (Figure 1.1), which have previously been considered too fine to examine individually (Yeomans 2005). Although previous micromorphological work by Matthews et al. (1996) has identified possible microremains relating to activities such as wood working, possible cereal parching, and floor sweepings. More often such micro deposits, for example phytoliths, are analysed out of context (Madella 2001, Rosen 2005). The context and associations of midden components are essential sources of information, as they enable the interpretation of exactly how the components were discarded as well as their covariance and context, which are fundamental to the investigation of different activities.

There is a suggestion of increasing dryness after 7000 BC based on an increase in juniper (Asouti 2005), with earlier levels showing a greater proportion of riverine species, and a greater proportion of amphibian remains in the microfaunal record (Jenkins 2005b). By examining phytoliths from sequences in Levels VII and VI, c. 6,600400 BC, this research will examine whether this hypothesis is supported by changes in fuel use from the phytolith record.

Figure 1.1: Multiple fine layers in Midden 1 in the South Area.

People and environment – resource use and seasonality Studying midden formation processes and associated activities has the potential to inform on the use of natural resources at Çatalhöyük, and their associations with specific activities through analysis of material from individual deposits rather than excavation units. This research investigates resource use, including for fuel and food, from individual activities, by examining phytolith plant remains in their precise depositional context, as individual deposits. By examining phytolith associations

Seasonality As well as identifying activities, patterns in deposition/activity and their frequency will be investigated in this research. These patterns may be cyclical, with some deposits being observed more frequently than others, indicating more frequent discard from specific activities. Deposits which occur less 2

frequently may indicate an activity that occurs only occasionally at specific times. By examining possible “seasonal” indicators in deposits, it may be possible to link these activities to particular times of the year, and help establish a seasonal pattern of occurrence. Such indicators may be fruit stones from seasonal abundance or use, such as hackberry which is found abundantly at the site and ripens in late summer/early autumn, but which has never been examined in its precise context, or phytoliths from the flowering parts of plants, such as husks and dendritic long cells, proposed as a seasonal indicator for spring (Rosen 2005). Other potential seasonal inclusions suggested by previous research include eggshell, and the hypothesis that craft debris may be linked to production in winter (Fairbairn et al. 2005a).

particular, as previous research has shown evidence of storage of cereals (Bogaard et al. 2005, Jenkins 2005a). Although these and other plant and animal remains may be stored year round, processing and the resulting waste may occur at seasonal intervals. Phytoliths have previously been used as indicators of crop processing with rice and millet (Harvey and Fuller 2005). By studying these signals and others such as fruit seeds, the present research expands on previous seasonality research at Çatalhöyük. By analysing individual deposits, the precise location of residues from procuring of these “stored” remains can be seen, and an assessment made of their frequency. If stored, it is likely that they would occur regularly, whereas if they were used only when they were freshly available, deposits would occur less frequently and perhaps in association with other seasonal indicators.

Seasonality refers to the way in which human activities and life cycles altered throughout the year in relation to seasonal change in the environment and available resources (Monks 1981). Studies of cyclicity and periodicity are similar to seasonality studies but refer to any patterns in activity over a period of time that are not necessarily linked to seasonal or environmental changes. The study of wall plasters at Çatalhöyük is an example of such cyclical or periodic patterns in activity, indicating that cyclical activity was an integral part of household life (Matthews et al. 1996). Paleoenvironmental studies suggest a seasonally fluctuating environment which was likely to have influenced people’s behavior (Rosen and Roberts 2005, Boyer et al. 2006, Rosen and Roberts 2009).

Resource use – fuel and fire Fire is argued to be a significant phenomenon in the lives of Çatalhöyük inhabitants (Cessford and Near 2005). As well as domestic use, evidenced by the presence of ovens in many of the buildings (Figure 1.2), there is evidence of the deliberate burning of buildings in the later levels of the site, particularly at the end of Level VII, though the purpose of this remains unclear (Cessford and Near 2005, Farid 2005). For an explanation of the levels and dates see Chapter 2. There is also some suggestion of the use of fire in the early levels from low temperature fired pottery and lightly fired figurines, and the production of lime plaster, suggested to occur at a household scale on the edge of the settlement (Cessford and Near 2005).

Seasonal change is an environmental change which occurs frequently in the timescale of the human lifespan. Seasonality of site occupation is an important issue as it gives information on the nature of early settlements and has implications for the timing of sedentary as opposed to nomadic settlement, or in some cases, permanent versus temporary settlement, and seasonal fission and fusion of populations, as well as management of resources as proposed for Çatalhöyük (Fairbairn et al. 2005, Roberts and Rosen 2009). Although it has been noted (Monks 1981) that the seasonality of midden formation processes is difficult to determine, midden assemblages have long been used to investigate the season of occupation for non permanent sites (Bailey 1975, Leacha 1979). For example in coastal shell middens present day ecological information has been used in conjunction with information on fish behaviour and distribution to identify the season of site occupation (Claassen 1998, Stein 1992). Non-shell middens, however, have been studied in much less detail.

Figure 1.2: Burning dung fuel in the reconstructed oven in the experimental house.

Some later midden deposits, in Levels VI/V have been observed to contain extensive burnt and ashy layers relating to large scale burning activities, the purpose of which has not been fully investigated nor incorporated into studies of fuel use and fire. This research addresses this by studying these ashes under the microscope to examine evidence for different fuel sources, such as dung, wood, reeds or a mixture of these, and other inclusions in the ash which may indicate their origin and purpose. It is essential to study these components

It is often animal remains such as fish and animal bones that are used in studies of seasonality, as the use of plants as an indictor of seasonality often proves problematic (Monks 1981). Cereals are often seen as being of little use as indictors of seasonal activities, due to issues such as storage. Although they are a seasonally available resource, they are easily stored and thus may be used at any time of the year. The storage issue is particularly important at Çatalhöyük and for this research in 3

pottery from storage and small vessels in Levels XII-X to include cooking in Level VII-I (Hodder 2006), which may also affect selection and types of fuel used and be detectible in discard in middens.

together, examining the ash as a whole rather than separating the components. The use of fuel is important in understanding the society at Çatalhöyük, particularly the distances people were travelling to collect fuel resources, which has implications for local environmental impacts, and also implications on changing fuel technology. For example the use of slow burning dung versus wood. Previous studies of fuel use at Çatalhöyük have focused on the plant macro remains in investigating this issue. Analysis of charcoal indicates that in earlier levels firewood was collected from nearby wet woodland areas and consisted of mixed species, with a shift to oak between Levels IX VII (Asouti 2005). This shift may suggest increased pressure on the more local wet woodland, perhaps as a result of increased fuel consumption, or greater consideration of burning properties as opposed to bulk fuel availability (Asouti 2005).

Craft activity has also been discussed as a possible seasonal activity occurring in winter and spring, when there would have been more time available away from fields and after gathering ripe fruits and nuts (Fairbairn et al. 2005a). By studying individual deposits in midden layers it will be possible to identify specific craft debris such as worked wood and obsidian fragments, and will help understand midden formation processes and cycles of activities. It is possible that the large scale burning activities observed in the middens may relate to craft activity, such as pottery production. Again this is possibly seasonal, as the clay would need to dry out before firing. By investigating ash composition through phytoliths and micromorphology, as well as other inclusions in the ash, this research aims to identify any evidence for such craft activity in middens.

Although Asouti mentions the use of dung as fuel, this is still an area under investigation. This research will examine whether there is any evidence to suggest that dung and wood were used as fuel in a complimentary fashion, perhaps related to seasonal differences in fuel availability, or that these were used for different purposes due to their different burning properties, or were used together in the same burning activities (Matthews et al. 2006). This will be achieved by examining associations of charred wood, phytoliths and dung in specific ash layers throughout the middens, over long time periods by studying earlier and later middens, as well as shorter timescales within middens, and with regards to pottery production which is closely linked to fuel use.

Origins of Agriculture and Diet Related to questions concerning the human relationship with the environment are the debates over the origins of agriculture and domestication. Dietary studies, for example the consumption of wild versus domesticated plants are also inherent to these questions, as well as being an important component of daily activity. The traditional model of Neolithic subsistence describes the exploitation of moist alluvial soils, with subsistence agriculture being the deciding factor in settlement location (Roberts 1991). This, however, is debated for Çatalhöyük, by Roberts et al. (1999), due to the seasonal flooding indicated by studies of sediments, which argue this would be an unfavourable environment for growing cereals.

Studies of charcoal and burnt plant macro remains are limited in that they only sample remains which have been carbonised (Van der Veen 2006). It is also important to consider the composition of ash, which may contain evidence in the form of plant phytoliths and dung spherulites. By studying the context of fuel through micromorphology of ash layers in middens, and analysing phytoliths and spherulites from these ash deposits, the work presented here will contribute to research into fuel use and fire at Çatalhöyük.

Although there is phytolith and macrobotanical evidence of large quantities of cereals in storage bins (Bogaard et al. 2005, Jenkins 2005a), current research at Çatalhöyük also debates the importance of cereals as a food source, and the region in which these may have been grown. For example Fairbairn (2006) argues for agricultural production of wheat and barley as a key component of the site’s economy, but also recognises the lack of suitable land within a 5km radius. Rosen and Robert’s most recent hypothesis (2009) suggests the seasonal movement of part of the population to manage crop fields, with an equal if not greater emphasis on wild resources.

Resource use – craft activities As well as domestic activity, previous research at Çatalhöyük has detected evidence for craft activities in middens, for example wood working debris identified by Matthews et al. (1996), abundant obsidian (Carter et al. 2006), pottery, and clay figurines, though details of pottery production methods are poorly understood (Akça et al. 2009). The presence of more highly fired pottery is noted particularly after Level VII (Hodder and Cessford 2004), and may be associated with changes in the use of fire as discussed in Section 1.2.3. Interestingly, this is the level where fuel use is argued to shift to a dominance of oak rather than mixed species (Asouti 2005). However, previous research has not examined any links between these phenomena. There is also a change in the use of

The evidence from the phytoliths remains unclear, due to a lack of taphonomic considerations. Although Rosen (2005) suggests an association of barley with weed species, which suggests this was not deliberately cultivated as a food crop, the same report discusses the presence of barley phytoliths in storage bins. This report relies on small numbers of phytoliths, and does not take into account taphonomic processes which affect phytolith size (Jenkins 2009). This is discussed in detail in Chapter 5, section 5.4. This research contributes to this debate by 4

respiratory mechanism of the plant, with plants such as wheat being C3, and corn being C4. C4 plants tend to be better adapted to hot, dry environments with greater oxygen availability and will be inefficient in shady or cool environments, whilst C3 are better suited to cool, wet environments with higher carbon dioxide levels (Hibberd and Quick 2002).

examining the phytolith record of middens in detail and in context, to assess the frequency of cereal use, and the taphonomic processes affecting size. Other plant resources exploited for food, preserved as charred remains, include fresh tubers, legumes, fruits such as hackberry (Celtis), almond (Amygdalus), plum (Prunus) and other berries , nuts such as pistachio (Pistacia) and acorn (Quercus), leafy greens such as Chenopodium and Labiatae, lentils (Lens culinaris) and peas (Pisum sativum) (Fairbairn et al 2005b). It is interesting to note that Clubrush (Bolboschoenus maritimus) and Brassicas are present in equal or larger quantities than wheat in the charred macrobotanical record. A seasonal cycle of use for clubrush has been suggested based on their probable availability throughout the year (Atalay and Hastorf 2006), though the variation of these in precise depositional units has not been investigated. By identifying the frequency of such remains in context through micromorphology, this research will test the hypothesis that plants such as hackberry and clubrush were exploited on a seasonal basis (although smallness of sample size needs to be considered, as discussed below).

Whilst these studies give an overall picture of food use at the site which can be inferred through the species present, it is difficult to establish a seasonal signal due to the analysis of material from bulk flotation, which mixes large volumes of deposits which may represent years of material build up. Similarly, studies of diet from skeletal isotopes give an average dietary signal of 10 years when analysing collagen depending on the density of the bone (Ambrose and Norr 1993), which cannot establish how this diet varied on a seasonal or even yearly basis. By studying phytolith deposits from middens, this research will examine evidence for cereals in the middens, and will be able to link these deposits to their precise depositional context, and thus distinguish between remains from activities e.g. crop processing and animal fodder. Analysis of individual units will investigate whether seasonal signals can be more readily detected, if they are present. Analysing these in context is essential to understand the origin of plant remains, for example it is suggested that many seeds recovered from flotation and interpreted as food remains may actually derive from animal dung being used as fuel (Miller and Smart 1984). Ethnographic studies of the use of dung as fuel in Anatolia support this (Anderson and Ertug-Yaras 1998). By studying individual deposits, the frequency of cereal use at Çatalhöyük will be investigated, which could help resolve the debate over the importance of cereals versus wild plants, and further test the recent hypothesis of Roberts and Rosen that cereals were grown in dryland conditions (2009).

Tooth wear analysis suggests less ground cereals were consumed, with more regular consumption of tubers, grains and nuts (Molleson et al. 2005). Although Fairbairn et al. (2005) recognise the ubiquity and abundance of clubrush; they interpret this as deriving from animal fodder. However it has been suggested as a seasonally available human food source at the site of Abu Hureyra (Hillman 2000), and concentrations of this in specific deposits could link the deposit to a seasonal cycle. This also illustrates the importance of examining the precise context of such remains to be able to interpret them. Examining remains in thin section will investigate whether clubrush deposits relate to human consumption (as suggested by Atalay and Hastorf 2006) or animal fodder (as suggested by Fairbairn et al. 2005b).

Coprolites are also an important component of middens which have not been considered at Çatalhöyük when investigating diet, perhaps due to difficulties in recognising these in the field. In addition to crop processing deposits, direct evidence for cereal consumption may be possible through the analysis of phytoliths from coprolites and other distinctive phytolith types which may be used to indicate diet, such as C3 versus C4 types. By studying coprolites it will also be possible to get a better understanding of animal versus human faecal inputs to middens, which can be linked to studies of fuel use discussed in the previous section.

Evidence for consumption of animals is based on the study of animal bone assemblages and isotopic studies on human remains (O’Connor 2004). The animal bone data suggest a dominance of sheep/goat (domesticated), with smaller numbers of cattle, equids, cervids and boar (wild), though seasonal variations in exploitation have not been investigated. Also present in the animal bone assemblage are fish (carp and loach), and water birds such as geese and ducks (Russell and Martin 2005). Isotope studies of human remains suggest cattle were unlikely to have been the main source of dietary protein for all occupants, with C3 feeding goat and sheep being the main source of protein. C3 plants are the main source of plant protein, though a C4 plant input into human diet is recognised. This is suggested to be via C4 consuming sheep due to the small number of C4 plants recovered from charred macrobotanical remains at the site, or from the off-site consumption of C4 plants (Richards et al. 2005). This suggestion will be tested in this research by examining phytolith evidence for C3 versus C4 consumption in coprolites. C3 and C4 refers to the

The research described here contributes to the question of diet in using a duel approach – firstly through examining food processing, preparation and cooking residues from middens, and secondly by directly examining plant indicators of diet through extraction of phytoliths from coprolites, in conjunction with analysis of organic residues from coprolites to identify these as human or otherwise. Coprolites have the added advantages of

5

representing a single dietary event, compared to isotopes which give longer signals.

which addresses the problem of fine stratification and context.

Methods of enquiry

Thin section micromorphology

Understanding human activity in the past can be difficult, and often it is possible only to understand general trends over long time periods. However, to understand the origin of complex processes such as the development of agriculture and technological developments such as ceramics, we need to understand human activity at a higher resolution. Understanding everyday, seasonal, annual and lifecycle activities, and how these were linked to a seasonally changing environment is difficult at a site like Çatalhöyük, a) because of the scarcity of accumulated deposits from human activities in building contexts (Matthews 1995a) and b) the microscopic nature of deposits associated with everyday activities and individual depositional events in middens (Matthews et al. 2004). This research utilises a specific set of techniques which aim to address such problems, by studying middens from the macro to the micro scale. Macro scale analysis has been achieved through observation and recording of the overall extent of deposits in middens in the field (through photography, section drawings and excavation records), followed by microscale analysis of thin section micromorphology blocks to observe the fine layers which are difficult or impossible to observe at the macroscale.

Traditional analytical techniques in archaeology have the unfortunate effect of removing components from their depositional context, and macro scale analysis of stratigraphic units in the field can often fail to identify single small scale depositional events, particularly deposits that are thin and difficult to excavate or identify in the field (Matthews et al. 1997). At Çatalhöyük this is evident in the excavation reports which refer simply to fine layering, and class such layers as one large unit (McCann and Brown 2006, Yeomans 2006). Micromorphology is a technique that has proved invaluable in the past two decades at providing contextual information and revealing differences between site contexts which are not obvious at the macroscale (Courty et al. 1989, Matthews et al. 1997). It has been used in a wide variety of studies in order to examine stratigraphic features in situ and at the micro scale, including the study of buried landscapes and ancient soils (Guttmann et al. 2003), site formation processes (Simpson and Barrett 1996) and the urban use of space (Shahack-Gross et al. 2005). In Turkey, the majority of micromorphological work has been conducted by Matthews, for example at the sites of Aşıklı Höyük, Kale Tepe, Hattusas, Kilise Tepe and Kerkenes Dağı, and many contexts from Çatalhöyük itself have been studied in depth (Matthews et al. 1994, Matthews et al. 1997, Matthews 2005). In particular wall and floor plasters are now understood in much greater detail due to this work. Wall plasters have been revealed to consist of hundreds of micro layers, applied in probably distinct seasonal and annual patterns (Matthews 2005, Wiles 2009).

Sub sampling of these blocks in the field and in the laboratory has been carried out as close as possible to individual layers for phytolith, FT-IR and GC-MS analysis. Phytoliths will be used to examine an important aspect of plant remains which are difficult to see and quantify in thin section, FT-IR to identify specific mineral components which are difficult to characterise in thin section, and GC-MS for the identification of coprolites, an important component of middens that can only be identified without ambiguity with organic residue analysis, and which are key deposits in approaching seasonal/high-resolution temporal scale diet. A summary of the techniques used is given in Table 1.1, with further details of methods in Chapter 3.

Under a petrographic microscope, individual layers may be examined at up to 400x magnification. These layers may be less than a mm thick, but they are often indicative of site formation processes and smaller-scale activities. As well as the individual layers it is the context and associations of materials recognised through thin section analysis that are most informative. At the macroscale during excavation, context is important in deciding how different features are related. The same principle is applicable at the microscale, using a microscope to establish the relationship between smaller scale features and components. Although thin sections are comparatively small at 14 x 7 cm and 30 μm thick, the smaller the sample size, often the greater the specificity of the time signal (Monks 1981). They represent a high resolution “snapshot” of activities.

Midden formation processes There are a number of methodological problems traditionally associated with the study of midden formation processes, which tend to be excavated in arbitrary units because of the fine nature of the deposits. It has been noted impossible to excavate and understand the individual units of deposition in the field (Yeomans 2005). Seasonality of formation is particularly difficult to determine on an absolute timeframe, due to ambiguities arising from potential storage and transport of seasonal indictors (Monks 1981). Dating midden sequences is also problematic, which leads to difficulties in assessing the timescale of formation for these deposits (Stein and Deo 2003). This research uses thin section micromorphology as the primary technique with which to examine and understand midden formation processes, a technique

Although micromorphology has become a well established technique in archaeology, its application to the study of midden deposits is an area which is less well developed, possibly due to the complexity and great variability of these deposits. Conversely it could be argued that it is this which makes midden deposits particularly well suited to this method of analysis. Some 6

studies have been carried out at the medieval site of Robert's Haven, Caithness, Scotland to examine midden formation processes as an indicator of domestic versus economic activity, by comparing human accumulation of fish bone (Simpson and Barrett 1996). They have also featured as part of a study of manuring practices, through observations of anthropogenic additions to soils (Davidson and Carter 1998) and the use of fuel ash as fertiliser at the Iron Age site of Jarlshof, Scotland (Guttmann et al. 2008). Micromorphology of middens has also been studied as part of larger investigations of site formation processes comparing micromorphology from a number of different contexts (Matthews 1995).

other techniques, and examining continuous detailed sequences. Resource use, seasonality and diet. Middens contain a large variety of microscopic deposits which are often underutilised. Although thin section micromorphology provides a means of understanding individual deposits in their precise depositional context, there are a number of problems associated with viewing a one dimensional slide (Matthews et al. 2004). These slides represent relatively small samples and emphasis is on existing visible attributes. In addition, resin impregnation means limited further work can be carried out.

However, the potential of these deposits for revealing human activities has not been fully investigated, especially at sites like Çatalhöyük where these deposits are incredibly extensive (a single midden may be many metres high and wide – see Figure 1.3), forming one of the largest and richest contexts at the site. Previous work has examined these deposits at the macroscale, through the analysis of a specific component such as animal bone assemblages, to understand the nature of animal resource use (Russell and Martin 2005), plant macro remains and charcoal to investigate the use of natural resources as fuel (Asouti 2005, Fairbairn et al. 2005b) or phytolith remains (Rosen 2005, Jenkins 2005). All of these analyses have analysed material recovered from bulk excavation and processing techniques, which separates the components being analysed from their associated material. This research addresses questions of plant resource use through the analysis of phytoliths and microcharcoal in context. In this way variations between individual deposits will be seen that give higher specificity of time signal, rather than blurring any potential signals.

In this study the focus is on integrated micromorphology and phytolith analysis as a new method for characterising the plant component of micro layers. Phytoliths are important micro remains/artefacts at a site like Çatalhöyük, where more traditional techniques such as pollen analyses cannot be used due to unfavourable oxidising preservation conditions. By identifying and quantifying phytolith remains from thin section sediments, we can tackle questions relating to agriculture, diet and resource use as well as paleoenvironment (Trombols and Israde-Alcantara 2005, Piperno 2006). By themselves, phytoliths can tell us the range of plants that were present, but by looking at their context through micromorphology we can investigate the different ways in which plants were being used and for which activities they were being used, and other remains they are associated with. Phytolith analysis potentially provides evidence of a different variety of plant remains compared to pollen or macrofossil remains, where only certain parts of the plant may be preserved (Horrocks and Lawlor 2006). The technique is not without problems, particularly with regard to the different rates of phytolith production between dicotyledonous and monocotyledonous plants and the difficulty of identifying beyond genus (Piperno 2006) which could skew the record. This can be overcome to a degree through thin section micromorphology, which enables the investigation of a wide range of plant material in a deposit, including charred plant remains. These limitations are taken into consideration when interpreting the data in this research, and are considered in detail in the discussion.

Figure 1.3: Photograph to illustrate the dimensions of a single midden (Midden 2, South Area).

Phytoliths can be difficult to distinguish in thin section depending on the angle of cut and masking by other components. In this research, in addition to studying thin sections of deposits, blocks are sub sampled before resin impregnation, and phytoliths are extracted from individual layers within the middens in order to enhance the information that can be seen in thin section, and to provide statistically significant counts of phytoliths in the deposits. This is important to investigate questions of resource use and seasonality, as plant remains are potentially an important seasonal indicator, and an important natural resource.

Initial micromorphological work in the Deep Sounding and South Area middens (the location of these areas can be seen in Chapter 2, Figures 2.2 and 2.3) has revealed complex sequences of deposit types that relate to different activities, such as hearth rake out, cooking debris and building waste material (Matthews 1996, Matthews 2005, Shillito 2004). The present study aims to add much greater depth to the interpretation of midden deposits by using thin section micromorphology with

7

oxalate (CaC2O4) phytoliths. Silica is present in the soil in a solid (e.g. quartz or feldspar, SiO2) or as a soluble liquid form (monosilicic acid Si(OH)4). There is equilibrium between these two forms, with silica being eroded by water and then precipitated from solution.

The present research addresses this limitation by using a highly targeted high resolution sampling strategy to extract samples from individual microlayers, in addition to microanalysis on impregnated resin blocks in situ where possible. Micromorphology provides an excellent contextual description of deposits, however it is sometimes not sufficient for the complete identification of material, for example coprolitic material cannot be analyzed beyond its physical morphology (Courty et al. 1989). In addition the identification of a certain feature may not be straightforward, for example phytolith identification is often restricted in thin section due to the two dimensional nature of the cut, and organic residues cannot be observed. In order to understand these components in more detail, infra red spectroscopy and gas chromatography-mass spectrometry have been selected to analyse specific components of interest in middens, for example, coprolites. These are an important component of middens, and are also of potential use in the study of diet.

SiO2 + 2H2O

Si(OH)4

Phytolith analysis Near Eastern sites are ideal for phytolith analysis, as the dry summers and high rates of evaporation, and thus transpiration, lead to a high concentration of silica within the plant epidermis (Hillman 1984). Phytolith analysis has therefore successfully been used in studying ancient agriculture in this region. It was Rosen who recognised the great potential for phytolith research in the Near East for answering questions related to the origins of wheat and barley agriculture, and the fact that such sites are ideally suited to this type of analysis (Rosen 2001, Rosen 2005). Phytolith analysis has been selected to understand the plant component of microlayers. Although charred plant remains have been studied in detail (Asouti et al. 2005, Bogaard et al. 2005, Fairbairn et al. 2005b), middens contain a range of non charred plant material which is preserved as phytoliths. Phytoliths have been studied from Çatalhöyük middens (Rosen 2005, Jenkins 2005) as a general overview, in comparison with other contexts such as storage bins and floors. Phytoliths from distinct deposits have contributed to understanding craft activity including recognition of the use of sedges in basketry (examples can be seen in Figure 1.4). This previous research has contributed to questions of environment and agriculture by suggesting a lack of large conjoined phytoliths indicating irrigation or cultivation in a marshy environment. The association of barley with weed species suggests it was not deliberately cultivated as a food crop, when compared to wheat which shows low correlation with weed grasses in the samples analysed (Rosen 2005). However, as discussed earlier, there are taphonomic problems which are not considered.

Figure 1.4: Phytolith basketry impression from unit 3228, Building 5, in the North Area (above), and matting impression from unit 10406, Building 42, in the South Area (below).

The term phytolith refers to any mineral deposited within a plant (Rovner 1971), though in most archaeological studies the term refers to opal or amorphous silica phytoliths (SiO2.nH2O), and occasionally to calcium 8

and more experimental work needs to be done to confirm exactly how this varies between species, and whether other environmental factors such as flooding may have similar effects. Currently further experimental work assessing a range of factors on phytolith size is being carried out as part of the Leverhulme funded Water Life Civilisation project, the results of this are eagerly anticipated (Jenkins et al. forthcoming, Mithen et al. 2008). This research (Rosen and Weiner 1994) is used for the basis of Roberts and Rosen (2009) argument that cereals were being grown over 5km from the site. However, Rosen’s experimental work on modern samples does not account for variation in phytolith size from taphonomic and methodological processes (Jenkins 2009), which will be investigated in this research.

The soluble form of silica is found in groundwater and is absorbed by plants as monosilicic acid through their roots. As the water passes through plants cells the silica in it is deposited. The site of deposition depends on the species and can occur between cells, within the cell walls, or sometimes completely infilling the cells (Pearsall 1982). The process is controlled physiologically within designated cells and environmentally by temperature and evapotranspiration (Piperno 1988) and by soil type as well as by anthropogenic factors such as irrigation (Rosen and Weiner 1994). The deposition of silica leads to a three dimensional replica of the plant cells that remain preserved whilst the organic plant matter itself decays. Phytoliths can be formed in the roots, leaves, stem, fruit etc, depending on the species, though aerial parts produce more than subterranean parts. Species which are particularly prolific producers of phytoliths include Gramineae, Cyperaceae and Equisetaceae (Piperno 1988), i.e. monocotyledonous plants. Dicotyledonous plants are also silica depositors but the forms are less distinct, though the ratio of dicotyledonous to monocotyledonous types can indicate phytolith sources. For example, wood has a high amount of variable morphology phytoliths compared to grasses, so a higher proportion of variable forms would indicate a wood source (Ollendorf 1987). This is useful if charcoal is poorly preserved, otherwise it is more useful to use charcoal analysis for such deposits.

Phytolith analysis is a relatively new but very important area of research in archaeology. The inorganic nature of phytoliths means that they are not susceptible to breakdown by microbes, and do not have to be burnt nor waterlogged to be preserved. This is a major advantage over other more commonly studied botanical remains such as pollen and seeds, though dissolution can occur at pH > 9.0 in some contexts (Piperno 1988). Phytoliths are particularly important in the investigation of the Çatalhöyük middens, as they form a very large component of the deposits, in many cases forming entire depositional units. Whilst plant macro fossil analysis can give large scale trends in plant use, phytoliths can provide important complementary additional data on different aspects and depositional pathways of plant material, for example of non burnt plant deposits and finely layered deposits.

Phytoliths can be present either as single or multi cellular forms – the latter sometimes being referred to as silica skeletons or conjoined phytoliths. Single cells are nearly impossible to identify beyond genus level in most cases, but are specific to different parts of a plant, and the morphology of the short cell can distinguish between C3 and C4 photosynthetic pathways. For example bilobe short cells are considered a feature of C4 plants, whereas rondels are a feature of C3 plants (e.g. Bremond et al. 2008).

There have been significant developments in developing and refining extraction techniques (Piperno 1984, Zhao and Pearsall 1998), and to improving identification and classification problems. Much work on phytolith taphonomy is still in progress (Lentfer and Boyd 1999, Madella et al. 2005). Phytoliths have been applied to a variety of other studies, including paleovegetation reconstruction (Bowdery et al. 2001), paleodietary studies (Elbaum et al. 2003) and fire detection through analysis of changes in the refractive indices of phytoliths (Delhon et al. 2003).

Analysis of phytoliths in the study of plant ecology dates back to the mid 20th century (Twiss 1969, Parry et al. 1984, Twiss 1992), with the first uses of the technique in archaeology being to identify cultivated grasses in old world archaeology (Parmente and Folger 1974). Such studies however were limited, and it was not until Rovner’s article (Rovner 1971) that interest developed in the potential of phytolith analysis as a paleoecological and archaeological technique. The earliest significant phytolith work in archaeology was therefore concentrated on looking at soil phytoliths and dates from the 1970s, with researchers such as Pearsall (1982), Piperno (1988) and Rovner concentrating on the Americas.

Spectroscopic techniques in archaeology Other components of middens are difficult to fully assess in thin section, for example organic material. In this research a range of analytical techniques are considered which may be able to address some of these problems. The spectroscopic features of individual materials are often highly specific, and as such, spectroscopic techniques are often used to analyse and identify samples. Techniques such as Infra Red (FT-IR) for example have been used to investigate mineralization of deposits and the characterisation of archaeological materials such as pigments in artwork (Cassadio and Toniolo 2001), ochre from Çatalhöyük and Clearwell Caves, UK (Mortimore et al. 2004), and mineralised insects and fruit pips from Silchester Roman Town, UK (Marshall et al. 2008).

Studies have suggested that irrigation may have an effect on the extent of silicification in the presence of other factors such as climate. The number of cells in multi cell silica “skeletons” in particular has been shown to increase in the presence of irrigation (Rosen and Weiner 1994, Mithen et al. 2008, Madella et al. 2009), although there are many other factors which are involved in the process, 9

high spatial resolution. By contrast, traditional “bulk” FT-IR requires the sample to be removed from its context for analysis. Whilst bulk FT-IR is useful for larger samples, for some of the finer deposits such as wall plasters, and the finest midden layers, many inclusions are just too small to be extracted for individual analysis, and fine layers may be aggregated. The drawback to IR microscopy is that samples need to be very thin for transmission spectroscopy, which is the easiest mode to utilise. Thus such contextual analysis is done through reflectance mode infra red, which, whilst giving rise to spectra which are more difficult to interpret, shows much potential.

A review of the literature suggested FT-IR could be a useful technique in conjunction with thin section micromorphology, having previously been successfully used with phytolith analysis in characterising ash layers in cave sequences such as Hayonim, Israel (Steiner et al. 2001, Weiner et al. 2002). In addition, FT-IR with SEMEDX has previously been used in the characterisation of coprolitic material from Brean Down, UK (Allen et al. 2002). It was reasoned that these techniques could therefore be useful in characterising specific components in the Çatalhöyük middens, particularly coprolites, ashes and unidentified mineral nodules, which would aid in understanding midden formation processes in the layers in which these components occur.

One use of IR microscopy considered in this project is to investigate the mineralogy of archaeological phytolith samples from Çatalhöyük middens, to assess the potential to use this as an indictor of phytolith source and thus contribute to the agriculture debate by suggesting possible regions of crop growth, and as a more detailed characterisation of phytolith types that are difficult to identify by physical morphology. Studies examining plant physiology have found that different crystalline forms of silica may occur in plants (Lenain 2000, Monje and Baran 2000, Smith and Clark 2004). Previous studies on mire systems in Malaysia have suggested that phytolith mineralogy and elemental composition can be affected by the soil substrate (Wüst and Bustin 2003). Although it was not possible to study mineralogy and trace element composition in this study due to limitations of the equipment available, a discussion of the potential of this is given in Chapter 8.

The theory of infra red spectroscopy is that a molecule can absorb IR radiation at an appropriate frequency that will excite it from one vibrational state to another. A molecule can have a number of different vibrational modes. For IR activity to occur there needs to be some change in the permanent dipole moment of the molecule or ion. For example, the symmetric stretches of the free carbonate (CO32-) or silicate (SiO44-) ions show no change in dipole moment and the vibrations are IR inactive (Figure 1.5). Asymmetric stretches are IR active and for molecules of low symmetry, the symmetric stretches may also show IR activity. 2

-

4

IR spectroscopy of coprolites, in combination with SEMEDX, has previously been applied to samples from Brean Down, a Bronze Age settlement in the UK (Allen et al. 2002). This work has been successful in identifying calcite, apatite and occasionally quartz in the concretions that were suspected to be coprolites. Comparison with surrounding soil samples show that the apatite is unique to the coprolites, and it suggested that the phosphate in the mineralised faecal remains has its origin in small bone fragments.

Si

C O

-

O

O

O

O

O O

Figure 1.5: The symmetric stretches of the free carbonate (CO3 2-) and silicate (SiO4 4-) ions.

If broad beam IR energy passes through a sample, the energy from certain frequencies will be absorbed by that sample. The mid-infrared range between 4000-400 cm-1, is used to study fundamental vibrations and structure. A spectrum is produced of the intensity absorbed against the frequency, which is referred to as the absorption spectrum of the sample; the spectrum will have peaks that indicate certain bonds or functional groups, as well as a fingerprint region unique to each molecule. In small molecules the molecular structure may be determined by looking at an IR spectra, but for larger molecules, the pattern of absorbance is normally used simply as a characteristic of the functional groups present (Christian 2004).

A further methodological development in this research is the use of IR spectroscopy as a quick and inexpensive method for identifying potential coprolite samples in the Çatalhöyük middens through examining the presence of phosphate, as well as providing an overview of the bulk mineralogy of layers from thin sections. This could be useful for targeting samples for more detailed observation such as GC-MS or detecting high levels of post depositional disturbance from mineral crystallisation. Spectroscopic and diffraction work has previously been carried out on calcareous spherulites, using FT-IR, XRD and SEM. Spherulites are microscopic particles found in coprolites from certain animal species and range from 520 μm in diameter and which in thin section can be very diagnostic of the presence of faecal material (Canti 1997, Canti 1998, Canti 1999). Examples can be seen in Figure 1.6. Spherulites are formed of a radial microcrystal mass

The development of an IR spectrometer coupled to an optical microscope is an area of potential importance in allowing non destructive analysis of selected areas of a sample by transmission or reflectance spectroscopy. This approach allows the in situ analysis of materials with a

10

in an approximately spherical shape. Anisotropic spherulites under a petrological microscope have a permanent dark cross in their centre due to the constant presence of crystallites in the four extinction angles. XRD analysis has shown there to be a strong calcite component to spherulites (Canti 1998).

focus on much smaller particles than a conventional IR microscope. However a number of other methodological problems were encountered during this research. Suggestions for further work and improvements on the experiments carried out in this research are given in Chapter 8.

Canti suggests that a significant factor in spherulite production could be the mineral content of the local soils. For example sheep that had been grazed on acidic soils do not produce spherulites, though he also observed that calcareous grazing does not necessarily lead to spherulite production, suggesting a more complex number of factors is at work. Interestingly, Canti has identified 88 other materials that are spherical, some with extinction crosses (Canti 1997, Canti 1998, Canti 1999). Thus techniques for the unambiguous identification of coprolites are all important.

Organic Residue Analysis In the midden deposits studied in this research, distinct orange inclusions could be seen in the field, which were suspected to be coprolitic material. Organic residue analysis by GC-MS was therefore selected in this study to identify these a) as being coprolites and b) as human or otherwise. Identification of these to species level is essential in understanding midden layers containing this material, for example, to establish whether these deposits indicate animal waste from penning, or human waste, and for interpreting these as indicators of human diet. The term organic residue analysis covers a range of chemical techniques that are used to separate and identify organic compounds, including chromatographic techniques such as gas chromatography (GC), high performance liquid chromatography (HPLC), couple to mass spectrometry (MS). GC-MS in particular is successful in separating volatile mixtures and identifying the residues present, and thus is a powerful tool in the petrochemical and agrochemical industries. With the aid of an established reference collection and knowledge of the breakdown pathways of archaeological materials, it is possible to determine the use of a pottery fragment (Dudd et al. 1999, Evershed et al. 2003), or which species produced faecal material (Bull et al. 2002, Bull et al. 2003), or whether soil was manured (Bull et al. 1999, Simpson et al. 1999). Much of the work in this area has been carried out through the NERC Life Sciences Mass Spectrometry Facility (LSMSF) at the University of Bristol. The approach is to match properties such as the molecular structure of compounds extracted in archaeological materials with samples produced by modern plants and animals that are likely to have existed at the time of a site’s occupation. This information can be gained by studying the faunal remains and through pollen and phytolith analyses, and the analysis of bone assemblages. Much of this work has also focused on the degradation of compounds and the construction of an extensive database of reference data, which is critical to interpretations of archaeological residues (Charters et al. 1997, Evershed et al. 1997, Evershed et al. 1997).

Figure 1.6: Faecal spherulites in thin section at x100 (above) and x200 (below). An individual spherulite is circled in red.

Residue analysis has become established in archaeology is in the analysis of pottery residues (Evershed et al. 1990, Evershed et al. 1991), with further applications including analysis of ancient tars and resins, such as the determination of a pine wood origin for pitch from Henry VIII’s flagship, the Mary Rose (Evershed et al. 1985), analysis of the composition of bog butters from peat bogs in Ireland and Scotland (e.g. Berstan et al. 2004) and determining the composition of other materials, for

The limitations of using FT-IR and XRD to investigate spherulites is the same as the problem presented by smaller phytoliths, that is, the small size of these particles, at around 20 microns for an individual phytolith and 5 – 20 microns for faecal spherulites. It was hoped to try and address these problems by using the synchrotron IR microscope at the Daresbury facility, which is able to

11

example the identification of processed animal fats in a Roman cream formulation (Evershed et al. 2004).

the gut (hence the 5β rather than aerobic 5α products are formed). Bile acids are a group of C24, C27 and C28 steroidal acids which assist the enzyme mediated deposition of fat (Berg et al. 2006). They ensure that body cholesterol is maintained by eliminating any excess sterols that may be present. 5β stanols and bile acids are relatively resistant to degradation, especially when buried, and hence the interest in these compounds as archaeological markers (Bull et al. 1999).

An interesting development in organic residue analysis is the investigation of the origin of dairying and the use of secondary animal products. Much of this work has been carried out on UK sites, for example a number of pottery sherds from Iron Age, Bronze Age and Neolithic sites have been investigated and the data compared with the archaeological faunal data (Copley et al. 2005 a,b,c). Recently GC-MS analysis of sterols has been used in combination with elemental analysis to review organic and inorganic signatures that could be useful for recognizing space use and identifying daily activities in the reconstructed Iron Age village at Lejre, Denmark. Results suggest that whilst elemental analysis could distinguish between the smithy and the stable areas, lipid analysis was better able to distinguish dwelling areas (Hjulström and Isaksson 2009).

Analysis of organic residues on Turkish sites has been carried out both at Çatalhöyük and at a number of other sites, for example the multi period site of Sagalassos in south west Turkey . The lipid fractions of residues in different vessels found at Sagalassos were analysed using GC-MS, and found to contain animal and plant derived residues (Kimpe et al. 2004). In a previous pilot study on seven samples from Çatalhöyük , on two coprolites, two midden deposits, three stabling deposits and one mudbrick control (Bull et al. 2005) coprostanol was found in suspected coprolite samples (Figure 1.8). The predominance of coprostanol compared to higher 5βstanols and the lack of 5β-stanol epimers indicate that the samples in this case are either human or pig as opposed to ruminant derived. An absence of hyodeoxycholic acid indicates that the sample was human in origin, as opposed to pig (Bull et al. 1999). This study showed the technique could be successfully applied to samples of this age and that at least some of the yellow material found on site is human and promising for further integrated analysis. Further applications of biomolecular analysis of faecal residues are discussed further in Chapter 7.

Early work was also carried out on soils as a more reliable alternative to phosphate analysis in looking an ancient manuring, for example experimental work at Butser Ancient Farm which highlighted the possibility of using 5β-stanols as biomarkers of manuring (Evershed et al. 1997), and an archaeological study of relict twelfth-to nineteenth-century anthropogenic deep top soil in West Mainland Orkney (Simpson et al. 1999). Phosphorus has long been considered an important indicator of past human activity (Holliday and Gartner 2007). High phosphorus, for example, has been used to identify kitchen areas at a colonial house in Virginia (Sullivan and Kealhofer 2004), and to delineate the site boundary at a prehistoric Indian site at Cape Cod (Schlezinger and Howes 2000). However, phosphate analysis is a non specific technique, and the phosphate could potentially come from a number of sources, including food remains, faecal material and bone.

COOH

HO

The persistence of phosphate in different soils and its ability to act as a marker for human activity or burials is also debated. For example studies at the Experimental Earthwork at Wareham, Dorset indicate phosphate from bone in acidic heathland soils is poorly preserved, sometimes with no traces remaining after 30 years of burial (Crowther 2002). Phosphate analysis is also not able to distinguish between species that produced coprolitic material, in contrast to GC/MS analysis of coprolites, which can detect species specific sterols and bile acids.

H

HO

Figure 1.7: Structure of 5β-coprostanol (left) and lithocholic acid (right).

There are two main groups of organic compounds that can be found in faecal material, these are 5β-stanols and bile acids (Haslewood 1967, Hill and Drasar 1968). Examples of major human faecal compounds can be seen in Figure 1.7. The stanols are reduction products of cholesterol (cholest-5-en-3β-ol) and a number of other analogues: 24-methylcholest-5-en-3β-ol, 24-ethylcholest5-en-3β-ol and 24-ethylcholest-5,22-dien-3β-ol (campesterol, sitosterol and stigmasterol, respectively) which are found in the food ingested by higher mammals. The reduction is mediated by enteric bacteria present in

Figure 1.8: Coprolite material in thin section, showing pseudomorphic voids and a fish tooth. The coprolite is suggested as human (Matthews et al. 1996).

12

burning in the archaeological record (Weiner et al. 2002). Results suggest that burning alters the mineralogy of the sediments, and thus these techniques can be used to detect burning in the archaeological record (Weiner et al. 2002).

Integration of analytical techniques This research is one of the first examples of the use of micromorphology to study the fine layering of midden deposits, and the first to study midden deposits with a range of other techniques such as phytolith analysis and organic residue analysis to investigate questions of periodicity and cyclicity of discard, resource use and diet. There are a number of advantages to using techniques such as GC-MS as an analytical tool in combination with other traditional archaeological techniques. In Figure 1.8 coprolitic material is illustrated which has been identified in thin-section as potentially human on the basis of the fine fabric and comparison to modern samples (Matthews et al. 1996, Courty et al. 1989). The thin section analysis provides the context for this coprolite and its contents. In this research residue analysis is highly targeted on deposits which have been studied in their precise depositional context, as part of the aim of identifying specific components and deposit types and relating them to seasonal and periodic activities.

The research presented here aims to apply an integrated methodology, by using in situ or spot microanalysis where appropriate, to target individual features, rather than simply looking at bulk chemical properties. No such studies have been previously conducted on midden deposits. This novel methodology is particularly relevant due to the finely laminated nature of the midden deposits at Çatalhöyük. This method allows multi-scalar interdisciplinary investigation of middens. Analysis begins at the macroscale through visual examination of midden deposits in the field, which allows an assessment of the spatial extent of deposits and patterns in large scale depositional events, to microscopic observation using thin section micromorphology (for microstructure and depositional characteristics) and phytolith analysis (for detailed observation of microscopic plant remains and to complement previous studies of charred remains from flotation).

The combined analysis of thin sections in conjunction with phytolith and chemical analysis from these sections in particular is an innovative technique. Basic studies have been carried out using phytolith analysis in conjunction with soil chemistry analysis, but so far these have been limited to identifying general activity areas within buildings (Sullivan and Kealhofer 2004). Chemical analysis in particular suffers from a lack of contextual analysis, with samples invariably being removed from their original context, with the focus being on the sample itself rather than on the depositional context.

Further analysis of selected components is then made with a selection of chemical techniques to identity specific components and non visible properties such as the presence of organic residues. Results from chemical and microscopic analysis can then be related back to observations at the macroscale to aid interpretation of midden deposits. A summary of the techniques used and the rationale for selection is given in table 1.1, along with a summary of how these can answer specific questions relating to midden formation processes.

Integrated studies of phytoliths, mineralogy and thin section micromorphology have been carried out in the past 5-10 years, initially focusing largely on the mineralogy of phytolith and adjacent layers (Shiegl et al. 1996, Karkanas et al. 1999) and more recently looking at the phytolith assemblages. These studies have focused particularly on cave sites with a large emphasis on diagenesis of deposits in the cave environment (Albert et al. 2000, Weiner et al. 2002, Karkanas et al. 2002). IR spectroscopy has proved to be a useful tool in distinguishing between different mineral types associated with hearth layers and bone material (Albert et al. 2000), and for assessing the preservation state of the archaeological record, through identifying stages of mineral post depositional transformations. Phytolith analysis is seen to be most informative when related to specific deposits such as hearths.

The methodological objectives in this research are therefore to develop an integration of analytical chemical techniques such as IR, XRD, SEM, and residue analysis, with traditional archaeological methods of thin section and phytolith analysis, to characterise midden samples, in particular coprolites and phytoliths. By characterising sequences of deposits, it is hypothesised that it will be easier to understand midden formation processes and human activity at Çatalhöyük and the sequential nature of deposition potentially allows the elucidation of cycles in types of deposition. The results of this research into midden formation processes will be applied to archaeological research questions and issues that can be investigated though the analysis of these processes, such as cyclicity and seasonality of activities and resource use at the Neolithic site of Çatalhöyük in central Turkey.

A large number of these studies have been carried out at the Kebara and Hayonim cave sites in Israel (Schiegl et al. 1996, Karkanas et al. 1999) and the Olduvai Gorge site in Tanzania (Karkanas et al. 2002). More recently Bronze and Iron Age sediments have been studied from Tel Dor in Israel to look at the effects of burning on the mineralogy of these sediments, using FT-IR and XRD. Results suggest that burning alters the mineraology of the sediments, and thus these techniques can e used to detect

Summary of analytical techniques used in this research This research aims to address the problems of the fine stratification of middens and the lack of contextual analysis through the application of thin section micromorphology, in conjunction with a number of micro 13

analytical techniques that target individual layers and components within middens. The techniques used have been selected to characterise fine layers within complex midden deposits. Specifically these micro analytical techniques are phytolith analysis of the plant components of middens which has been targeted as a major indicator of activity/formation processes and one of the largest contributors to midden deposits at Çatalhöyük (Matthews2005), organic residue analysis of faecal material (the identification of which has previously been ambiguous in the field and in thin-section) and spectroscopic analysis of minerals and other components to narrow possible interpretations of deposits arising from micromorphological analysis. In addition, the analysis of each of these specific components will provide information relating to general plant resource use and diet at the site.

It is expected that at least some of the specific activities identified in previous research will be identified, including crafts, food processing, fuel, discard, floor sweepings and building construction/demolition.

Specific research questions and hypotheses



Considering the research background previously discussed, a number of research questions are considered in this research, and specific hypotheses examined. The research questions are specific to Çatalhöyük, used as a case study to illustrate general issues of the Neolithic in Anatolia and the Near East. Chapter 2 considers Çatalhöyük itself in more detail, and the midden sampling strategy that was used to investigate these questions. There are three major aims.



The second aim is to investigate cyclicity and seasonality of resource use and activities, through the investigation of the abundance and frequency of discarded remains and potential “seasonal” indicators such as food processing residues, food remains which are not readily storable (for example fruits, leaves), wind/water laid sediments relating to annual changes in climate and storm events, and particular component assemblages which may relate to cyclical activities, such as crafts. Hypotheses relating to periodicity/seasonality of activities and resource use

  

The first major aim is to develop an integrated methodology for the study of midden formation processes and discard from specific activities by linking high precision geochemical analysis of archaeological deposits with high-resolution microscopic analysis of deposit materials, morphology and precise-depositional context to provide a more robust interdisciplinary characterisation of the origin, deposition and post-depositional alterations of archaeological deposits. The specific objective is to combine high-precision spot sampling for phytolith, FTIR and GC-MS analysis of specific components with thin section micromorphology of components precise depositional context and associations, in order that midden formation processes can be better understood.

 

The third major aim is to investigate longer term changes in settlement, ecology, diet and food processing through analysis of middens from early-middle to late levels of Çatalhöyük, Levels VII to 0 (dates c. 6690 cal BC to 6090 cal BC and later) and any variation between neighbourhoods through the study of contemporary middens from the North (4040) and South areas of the settlement, in Levels VI.

Hypotheses relating to midden formation processes and identification of specific activities   

Observations of the frequency and sequence of deposit types will indicate cycles in activity. Some deposit types occur more frequently than others and can be related to more frequent ‘everyday’ activities. Identification of specific seasonal indicators in the deposit types may indicate a seasonal aspect to cycles of activity. Midden deposits can be used to further elucidate the nature of plant resource use at Çatalhöyük. Integrated micromorphological and phytolith analysis will enable identification of dung and its use as fuel, as well as non wood plants not preserved in the charred plant record. Differences in fuel selection are related to different activities, e.g. use of hearths/ovens and pottery firing. Differences in fuel selection may also be related to the seasonal availability of different fuel types, which can be distinguished by micromorphological features and inclusions.

Thin section micromorphology can enable the identification of individual depositional events in fine layers in middens. Individual midden deposit types can be used to identify specific human activities at Çatalhöyük, based on their inclusions and structure. The use of phytolith analysis in combination with micromorphology shows that similar phytolith assemblages can occur from bulk extractions, which are a result of distinctly different activities, detectable in thin section.

Hypotheses relating to the origins of agriculture and diet 

 

14

Observing the presence and frequency of cereal phytoliths in individual deposits will indicate whether cereal processing was conducted on or offsite and periodically, perhaps seasonally. Phytolith analysis will allow the identification of specific crop processing residues. Study of the taphonomy of cereal phytoliths will contribute to investigation of whether cereals were cultivated in wetland or dryland habitats.

   

Table 1.1: Summary of analytical techniques used in this research and rationale for their selection.

The nature and frequency of crop and food processing residues will contribute to establishing the relative importance of cereals versus wild resources. Individual midden components, specifically phytoliths and coprolites, can provide information on diet. Phytoliths extracted from coprolites are direct indicators of plant material being consumed. GC-MS analysis of these coprolites can confirm these as human or otherwise.

Technique

Analytical capacity and rational for selection

Samples analysed

Questions relating to midden formation

Macroscopic observations in the field

Allows observation and assessment of the spatial extent of deposits and macrolayers. Allows observation of component microstructure and associations within individual fine layering in middens, compared to excavation and flotation which cannot resolve fine layering.

Section faces of 7 middens

Nature and patterns of large scale individual depositional events and patterns of microlayers.

Blocks of deposits taken from section faces

Nature and patterns of individual depositional events, and comparisons of these events spatially and temporally.

Phytolith Analysis

Phytolith remains are difficult to assess quantitatively in thin section. Allows semi quantitative and qualitative description and comparisons of the microscopic plant remains from individual microlayers and discrete components such as coprolites.

Sub samples taken from micromorpholog y blocks, and from massive ash layers in section and from coprolites

Plant resource use, and discard and disposal of plant remains such as fuel and food remains.

Spectroscopy and diffraction (FT IR, XRD, SEM EDX)

Identification of inclusions and components in individual microlayers which are difficult to identify in thin section, and assessment of non visible properties e.g. degree of heating and alteration, elemental analysis. Identification and quantification of organic residues.

Sub samples taken from micromorpholog y blocks and from massive ash layers in section

Identification of components which are difficult to identify in thin section, and assessment of non visible properties e.g. degree of heating and alteration, elemental composition.

Sub samples taken from micromorpholog y blocks and from suspected coprolite deposits in section

Identification of coprolitic material and potential indicators of plant and non plant component of diet.

Thin section micromorpho logy

Summary This introductory chapter has examined the research questions under investigation, and the methodological approach used in this research, along with the rationale for selecting this methodology, and how this will contribute to previous work at Çatalhöyük. In the following chapter an overview is given of the case study, Çatalhöyük, including details of the sampling strategy employed to study the middens at this site. Chapter 3 discusses the methods selected in order to address these questions. Results are then presented in order of scale. Starting with macroscale observations of middens and thin section micromorphology, followed by microscopic examination of phytoliths, then chemical analysis using spectroscopic and bimolecular techniques, in chapters 4 – 7 respectively. The discussion in Chapter 8 brings together key results from the integration of these techniques to show how this research has contributed to the understanding of midden formation processes at Çatalhöyük, and the implications for understanding the development of human and environmental interactions in the Near Eastern Neolithic and diet. This is followed by a final section of future work that has been identified from this research.

Organic residue analysis by GC MS

15

THE CASE STUDY AND SAMPLING STRATEGY The Case Study: Çatalhöyük, Turkey

Figure 2.1: Map showing the location of Çatalhöyük in Turkey.

The Neolithic site of Çatalhöyük in central Anatolia, Turkey (Figure 2.1) dates from 7400 – 6000 BC (Cessford et al. 2005), and is an excellent case study for understanding the Neolithic of Anatolia and the Near East, both because of the world significance of the site (currently on the World Heritage tentative list) and for investigation of midden deposits due to their extent and excellent preservation. The occupation on the East Mound at Çatalhöyük spans approximately 1400 years from the early Neolithic to the early Chalcolithic. The site has traditionally been seen as one of the earliest areas of agriculture, though recently this has been debated. Roberts and Rosen (2005) for example, argue that the location of Çatalhöyük in an agriculturally unfavourable area suggests agriculture was not the main focus of the site. The special significance of Çatalhöyük is its remarkable preservation and the magnificent paintings and artefacts, which are rare for such an early site and provides evidence for complex social organisation (Mellaart 1967).

by Ian Hodder, has been carrying out new excavations and research, in order to understand the economy, society and material culture of the people that inhabited the site. Current research at Çatalhöyük is focused on the relationship between the site and the environment with current interpretations being based on faunal, charred macrobotanical, phytolith and charcoal evidence from excavation and flotation. Another focus is diet and life ways, with current interpretations from human remains being used to reconstruct population dynamics and social structures, and settlement structure, concerning buildings and open spaces, and how these were used and lived in (Hodder 2006). Çatalhöyük midden deposits are rich in refuse, with less tangible archaeological components such as decayed organic material, and are formed through deliberate and sequential accumulation of material at a specific location, often between clusters of buildings or within abandoned buildings (Russell and Martin 2005, Yeomans 2005). Midden deposits occur throughout the entire occupation history of the site, and this allows a comparison to be made between different periods and levels of occupation, where there are few other records available about aspects of day to day life, due to the cleanliness of the floors in buildings (Matthews 2005). Initial micromorphological studies of middens at Çatalhöyük, indicate that they contain a variety of deposit types that are not found in the “clean” building deposits (Matthews 2005), and which are related to activities such as food processing, cooking and building construction.

The site is a complex tell site over 20 m high, and covers over 13.5 hectares. It is estimated that as many as 8,000 people may have lived here (Mellaart 1967, Hodder 2006). Discovered by James Mellaart in the late 1950s, the first excavations were carried out between 1961 and 1965 (Mellaart 1962, 1963, 1964, 1966). Çatalhöyük became recognised internationally due to the size and density of the settlement and the wealth of the wall paintings and other artwork uncovered within the buildings. The site comprises two mounds – the early Neolithic East mound and the later Chalcolithic West mound (Figure 2.2). Since 1993 an international team led

16

Figure 2.2: Site plan of Çatalhöyük showing the different excavation areas.

In recent years much effort has been made to bring in a wide range of specialists in order to obtain detailed interdisciplinary information about the origins of, and occupation at, the site; in particular the daily lives of the inhabitants, such as food consumption and the relationship with the environment, are seen as a major focus (Hodder 1996), hence the research presented here is a major aspect of current research at Çatalhöyük, and expands on the previous work as detailed in Chapter 1. Çatalhöyük was selected as the case study due to the excellent preservation and extent of the midden deposits, which provide an extensive record of activities, and the uninterrupted temporal sequence, which spans the early Neolithic to Chalcolithic, and thus has potential for investigating issues of diet, resource use and seasonality in the Neolithic. Previous work on other sources of information such as the charred plant remains and animal bone also allow a useful comparison to be made between the information gained from these techniques and the micro analytical approach used in this research.

years before being demolished (Cessford et al. 2005). Middens are located both between buildings in “open areas”, and within buildings that are no longer used for habitation. Table 2.1: Summary of the Çatalhöyük excavation areas. See Figure 2.3 for an aerial photo showing these areas.

Excavation area

Overview

BACH

Berkeley Archaeologists at Çatalhöyük

Forty-forty (4040)

South

Originally called Mellaart area, this is where the original excavations were carried out. The Deep Sounding is also located in this area. Span Levels IX to IV at present. Excavation aim is to investigate earlier levels.

TP

Area being excavated since 2001 by a team from Poznań, Poland. Located at the highest point of the east mound i.e. the latest levels of occupation, levels III – 0

The organisation of excavation at Çatalhöyük In order to understand the context of samples studied in this research, a brief summary of the organisation of excavation at Çatalhöyük is given here to help the reader to understand the site. Çatalhöyük is divided into a number of main excavation areas (Figure 2.2 and 2.3, Table 2.1), each of which is divided into buildings and spaces. The vertical extent of the tell is divided into levels which are based roughly on a chronological sequence devised by Mellaart (currently under revision). Excavations have revealed at least 16 levels at the site. It is an example of a tell site, where older buildings are demolished, filled in, and new buildings are constructed on top, thus the site grows vertically over time. In general a building is thought to have had a life span of 70 - 120

West

KOPAL

17

North Area. 2004 excavations investigated large areas of buildings and possible “street” layers

Limited excavations have been carried out on the later west mound. Post Neolithic deposits. Konya basin Palaeoenvironment research. Not shown on map – offsite location for paleoecological samples, at the northern edge of the East mound.

was first occupied on the alluvial layers which accumulated in the early Holocene. The onset of the Holocene in this region around 9500 cal BC led to a warmer and moister environment in the Konya plain and the formation of alluvial fans and wetland which would provide attractive resources to the first settlers at Çatalhöyük.

Geology, soils and climate of the region As aspects of this research concern the human relationship with the environment and resource use, it is necessary to understand the local geology and soils, both at present and during the occupation of Çatalhöyük. Seasonality of activities and resource use is fundamentally linked to the environment, particularly the availability of plant, animal and water resources. Here is given a brief summary of the environment at Çatalhöyük. This is understood largely through an intensive survey and paleoenvironmental work as part of KOPAL.

The backswamp clay indicates a very wet environment with seasonal or semi permanent flooding. Quarrying of the lake marl suggests seasonally drier periods, most likely in the summer periods when flooding is less likely, which shows how environment is linked to seasonality. Work on the 1999 cores also shows anthropogenic deposits sealed by further backswamp clays, suggesting a more permanent flooding in the later Neolithic occupation phase. Above the backswamp there are possible alluvium/colluvium and buried soil horizons indicating drier periods at the very end of the Neolithic. These results show that the environment of Neolithic Çatalhöyük varied considerably over the lifetime of the settlement, and perhaps even during the lifetime of the inhabitants.

The KOPAL project (KOnya basin PALaeoenvironmental project), including pollen and macrofossil analysis of lake cores, has been used as a means of vegetation and paleoenvironmental reconstruction in central and south Turkey (Roberts et al. 1999). This has been carried out to determine the hNeolithic environment at Çatalhöyük in order that questions about early agriculture and the surrounding landscape may be better addressed (Roberts et al. 1999, Boyer et al. 2006). Pollen and macrofossil data indicates that the onset of the Holocene was rapid, with a distinct shift from herb to grass steppe, though the change from non arboreal to arboreal vegetation was much slower, taking 3000 years to reach the arboreal pollen maximum (Boyer et al. 2006). Although dry today, up until the 20th century soils remained waterlogged for a large part of the year (Driessen and de Meester 1969).

Changes from drier to wetter periods and corresponding changes in plant and animal resource availability suggest the inhabitants’ activities may have had to respond to cope with such changes, for example it is suggested that changes in fuel use may be a response to increased aridity (Asouti and Hather 2001). An interesting question is where was the location of crop growing? With such a wet and fluctuating environment, the possibility of growing crops seems unlikely, and it is suggested that this occurred c.12 km off site (Rosen and Roberts 2009). The debate on the use of cereals will be examined in this research by looking for evidence of the frequency of cereal consumption in individual midden deposits, and through extraction of phytoliths from coprolites.

Çatalhöyük is situated in the Çumra area of the Konya basin, itself a part of the Central Anatolian Plateau (Figure 2.3). The Central Anatolian Plateau is around 10,000 km2 in area and includes Konya, Karaman, Karapınar, Ereğli and Bar as well as the Çumra plain. The plateau is surrounded in the south by the Taros Mountains, composed of Upper Cretaceous limestone, and in the North and West by the Anatolides, composed of Palaeozoic limestone and schist. During the Pleistocene, areas of the Konya basin were covered by a shallow lake, indicated by relict cliffs and beach ridges (Driessen and de Meester 1969). This lake became gradually infilled by calcareous material and eventually dried up, with the shorelines receding towards the middle of the basin. Material was also brought into the system from upland rivers which deposited coarse sediments on the shores, forming the May and Çarşamba bajadas (alluvial features formed by the lateral merging of a series of alluvial fans) in the South and East.

This wetland environment provided a range of plant and animal and plant resource use such as wetland birds, wood and reeds. Previous research at Çatalhöyük has discussed the use of these resources, for example, through animal bone studies which show the presence of geese, ducks and other water birds (Russell and McGowen 2005), macrobotanical analysis showing a range of wetland species in use (Fairbairn et al. 2005), and phytolith studies indicating the presence of Phragmites reeds (Rosen 2005). An integration of these studies has been attempted to suggest ways in which these resources were used on a seasonal basis. This research aims to contribute to these previous studies by examining these materials in their precise depositional context in individual layers in middens, to see if the precise context and association can give more detailed information of exactly how these resources were being used for different activities, and to examine possible cycles of use which may be seasonal.

The alluvial fan of the Çarşamba overlies the lacustrine bed of palaeo Lake Konya, and a distributary of the Çarşamba ran between the 2 mounds before drainage was modified. The whole fan is dotted with a number of “höyüks” or mounds, many of which have been buried by Holocene alluviation (Baird 2005, Boyer et al. 2006). Dating and sedimentary analyses show Çatalhöyük is situated on riverine clay silts that overlay the Pleistocene lake marl which indicates that the site

18

Figure 2.3: Map showing the geomorphology of Central Anatolia (Kuzucuoğlu 2002). Dating sequence at Çatalhöyük Chronological change is a significant aspect of the research aims at Çatalhöyük (Hodder 2006) and in the study of middens in this research. Previous research suggests increasing technological strategies post Level VII (Conolly 1999, Carter and Shackley 2007). By examining evidence for craft activities in middens, this hypothesis is investigated further to see if there are corresponding changes in activities and resource use, such as fuel use, which may be linked to technological changes.

Currently the timeframe of midden formation is understood only in broad terms. Problems in understanding the absolute rate of midden formation processes have been recognised (Stein and Deo 2003). By examining individual fine layers for distinctly seasonal deposits, it may be possible to link individual layers to different times of the year, for example concentrations of dendritic phytoliths have been suggested as an indicator of spring deposition (Rosen 2005). These have the potential to provide a relative chronology of deposit build up between these seasonal marker deposits.

The precise dating sequence for Çatalhöyük is currently under revision due to methodological problems at the Oxford Radiocarbon Accelerator Unit (Bayliss and Farid 2007). A technical problem with the method of bone pretreatment on samples analysed between 2000 – 2002 means that these dates are 100 – 300 radiocarbon years too old (Bronk Ramsey et al. 2004). Current estimations of the dates that each level represents can be seen in Figure 2.4 (Cessford et al. 2005). Samples have been dated from the South Area sequence, the north area, and the KOPAL area. The number of years that is represented by each level of occupation is estimated in the region of 50 to 80 (68% probability) or 45 to 90 (95% probability). The middens sampled span levels VII, VI, V and III to 0 at the latest. 19

Figure 2.4: Dating sequence (Cessford et al.)

micromorphology. Undisturbed micromorphology samples for thin section micromorphology were collected according to a standard procedure (Bullock et al. 1985, Courty et al. 1989).

Field work and sampling strategy As well as investigating deposits within a single midden, the sampling strategy was devised to investigate longer term change over the entire life cycle of the site, by selecting samples from seven different middens, spanning levels VII to III/0. Middens were selected to cover a wide spatial and temporal range. These have been assigned numbers 1 to 7. The precise location of the middens was determined by the limits of excavation in the two field seasons when sampling was carried out (2004 and 2006), as it is necessary to have an entire section of a midden exposed to collect micromorphology samples. Associated section and plan drawings are referred to in Table 2.2. Photographs of the middens and descriptions of these at the macroscale are discussed alongside thin section microscale observations in Chapter 4.

The South Area middens are the earliest samples analysed (Levels VII, VII, VI) followed by the 4040 area middens (Levels VI, V, dated at 6550 cal BC at the earliest, and finally the TP area midden (Levels III – 0, not dated but estimated at later than 6090 cal BC), which represents the latest level of occupation at the site prior to abandonment and burial by post Neolithic activity. The aim is to investigate whether there are any changes in activity deposits associated with other major changes that have previously been identified at the site, such as the introduction of more and finer pottery (post Level VII) and changes in settlement organisation, with more architectural variation and open spaces from Level V (Hodder 2006). These changes may have impacts on the deposits in the middens, for example the activity of pottery production may be represented by large ash layers with clay debris. Examining the frequency of such deposits in the middens will help understand the possibly cyclical nature of these activities.

For older samples such as the Deep Sounding area, sampling has been limited by the fact that these levels were excavated during the 1994 – 1999 field seasons, and have now been backfilled for safety reasons. The sampling strategy for the new midden samples from the excavation seasons 2004 and 2006 has been carefully devised so that a number of analytical methods can be applied to samples from the same contexts, so that the results from one analysis can be compared with confidence to results from another analysis.

Midden 1 (Level VII/VIII) is the earliest of the South Area middens examined here and samples from here have been examined previously (Shillito 2004). In this study, a further sample block was analysed from this area for phytoliths (Unit 1668). Midden 2 (Level VI) is from the level of occupation immediately above Midden 1, and Midden 3 (Level VI, III) in the 4040 area is either contemporary with Midden 2 or the level immediately

The samples available from previous field seasons at the site, in storage in Turkey and Cambridge, include suspected coprolites for biomolecular analysis of organic residues (see Chapter 7). Samples were selected with the aim of producing slides for thin section

Figure 2.4: Section drawing of Midden 1, South Area, Unit 1668, East face.

20

Figure 2.5: Section drawing of the South Area Midden 2, West and North faces 2006, showing positions of thin section block samples and organic residue samples (marked with crosses).2.2.2 4040 Area

Figure 2.6: Section drawing of Midden 6, West face, showing positions of micromorphology block samples and organic residue samples (marked with crosses).

analysis were taken both from the thin section blocks, and from adjacent deposits in the field, from Middens 2 and 6, in addition to possible coprolites from graves (see Chapter 7). Sample locations were recorded in detail on section drawings and photographs, to allow direct comparison between analysis of sub samples and micromorphology. For analysis and interpretation of results, samples are considered in order of their temporal position, from the earliest to the latest levels. Figure 2.11 gives an example of how samples were collected, and how the sample collection in the field relates to the final thin section.

above Midden 2. Dates of middens 4 and 5 are slightly unclear but are estimated to be levels VII – VI and so are contemporary with, or immediately above, Middens 2 and 3. Midden 6 is also unassigned at present, but is estimated to be level VI/V, making it contemporary with 3 and 4, and Midden 7 in the TP Area is the latest, levels III – 0. A new program of dating is currently in progress as discussed earlier. Within a single midden, areas for sampling were chosen by cleaning and surveying the entire exposed section of the midden and selecting an area that seemed most representative, and that showed the least sign of disturbance by root or animal action. A high resolution photograph was taken of the exposed face, as well as detailed section drawings by the excavators, on which sample locations were marked. Table 2.2 summarises the thin section blocks that were collected in the field from each of the seven middens.

South Area Seven blocks were collected from the South Area – 1 block from Midden 1 and 6 blocks from Midden 2. The location of the middens can be seen in the plans in Figure 2.7 – 2.9. Section drawings and photographs of different sections are shown in Figures 2.4 – 2.5. Midden 1 was excavated in 1996 and extends across the whole length of the area called Space 115, on a gradual slope from east to west and a slight slope from north to south. It is classed

Further sub samples taken from these blocks for phytolith and chemical microanalysis are detailed in the relevant results chapters. Spot samples for organic residue

21

as an external midden area, with Mellaart’s horizon of Level VII buildings being constructed over the midden (Farid 1996). The Çatalhöyük excavation database gives the dimensions as 2.8m (N-S) by 2.2m (E-W) with a depth of 0.16m (E) and 0.23m (W). Macroscopically Midden 1 appeared to have some extensive charcoal layers. Midden 2 covers Space 261, and is bounded to the west by an external wall and to the north by an eroded slope from post-Mellaart excavations. The southern and eastern extent of the midden is arbitrarily defined by the limit of excavation. The dimensions are 5.5 m by 3.08 m, east to west and north to south respectively. The space has been given 4 life phases which are discussed further in Chapter 4. In the field Midden 2 was observed to be particularly rich in possible coprolitic material, containing several rounded orange inclusions of c. 4-5cm. It could be that these were particularly well preserved having only been exposed at the end of the 2005, with sample collection in the 2006 season. It was also noted that this midden contained particularly extensive layers of repeated charcoal and reddish sediments overlain by very thick white ash layers, suggested by the excavation report to be areas of lime burning for plaster production (McCann and Brown 2006).

Figure 2.8: Plan of buildings around Space 280, showing location of Midden 3, 4, 5 and 6

4040 Area Eight sample blocks were collected from three middens in the 4040 area, labelled Middens 3, 4, 5 and 6; see Table 2.2 for sample details. Plans showing the location of these middens and the surrounding buildings can be seen in Figures 2.8 – 2.9. A section drawing and photograph of Midden 6 can be seen in Figure 2.6.

Samples were selected to cover a range of multiple fine layers from the base to the top of the excavated midden, in both the pre and post cut phases. Sub samples were also carefully collected from the ash layers to investigate phytolith and dung remains which could indicate the type of fuel used, as well as the reddish sediments, which could be analysed using FT-IR to estimate the temperature at which these fires were burning. An important observation in the field which is not mentioned in the excavation report is the presence of numerous orange lumps of clay like material containing pseudomorphic voids from plant stems. A sample was also collected of this material. Results of this analysis can be found in Chapter 6.

Figure 2.7: Plan of buildings in the South Area. Figure 2.9: Details of features around Space 287

22

Table 2.2: Summary of the micromorphology samples. Year Area Space Level Excavation Unit 2004

Context/field observations

Thin sections analysed

Midden number

Associated figures

TP

None

III-0

8932

Upper middle band of grey ashy lenses

8932 S7

7

Figure 2.19 Figure 2.20

TP

None

III-0

8932

South section, north facing, lowermost lenses of sediment and ash on top of brick/rubble

8932 S3 (1 and2)

7

Figure 2.19 Figure 2.20

TP

None

III-0

8932

South section, north facing, upper middle, grey ashy

8932 S9

7

Figure 2.19 Figure 2.20

2003

TP

none

III-0

7867

7867 S2

7

2004

4040

100

III-0

7931

?roof collapse middle sample, last section of midden above fill Last remaining segment of midden above blocky/bricky fill

7931 S3 (1 and 2)

5

Figure 2.19 Figure 2.20 Figure 4.35

2004

4040 4040

232 232

VI, III VI, III

11016 11017

Midden like ?street layers ?street long sequence of multiple lenses and in situ burning

11016 11017 S1

3 3

Figure 4.33 Figure 4.33

4040 South area South area

229 115

VI, III VI, VIII

10711 1668

4 1

261

VI

12558

South area

261

VI

12504

fine layers over ash and another burning/ash sequence

2

Figure 4.34 Figure 2.10 Figure 2.15 Figure 2.11 Figure 2.12 Figure 2.14 Figure 2.11 Figure 2.12 Figure 2.14

South area

261

VI

12504

Continuation of fine layering and burning/ash sequence

2

Figure 2.11 Figure 2.12 Figure 2.14

South area

261

VI

12558

Very fine layers of burnt and ashy material

S2

2

Figure 2.11 Figure 2.12 Figure 2.14

South area

261

VI

12519

Continuation of sequence, very fine layers of deposits

S9

2

Figure 2.10 Figure 2.11 Figure 2.12 Figure 2.14

South area

261

VI

12524

Continuation of sequence of fine layers, base of midden

2

Figure 2.11 Figure 2.12 Figure 2.13 Figure 2.14

4040

279

Unassig ned, c. VI/V

13103

Near top of midden, large burnt/ash sequence

S22

6

Figure 2.16 Figure 2.17 Figure 2.18

4040

279

Unassig ned, c. VI/V

13103

S20

6

Figure 2.16 Figure 2.17 Figure 2.18

1996 2006

2006

Fine layering and repeated burning/ash sequence Fine layering and repeated burning/ash sequence

2

Smaller burnt/ash sequence with finely stratified layers

4040

279

Unassig ned, c. VI/V

13103

Very finely stratified layers

S32

6

Figure 2.16 Figure 2.17 Figure 2.18

4040

279

Unassig ned, c. VI/V

13103

Continuation of sequence above S 25, base of block includes large ashy layer

S28

6

Figure 2.16 Figure 2.17 Figure 2.18

4040

279

Unassig ned, c. VI/V

13103

Section through burnt/ash sequence

S25

6

Figure 2.16 Figure 2.17 Figure 2.18

4040

279

Unassig ned, c. VI/V

13103

Continuation of sequence, finely stratified, base of midden

S26

6

Figure 2.16 Figure 2.17 Figure 2.18

23

Figure 2.10: TP area section, Midden 7.

Figure 2.11: Sample collection procedure.

24

location of sub samples for other analyses, and in turn the section photos and section drawings. The locations of spot phytolith and chemical samples were plotted on the thin section scans. These photographs can be found in the Appendix.

TP Area Six samples were taken from the TP area, from one midden labelled Midden 7. See Table 2.3 for sample details. A section drawing is shown in Figure 2.2. Plans of the TP area are not currently available.

Summary of the case study and sampling Comparison of microanalysis data and field data Çatalhöyük has been chosen as a case study for which questions regarding the development of resource use, subsistence and diet in the Neolithic can be examined. The site provides an extensive spatial and temporal range of deposits which can be examined. Middens are particularly rich in material which can be used to answer these questions, such as plant remains, with the added advantage that these deposits can be examined in their precise depositional context due to the methodology adopted in this research. This is an approach which has not previously been utilised at the site, and which it is hoped will contribute to other methods of enquiry such as macrobotanical remains and charcoal. Sampling has covered seven middens. Chapter 3 gives an overview of the methods used and previous applications of these methods in archaeology.

The approach being used in this research is a detailed multi-scalar and contextual approach to understanding midden formation processes. Before beginning microscopic analysis, samples were studied at the mesoscopic level by eye and through scanned high resolution images of the slides, which allows quick and easy comparison with field sections and photographs (Arpin et al. 2002). Print outs of the scanned images were used alongside microscopic study to record initial observations on deposit types and boundaries. This level of comparison was essential to compare the thin sections with the field photographs, which gives a better overview of the sample context and any surrounding features, and the interrelationships of different scales of analysis. These images were also compared to the original photos of the unprepared sample blocks, which show the precise

25

CHAPTER 3: INSTRUMENTATION

METHODS

phytoliths are not informative for certain deposit types, discussed in Chapter 5.

AND

Introduction

Thin section methodology

The following chapter describes the methods used in this research, which were introduced in Chapter 1. This includes thin section micromorphology, phytolith analysis, bimolecular analysis of organic residues by gas chromatography mass spectrometry (GC/GC-MS), infra red analysis (FT-IR), scanning electron microscopy (SEM-EDX) and X-ray diffraction (XRD). Micromorphology, phytolith and FT-IR analyses were carried out at the University of Reading in the departments of archaeology, soil science and chemistry. The SEM-EDX was carried out at the University of Reading Centre for Advance Microscopy (CFAM), and the organic residue analysis was carried out at the NERC Life Sciences Mass Spectrometry Facility (LSMSF) in Bristol (funded by 2 NERC LSMSF awards). XRD analyses (and some FT-IR) were carried out at the Central Laboratory of the Research Councils Daresbury Laboratory using synchrotron radiation source (SRS) XRD, with a project facility grant.

Thin section micromorphology involves the impregnation of large blocks of sediments taken from a soil or occupation deposit sequence. After field collection, the blocks were oven dried for a period of 2 weeks or until all moisture had evaporated. This was checked by periodically weighing the samples to constant mass. Thin section samples were prepared in six stages (Table 3.1) using a methodology developed by Mr John Jack (Geoscience Technician) at the University of Reading (unpublished). Table 3.1: Summary of stages in thin section methodology Stage 1 Stage 2 Stage 3: Stage 4: Stage 5: Stage 6:

Resin impregnation Slice cutting and temporary mounting Grinding and polishing face Permanent mounting to a glass slide with UV glue Fine grinding to a thickness of 30 μm Hand finishing and coverslipping

Stage 1: resin impregnation

Laboratory sub-sampling for secondary analyses

The dried sample was placed in a made to measure foil box and placed inside a desiccator. The equipment set up can be seen in the diagram below (Figure 3.1). A vacuum was applied to the desiccator by closing tap 1 and 2 and opening tap 3, for at least 12 h to ensure that all air is removed from the sample. When the desiccator was under full vacuum, epoxy resin was prepared and added to the separating funnel attached to the desiccator. This was done by closing tap 3 to keep the desiccator under vacuum, removing the tubing from the top of the separating funnel, and pouring the resin in through a funnel. The tubing was replaced, and the vacuum pump was switched to the funnel by slowly opening tap 1, and the air was slowly removed from the resin. Once the resin chamber and desiccator were both under vacuum, tap number 2 was opened slowly and the resin allowed to drip through into the desiccator. More resin was added (with slow removal of air each time) until the entire sample was covered in resin. The sample was then left under vacuum for another 12 h (or until the resin in the sample had stopped bubbling completely) to ensure that any remaining air was removed and that the entire sample was completely impregnated with the resin. The next day the sample was carefully removed and placed into an oven at 70 °C for 18 h to harden the resin.

The aim of the laboratory sampling was to enable comparison of the results from sub-sample analyses with the results from thin sections analysis of the block samples collected in the field. When sub sampling, great care was taken to extract sub samples directly from individual layers. Where possible up to 10 g of sub sample were taken, though for the finer layers this was not always possible, and limited sub sample analyses were possible. Visual examination in the field gives a first glimpse into the layering present in the middens. Midden deposits at Çatalhöyük are very finely layered, with some layers only a few mm thick. The laboratory sampling strategy was devised to extract these fine layers individually, so that each can be studied separately using a range of analytical methods, before studying them in situ as thin sections. The face of each block was cleared by scraping away the top of the block face, so that any contamination is removed. This was achieved using a sharp scalpel and by gently blowing away excess material. After a clean face was achieved and the layers were clearly visible, a digital photograph was taken with a scale included. These photographs were printed out, so that when sub samples were taken, their exact location could be marked on the photograph for future comparison with thin section micromorphology slides. The layers were removed using a scalpel and spatula, and transferred to labelled glass jars. These sub samples were then subjected to phytolith and chemical analyses. It was initially proposed to carry out all of the analytical techniques on all of the sub samples, but time constraints did not allow this. Future work will target phytolith analysis in particular after examination in thin section, as this research suggests

Stage 2: slice cutting and temporary mounting After impregnation a slice was cut from the sample in the hardened block of resin. The sample was carefully secured in a saw, and a slice of around 1cm was removed from the face of interest. This slice was mounted to a glass slide by using temporary glue. A glass slide was placed on a hotplate at 70 °C, and the glue stick is carefully rubbed over the surface of the slide. The glue melts onto the slide at this temperature, and the sample

26

Brot machine for fine grinding. As the distance between the sample and the grinding wheel is known, the Brot was set to grind the sample to a selected thickness of 30 μm. This was checked at regular intervals using a micrometer.

was then pressed onto the glue. The slide with the sample slice attached was then placed under a mounting jig at high pressure for a few minutes to allow the glue to cool and set.

Stage 6: hand finishing and coverslipping For some samples it was necessary to hand finish the sections before cover slipping, for example if the slide contained material of very different hardnesses, the surface tends to be thicker in those areas which are harder. Hand finishing was done by lubricating the surface with Brot oil and polishing with silicon carbide paper, checking the surface regularly under a microscope to judge how close it is to a thickness of 30 μm. When the entire surface was at 30 μm, a glass coverslip was added using the UV curing glue. A layer of glue was added to one side of the slide, and the coverslip carefully lowered with tweezers to ensure that no air bubbles are present. The glue was then cured under a UV lamp. Analysis by optical microscopy Thin sections were analysed by examination under an optical polarising light microscope. The microscope used was a Leica DMLP microscope with an integrated Leica DFC320 microscope camera using the Leica digital capture and image analysis software (IM50 and IM1000) which allows high resolution image capture with measurement functions (Leica Microsystems GmbH, Germany). Examination of the slides was carried out over a range of magnifications from 10 to 400 x, using mainly plane polarised (PPL) and cross polarised (XPL) transmitted light. Archaeological thin section analysis requires the use of polarising light to identify minerals and the sedimentary matrix, as well as to distinguish between organic and inorganic silica, and to identify other important components such as calcareous spherulites present in faecal material.

Figure 3.1: Equipment set up for the addition of epoxy resin under vacuum to micromorphology samples.

Stage 3: grinding and polishing face The face up part of the sample is the sample face. It is necessary to prepare this surface so it is completely flat and smooth, so that it can be glued permanently to a glass slide. This was done using a Brot machine (an oil-cooled precision grinder-polisher which can grind samples to 30 μm). The samples were attached to a sample holder using sciron oil to create a sealed surface against a metal plate. The sample plate was then rotated (three samples can be held at a time), and a grinding plate was gradually moved closer and closer to slowly grind the surface. The surface of the samples was marked with ink so that it was possible to see when the entire surface has been completely ground. After polishing the slide was removed from the temporary slide holder by placing the sample on a hot plate at 50 °C and melting the glue.

The microscope is equipped with a large rotating 360° stage suitable for the analysis of large thin section slides. Oblique incident light (OIL) was used where necessary to examine opaque minerals and the presence of ochre. Deposits are described using standard terminology (Bullock et al. 1985, Courty et al. 1989).

Stage 4: permanent mounting The smooth face of the slide was blown gently to remove any debris and wiped with alcohol to remove any traces of oil, and a thin layer of UV setting glue was applied. A pre-prepared frosted glass slide was carefully lowered onto the sample, taking care not to introduce any air bubbles. The sample was placed under a mounting jig under high pressure for 5 min, and then the whole jig was placed under a UV lamp, where the glue was allowed to set for 3 min. The sample was removed from the jig and any excess glue scraped away using a sharp blade.

Phytolith methodology Processing of phytolith containing samples was done in batches of 10 samples. There are a number of methods to extract phytoliths from the archaeological matrix. The following is a method developed by Rosen (pers. comm.) based on Albert and Weiner (2001) and which has already been used in previous phytolith work at Çatalhöyük (Rosen 2005, Jenkins 2005). The method is summarised in Table 3.3.

Stage 5: fine grinding to 30 μm The block was first trimmed down to 1 mm thickness using a hand saw before it was mounted back onto the

27

Table 3.3: Summary of the stages in phytolith sample preparation. Stage 1 Carbonate Removal Stage 2 Clay removal Stage 3 Organic matter removal Stage 4 Removal of non phytolith mineral material Stage 5 Weighing and mounting extracted phytolith material

[Na6(H2W12O40).H2O]. The amount of sodium polytungstate was previously calibrated to give a density of 2.3 g cm3 (phytoliths have densities between 2.1 and 2.2 g cm3). The sample was added to the tube, the cap closed and the samples were shaken vigorously using a vortex mixer. The tubes were centrifuged at 800 rpm for 10 min, then the suspense containing the phytoliths was poured off into clean 15 ml tubes. Distilled water was added to the tubes containing the phytoliths to adjust the density, and they were centrifuged at 2000 rpm for 5 min. At this stage the phytoliths were at the bottom of the tube. The suspense containing the sodium polytungstate was poured off through a filter into a wash container, was then filtered again into a measuring cylinder, then was finally filtered into a storage container for reuse. Distilled water was added to the samples that remain in the tubes to wash them, and then they were pipetted into a small container and dried. After drying was complete the total mass of phytoliths recovered from each sample was determined by weighing.

Stage 1: Carbonate removal The first step involves the removal of carbonates. Approximately 800 mg of the sample was passed through a sieve of 0.5 mm, onto paper with a shiny surface, and was then transferred from the paper into a 50ml centrifuge tube. The total mass of the samples was obtained by using an analytical pan balance and subtracting the weight of the centrifuge tube. To remove carbonates 10% HCl was added into the tube. The sample stops effervescing when all carbonate has been removed. It was found that usually less than 7.5 ml HCl is sufficient. Distilled water was then added to dilute the acid and the sample was centrifuged at 2000 rpm for 5 min. After the first spin, the supernatant was poured off and the rinsing and centrifuging repeated two more times. The samples were then left overnight in a little distilled water to help disperse the clays.

Stage 5: Weighing and mounting extracted phytolith material To enable a quantitative analysis to be made it was necessary to be specific in the way in which the samples were mounted. A 3 x 1 inch slide was labelled and placed over a beaker on a digital pan balance. The balance was tared and a few drops of Entellan mounting agent were added to the slide using a dropper bottle. Approximately 3 mg of phytoliths were added to the slide, with the exact weigh being recorded and added to a spreadsheet in order to calculate the total number of phytoliths per weight of sample. The slides were mixed well with a tooth pick to get an even distribution on the slide, and a cover slip was added. Care was taken not to press down and break the slide, and to make sure that no air bubbles were present. The slides were labelled with pencil and left to dry for a day or so.

Stage 2: Clay removal Excess water was pipetted off and 15-20 ml sodium hexametaphosphate was added. The samples were stirred vigorously and poured into a tall 400 ml beaker, and distilled water was added to make the height to 8 cm. Stoke’s Law was used to estimate the time that the samples were left to allow all the clay particles to settle. They were left for 1h and 10 min, 10 minutes being added to compensate for the slight change in density caused by the addition of sodium hexametaphosphate. After leaving the samples for this time, the suspense was poured off down to 100 ml, refilled to an 8 cm depth again, and allowed to stand for another 1 h. This procedure was repeated until the suspense was clear. Any remaining liquid was pipetted off, and the samples were transferred to crucibles and left to dry in a drying oven overnight at 50 ºC.

Quantifying phytoliths and interpretation of results In order to quantify the results, measurements were made at different stages of the extraction method, which allows the number of each phytolith type per gram of sediment to be calculated (Albert and Weiner 2001). An Excel spreadsheet had already been prepared to allow this to be done quickly for a large number of samples (courtesy of Dr Rosen, UCL). An extensive number of phytolith reference slides were prepared using material from the University of Reading Herbarium, whilst a number of up to date references have been acquired to help with the full identification of species present. Details of the reference species are given in Chapter 5.

Stage 3: Organic matter removal Any lumps in the dried samples were broken up before being placed in a muffle furnace for 2 h at 500 ºC. The oven was then turned off and the samples were allowed to cool. Organic material may also be removed by adding concentrated HNO3 and heating in a water bath at 100 °C for approximately 1h. This was tried for one batch but was time consuming and difficult, so all the following batches used the muffle furnace method.

The slides were prepared by mounting a known weight onto a 22 x 22 mm coverslipped slide. At a magnification of x400 there are 48 fields of view in one 22mm column of the slide, which equals 2304 total fields of view on the slide (sometimes a few extra fields are added if the mounting agent spreads beyond the boundaries of the

Stage 4: Removal of non phytolith mineral material A 15 ml polypropylene centrifuge tube was filled with exactly 3 ml of sodium polytungstate solution

28

any contamination of the samples, including cleaning of all glassware using Decon solution followed by dichloromethane (DCM) extracted double distilled water, HPLC grade acetone then drying in an oven. Sample vials are further cleaned in a furnace.

coverslip). Thus we can calculate the number of phytoliths per slide as follows: Phytolith count Number of fields counted x total number of fields on slide

Table 3.4: Summary of the stages in the residue extraction method Stage 1 Soxhlet extraction Stage 2 Saponification Stage 3 Water removal Stage 4 Aminopropyl SPE extraction Stage 5 Neutral fraction processing Stage 6 Acid fraction processing Stage 7 Analysis of extracts by GC and GC-MS

Then the number of phytoliths per gram of sediment can be calculated as follows: Number per slide Mass of phytoliths mounted

x

Mass phytoliths extracted Total sediment weight

x1000

A known number of fields were studied at x 400 magnification, and between 200 to 300 single cell and between 50 to100 multi cell phytoliths were counted. It has been demonstrated that counting 194 phytoliths with consistent morphology gives a 23% error margin, which is reduced to 12% for 265 phytoliths (Albert and Weiner 2001). Phytoliths were quantified using the Leica DMLP microscope as described earlier, with an XY mechanical stage (slide holder) attached for holding and moving the slides at fixed intervals.

Stage 1: Soxhlet extraction The first stage was to extract as much residue as possible from the sample using a Soxhlet apparatus. The finely ground sample was weighed into an extracted cellulose thimble, and plugged lightly with extracted glass wool to stop the sample being splashed out of the thimble during extraction, and placed inside the Soxhlet. A round bottom flask with a few anti bumping granules was filled with 200 ml DCM: acetone 9:1 v/v, and 200μl of internal standard was added to the round bottom flask. The standards are hycholic acid and preg-5-en-3β-ol. The Soxhlet apparatus was set up and left to run for at least 8 hours overnight. After extraction, the round bottom flasks were removed and a rotary evaporator was used to remove the solvent under reduced pressure at 65 °C.

Fourier Transform Infra Red Spectroscopy (FT-IR) For infra red spectroscopic analysis samples were ground with dried KBr powder and pressed (10 tons in-2) into thin discs. The FT-IR spectra were obtained using a Perkin-Elmer 1720-X Fourier Transform spectrometer with a deuterated triglycerine sulfate detector operating between 400 – 4000 cm-1 with a resolution of 4 cm-1. For examination under the infra red microscope, a Bruker Equinox 55 infrared spectrometer with a Bruker IRscope II Microscope Attachment was used. Extracted phytolith samples were placed onto a BaF2 window on the microscope stage, located using the visible light microscope, then targeted using the software available with the IR microscope. At Daresbury the samples were analysed using the Synchrotron Radiation Source (SRS), as the IR source. This gave a minimum spatial resolution of about 10x10 μm. Spectra were recorded between 600 and 400 cm-1 with a typical resolution of 8 cm-1.

Stage 2: Saponification The dried total lipid extract (TLE) was redissolved in 3 ml of DCM/isopropanol 2:1 v/v, and transferred to tall glass vials using a Pasteur pipette. The round bottom flask was rinsed with a further 3 ml of solvent which was also added to the tube. The solvent was then evaporated to dryness using a Techne dry block at 40 °C under nitrogen. When the solvent was fully evaporated 3 ml of 5M KOH in 90% methanol was added to the sample, which was heated at 110 °C for 1h. The hydrolyzed sample was allowed to cool, and 2 ml DDW were added. The pH was then adjusted to 3-4 using 6M HCl. The HCl is added carefully 1 drop at a time, while mixing with a whirly mixer and checking the pH carefully after each addition. The exact pH is important, as a too high pH means the carboxylic acids are deprotonated and will dissolve in aqueous media rather than organic solvents, whereas at too low a pH compounds with hydroxy groups will protonate and become hydrophilic.

Scanning Electron Microscopy and Energy Dispersive X-ray analysis SEM-EDX was carried out using an FEI Quanta 600 FEG Environmental SEM equipped with an Oxford INCA energy and wavelength dispersive X-ray system, at the Centre for Advanced Microscopy, University of Reading.

Stage 3: Water removal

Coprolite residue extraction method

3 ml diethyl ether was added and the sample was mixed thoroughly with a whirly mixer. The compounds dissolve in the organic solvent layer. Residual water was removed by passing the top layer of the samples through a short glass column filled with anhydrous Na2SO4. A second 3 ml portion of diethyl ether was used to rinse the tall vials and this is added to the Na2SO4 column. The solvent was then evaporated under nitrogen.

The method used in this research was developed by the Organic Geochemistry Unit and the University of Bristol (Bull et al. 2005) and is summarised in Table 3.4 and Figure 3.2. Training in this method was given at Bristol University through a grant provided by the NERC Life Sciences Mass Spectrometry Facility (LSMSF). Throughout this method the utmost care is taken to avoid

29

dichloromethane/hexane and further fractionated on activated silica gel. The samples were eluted with a further 5ml aliquot of dichloromethane/hexane then with dichloromethane/methanol. The solvent was removed under nitrogen, and the acids and sterols were converted to trimethylsilyl (TMS) derivatives by adding 100 μl TMS reagent and then leaving to stand under nitrogen at 70 ºC for 1h. The fully extracted samples were then diluted and the hexane phase was analysed.

Stage 4: Aminopropyl SPE extraction Phenomenex strata NH2 aminoproyl bonded-phase SPE cartridges were used. Two sets of vials were labelled to elute into – one set labelled n for the neutral fraction, and another labelled a for the acid fraction. The columns were washed using 6 ml of DCM/isopropanol 2:1 v/v. 1 ml DCM/isopropanol 2:1 v/v was used to redissolve the residue, and this was added to the washed SPE cartridge. The vial was rinsed through with a further 4 ml DCM/isopropanol 2:1 v/v which was also added to the cartridge. The first eluate collected with the DCM/isopropanol 2:1 v/v is the neutral fraction containing n-alkyl alcohols and sterols, with the more polar acid fraction remaining on the column. The acid fraction was eluted separately using 6 ml MeOH + 5% acetic acid. Both sets of vials were then dried under nitrogen. Stage 5: Neutral fraction processing The neutral fraction was further split into mixed neutrals and the important alcohol fraction using a silica gel 60 column. The column was rinsed through with 6 ml DCM. 1 ml DCM was added to the sample to redissolve the residue, which was sonicated to help it dissolve. The sample was then transferred to the column, and the sample vial rinsed with a further 1 ml DCM, and also added to the column. The column was rinsed through with 6 ml DCM and the eluate was discarded. The column was then rinsed with 2 ml DCM: methanol, and the eluate was collected in a vial labelled alc, and the vials were evaporated to dryness under nitrogen. The alcohol fraction was subjected to urea adduction to remove unwanted linear alcohols – the urea crystalises around linear compounds, leaving the cyclic compounds in solution. Urea solution was heated on a hotplate to dissolve all crystals into MeOH. 1 ml of hexane was added to the dried samples, then 0.5 ml of acetone added. The sample was transferred to a tall culture tube, and held on a vortex mixer. 1.5 ml urea solution was dropped into the centre of the vortex whilst mixing, and the sample was centrifuged for 5 min at 2500 rpm. The liquid was then transferred to a vial, taking care not to contaminate with urea crystals. 2 ml DDW were added to the sample to dissolve any urea crystals, and DCM to dissolve organic components. The sample was shaken vigorously and the top layer of water was removed and discarded. This step was omitted for the second phase samples due to the low concentrations of biomarkers observed in the first phase.

Figure 3.2: Diagrammatic summary of the GC-MS extraction method utilised in this work (after Bull, pers. comm.).

GC and GC-MS Instrumentation Analysis was carried out at Bristol using the Thermoquest Trace MS at the University of Bristol Organic Geochemistry Unit. This is a single quadropole GC-MS, fitted with programmable temperature vaporising and on column injectors. It operates in electron ionisation (IE) mode and has a CTC A200S autosampler. It is capable of analysing mass ranges from 2-1023 Daltons, and the mass resolution is adjustable up top 2500 at 100 Daltons. The mass stability is +/- 0.1 Daltons over 12 h, and the sensitivity is given at EI+ 50:1 on 10 pg benzophenone.

Stage 6: Acid fraction processing The solvent from the polar fraction (including bile acids) was removed under nitrogen and redissolved in 1ml methanol and methylated with 10 ml diazomethane in diethylether at room temperature overnight. The diethylether and excess diazomethane were removed under nitrogen and the residue was dissolved in

Electron ionisation uses a beam of electrons to ionise the sample. When the molecule loses one electron it forms the molecular ion, M+. When this peak is observed in the spectrum it gives us the molecular weight of the parent

30

molecule. It is usual for the molecule to fragment, producing further ions of smaller masses. The relative abundance of these secondary ions is characteristic of individual molecules, and so this information can help identify compounds of interest. After the sample is ionised the mass analyser separates the positively charged ions according to mass properties. The instrument used in this research has a single quadropole analyser. After separation the ions pass through a detector, which sends the information to a PC which converts the signals into visual outputs.

Summary of techniques used in this research The techniques used during this research were introduced in Chapter 1, and here in Chapter 3 have been presented with details on the specific methodology. The methods used are summarised in Table 3.5. For each technique the type of sample studied and the basic rationale for employing the method is given. Some indication as to what information may be forthcoming from the particular method is also given in the table.

GC-MS conditions The samples were injected into a GC separated with a silica capillary column. The oven was held for 1 min at 40 ºC, then the temperature was increased from 40 to 230 ºC at 20ºC min -1. The temperature was then increased to 300 ºC at 2 ºC min -1 for 20 minutes. He was used as a carrier gas, with a flame ionisation detector to monitor eluent. GC-MS peak assignments were made by comparison with known mass spectra and comparing retention times of authentic compounds followed by coinjection. Table 3.5: Summary of techniques used and research rationale. Sample type

Technique

Reason for analysis

What will results show?

Phytoliths

Microscopy

Species types and quantification

SEM-EDX

Morphology and trace elements within silica structure

FT-IR

To test the suitability of this method for determining the mineralogy of phytoliths Detailed mineralogy of individual phytoliths

Variations in plant types and plant parts represented spatially and temporally within middens Detailed morphology may show pitting, erosion etc, whilst trace elements may indicate growing region/conditions Major mineral components – characterisation of the sample matrix

IR microscopy

To investigate possible variations in mineralogy between phytolith samples, which may indicate phosphate and postdepositional processes e.g. gypsum formation.

SEM-EDX

Morphology and elemental analysis

GC-MS

Organic residue analysis

XRD and FT-IR

Mineralogy and crystalinity

Midden blocks

Thin section micromorpholog y

Microstructure

To investigate deposit types, activity types, post depositional alterations etc within blocks, and to make comparisons between blocks from different spatial and temporal contexts

Hackberry pericarps

XRD/IR

Mineralogy and crystalinity

Confirmation of hackberry as species, and preservation.

Coprolites

To support FT-IR analysis by confirming the presence of phosphate, and observe inclusions for possible dietary indicators e.g. phytoliths, bone fragments, seeds. To identify species types which can be used along with micromorphology and phytolith analysis to investigate diet. To investigate the preservation conditions and the process of coprolite mineralisation.

31

2 for details of the excavation areas and sampling strategy and Table 4.1 for a summary of the micromorphology samples). As well as representing different areas of the site, the middens examined are from different occupation levels, to allow comparison of activity residues from the middle phases of occupation with the latest.

4: THIN SECTION MICROMORPHOLOGY Introduction Currently midden formation processes at Çatalhöyük are poorly understood due to their complex stratigraphy (Yeomans 2005), and a lack of information on their timescale of accumulation (Stein and Deo 2003). Middens are currently excavated in large bulk units, and components such as plant remains and bones are analysed without reference to their specific micro-context and associations (e.g. Fairbairn et al. 2005b, Russell and Martin 2005). Previously thin section analysis has been used to distinguish individual layers (Matthews 2005), but only with a limited sample set, and there are problems in identifying some components, particularly phytoliths and coprolites, which are difficult to distinguish by thin section analysis alone.

Results A total of twenty thin sections have been studied, supported by the analysis of specific components – phytoliths, mineralogy and organic residues, detailed in Chapters 4 to 7. Results are presented here in chronological order of middens 1 to 7, beginning with the earliest levels of the South Area and working upwards to the latest samples studied from the TP area. Although traditional thin section micromorphology focuses on attributes such as structure and sorting, this approach was seen to be of limited use in these samples as the majority of deposits were unorientated and unsorted. A new system of classification was devised based on major components, and used to classify layers into deposit types.

In this research sequences of micromorphology blocks have been analysed to distinguish sequences of fine stratigraphy, supported by extracted phytolith and chemical analyses to complement the information seen in thin section, by identifying these components with greater certainty. Thin section micromorphology is well suited to investigating midden formation processes, as it enables the identification of single depositional events, and the examination of midden components in their precise depositional context (Matthews 2005). This enables investigation of the pre-depositional history, mode of deposition and post depositional alterations of the finely stratified deposit and the activity that produced it.

The classification of layers into individual deposit types allows a comparison of similar deposits within and between different middens. Deposit types have been classified primarily on the major inclusion type (e.g. plant material, aggregates) and secondly on the structural characteristics (e.g. in situ or redeposited). These deposit type classifications are presented then summarised in Table 4.3, after giving an overview of midden micro inclusions and structure, and the key micromorphological features of different middens on which the deposit type classifications are based.

Hypotheses to be tested It is hypothesised that observations of finely stratified midden deposits, using thin section micromorphology, will enable the identification of individual depositional events in a range of middens, and that the relative frequencies of different deposit types can be established. It is further hypothesised that seasonal “marker” deposits, such as dendritic phytoliths and hackberry pericarps, will be found in specific concentrations, rather than distributed evenly throughout the middens.

Table 4.1: Area and level of samples studied (see Chapter 2 for an explanation of area, space and level).

The aim is to identify and understand spatial and temporal trends in midden formation processes, to investigate resource use and diet at a high resolution timescale. This is achieved by examining midden deposits in their precise depositional context using thin section micromorphology. A further aim is to understand temporal patterns in midden formation, i.e. cyclicity and seasonality of midden formation, which is achieved by examining deposits from a wide spatial and temporal range, and observing concentrations of potential seasonal marker deposits as discussed in Chapter 1. The samples analysed are from three of the major excavation areas at Çatalhöyük – South Area, 4040 and TP Area (see Chapter

32

Midden number

Area

Space

Level

Slides analysed

1 2 3

South South 4040

VII/VIII VI III, VI

2 4 3

4

4040

115 261 232/240/ 60 229

VI, V

1

5 6

4040 4040

100 279

1 6

7

TP

none

VII-VI Unassigned, c. VI/V III-0

6

Table 4.2: Summary of midden inclusion types. Inclusion type Bone

Unburnt Burnt

Description

Variations

Significance

PPL: yellow appearance, varies from microscopic fragments to large inclusions with visible cell structure XPL: grey

Size and shape, roundness, preservation

Indicates waste from activity involving animal resource. Predepositonal burning may indicate cooking/hearth remains.

PPL: yellow to orange appearance, varies from microscopic fragments to large inclusions with visible cell structure XPL: bright orange

Post depositional burning may be a result of in situ burning in midden as part of a different activity.

Plant material Charred PPL: black charcoal fragments, often with cell structure intact Partially charred

PPL: brown-black

Phytoliths

PPL: siliceous, semi-transparent impressions of plant cells XPL: non-birefringent

Pseudomorphic voids

PPL: white, voids spaces where plant material was once present but has decayed in situ, leaving an impression of its former shape in the surrounding fine material. Often seen as impressions in building materials.

Size and shape, roundness, preservation, species

Plant burning activity. Partially charred plant material rather than fully burnt may indicate accidental burning.

Plant part/species, articulation, multi or single cells Size, shape

Plant decay in situ or burning in situ if associated with ash or rubified deposits. Plant decay in situ.

Coprolitic material/dung Amorphous, non-burnt PPL – yellow/orange, smooth, amorphous XPL – dark, often non-birefringent.

Size, shape, spherulites, plant and bone inclusions

Faecal waste deposition – cleaning

Charred 30%

Mixed hearth/floor sweepings

8d like 8c but inclusions < 30% of unit area

Sweepings from unburnt deposits e.g. floor, food processing area, storage area

8e plant and aggregate (unburnt), small rounded fragments >30% 9

Bone (burnt and unburnt)

Dumping from food processing, feasting remains, non food animal carcass

9 a large fragments of unburnt bone 9b large fragments of burnt bone 9c small burnt bone fragments

Dumping from food cooking – large debris clearout

9d small unburnt bone fragments

Fragments from food cooking Fragments from food processing

10

Mixed inclusions

10

Deposits contains a mixture of a number of inclusion types which are embedded and randomly orientated. These deposits may represent large scale tertiary deposition, and bioturbated deposits

51

Redeposited midden material from midden clearance in another area, e.g. for new building

thin section, and phytoliths are a major contribution to middens that need to be understood in terms of individual layers. FT-IR is used to characterise specific mineral components, and GC-MS is used to identify orange amorphous organic material suspected to be coprolites, which form a large proportion of midden deposits. The implications for questions relating to environment, diet and resource use, and periodicity of deposition, are discussed in Chapter 8.

Thin section observations have identified ten major deposit types, sub divided into thirty one sub types (see Table 4.4). In summary these comprise of deposits dominated by the following inclusions: charred plant material, phytolith plant material, calcitic ash, dung, amorphous organic material, burnt and unburnt aggregates, rock fragments, burnt and unburnt bone, and mixed inclusions (either two major types or no dominant types i.e. equal mixes of a number of inclusion types). Three of the major deposit types are present in all middens, comprising deposits dominated by ashy and charcoal rich deposits (major deposit types 1 and 3), which supports previous ideas about the importance of fire at Çatalhöyük (Cessford and Near 2005). This is also supported by the omnipresence of microcharcoal throughout the deposits. These are interspersed with burnt and unburnt aggregate material (major deposit type 6) and archaeozoological and archaeobotanical material. Less common but present in Middens 2 and 6 are large layers of repeated ash and in situ burning. Phytolith analysis (Chapter 5) suggests much of the ash layers to be largely grass/reed derived, and micromorphological identification of calcareous spherulites in some deposits shows that dung was also being burnt as fuel. There are some indications that the reeds seen in ash may be dung derived, supported by discrete animal dung deposits with embedded grass and reed phytoliths, for example in Midden 7, 8932 S7. However there are instances where reeds are seen with no evidence of the presence of dung. It is suggested that a mixture of dung containing grass and reeds as well as pure reed fuel was being used. There are also some important differences in observations between middens, which have implications for the interpretation of changing midden formation processes over time, as well as for seasonality and cyclicity of activities, fuel resources and diet. In particular, some differences are observed between the earlier South Area middens and later TP Area middens, which may be a result of changing intensity of occupation and different preservation conditions. On a broader scale thin section micromorphology and macroscale comparisons have distinguished between four major types of depositions:    

Sequences of multiple fine layers of ash, organics, phytoliths and coprolites Large aggregate rich layers of burnt and unburnt aggregates Large ash layers with underlying charcoal and rubified material from in situ burning Large layers of mixed redeposited material

The following Chapters 5 to 7 present results of analyses of sub samples from these micromorphology blocks, including phytolith analysis, FT-IR and GC-MS, to further understand and clarify information on formation processes with can be observed in thin section. Phytolith analysis is used as this component is difficult to see in 52

useful for gaining an overview of plant use and making general comparisons between major context types (Jenkins 2005), it does not give information on the variations between micro units, which relate to different activity types. This makes it impossible to relate the phytoliths seen in middens to a particular activity or use. Previously activity has been inferred only by associations of different phytolith types from bulk units – as these units may mix several deposits from different activities, there is no way of distinguishing between activities.

5: PHYTOLITH ANALYSIS Introduction Previous phytolith research Phytoliths from Çatalhöyük have been used to identify craft activities and the materials used in the construction of basketry and matting in distinct deposits adjacent to storage bins, indicating the use of Scirpus as matting material (Rosen 1998, 1999, 2005, Jenkins 2005). This activity is also inferred in other areas on the basis of large concentrations of Scirpus in platform deposits. Analysis of floors near ovens identified wheat husks associated with Phragmites, interpreted as fuel, though it is not clear whether this means just the reeds as fuel, or both the reeds and wheat. Barley has also been identified in small quantities on floors near storage bins both by itself and with wheat husks, in unit 3858, Building 5, suggested as remains of barley grain storage in one bin and alternating mixed storage in another. But Rosen also suggests barley was entering the site primarily as a weed grass in dung and dung fuel from animal fodder due to its association with stem and leaf phytoliths and wild grass husks in Building 1, and the lack of correlation with wheat in Building 5 (Rosen 2005).

Rosen notes concentrations of phytoliths from husks and floral parts of grasses are a possible indicator of seasonality, as grasses flower in spring, and thus the presence of husks indicates collection and use in spring, or from dung from animals grazing in spring. However the association of these concentrations with either dung or human use is not clear. The analysis of samples from bulk units mixes several deposits containing these husks and floral parts and blur any seasonal signal. A larger sample set is needed to investigate questions on longer timescales, such as seasonality and changing resource use between the early and late levels of the site, which, like other macrobotanical analyses such as pollen and macrofossils, requires a systematic and high resolution sequence of samples. Although comparisons are made between phytolith and plant macro data, for example a comparison between wheat phytoliths and macrobotanical remains in unit 5317, South Area Space 181, midden sequence, the lack of high precision contextual information makes this data difficult to interpret, particularly considering the low numbers of some phytolith types. For example, although wheat husks were found to be most numerous in Space 181, Unit 5317, than in most other locations studied, the numbers per gram for wheat husks (15942 n/gm) are still smaller than, or equal to, bilobes (17536 n/gm), Setaria type husks (15942 n/gm), barley husks (38261 n/gm), and sedges (15942 n/gm) for example, and much smaller than the majority of common single cells such as hairs, long and dentritic stems and wild grass husks. The macrobotanical data refers only to cereal grain (being almost 50% of the remains recovered from the unit) rather than wheat specifically. The macrobotanical remains are recovered from 30 litre samples (Hastorf 2005), and so it is impossible to say whether the phytolith and macrobotanical remains are actually associated with each other. This means that current inferences about cereal use based on phytolith in middens are difficult to support. More recently phytoliths from Çatalhöyük have been used as environmental indicators. Roberts and Rosen (2009) argue on the basis of the size of cereal multicell phytoliths, that these were grown in a dryland region. This hypothesis is based on comparison with experimental growing of crops in Israel on emmer wheat, showing irrigated cereals typically have husk phytoliths of 100 to 300 conjoined cells, whereas non irrigated cereals have less than 100 (Rosen and Weiner 1994). This is recently supported by further experimental wheat studies in Jordan, though these suggest controlling factors are more complex (Mithen et al 2008, Madella et al

Six samples from the midden deposits at Çatalhöyük have also previously been examined to gain general information about plant use at the neighbourhood level (Rosen 2005). This research concluded that midden contexts have a much richer assemblage than other contexts such as floors, with a greater diversity in the types present (Rosen 2005). This is logical as there are a large number of different activities and deposit types present in the middens, and supports the fact that building floors at Çatalhöyük were kept very clean. Species identified from phytoliths in Jenkins’ field assessment (2005) and Rosen’s report include wheat, barley, Phragmites, Aegilops and Avena as well as wild grasses, the largest concentrations of which are found in midden contexts. In addition Setaria sp. is identified in BACH area samples such as unit 6208 (Jenkins et al. in press) though this is not present in any of the macrobotanical reports. Sedges, however, are said to occur in low numbers in middens despite being commonly used as matting, though there is no clear explanation for this. Other suggested activities include the use of reeds as fuel, roofing or screens based on their large quantity in middens, but this cannot be verified due to a lack of specific contextual information. Rosen notes a general phytolith “noise” due to the spread and mixing of ash around the settlement, and notes that strong peaks in certain samples can be more informative. However this “noise” is not taken into consideration in the analysis of midden samples, contexts likely to have a very large noise from spreading of ash. It is clear from these studies that interpreting phytolith remains can be problematic. The samples from middens in Rosen’s study analysed bulk samples from excavation units, which combine a number of different micro units. Whilst this approach is 53

these really do represent single “seasonal” deposits or if they occur in mixed deposits throughout the sequences.

2009). An analysis of wheat phytoliths at Çatalhöyük shows them to typically have less than 100 conjoined cells (Rosen and Roberts 2009). This contradicts earlier field observations of “abundant” large wheat and barley husks that are said to support the hypothesis that cereals were grown on alluvium in marshlands. (Rosen 1998). There is no explanation in any subsequent work for this complete change in observations.

By looking at these results in conjunction with the corresponding micromorphology slides, we can examine the precise depositional context of the phytoliths, and thus infer the depositional agencies and post depositional taphonomy, and how the findings from the phytolith investigations relate to this, in order to develop a more complete understanding of the use and discard patterns of plant materials. The plant component is an important midden component in determining the deposit and activity type, as plants were used at the site for a wide range of activities, including food, fuel, stabilisers in plasters and mudbrick, matting, basketry, and animal fodder (Fairbain et al 2002, Matthews 2005, Rosen 2005).

The comparison with archaeological data has a major flaw in that it does not consider taphonomic processes that affect phytolith size, or different methods of processing modern and archaeological phytolith remains that also affect the size of aggregated phytoliths. Recent experiments on modern phytolith material show that processing methods have an impact on multicell sizes, with dry ashing producing a greater number of multi cells than acid extraction in Triticum durum (Jenkins 2009). This implies that taphonomic and laboratory processes will also have an impact on multicell phytolith size.

Phytolith terminology Unlike microfossils such as pollen, until recently there has been no systematic or established protocol for the description of phytolith types. The terms used in this research are based on previous archaeological studies in the Near East and at Çatalhöyük in particular. Recently at the International Meeting on Phytolith Research (Bruxelles, August 2000), the International Code for Phytolith Nomenclature (ICPN) was proposed, and has produced a code for the naming of phytolith morphotypes, and published in 2005 (Madella et al. 2006). Table 5.1 gives the names of the different phytolith types identified in this study and their corresponding ICPN descriptions. The ICPN terminology was not followed when analysing samples in this study, as phytolith analysis began before the code was published.

Advantages of the integrated approach The analytical approach in this research of using thin section micromorphology in combination with complementary phytolith and chemical analysis of specific layers allows comparison of the phytolith assemblage with high precision analysis of the context in thin section, which will allow taphonomic problems to be better understood. The aim of the phytolith analysis in this research is to provide detailed information on the phytolith assemblages in, as close as possible, individual depositional events within middens, rather than the arbitrary sampling used in previous studies, to better understand midden formation processes. Phytoliths have also been analysed from specific features in middens, including coprolites, as a potential indicator of diet, and the sequence of ashes in the South Area, as a possible indicator of fuel type and the nature of activities represented by deposits from a large scale repeated activity within midden areas. Phytoliths are important as they represent the non charred portion of fuel remains which have not previously been considered. However, unless these are studied in context with associated materials, they are difficult to interpret. Middens are seen to contain abundant ash deposits which could help further the understanding of fuel use for different activities. As discussed previously, coprolites are an important indictor of diet, as they provide a single event that is directly related to what an individual has been eating. Along with biomolecular analysis of organic residues presented in Chapter 7 to identify species, this research will examine whether these can give any dietary information for animals and humans.

Hypotheses related to phytolith analysis of middens As outlined in Chapter 1, phytolith analysis is carried out in this research to help characterise individual fine layers as well as to test a number of hypotheses. By examining phytoliths in thin section alongside phytolith extracted from specific layers in the sections examined, it is hypothesised that multicell size is affected by taphonomic processes of burning, dumping and mixing. This is tested by comparing in situ decay deposits (identified in thin section) with extracted samples to observe differences in conjoined forms. By examining frequencies of cereal phytoliths from a large number of individual depositional events, this research will test the hypothesis that cereals were either a major part of the diet at Çatalhöyük, as suggested by Fairbairn et al 2005, or that they were only a minor contribution, as suggested by Atalay and Hastorf (2006), and Roberts and Rosen (2009). By examining phytoliths from coprolites and dung, identified to species by GCMS, phytoliths can contribute to understanding diet on short term timescales. And finally, by reducing the taphonomic problems and comparing phytoliths with associated material, phytoliths can contribute to the understanding of plant and fuel use at Çatalhöyük.

Individual layers of middens may represent discard from seasonal activities, compared to contexts such as floors and storage bins, which present difficulties from re-use and storage, as well as possible contamination during excavation. In thin section it has been possible to observe husk phytoliths in context, which will help determine if 54

Table 5.1: Common phytolith names used in this research and the official ICPN terminology (ICPN terms Madella et al. 2005). Common term

ICPN term

Schematic drawing key

Dedritic long cell

Elongate dendriform/dendritic

a

Smooth long cell

Elongate rectangle

b

Trichome

Unciform hair cell

c

Rondel

Rondel

d

Bilobe

Bilobate short cell

e

Saddle

Saddle

f

Keystone bulliform

Cuneiform bulliform cell

g

Bulliform

Parallepipedal bulliform cell

h

Crenate

Globular echinate

i

Rugulose spheroid

Globular granulate

j

Trachied

Cylindric sulcate trachied

k

phytoliths extracted (for example diatoms are sometime present), and can also give a false impression of the numbers recovered by multiplying figures up considerably. However the analyses were started out using this method as it had previously been used at Çatalhöyük, and so was used for all samples for consistency.

Methods Methods for extracting and quantifying phytoliths were described in detail in Chapter 3. In brief this involved carbonate removal with 10% HCl, clay removal by settling, organic removal in a muffle furnace at 500C, and non biogenic mineral separation by centrifuging with heavy density solution calibrated to the specific gravity of phytoliths, accepted as 2.3 sg in the literature (Piperno 2000). Phytoliths were counted across the slides and the quantities of different types and species were recorded in detail on a tally recording sheet (see Appendix for an example of the recording sheet used). The results from these recording sheets were then entered into an Excel spreadsheet, where percentage weights of total phytoliths per sample, and of individual types, were calculated and displayed graphically. This methodology is the same as that used on previous Çatalhöyük samples by Rosen (UCL), based on Albert and Weiner (2001) which compare phytolith assemblages based on numbers of different phytolith types per gram of sample, and which have previously been used with Çatalhöyük samples (Rosen 2005). Details of the calculations used can be found in Chapter 3 section 3.8. The number per gram method is not ideal as it does not take into account imperfect mineral separation which affects the weight of

Results Before presentation of results by Area and Midden, a summary is given of all the different phytolith types and corresponding plant types that were identified during the course of this study, in order that the reader has some familiarity with the species and significance of each phytolith type, and to avoid repetition during discussion of the results. Results relating to the assemblages in the high resolution sequence samples are presented by excavation area, and within areas, divided between middens from the earliest to the latest deposits. A summary of the samples analysed can be seen in Table 5.2. Diagrams showing the location of where phytolith samples were taken from micromorphology blocks are given in the Appendix. General trends in each midden are then described.

55

likely hackberry phytoliths from the seeds and fruit of Celtis (Gobetz and Bozarth 2001; Wallis 2003). This is supported by the presence of abundant hackberry pericarps in this sample, which are discussed in Chapter 6 section 6.3.3.2.

The data are presented by showing variations in the total percentage of phytoliths per weight of samples, followed by information on the different phytolith types identified and the variations in the number of each individual phytolith type per gram of sample. Phytolith assemblages from specific features including the coprolites that were analysed by GC-MS (discussed in Chapter 7), and the large scale ash deposits discussed in the spectroscopy chapter, are presented after the midden sequences.

A small number of rugulose spheroid phytoliths are present, and are likely to be from date palm, Phoenix dactyliferia. Phoenix species occur in dry seasonal forests and swamp habitats, as well as mixed forest, and have previously been identified at Çatalhöyük, suggested as palm leaf basketry (Rosen 2005). Tracheids are present in a large number of taxa, including Cyperus (Kealhofer and Piperno 1998; Thorn 2004) and are produced in the xylem tissue of vascular plants. These are present occasionally in the samples studied in this research.

Major Phytolith types identified in midden deposits The photographs in Figure 5.1 show the major single-cell and multi-cell phytolith types identified, as well as some of the less common types that are only found in certain units. The species/family and plant parts that these phytoliths represent, as well as their relative frequencies and variability in the samples studied, are given in Table 5.3. The frequency and variability summaries in this table are visual estimates after counting all of the slides. Phytolith identifications are based on a number of published references (Twiss 1969; Mulholland and Rapp 1992; Pearsall and Dinan 1992; Rosen 1992; Bowdery, Hart et al. 2001; Lu and Liu 2003; Piperno 2006), as well as through comparison with reference material prepared by the author using plant material obtained from the University of Reading Plant Sciences collections in consultation with botanist Dr Keith-Lucas. As expected considering taphonomic issues such as variability in phytolith production between species, monocotyledons are represented to a much greater extent than dicotyledons.

Multi cell phytoliths identified Multi cell phytoliths are also referred to as “silica skeletons”, and are impressions of larger sections of plant tissue rather than individual cells, and so can be identified to genus or species in some cases. Multi cell phytoliths in these samples were largely in the form of leaf and stem tissues from grasses and sedges. Larger types included multiple smooth long cells, occasionally with bulliforms and smaller short cells attached. A large number of these tissues have been identified as Phragmites through comparison with reference material, and discussions with Dr Arlene Rosen (UCL) and Dr Emma Jenkins (University of Reading). Phragmites leaves and stems are characterised by abundant stomata, with the stems having almost husk-like waves similar to the Setaria wave, but are distinguishable at high magnifications due to the waveform, the lack of papillae, and the presence of stomata. The most abundant multi cell form was Phragmites leaf and stem cells, followed by sedges.

Single cell phytoliths identified The most abundant single cell phytoliths were found to be smooth long cells, which are found in the leaves and stems of all grasses, followed by bulliform cells, which are large cells from the epidermis of grass leaves, with abundant vacuoles (see Table 5.3). Also abundant were keystone bulliform cells, a characteristic type of bulliform cell with a distinct shape that is found in Phragmites and Oryza (rice) leaves (Houyuan et al 2002, Harvey and Fuller 2002) and rondel short cells. In this study keystone bulliforms are assumed to be from Phragmites rather than Oryza as rice was not present in this region. Dendritic long cells indicative of flowering parts of grasses were present in more variable quantities. The floral:stem ratio was used here to indicate relative proportions of floral and non floral inputs, which are hypothesised to vary seasonally.

Table 5.5 gives a summary of common species referred to in Near Eastern archaeological literature. A variety of wild grass husks were present, identifiable due to the characteristic “wavy” morphology and papillae. These are distinguishable from cereal husks as the papillae and wave pattern of the husks are unique to each species. Previous research has fully characterised these wave patterns in archaeologically important cereal species such as wheat (Triticum), barley (Hordeum), and rye (Secale) (Rosen 1992). Cereal husks were largely absent from the samples analysed. Of all the cereals previously found at Çatalhöyük through floatation and phytolith analyses (Faribairn et al 2002, Rosen 2006) only Triticum (wheat) was seen in these samples, and in very small quantities.

Rondels are a type of short cell that are found in the leaves and stems of Pooid grasses. In Panicoid and Arundonoid grasses these short cells take the form of bilobate and saddle shaped cells. Bilobe and polylobate phytoliths were noticeably less abundant in the samples analysed, whereas rondels were very abundant, with a lesser number of saddles. One sample, 1542, contained a number of polygonal single cells with a unique surface texture. After examining reference material these have been identified as Ulmaceae verrucate spheroids, most

Although this would seem to refute previous phytolith research which identifies wheat and barley in a number of samples, when considering the relatively small numbers per gram in Rosen’s study and the difference in sampling strategy used in this research, it is likely that concentrations in the individual deposits sampled in this research were simply too low to register. In Rosen’s study much larger bulk units were analysed, which may 56

though it is generally rare that they form a significant part of the assemblage. In cases where there is a larger proportion of variable to consistent forms, this is argued to indicate a wood source for the deposit (Albert, BarYosef et al. 2003).

have mixed several individual units and thus given a high “cereal” signal. This highlights the importance of examining specific contexts of phytoliths, and suggests further work needs to be done to understand the scarcity of cereal phytoliths in middens compared to plant macrobotanical data.

Phytolith assemblages of high resolution sequences in middens

8

7

In order to study sequences of phytolith deposits and to compare them to their depositional context, phytolith samples were analysed as chronological sequences from individual thin section blocks. In the diagrams for each area and midden, each graph corresponds to an individual thin section block (i.e. microstratigraphic sequence), with varying numbers of sub samples between each of the blocks depending on the number of fine layers present. These individual micro layers are composed of often very different material, for example some are composed entirely of ash, whereas others may be composed of charred material or burnt/unburnt aggregates. Each block itself is a sampled sequence from within one midden. Data is presented with multiple blocks from the same midden in order of the stratigraphic sequence.

Weight percent

6

5

4

3

2

1

0 1668 upper 1

1668 upper 2

1668 upper 3

1668/02

1668/03

1668/07

Sub sample number

Figure 5.1: Weight percent phytoliths per gram of sediment for block 1668 sequence, Midden 1.

A number of multi cell husks have been classified as “unidentified”, as they were too fragmented to identify as either cereals or non cereal types (for example the papillae may have been absent). When developing the methodology it was considered unnecessary to try and classify or identify individual wild grass husks beyond family, as it was expected that these would be low in numbers and present as general weeds, and identification would be difficult without a large reference collection. However, wild grass species appear to be quite abundant. Attempts have been made to try and classify the types present in these samples through comparison with reference materials. There are some similarities between the sample husks and references of Agropyron and Aegilops. None of the wild grasses appeared similar to Bromus. This result is similar to Rosen’s data, which shows high concentrations of wild grass husks in bulk midden samples. The difference between wild grasses and cereals is very interesting, and has not been considered previously as these are not well preserved in the macrobotanical record. This is discussed further in Chapter 8.

South Area Samples from the South Area include some of the earliest samples studied, including a sequence of samples from Midden 1 which was excavated in 1996 (Space 115, Unit 1668), and samples collected in 2006 from Midden 2 (Space 261, Units 12524 and 12519). A number of coprolite samples were also examined from this area; the results for these are discussed separately. Figure 5.2 shows the variations in the percentage weight of phytoliths per gram of sediment for the sequence from micromorphology block 1668 from Midden 1. The percentage weight of total phytoliths per gram of sample was calculated by dividing the weight of phytoliths extracted by the weight of the original sub sample, and indicates the overall contribution of phytoliths to the deposit type. These data indicate significant differences in the concentrations and abundance of phytoliths between deposits. It is worth noting that the deposit type affects the weight percent depending on the weight of other components in the sample.

Amorphous single cell phytoliths from dicotyledonous species

The sequence from 1668, Midden 1, is dominated by vast numbers of grass phytoliths for both the multi cell and single cell phytoliths. The single cell phytoliths from this sequence are dominated by long smooth cells, forming between 30 and 45% of each assemblage, though the sequence also contains a relatively high number of dendritic phytoliths (Figure 5.2). In 1668/07 these are more frequent than smooth long cells. The saddles observed in subsample 1668/01 are likely to be from Phragmites as this is the only species present that produces this morphology, although it should be noted that statistics showed no correlation between the occurrence of multi cell Phragmites and saddles. The multi cells are also dominated by general leaf/stem

Phytoliths occur in woody trees and other dicotyledons, but in these plants they form irregular shapes and are difficult or impossible to distinguish between species. Amorphous types in this study have all been classified under one category, as insufficient references are currently available to distinguish different types. Amorphous phytoliths are not diagnostic of species, but are identified as occurring in tree bark and leaves, which in itself can be used to distinguish a wood or grass source for deposits such as fuel ash. The large amorphous phytoliths in these samples have occluded brown material and occur with varying frequency between the samples. They are present to an extent in the majority of samples,

57

Table 5.3: Summary of phytolith types encountered and their relative frequencies. Phytolith type

Species/subfa mily

Plant part

Overall frequenc y in samples studied

phytoliths, with a smaller number of Phragmites and sedge multi cells than in some other sequences (Figure 5.3). The proportion of each type remains similar, suggesting repeated inputs of leaves and stems of reeds and grasses

Variabilit y of frequenc y between samples

100%

Single cells

90%

Smooth long cell Dendritic long cell Bulliform Keystone bulliform Saddle (short cell) Rondel (short cell) Bilobe (short cell) Crenate (short cell) Smooth spheroid Rugulose spheroid Polygonal/t extured Trichome/h air

Hair (with base)

Tracheid (scalariform )

Amorphous

Monocot/grass (all) Monocot/grass (all) Monocot/grass (all) Phragmites and Oryza Monocot/grass (Arundoinoidea e) Monocot/grass (Pooaceae) Monocot/grass (Paniceae) Monocot/grass

Leaf/st em Floral/ husk Leaf

●●●●

Low

●●●

High

●●●●

Low

Leaf

●●●

Low

Leaf/st em

●●

Medium

Leaf/st em Leaf/st em Leaf/st em

●●●●

Low

●

High

●●

High

●●

High

Leaf/fr uit

●●

High

Leaf/fr uit Hair cells of leaf and stem Hair cells of leaf and stem Elongat ed cells in the xylem of vascula r plants Wood/ bark

●

High

●●●

Medium

●●●

Medium

Husk

●●● (cereals ●) ●● ●●●

High

80% 70%

50% 40% 30% 20% 10% 0% 1668/02

1668/03

1668/07

1668 upper 1

1668 upper 2

1668 upper 3

Sub sample number

Figure 5.2: Percentage contribution of each phytolith type to the overall phytolith assemblage in block 1668, Midden 1 (single cells). 100%

Palmae (Phoenix dactylifera) Celtis (hackberry) Present in a large number of taxa Present in a large number of taxa Present in a large number of taxa

Dicot/tree

80%

Cereal /wild grass

Stacked bulliform Cyperaceae Phragmites leaf Phragmites stem Wild grass husk Unident. husk Leaf/stem

60%

40%

●●

20%

0% 1668/02

●

1668/03

1668/07

1668 upper 1

1668 upper 2

1668 upper 3

Sub sample number

High

Figures 5.20: Percentage contribution of each phytolith type to the overall phytolith assemblage in block 1668 Midden 1 (multi cells).

South area summary of assemblage 1668/07 from the Midden 1 sub samples has a particularly distinctive assemblage, with a large percentage of dendritic long cells and multi cell husks. In addition there is a complete absence of amorphous dicotyledonous phytoliths. In contrast, 1668 U1 shows a much larger dicotyledonous input. 1668 U1 contains largely smooth long cells (from stems) and bulliforms (from leaves), with a large proportion of multi cell types suggesting less disturbance.

Multi cells Wave/husk

Dicots. Rondels Crenates Bulliform Trichomes Hairs Long (dendritic) Long (smooth)

60%

Cyperaceae Wave/papill Phragmites Stem ae communis Multi Phragmites Leaf ●●● papillae communis Stacked Phragmites Stem/le ●●● bulliforms communis af Smooth Monocot/grass Stem/le ●●●● multi cells af Long cells Monocot/grass Stem ●● with hairs ●●●● Very common ●●● Common ●● Uncommon ● Rare

High Medium Medium

There are a relatively high proportion of dicotyledonous types in this sample, but the overall weight percentage for the sample is low at around 4%. The dominance of leaf and stems along with the dicotyledonous types and macroscopic observations of charcoal flecks suggest a classification of type 1/5 – fuel burning with some mixed material. 1668 U2 seems to be dominated by Phragmites and stem cells, suggesting a reed rich deposit. 1668 U3 is a mix of stems, husks, sedge and dicotyledonous types.

Medium Medium Medium

58

Table 5.2: Summary of phytolith samples analysed and associated thin section blocks. Midden Number 1 1 2 2 2 6 5 3 7 7 7 7

Site area

Field unit

South South South South South South 4040 4040 4040 North TP TP TP TP

1668 4477 1542 12519 12504 12524 13103 7931 S3 11017 1494 S2 8932 8932 8932 7867

Number of block samples 1 1 1 S7 S5 S3 S3

Year collected

Context

1996 1999 1996 2006 2006 2006 2006 2004 2004

Midden block Coprolite Coprolite Coprolite Coprolite Ash sequence

2004 2004 2004 2004

Midden block Midden block Coprolite Midden block Midden block Midden block Midden block

Number of phytolith sub samples per block 6 1 1 2 1 12 4 5 10 1 11 3 13 6

Table 5.5: A list of common Gramineae/Poaceae from archaeological literature and some important characteristics. Common name

Typical phytolith types

Scientific name

Sub family

Ecology and distribution

Physiological group

Phragmites communis

Arundinoideae

Fresh to brackish wetlands from temperature to tropical, large colonies

C3

Tall saddles, keystone bulliforms, abundant stomata

Common reed

Arundo donax

Arundinoideae

Fresh to brackish wetlands from temperature to tropical, large colonies

C3

Bilobes

Cereals Barley

Hordeum vulgare

Pooideae

Temperate

C3

Wheat

Triticum spp.

Pooideae

Temperate

C3

Millet

Setaria italica

Panicoideae

Tropical and warm temperate

C4

Rondels, distinct husks Rondels, distinct husks Bilobes

Sorghum

Sorghum

Panicoideae

Arid tolerance, warm and dry, tropical to sub tropical

C4

Bilobes, cross

Maize

Zea mays

Panicoideae

Arid tolerance, warm and dry

C4

Cross

Aegilops Agropyron

Pooideae Pooideae

Temperate to cool

C3

Rondels Rondels

Bromus

Pooideae

Temperate

C3

Rondels

Scirpus Carex Cyperus

Cyperaceae Cyperaceae Cyperaceae

Marshy, wet

C3 C3 C3

Reeds Common reed

Wild grasses Goat grass Crested-wheat grass/ desert wheatgrass Brome grass Sedges Bulrush True sedge Sedge

Data from Drum 1968, Ollendorf et al. 1988, Lux et al. 2002, Lu et al. 2009, Harvey and Fuller 2005, Rosen and Weiner 1994, Schellenberg 1908, Rosen 1992, Mulholland and Rapp 1992, Piperno 1984, Twiss 1969, Twiss 199

59

60

Figure 5.3: Microscope photographs of the major phytolith types present in the samples. Starting top left and reading downwards: 1. Rugulose spheroid 2. Keystone bulliform 3. Smooth long cell 4. Crenate 5. Trichome 6. Rondel (tower type) 7. Amorphous phytoliths from wood 8. Smooth long cell, bulliform and dendritic long cell 9. Wild grass husk 10. Saddle 11. Phragmites leaf 12. Reference of Setaria italica showing hairs/trichomes and bilobes 13. Cyperaceae multi cell 14. Celtis type. 15. Conjoined wheat husk

61

Figure 5.4: Extracted Phragmites multi cell phytolith. Midden 7, 8932 S7 /05 (observed in thin section as yellowish amorphous fine fabric with ashy grey areas).

Figure 5.8: Extracted husk phytolith and dendritic long cells from coprolite sample 12519 S7, South Area Midden 2.

Figure 5.9: Extracted grass and reed stem cells from ash layer 12524 S15, South Area Midden 2.

Figure 5.5: Extracted sedge multi cell, Midden 7, 8932 S7/ 08 (sub sample observed in thin section as mixed charred plants and

Figure 5.10: Organic material with articulated stem cells. Midden 2, 12558 S2.

Figure 5.6: Phragmites and grass leaf/stem cells, Midden 7, 8932 S7/08 (observed in thin section as mixed charred plants)

Figure 5.11: Husk phytolith in mixed deposit. Midden 7, 8932 S7. Figure 5.7: Phragmites stem, Midden 7, 8932 S7/11 (observed in thin section as containing large bone and charcoal fragments, underneath ashy layer).

62

Figure 5.12: Articulated stem with hair cells in phytolith/charcoal layer. Midden 2, 12558 S2.

Figure 5.16: 13103 S29 Phragmites stem showing bulliforms and wave

Figure 5.13: Phragmites multi cell within ash deposit. Midden 2, 12558 S2.

Figure 5.17: Wheat husks from in situ decay sample 12519 S9

Figure 5.14: Phragmites stacked bulliforms in partially mixed ashy/organic layer, Midden 7, 8932 S9.

Figure 5.18: In situ decay of plants in 13193 S26, showing long cells and rondels

Figure 5.15: 8932 S7 partially charred reeds and grasses

Figure 5.19: In situ decay of reeds in 13103 S26 showing stacked bulliforms

63

Table 5.4: Number of phytoliths per gram (n/gm) for 1668 samples, Midden 1.

1668/02 is husk and dendritic rich, type 2, which is suggested as a possible seasonal indictor – at the macroscale this sample is seen to be ash. 1668/03 is a mix of sedge, leaves and dicotyledonous types, whilst 1668/07 is similar to 1668/02 in that there are many husks and dendritic long cells, both of these are observed to be ash layers with charcoal fleks.

Sample number Phytolith type (single cell)

Long cell smooth Long cell sinuate Long cell dendritic Papillae Hairs Trichomes Bulliform Keystone bulliform Crenates Bilobes Rondels Saddles Cones Rugulose spheroid Smooth spheroid Trachied scalloped Phytolith type (multi cell) Leaf/ stem joined long cells Unidentifie d husks Wheat husks Barley husks Aegilops Avena husks Setaria husks Wild grass husk Cyperaceae Phragmites stem Phragmites leaf General awn Panicoid Stacked buliform Verrucate Polyhedral

1668 / 01

1668 / 03

1668 / 07

1668 Upper 1

1668 upper 2

1668 upper 3

8574

2235 8

3041

7611

30959

20800

0

0

0

0

0

0

5276

4268

4268

2669

18877

8045

0 513 366 440

0 916 0 2382

133 187 240 587

0 0 99 2372

0 755 0 8684

0 981 589 5887

147

183

53

198

378

392

440 0 2638 73 0

1466 0 6414 0 0

0 0 1254 0 0

494 0 4250 0 0

755 0 23408 0 0

1177 0 16287 0 0

0

0

0

0

378

0

0

0

0

0

0

0

147 0

550 0

0 0

0 297

758 0

0 0

1668 / 01

1668 / 03

1668 / 07

1668 Upper 1

1668 upper 2

1668 upper 3

7695

7147

774

3163

13592

6868

953

550

1280

99

755

981

0

0

0

0

0

0

0

0

0

0

0

0

0

0

0

0

0

0

0

0

0

0

0

0

0

0

0

0

0

0

73

0

0

0

0

0

916

147 73

0

99

1133

589

107

99

755

196

187

0

755

0

0

0

0

0

0

0

0

392

550

27

890

755

0

367

0 0

0 0

0 0

0 0

Phytolith type (variable morpholog y)

1668 / 01

1668 / 03

1668 / 07

1668 Upper 1

1668 upper 2

1668 upper 3

dicot

73

1833

0

2570

755

1962

In thin section, a sample from the South Area, Unit 12519, was observed to contain highly silcified cereal husks. The phytoliths from this deposit are discussed in more detail in the overview section. 4040 Area One detailed sequence was studied from the 4040 area, from Midden 3 (unit 11017). Although initial field interpretations suggested this as a midden deposit, micromorphology suggests that this is a homogenous redeposited unit (Chapter 4 section 4.7.2.3), perhaps packing material. The weight percentage shows that these samples contain a large proportion of phytolith material (Figure 5.5), which is consistent with the ashy nature observed in the field and in thin section; however individual phytolith types were difficult to distinguish in thin section (Chapter 4 Table 4.8). This illustrates the importance of using extracted phytolith analysis in conjunction with thin section micromorphology to obtain an accurate picture of deposit components. The weight percentage of phytoliths in 11017, Midden 3, varies from 10-15% to over 60% (Figure 5.6 and 5.7). The numbers of phytoliths per gram in the 11017 sequence seems to be fairly homogenous across the unit, with a dominance of grass phytoliths. Dendritic phytoliths are consistent across this unit also, suggesting there is no seasonal signal in this sequence of deposits, or that the whole sequence represents deposition at the same time of the year. This would be consistent with the suggestion from the micromorphology studies (Chapter 4, section 4.7.2.3) that this is a homogenous, redeposited material. The variability between the sub samples also shows the importance of microsampling in non distinct phytolith deposits in middens. 4040 area summary of assemblages In summary the phytoliths from 11017, Midden 3, show a dominance of assemblage types 5 and 6 i.e. mixed homogenous material. Overall percentage weights are variable (Figure 5.9), with those showing lower weight percentages having larger aggregate components. The most interesting finding from the 4040 area assemblages is the presence of relatively large amounts of C4 types (Figure 5.18), and the presence of wheat (Figure 5.14 and 5.15), albeit in small quantities. Unfortunately the mixed redeposited nature of this material makes interpretation difficult.

64

TP Area

60

Samples from the TP area come from Midden 7 (Space 100, Units 8932 and 7867). 8932 is the most extensively sampled unit for phytolith sequences, with four high resolution sequences from four micromorphology blocks. The overall number of phytoliths per gram varies quite significantly, with some units containing very few phytoliths such as 8932 S7/09, and others showing a high abundance such as 8932 S3/07(Figure 5.8). These data shows the largest variations in assemblage between different individual depositional events in the midden.

50

Weight percent

40

30

20

10

0 11017/01

11017/02

11017/03

11017/04

11017/05

11017/06

11017/07

11017/08

11017/09

11017/10

Figure 5.21: Graph showing the weight percent of phytoliths from the 11017 sequence, Midden 3. 100%

80% Dicots Rondels Crenates Bulliforms Trichomes Hairs Long (dendritic) Long (smooth)

60%

40%

20%

11 01 7s 1/ 01 11 01 7s 1/ 02 11 01 7s 1/ 03 11 01 7s 1/ 04 11 01 7s 1/ 05 11 01 7s 1/ 06 11 01 7s 1/ 07 11 01 7s 1/ 08 11 01 7s 1/ 09 11 01 7s 1/ 10

0%

Sub sample number

Figure 5.22: Percentage of each phytolith type of the total assemblage for the 11017 sequence, Midden 3 (single cells). 100%

80% Stacked bulliform Cyperaceae Phragmites leaf Phragmites stem Wild grass husk Wheat husk Unident. husk Leaf/Stem

60%

40%

20%

11 01 7s 1/ 01 11 01 7s 1/ 02 11 01 7s 1/ 03 11 01 7s 1/ 04 11 01 7s 1/ 05 11 01 7s 1/ 06 11 01 7s 1/ 07 11 01 7s 1/ 08 11 01 7s 1/ 09 11 01 7s 1/ 10

0%

Sub sample number

Figure 5.23: Percentage of each phytolith type of the total assemblage for the 11017 sequence, Midden 3 (multi cells). 50

Weight percent

40

30

20

10

8932s3/13

8932s3/12

8932s3/11

8932s3/09

8932s3/08

8932s3/07

8932s3/06

8932s3/05

8932s3/04

8932s3/03

8932s3/02

8932s3/01

8932 S7/12

8932 S7/11

8932 S7/10

8932 S7/09

8932 S7/08

8932 S7/07

8932 S7/06

8932 S7/05

8932 S7/03

8932 S7/02

8932 S7/01

0

Figure 5.24: Weight percentage of phytoliths in the 8932 sequence, Midden 7 (2 thin section blocks).

65

The Midden 7 samples have a noticeably high percentage weight of phytoliths per gram of sediment (Figure 5.8), with sample 8932 S3/07 having over 50% of the weight composed of phytolith material. This is seen in thin section to be highly mixed, and individual phytoliths are hard to distinguish (Chapter 4 Table 4.15). As in the earlier middens (South area, Space 115, Midden 1, Unit 1668) the assemblages are dominated by the leaves and stems of grasses. 8932 S7 (towards the base of the TP Midden 7) is noticeably lacking in dendritic long cells (Figure 5.20), with very small numbers of wild grass husks.

Table 5.6: Phytolith numbers per gram for the 11017 sequence, Midden

Sample number Phytolith type (single cell)

11017 1

11017 2

11017 3

11017 4

11017 5

11017 6

11017 7

11017 8

11017 9

11017 10

Long cell smooth Long cell dendritic Papillae Hairs Trichomes Bulliform Keystone bulliform Crenates Bilobes Rondels Saddles Rugulose spheroid Smooth spheroid Trachied jigsaw

8408 3562 0 117 876 1051 117 525 0 4262 0 0 234 0 0

23509 7895 0 1404 526 4561 1930 351 0 12105 175 0 0 0 0

1293 303 0 13 79 515 330 26 0 369 13 0 0 0 40

48579 22152 0 2720 777 8161 2720 1555 0 20597 0 0 0 0 0

29389 12263 0 211 634 2326 846 211 0 11629 211 0 0 0 0

9221 2468 0 325 130 1818 325 130 0 2143 0 0 0 0 0

2136 773 0 147 37 221 74 74 0 810 0 0 0 0 37

7329 2527 0 0 51 404 303 101 0 1719 0 0 0 0 0

178384 52180 0 6067 2427 15775 0 4854 0 185665 1213 0 0 0 0

30146 9737 0 936 374 2434 374 936 0 16852 562 0 0 0 0

Phytolith type (multi cell)

11017 1

11017 2

11017 3

11017 4

11017 5

11017 6

11017 7

11017 8

11017 9

11017 10

4846

5764

646

33811

15012

2078

1105

4954

74023

11609

525 0 0 0 0 0 117 0 584 409 0 234 0

251 0 0 0 0 0 125 0 251 251 0 125 0

92 0 0 0 0 0 53 40 172 53 0 158 0

3886 389 0 0 0 0 2332 389 12048 3109 0 2332 0

3172 211 0 0 0 0 1057 634 634 846 0 423 0

455 0 0 0 0 0 0 0 130 130 0 130 0

331 0 0 0 0 0 0 0 37 37 0 0 0

607 0 0 0 0 0 0 51 354 303 0 0 0

6067 0 0 0 0 0 0 1213 2427 2427 0 0 0

1685 0 0 0 0 0 0 0 374 936 0 374 0

11017 1

11017 2

11017 3

11017 4

11017 5

11017 6

11017 7

11017 8

11017 9

11017 10

7018

409

10493

4229

909

589

859

8494

1311

Leaf/ stem joined long cells Unidentified husks Wheat husks Barley husks Aegilops Avena husks Setaria husks Wild grass husk Cyperaceae Phragmites stem Phragmites leaf General awn Stacked buliform Verrucate Phytolith type (variable morphology) dicot

170

66

GC-MS indicated only the presence of cholesterol, 5βstigmastanol and sitosterol, with no coprostanol or cholestanol (see Chapter 7, Table 7.5). Interpretation of this sample is unclear, a suggestion is that this is non coprolitic organic material.

20 18 16

Weight percent

14

Figure 5.25: Microscope photograph of phytoliths from sample 13103 S24, Midden 6.

12 10 8 6 4

Phytoliths from Coprolites

2 0

Coprolites have been identified through GC-MS analysis (Chapter 7), which has been further supported by observation in thin section (Chapter 4). Analysis of phytoliths from within the coprolites has the potential to give information on diet. Samples examined for phytolith content include three coprolites from the 4040 midden sampled in 2006 (unit 13103, Midden 6), two samples from the South area midden sampled in 2006 (Units 12504 and 12519, Midden 2), and two samples from earlier contexts, including the hackberry rich samples 1542 and 4477.

4477

1542

12504s16

12519s9

13103s21

13103s33

13103s34

Figure 5.26: Graph showing the weight percent phytoliths per gram of sediment for coprolite samples.

The coprolite samples contain a smaller percentage of phytoliths per weight of sample than other samples analysed, ranging from 2% to just fewer than 20% (Figure 5.10), compared to some of the midden sub samples such as 8932 S3 which are greater than 50%. These figures are likely to be slightly higher than the actual phytolith content, as all of the coprolites contained a large amount of non-biogenic mineral material even after heavy density separation, which increases the n/gm. This is illustrated in the Figure 5.9. Dendritic long cells and a multi cell leaf/stem fragments can be seen amongst the large amount of non-biogenic mineral material. This problem was encountered in all the coprolite samples, but is rarely seen in non-coprolite samples. This is unexpected in human diet, and it is unclear if this is from ingestion or a result of coprolite mineralization, though it is more likely to be the latter.

Figure 5.27: Stacked chart showing the relative percentages that each phytolith type contributes to the overall assemblage in coprolite samples (single cells). 100%

80%

Stacked bulliform Cyperaceae Phragmites leaf Phragmites stem Wild grass husk Unident. husk Leaf/stem

60%

40%

Despite relatively low absolute counts, a wide range of phytolith types are observed in the coprolite samples, including a variety of short cell types as well as long cells and trachieds (Figures 5.24 and 5.25, Table 5.8). Dicotyledonous types are present only in small quantities, except in 12504 S16 where they comprise a large percentage of the total phytolith assemblage (seen in Figure 5.11). This sample shows possible phosphate peaks in the FT-IR (see Chapter 6, section 6.3.1.1), but

20%

0% 1542

4477

13103 s21

13103 s33

13103 s34

12504 s16

12519 s9

Figure 5.28: Stacked chart showing the relative percentages that each phytolith type contributes to the overall assemblage in coprolite samples (multi cells).

67

Table 5.7: Numbers of phytolith per gram for the coprolite samples. Sample number (coprolites) Phytolith type (single cell) 4477

1542

12504 s16

12519 s9

13103 S21

13103 S33

13103 s34

84195 163073 0 0 886 886 886 0 0 40768 0 0 0 0 0 0

98182 22091 0 3682 4909 23318 0 8591 0 67500 0 0 0 0 2455 0

44114 43402 0 0 0 0 0 1067 0 13163 0 0 0 0 0 0

55512 113997 0 0 496 496 0 0 0 30730 1983 0 0 0 0 2478

25696 1960 0 1307 218 436 0 653 0 7404 218 0 0 1089 0 0

421350 244655 0 22653 27184 45306 31715 40776 4531 729434 9061 0 18123 67960 9061 4531

380672 93372 0 10774 10774 10774 10774 7182 0 736206 25139 0 10774 14365 0 0

4477

1542

12504 s16

12519 s9

13103 S21

13103 S33

13103 s34

Leaf/ stem joined long cells Unidentified husks Wheat husks Barley husks Aegilops Avena husks Setaria husks Wild grass husk Cyperaceae Phragmites stem Phragmites leaf General awn Panicoid Stacked buliform Verrucate

2216 1773 0 0 0 0 0 222 0 0 0 0 0 222 0

68727 6136 0 0 0 0 0 0 0 3682 7364 0 0 0 0

1423 0 0 0 0 0 0 0 0 0 0 0 0 0 0

28747 2974 0 0 0 0 0 1487 0 496 0 0 0 0 0

30486 0 0 0 0 0 0 0 0 436 0 0 0 0 0

366982 0 0 0 0 0 0 0 0 13592 0 0 0 4531 0

183154 0 0 0 0 0 0 0 0 0 3591 0 0 3591 0

Phytolith type (variable morphology)

4477

1542

12504 s16

12519 s9

13103 S21

13103 S33

13103 s34

Dicot. plates Hackberry polygon

2659 0

4909 95727

7471 0

0 0

13066 0

45306 0

7182 0

Long cell smooth Long cell dendritic Papillae Hairs Trichomes Bulliform Keystone bulliform Crenates Bilobes Rondels Saddles Cones Rugulose spheroid Smooth spheroid Trachied Jigsaw

Phytolith type (multi cell)

68

Table 5.8: Numbers of phytolith per gram for the ash samples. Phytolith Sample number (ash sequence) type (single cell) 12524 s15

12524 s16

1252 4 S17

12524 S18

12524 S19

Long cell smooth Long cell dendritic Papillae Hairs Trichomes Bulliform Keystone bulliform Crenates Bilobes Rondels

19895

66394

21972

44114

791

5242

5039 9 1989

4120

43402

0 395 2899 791 791

0 437 1310 5242 3058

0 1326 332 3316 332

0 549 2884 2060 0

0 0 0 0 0

0 0 9618

0 874 59842

275 0 6180

1067 0 13163

Saddles Cones Rugulose spheroid Smooth spheroid Trachied Jigsaw Phytolith type (multi cell) Leaf/ stem joined long cells Unidentifie d husks Wheat husks Barley husks Aegilops Avena husks Setaria husks Wild grass husk Cyperaceae Phragmites stem Phragmites leaf General awn Panicoid Stacked buliform Verrucate

395 0 0

13978 0 0

0 0 2088 9 995 0 995

1648 0 0

0 0 0

791

0

995

0

0

0 0 12524 s15

0 0 12524 s16

0 0 12524 S18

0 0 12524 S19

22531

28392

1326 0 1252 4 S17 3083 6

32949

1423

132

1310

0

824

0

0

0

0

0

0

0

0

0

0

0

0 0

0 0

0 0

0 0

0 0

0

0

0

0

0

132

437

0

275

0

395 659

1310 874

663 3979

1236 824

0 0

264

1310

2984

1099

0

0

0

0

0

0

0 132

0 2184

0 0

0 137

0 0

0

0

0

0

0

12524 s15

12524 s16

1252 4 S17

12524 S18

12524 S19

922

1747

6963

0

7471

Phytolith type (variable morpholog y) Dicot. plates

Phytoliths from repeated burning and ash layers The mineralogy of deposits in this sequence of samples is analysed by FT-IR and discussed in Chapter 6 (section 6.3.3.7 Sequence 12524, Midden 2). The sequence includes samples from the two large ash layers (samples 12524 S15 and S18) as well as the mixed charred material and charcoal layers between the ashes (samples 12524 S16, 17 and 19). Phytoliths have been recovered from the ash deposits as well as the burnt deposits immediately underlying the ash layers. Previous phytolith work at Çatalhöyük has only been able to suggest the origins of the phytolith inputs, for example the use of Phragmites as a fuel (Rosen 2005). The present work however can confirm the context of these ash deposits as fuel, as well as describing the phytolith assemblage. Both the ash layers have similar proportions of phytoliths at just over 20%. The charcoal layer contains just over 10% of the total weight as phytoliths, and the dark brown/burnt layers vary with one containing just over 10 % and the other over 45% of phytoliths by weight. This is illustrated in Figure 5.13. Total numbers per gram are shown in Table 5.8. The multicells show a leaf/stem assemblage in the ash as well as Phragmites leaf/stems and sedges. The darker layers have amorphous dicotyledonous types consistent with macroscale observations showing the presence of wood charcoal.

Figure 5.29: Graph showing the weight percent phytoliths per gram of sediment for the ash sequence (Midden 2, Unit 12524). A photograph of this ash sequence can be seen in Chapter 6, Figure 6.45.

Table 5.8: Numbers of phytoliths per gram for the ash sequence (12524, Midden 2).

69

a perfect negative correlation and 1.0 being a perfect positive correlation.

100%

80%

Dicot Saddle Rondel Bilobe Crenate Keystone Bulliform Trichomes Hairs Long (dendritic) Long (smooth)

60%

40%

20%

0% 12524 s15

12524 s16

12524 s17

12524 s18

12524 s19

Figure 5.30: Graph showing the relative percentage of each phytolith type in the burning/ash sequence (Midden 2, Unit 12524) from the South Area (single cells). 100%

90%

80%

70%

60%

Cyperaceae Phrgmites leaf Phragmites stem Wild grass husk Unident. husk Leaf/stem

50%

40%

Table 5.9: Correlations between selected phytolith data sets. Data sets Pearsons r Explanation compared (3.dp) (phytoliths n/gm) Keystone / saddle 0.468 Slight positive correlation Saddle / Phragmites -0.097 Slight negative correlation stem Phragmites Stem / Strong positive 0.924 Phragmites leaf correlation Phragmites leaf / -0.002 Slight negative correlation stacked bulliform Phragmites stem / 0.180 Slight positive correlation stacked bulliform Saddle / Phragmites -0.068 Slight negative correlation leaf Keystone / -0.066 Slight negative correlation Phragmites leaf Dendritic / total 0.154 Slight positive correlation husks Dendritic / unident. 0.148 Slight positive correlation husks Dendritic / wild 0.170 Slight positive correlation grass husk Wild grass husks / Strong positive 0.902 unident. husks correlation

30%

The results shown in Table 5.9 suggest a very strong correlation between Phragmites stem and Phragmites leaf multi cell phytoliths, suggesting that these occur as whole plants in the samples studied. Relationships between other potential reed phytoliths are less convincing. There is a slight correlation between stems and stacked bulliforms and keystones to saddles. These would be expected to co-occur in Phragmites. The negative correlations are all very small, to the extent that they can be interpreted as being no linear relationship between the data sets. There is also a strong positive correlation between wild grass husks and unidentified husks, suggesting that the unidentified husks may come from wild grasses.

20%

10%

0% 1

2

3

4

5

Figure 5.31: Graph showing the relative percentage of each phytolith type in the burning/ash sequence (Midden 2, Unit 12524) from the South Area (multi cells).

Discussion The assemblage based approach As can be seen in Table 5.3 a large proportion of phytolith types are not distinguishable beyond genus. Some phytolith types such as smooth long cells are produced by a number of different genera. This is a problem with phytolith analysis in general, and the approach here therefore is largely assemblage based rather than species based (Powers-Jones 1994). Although some forms are produced by many species, the proportions of the morphotypes vary, and the plant part can be just as important as the species.

Classification of phytolith assemblage types Phytolith assemblages have been classified into categories based on the dominant phytolith types present , and possible activities that would be expected to produce these deposit types are discussed. Discussion of the relationship between the phytolith signature and the depositional context as observed in thin section, are discussed further in Chapter 4. These detailed assemblages of individual layers will enhance previous phytolith investigations at Çatalhöyük by providing high resolution sequences that can be directly related to specific activities.

Descriptive statistics on the entire phytolith assemblages (sequences from units 1668, 11017, 8932 and 13103) analysed in this research have shown a relationship between certain phytolith types. The data were analysed to examine the relationship between Phragmites multi cell phytoliths and single cell phytoliths which potentially come from Phragmites such as saddles and keystone bulliforms. Comparisons have also been made of the relationship between dendritic long cells and husk phytoliths, which are both present in the flowering parts of grasses. The Pearson product moment correlation coefficient, r, was used. This is a dimensionless index that ranges from -1.0 to 1.0 and indicates the extent of a linear relationship between two data sets, with -1.0 being

The research presented here has examined the context of Phragmites reeds and suggests their use as fuel base on largely ashy contexts and mixed disaggregated phytoliths, though potentially also from crafts (matting/bedding) in cases where these phytolith form large articulated layers. The presence of Phragmites with spherulites suggests a dung origin for at least some of the reed inputs to fuel.

70

Phytolith assemblage types are shown in Table 5.10. Based on phytolith analysis alone these classifications are very general, and it is not possible to distinguish between different contexts that may have similar phytolith assemblages, particularly articulated deposits versus disaggregated redeposited types. Whilst this analysis is good for a general overview of plant species, and enables a semi quantitative analysis of the different types of phytoliths present in each deposit, questions of diet, resource use and seasonality can only be considered by contextual analysis. These results therefore are considered in conjunction with micromorphology in Chapter 4.

laminated (Figure 4.3), and represents the in situ dumping of fresh plant material, another is a high temperature burning ash deposit associated with animal dung and burnt clay aggregates. Another example is a mixed redeposited layer (Figure 5.23). In Figure 4.9 and 5.25 the Phragmites multi cells are black from occluded carbon, that is they have been burnt at low temperatures, so remain as charcoal, this is another feature which would be removed during phytolith extraction. This contrasts with high temperature burning, where carbon is removed, leaving just the silica phytoliths (Figure 4.41). Phytoliths embedded in coprolites can be seen in thin section in Figure 5.22, and in Chapter 7, Figures 7.18 – 7.21. This contrasts with the appearance of phytoliths extracted from coprolites (Figure 5.20), which appears the same as phytoliths extracted from other contexts. These have very different implications for interpretation, and this is a key example which illustrates the importance of integrating contextual analysis with analysis of the phytolith assemblage.

Table 5.10: Phytolith assemblage types and possible associated activities. Assemblage type Possible activities Dicot dominant

Wood burning/ wood decay

Rich in dendritic long cells and husks

Floral plant parts – seasonal indicator?

Rich in multi cell Phragmites

Reed deposit – fuel, basketry, matting/bedding?

Dominated by general leaf and stem cells

Leaves and stems of grasses fuel, basketry, matting/bedding?

Random mix of types

Mixed plant deposit – redeposited? Mixed contexts?

Few multi cells

Homogenised deposit– redeposited? Mixed contexts?

Comparison with contextual observations in thin section It is argued here that in deposits such as middens, the analysis of the phytolith context and articulation is essential in interpreting the phytolith assemblage. Phytolith analysis alone cannot inform on the use of the plant, the original size of the multi cell fragments (due to disaggregation during extraction), associated components, or the extent of burning. All of these factors are essential to the interpretation of a deposit. Results obtained during this research have shown that samples which have similar phytolith assemblages often have a very different appearance in thin section, for example laminated large multi cellular fragments versus ash samples, burnt at different temperatures. Examples include sample 8932 S7 from Midden 7, TP Area, and 12558 S2 from Midden 2, South Area.

Variations in phytolith types The ratio of long smooth cells to long dendritic cells has been proposed as a potential indicator of season, as the dendritic cells are found in the flowering parts of plants (Rosen 2005). There are issues concerning storage, of cereal husks for example that may obscure such a seasonal signal. It is argued here however that the lack of cereal remains observed in the multi cell phytolith assemblage could indicate that these deposits do not relate to cereal discard, and so the floral dendritic cells come from a plant that would not be stored, such as weeds, and so could indeed be a seasonal indicator. A similar proportion of smooth to dendritic long cells is observed in the entire set of sub samples from 1668 S12 (Midden 1), apart from sample 1668/07 which has a greater number of dendritic long cells (Figure 5.27). Rosen (2005) notes that a large number of the husks in Midden 1 come from wild grasses, and that these are a possible indicator of seasonality, as grass flowers in the spring, and thus infers that a large number of inflorescences are from a spring deposit, or from dung derived from spring grazing animals. However Rosen’s work only examines six bulk phytolith samples from middens, and with a small sample set it would be difficult to look for any seasonal pattern in the occurrence of these dendritic phytolith types. This contrasts with the present study which examines 75 sub samples as well as examining the context through micromorphology to investigate the source of the phytoliths in a deposit.

The Figures below shows the appearance of the phytoliths in thin section (see also Chapter 4, Figures 4.3 – 4.9) also how they appear in extracted phytolith slides (Figure 5.16 to 5.21, see also Figure 5.1). It can be seen that whilst the depositional context of these plant remains is quite different, for example mixed, ashy, coprolite, animal dung, after extraction, the phytolith assemblage appears very similar, and little can be said apart from that they are dominated by reeds and grasses. The micromorphology shows that one deposit is highly

The sequence from 1668 S12, Midden 1, shows variable ratios of dendritic:smooth long cells between the sub samples (Figure 5.27) which suggests that individual deposits could be linked to seasonal deposits. Comparison with sequences from other middens suggests that dendritic forms are only found in some deposits rather than in all midden deposits. There may be some

71

link with activity, but whether this is strictly seasonal is still unclear.

18000 16000

Discussion of results from the South Area

Long cells (dendritic) Unident. husks Wild grass husks

14000

n/gm

12000

This ratio is a general indicator of the source of the major phytolith inputs to a deposit, as it is hypothesised that a greater number of multi cell phytoliths would come from the discard of the entire plant, rather than plant material from cooking/food waste, as these remains would be largely disaggregated (Rosen 2005). Figure 5.29 shows this ratio for the samples from 1668 S12, Midden 1. The ratio is largely similar for all the sub samples except 1668/02 which has an increased ratio, showing more multi cells to single cells than the other sub samples. This suggests a non mixed deposit with more articulated plant material.

10000 8000 6000 4000 2000 0 1668/02

1668/03

1668/07

1668 upper 1

1668 upper 2

1668 upper 3

Sub sample number

Figure 5.33: Comparing the n/gm of dendritic and husk phytoliths from 1668 S12, Midden 1. 0.500

0.450

0.400

Multi cell:single cell ratio

0.350

1.40

1.20

0.300

0.250

0.200

0.150 1.00 Ratio floral/stem

0.100

0.80

0.050

0.000 0.60

1668/02

1668/03

1668/07

1668 upper 1

1668 upper 2

1668 upper 3

Sub sample number

Figure 5.34: Graph comparing the mutli cell : single cell ratio for the phytoliths from the 1668 samples, Midden 1.

0.40

0.20

0.00 1668/02

1668/03

1668/07

1668 upper 1

1668 upper 2

0.160

1668 upper 3

Sub sample number 0.140

Figure 5.32: Graph showing the floral:stem ratio for phytoliths from 1668 S12, Midden 1. Variable : consistent ratio

0.120

Variable to consistent ratio The variable to consistent ratio compares proportions of phytoliths from dicotyledonous species (producing consistent phytolith forms) and monocotyledonous species (producing amorphous or variable forms). This ratio was used to examine the relative proportions of woody inputs versus grass inputs. Due to the relatively low production of phytoliths in dicotyledonous plants, an increase in this phytolith type is significant and indicates a large input of wood, compared to the grass phytoliths, which if present in low numbers could be interpreted as a background signal. Figure 5.30 shows this ratio for the samples from unit 1668, Midden 1. This ratio is very variable, with 1668 upper 1 showing a much higher proportion of variable forms, suggesting perhaps a largely wood source for this plant material, though in deposits such as this, analysis of wood charcoal is more useful in determining activity as it is possible to identify this to species.

0.100

0.080

0.060

0.040

0.020

0.000 1668/02

1668/03

1668/07

1668 upper 1

1668 upper 2

1668 upper 3

Sub sample number

Figure 5.35: Graph showing the variable: consistent ratio for phytoliths from the 1668 samples, Midden 1.

Discussion of results from the 4040 Area Variations in phytolith types Although the overall numbers of phytoliths are variable in the 11017 sequence (Midden 3), with sample 11017s1/09 containing noticeably more smooth long cells than other samples (Figure 5.31), the ratio of floral: stem types is relatively consistent (Figure 5.32). Unit 11017 is one of the few sample sets studied that had any evidence of cereal phytoliths, unfortunately these were not visible in the thin section that these phytolith relate to, and so the context of the cereal phytolith could not be observed. The homogeneity of these deposits in thin section suggests redeposited material and so it is not possible to assess the

72

origin of these phytoliths. Figure 5.33 compares unidentified husks with wheat husks and grass husks – there does not appear to be a relationship between these forms.

50000

Long cells (dendritic) Unident. husk Wheat husks Wild grass husks

n/gm

40000

The multi-cell to single cell ratio however varies between these sub samples, with 11017s1/02 having a lower ratio (Figure 5.35). Thin section analysis shows this unit to contain largely charred plant material (Chapter 4 Table 4.8), though it is largely disturbed by modern root action. The variable to consistent ratio is also very variable, with samples 11017s1/01, 09 and 10 having low ratios (Figure 5.35). Again this is difficult to interpret, however, due to the highly disturbed and mixed nature of these layers. An interesting observation in these samples is the relatively high proportion of C4 type phytoliths, largely saddle type short cells. This is shown in Figure 5.37.

30000

20000

10000

Sub sample number

Figure 5.38: Graph comparing the numbers per gram of dendritic long cells and husks for the 11017 sequence, Midden 3.

Discussion of results from the TP Area Variations in phytolith types The ratio of floral to stem cells is highly variable in these sequences from Midden 7 (Figure 5.38). In some samples such as 8932S3/2, 8932S3/3, 8932S38, 8932S3/9 and 8932S7/5 and 8932S7/8, in particular, the ratio of dendritic to smooth is low, and 8932S3/9 also has overall large numbers of phytoliths per gram of dendritic types. This could possibly indicate a seasonal deposit. The context of these is very variable, ranging from ashy (8932S3/2), charred (8932S3/3) to amorphous yellow organics (8932S3/8 and 8932S7/05) and aggregate rich (8932S3/9) (Chapter 4 Table 4.13 and 4.15). The amorphous yellow organics are identified as coprolites in thin section through the presence of pseudomorphic voids and bone fragments, and due to their distinct context are much more useful as a potential seasonal indicator, compared to samples such as 8932S3/9 which are highly disturbed by root action (Chapter 4 Table 4.13), and again illustrates the importance of micromorphology in these deposits, otherwise the context is unclear.

180000

Long cells (smooth) Long cells (dendritic)

160000 140000

n/gm

120000 100000 80000 60000 40000 20000

11017s1/10

11017s1/09

11017s1/08

11017s1/07

11017s1/06

11017s1/05

11017s1/04

11017s1/03

11017s1/02

11017s1/01

0

Sub sample number

Figure 5.36: Graph comparing the numbers per gram of dendritic long cells and smooth long cells for the 11017 sequence, Midden 3. 0.500

0.450

0.400

Floral:stem ratio

0.350

0.300 4000

0.250

0.200

3500

0.150

3000

0.100 2500

n/gm

0.050 2000

0.000 11017s1/01

11017s1/02

11017s1/03

11017s1/04

11017s1/05

11017s1/06

11017s1/07

11017s1/08

11017s1/09

11017s1/

Sub sample number

Figure 5.37: Graph comparing the ratio of floral: stem phytoliths for the 11017 sequence, Midden 3.

1500

1000

500

0 11017s1/04

11017s1/05 Sub sample number

Unidentified husks

Wheat husks

Wild grass husks

Figure 5.39: Graph comparing the numbers of phytoliths per gram of different husk types in the two samples from 11017 containing wheat husks.

73

11017s1/10

11017s1/09

11017s1/08

11017s1/07

11017s1/06

11017s1/05

11017s1/04

11017s1/03

11017s1/02

11017s1/01

0

100000

0.600

Long cells (dendritic) Unident. husks Wild grass husks

90000 0.500

80000

Multi cell:single cell ratio

70000 0.400

60000 50000

0.300

40000 0.200

30000 20000

0.100

8932 S7/12

8932 S7/11

8932 S7/10

Figure 5.40: Graph comparing the multi cell: single cell ratio for the 11017 sequence, Midden 3.

8932 S7/09

0

11017s1/10

8932 S7/08

11017s1/09

8932 S7/05

11017s1/08

8932 S7/03

11017s1/07

8932 S7/02

11017s1/06

Sub sample number

8932 S7/01

11017s1/05

8932 S5/02

11017s1/04

8932 s3/09

11017s1/03

8932 s3/08

11017s1/02

8932 s3/03

11017s1/01

8932 s3/02

0.000

8932 s3/01

n/gm

10000

Figure 5.43: Graph comparing the n/gm of dendritic long cells and husk phytoliths for 8932 sequences, Midden 7

0.160

0.700 0.140

0.600

0.500

0.100

Ratio floral:stem

Variable:consistent ratio

0.120

0.080

0.060

0.400

0.300

0.040

0.200 0.020

0.100 0.000 11017s1/01

11017s1/02

11017s1/03

11017s1/04

11017s1/05

11017s1/06

11017s1/07

11017s1/08

11017s1/09

11017s1/10

0.000

Sub sample number

8932 s3/01

Figure 5.41: Graph comparing the variable: consistent ratio for the 11017 sequence, Midden 3.

8932 s3/02

8932 s3/03

8932 s3/08

8932 s3/09

8932 S5/02

8932 S7/01

8932 S7/02

8932 S7/03

8932 S7/05

8932 S7/08

8932 S7/09

8932 S7/10

8932 S7/11

Sub sample number

Figure 5.44: Graph showing the floral: stem ratio for phytoliths from the 8932 sequences, Midden 7.

20000

Variations in phytolith types

n/gm

15000

C3 C4

10000

5000

0 11017 s1/01 11017 s1/02 11017 s1/03 11017 s1/04 11017 s1/05 11017 s1/06 11017 s1/07 11017 s1/08 11017 s1/09 11017 s1/10 Sub sample number

Figure 5.42: Comparison of C3 and C4 phytolith types from the 11017 sequence, Midden 3.

Discussion of phytoliths from coprolites A notable feature of the phytolith assemblages from coprolites is the general low quantities of phytoliths compared to the number found in midden assemblages, and the low quantity of multi cell forms in particular. This would be expected due to disaggregation of the multi cell forms in the gut, though it could also be that the plants being consumed did not produce large multi cell phytoliths. This is an example of the importance of micro context in the interpretation of phytolith assemblages. The phytoliths from coprolites are typically poorly preserved, probably due to decomposition in the gut.

Of potential importance is the presence of a relatively high number of bilobe and saddle phytoliths in the coprolite samples from the 4040 area Midden 6, unit 13103 (shown along with other short cell types in Figure 5.40). These phytolith types are largely absent from the majority of samples, and their presence in all of the coprolites analysed from Midden 6 could indicate a localised consumption of C4 plants. Previous phytolith work at Çatalhöyük by Rosen (2005) has also noted that bilobes are relatively rare at Çatalhöyük. Rosen interprets these bilobes as the remains of decayed baskets used to store and/or cook grains. The presence of bilobes within coprolites suggests that these may also derive from food plants. The floral to stem ratio is also variable (Figure 5.44), though the low counts make this difficult to interpret. All coprolite samples except 12504 S16 have a low variable to consistent ratio (Figure 5.45) 12519 S9 has zero variable forms. 1542 shows a large number of polygonal type phytoliths (highlighted in yellow in Figure 5.11) which resemble hackberry phytoliths, which is consistent with the macrosopic observation of this sample containing hackberry pericarps. This highlights the usefulness of phytoliths when they occur in distinct deposits rather than from bulk samples.

74

8932 S7/12

2.50

700000 Bilobes Rondels Saddles

600000

2.00

Floral/stem ratio

n/gm

500000

400000

300000

1.50

1.00

200000

0.50

100000

0 1542

4477

13103 s21

13103 s33

13103 s34

12504 s16

12519 s9

0.00 1542

Sub sample number

13103 s21

13103 s33

13103 s34

12504 s16

12519 s9

Figure 5.48: Graph showing the floral: stem ratio in the coprolite samples.

450000

0.40

Long (smooth) Long (dendritic)

400000

4477

Sub sample number

Figure 5.45: Chart showing variations in the type of short cells in coprolite samples.

0.35

350000 0.30

Variable:consistent ratio

n/gm

300000 250000 200000 150000

0.25

0.20

0.15

100000

0.10

50000

0.05

0 1542

4477

13103 s21

13103 s33

13103 s34

12504 s16

12519 s9

0.00 1542

4477

13103 s21

13103 s33

13103 s34

12504 s16

12519 s9

Sub sample number

Sub sample number

Figure 5.49: Graph showing the variable: consistent ratio in the coprolite samples.

Figure 5.46: Graph showing variations in the numbers of smooth and dendritic long cells in the coprolite samples. 250000

Dietary implications of coprolite phytolith content

Long cells (dendritic) Unident. husk Wild grass husk

200000

Coprolites have a very high temporal resolution, of perhaps only a few days. Coprolites therefore have the potential to show variations in diet on a shorter timescale. Previous isotope work at Çatalhöyük suggests a C4 plant diet (Richards et al 2003), which contrasts with the assumption that C3 cereals such as wheat were being grown for consumption. The presence of bilobe phytoliths (an indictor of C4 plants) in coprolite sample 13103 S33 supports the stable isotope analyses, though it is unclear which plant types these originate from – although previous phytolith studies indicate the presence of the C4 plant Setaria sp (Jenkins et al in press) which contains bilobes (Lu et al 2009), this species is not seen in the macrobotanical record or discussed in other phytolith reports such as Rosen (2005), although the lab team data records do have records for “Setaria type” and Setaria husks in a number of the samples, such as CH-9826 from Unit 1668 (Midden 1) and CH-00-10 from Unit 1252 (a room fill deposit) (phytolith data available online in the Çatalhöyük database: http://www.catalhoyuk.com/database/catal/Search.asp).

n/gm

150000

100000

50000

0 1542

4477

13103 s21

13103 s33

13103 s34

12504 s16

12519 s9

Sub sample number

Figure 5.47: Variations in the numbers of dendritic long cells and husks in the coprolite samples. 0.70

0.60

Multi cell: single cell ratio

0.50

0.40

0.30

0.20

0.10

Isotope analysis of faunal remains conversely shows a C3 diet. This could indicate that some C3 plants found at the site were used for animal rather than human consumption. The very fragmented nature of the phytoliths suggests a large amount of erosion, both physical through process of eating, and in the gut through digestion. Therefore the interpretations made are speculative, and represent possibilities based on the data available. Further work is

0.00 1542

4477

13103 s21

13103 s33

13103 s34

12504 s16

12519 s9

Sub sample number

Figure 5.48: Variations in the multi cell: single cell ratio in the coprolite samples.

75

suggested on a larger sample set before any firm conclusions can be made.

1.20

1.00

0.80 Floral:stem ratio

Discussion of results from repeated burning and ash layers Variations in phytolith types

0.60

0.40

Comparison of the dendritic long cells and smooth cells in this sequence shows that in all samples from Midden 2 except 12524 S19, there is a dominance of smooth cells over dendritic cells (Figure 5.46). This is illustrated further by looking at the floral to stem ratio (Figure 5.47). Looking at the context of these samples, we can see that 12524 S19 is a mixed charred layer, with evidence of low temperature burning (Chapter 6 section 6.3.3.7). Whilst this sample has a high proportion of dendritic long cells, it has relatively few husks, as indicated in Figure 5.46, and the single-cell to multi-cell ratio shown in Figure 5.47.

0.20

0.00 12524 s15

12524 s17

12524 s18

12524 s19

Sub sample number

Figure 5.51: Graph showing the floral: stem ratio for the ash sequence (12524, Midden 2). Long cells (dendritic) Unident. husk Wild grass husk

40000 35000 30000

n/gm

25000

The charcoal layers have a larger proportion of variable or amorphous phytoliths, which would be expected due to the large wood charcoal content of these layers visible at the macroscale, and no mutli cell phytoliths. The ash layers have a relatively high proportion of very large multi cell phytoliths, suggesting that leaves and stems were added as whole plants to be used as fuel, in addition to wood fuel. 12524 S18 shows no variable forms (Figure 5.50), whereas S17 and 19 have high ratios, suggesting a more significant input from wood sources. This fits with the observation that these are mixed burnt layers with large amounts of wood charcoal. Further work is suggested on phytoliths from distinct ash deposits such as hearths to get a better idea of the phytolith assemblages of fuels for different activities.

20000 15000 10000 5000 0 12524 s15

12524 s16

12524 s17

12524 s18

12524 s19

Sub sample number

Figure 5.52: Graph comparing the numbers per gram of dendritic long cells and husks for ash sequence (12524, Midden 2). 1.00

0.90

0.80

Multi cell:single cell ratio

0.70

Long cells (smooth) Long cells (dendritic

60000

12524 s16

0.60

0.50

0.40

0.30

50000

0.20

0.10

n/gm

40000 0.00 12524 s15

12524 s16

12524 s17

12524 s18

12524 s19

Sub sample number

30000

Figure 5.53: Graph showing the multi cell: single cell ratio for the ash sequence (12524, Midden 2).

20000

0.09

10000 0.08

0 12524 s15

12524 s16

12524 s17

12524 s18

0.07

12524 s1

Sub sample number Variable:consitent ratio

0.06

Figure 5.50: Graph comparing the numbers per gram of dendritic long cells and smooth long cells for ash sequence (12524, Midden 2).

0.05

0.04

0.03

0.02

0.01

0.00 12524 s15

12524 s16

12524 s17

12524 s18

12524 s19

Sub sample number

Figure 5.54: Graph showing the variable: consistent ratio for the ash sequence, Midden 2.

76

comparison with the context in thin section (Chapter 4) that we can begin to understand the phytolith inputs.

General observations from phytolith analysis of middens

The % of phytoliths per gram varies significantly, from less than 1% (e.g. 1668 U2, Midden 1) to greater than 50% of the total weight (8932 S3/07). This variation can be seen within and between different layers in the same midden. Comparison with thin section micromorphology suggests that certain deposit types are much more abundant in phytolith types than others. Interesting 8932 S3/07 (Midden 7, TP Area) corresponds with mixed ashy deposit types, and abundant phytoliths were not as obvious in thin section, This suggests that targeting phytoliths for specific layers after thin section observation, especially as the technique is relatively time consuming and is seen to be useful for some deposit types. In addition the n/gm method of quantification is problematic and is proposed to be only useful when comparing samples from the same deposit types.

Taphonomic considerations These results indicate that extracted phytoliths show similar assemblages in different contexts, and supports the hypothesis that by examining phytoliths in conjunction with thin section micromprohlogy, taphonomic problems of phytolith analysis of middens can be reduced, by giving contextual information of the extracted samples. This has important implications for the interpretation of phytolith assemblages from middens, and also supports the hypothesis that the use of multicell size to infer growing conditions is problematic. Although Phragmites is seen as very large articulated types in thin section, this is only in contexts where they are primary deposits and have decayed in situ. In all other contexts they are mixed and broken up. Extracted phytoliths are all disaggregated to an extent, and none of the very large articulated layers are seen, likely to be a result of extraction methods.

Taphononmy and phytolith size In thin section there is a noticeable difference in the size of phytoliths, with larger multicell types than are seen after extraction. As well as processing methods impacting phytolith size in experimentally grown wheat, as demonstrated by Jenkins (2009), in thin section we can see effects such as trampling and post-depositional processes causing the disaggregation of conjoined phytoliths in archaeological samples. To demonstrate this, the size of conjoined phytoliths in the single wheat deposit from 12519 was measured in thin section and after extraction (using the extraction procedure discussed in chapter 3, and also by preparing a simple smear slide). Phytoliths were seen to be significantly larger in thin section, with over 600 conjoined cells.

Assessment of the phytolith assemblages indicates some general trends across the site for midden deposits, which are much firmer based on 75 samples rather than the six previously analysed. Firstly there is a distinct dominance of phytoliths from stems and leaves, in particular from Phragmites. Cereal multi cells are surprisingly sparse, being found only as small individual fragments in homogenised deposits, and there is little evidence of distinct “cereal” deposits from on-site cereal processing. The dominance of rondels as opposed to bilobe short cells is expected due to the dominance of C3 plants, supported by the macrofossil data. The dominance of pooid grasses (indicated by rondel short cells) rather than panicoid grasses (indicated by bilobe short cells) is expected for the cool and moist general environment at Çatalhöyük (Rosen, Chang et al. 2000), though the presence of a small number of bilobes indicate perhaps a more complex environment with dryer areas preferred by C4 types.

Consideration of phytolith types The low recovery of cereals in this research supports the hypothesis of Atalay and Hastorf (2006), and Roberts and Rosen (2009) rather than Fairbairn (2005), that cereals may have been less important resources at Çatalhöyük, though this research also suggests that taphonomic problems of cereal phytoliths are not very well understood which could be the reason for the apparently conflicting information from phytoliths and macrobotanical data. If these were consumed often, it would be expected to see them more frequently in individual layers in both extracted and thin section samples. However, examination of numbers per gram in all areas indicates a dominance of leaf/stem phytolith cells in the majority of midden phytolith assemblages. This is due to the fact that these parts are common to all plant species, and produce a large number of phytoliths. The most common phytolith types are smooth long cells, dendritic long cells, bulliform, and rondels. The charts illustrating the varying proportions of selected phytoliths between samples show similar patterns for the smooth long cells and bulliforms, with a slightly higher amount of long cells. This is expected as these cells occur together in stems and leaves.

The results also indicate that the phytolith concentrations per gram of the total deposit vary significantly even in deposits which are adjacent to each other. It is suggested that this is a result of each of the deposits being composed of different material and represents a different source material, and supports the hypothesis that phytolith deposits vary between individual fine layers in the middens, and that bulk samples group together a number of different deposits. This supports the suggestion that phytolith analysis of midden deposits by itself does not provide any contextual information, as material is brought together from a number of depositional units. Thus the phytolith signatures that are shown by such bulk analysis only give an estimation of overall phytolith input, with no information on where the phytoliths are from. Even systematic sub sampling of units in the field does not provide any contextual information – it is through

77

single cell phytoliths. The majority of samples tend towards having a greater proportion of single cell types rather than multi cell types, though there are some where the multi cell types are dominant (such as in sequence 12524). This pattern could be due largely to the extraction procedure, which may disaggregate multi cell phytoliths, but also due to redeposition or reworking of the deposits, or because the phytoliths come from plant material which was broken up before or during deposition, for example through burning. A higher proportion of multi cell phytolith indicates material that has decayed in situ. This hypothesis is tested through comparison with micromorphology samples, which shows large articulated multicells only in in situ deposits, and highlights the problem of using multicell size as an environmental indicator.

Figure 4.55: highly silicified wheat husk with c. 120 conjoined cells from 12519

The floral: stem ratio is an indicator of the dominance of either smooth long cells, or dendritic long cells. The dendritic types are present in the flowering parts of cereals and wild grasses, and this ratio represents the dominant plant part (floral or stem) in that deposit. The ratio is variable in the samples studied. Smooth long cells are present throughout all sample sequences, but dendritic cells are much more variable, ranging from being completely absent (for example 8932 S7) to being the dominant over the smooth cells (for example 1668). They are concentrated only in specific deposits rather than being ubiquitous throughout the middens. Contributions to the study of fuel use The presence of Phragmites phytoliths in ash layers suggests these may have been used as fuel, though more comparisons are needed between ash in middens and other primary contexts, such as hearths. These also occur with spherulites and are seen within animal dung, suggesting at least some of the Phragmites phytoliths in ashes are coming from animal dung.

Figure 4.56: 12519 wheat husks in thin section showing layers of husks possibly from crop processing

Some phytolith types occur less frequently and are sparse such as bilobe short cells, some occur less frequently but when they do occur are found in large amounts, for example the polygonal phytoliths from coprolite sample 1542 (highlighted in yellow in Figure 5.24). Grass/leaf phytoliths in the form of smooth long cells and bulliforms are present throughout and in some ways can be considered a “background” representing continuous input, perhaps from a variety of the most commonly occurring daily activities.

Dicot. plates

25000

20000

n/gm

15000

10000

Seasonality

5000

The multi cell comparison also shows a dominance of leaves and stems. The number of husks present seems to be quite variable, being completely absent in a large number of the samples studied. In samples that do have a presence of husk phytoliths, wild grass husks are dominant, with cereal husks being almost entirely absent. Wild husks are perhaps more important than cereals as seasonal indicators as it is unlikely these would be stored, except perhaps as dung burnt as fuel.

89 32 89 S7 32 /01 89 S7 32 /02 89 S7 32 /03 89 S7 32 /06 89 S7 32 /08 89 S7 32 /09 89 S7 32 /10 89 S7 3 /1 16 2 S 1 68 7/ 1 16 up 2 68 pe r 16 up 1 68 pe r up 2 pe 16 r 3 68 16 /02 68 16 /03 78 68/ 67 07 78 S3/ 67 02 78 S3/ 67 06 78 S3/ 67 07 S 89 3/ 32 08 89 s3/ 32 01 89 s3/ 32 02 79 s3/ 31 03 s 11 3/0 01 1 11 7/0 01 1 11 7/0 01 2 11 7/0 01 3 11 7/0 01 4 11 7/0 01 5 11 7/0 01 6 11 7/0 01 7 11 7/0 01 8 11 7/0 01 9 7/ 10

0

Sub sample

Figure 5.57: Graph showing variations in the number of amorphous dicotyledonous phytoliths per gram in all the samples sequences studied.

The variable: consistent ratio is again an indicator of the phytolith source. The variable morphology phytoliths come from dicotyledonous plants e.g. wood, and thus the ratio of variable to consistent can show whether the dominant phytolith input is from monocotyledonous or

The multi cell single cell ratio shows the relationship between larger articulated phytoliths and individual

78

conduct a detailed study of phytoliths from different hearths in buildings to examine differences between hearth samples. If hearth ash samples were characterised this could make it easier to distinguish these ash types in middens. It would also be interesting to compare the ash in the massive ash layers to see if different fuels were being used for different activities.

dicotyledonous species. Figure 5.51 compares the numbers per gram of dicotyledonous phytoliths in all of the sample sequences studied. Conclusions from phytolith analysis Major findings of the phytolith research can be divided into three overall conclusions. The first major finding is that phytoliths can be extracted from coprolites, and that the phytoliths can be linked directly to plant consumption. A particularly interesting result is the presence of bilobe phytoliths in one of the coprolites, which supports previous isotope research at Çatalhöyük showing a C4 plant diet (Richards et al 2003). This has also highlighted discrepancies between macrobotanical data which has found no Setaria and previous phytolith data (Rosen 2005, Jenkins et al in press) which reports Setaria husks, which could either be a result of different taphonomic processes for macrobotanical and phytolith remains, or problems with phytolith husk identification.

Although it was hoped to examine phytoliths from animal and human coprolites as indicators of diet, organic residue analysis of the samples selected showed the majority of samples were human. Those coprolites which were large enough to conduct both GC/MS and phytolith analysis were human. Thus inferences on animal diet can only be made through observations in thin section at present. Further work on phytoliths from a larger sample set of coprolites still has much potential for a short term diet indicator, as well as using these as seasonal indicators. There is also clearly a need for better integration between phytolith and macrobotanical data. These are both important lines of evidence for the use of plant resources, but currently the data is difficult to use together due to differences in sampling methods and different taphonomic processes that act on these assemblages.

A second major advance of the work reported here is the methodological finding indicating the importance of the depositional context in the interpretation of phytolith results from complex deposits like middens. By comparing phytoliths assemblages with thin section observations, it can be seen that similar phytolith assemblages are present in different depositional contexts. Taphonomy must also be more carefully considered in the interpretation of deposits containing very small absolute counts of phytoliths, for example the small number of cereals recovered in this research, and the relatively small numbers reported in previous research (Rosen 2005, Rosen and Roberts 2009). Caution must also be taken in using phytoliths as evidence of dryland cereal agriculture based on their size (Rosen and Roberts 2009), as opposed to wetland (Rosen 1998, 1999). The single wheat deposit observed here suggests that at least some wheat being used at the site was growing under conditions of high water availability, with over 600 conjoined cells being observed in thin section. A further finding is the proportion of phytolith material in the massive ash layers in two middens studied. The high percentage of Phragmites present in these deposits has implications for fuel use – previous research into fuel use at Çatalhöyük has been based largely upon charcoal and plant macro remains (Asouti 2003), which misses inputs from plants which leave no macroscopic or carbonised remains. This is discussed in Chapter 8 alongside evidence for dung fuel inputs. Further work on phytoliths This work has highlighted the necessity of integrating phytoliths with micromprhology when studying complex finely laminated deposits such as middens, however there are further areas of work which have become apparent from this research. Although it has been attempted to address the question of fuel use by looking at phytoliths in ash samples from middens, it would be useful to 79

not micro-analytical chemical techniques could be used to differentiate between these different species and types.

6: SPECTROSCOPY AND SEM-EDX Introduction

As previously discussed in Chapters 1 and 2, a major debate at Çatalhöyük concerns where crops were being grown, as it is argued that the area surrounding the site was unsuitable for cereal growth due to the marshy environment (Rosen and Roberts 2005). However, there is evidence of cereal use at the site in the form of abundant cereal macro remains (Fairbairn 2005) and possible crop processing deposits (Asouti et al. 1999), although these have not been examined contextually.

A number of spectroscopic analyses were carried out on midden deposits to characterise particular components and investigate the mineralogy of individual layers, and to clarify information that may be unclear in thin section, and thus aid in the interpretation of midden formation processes. The techniques used were Fourier Transform Infra Red Spectroscopy (FT-IR), Scanning Electron Microscopy and Energy Dispersive X-ray analysis (SEMEDX) and Synchrotron Radiation Source IR Microscopy (SRS FT-IR Microscopy) at the CCLRC Daresbury Laboratory. SRS Micro X-Ray Diffraction (SRS Micro XRD) was also used for a few selected samples during the experiments at Daresbury.

SEM-EDX was used on phytoliths to examine variations in their trace element composition. It is suggested here that, as plants absorb silica, they may also incorporate other elements during phytolith formation. Studies of phytoliths from plants in tropical peatlands have shown that the elemental composition of the phytoliths vary a) between plant species (deciduous trees having a high concentration of aluminium, whilst grasses, sedges etc are dominated by opaline silica), b) within the plant, and also c) depending on the substrate on which the plants grow, with variations in pH having a significant impact on the ratios of Si to Al (Wüst and Bustin 2003). It is known that plant opal can contain significant quantities of trace elements (Wilding et al. 1989).

As well as the major hypotheses of this research relating to midden formation processes, a number of specific questions were addressed related to the spectroscopic analysis of midden components. These questions and related hypotheses are stated below together with an indication of the experimental strategy used to address the question and a brief summary of the results obtained. As GC-MS is a time consuming and expensive technique, it was reasoned that using a quicker and cheaper technique to give a basic idea of the major minerals present in the samples would be a useful screening technique in selecting samples for organic residue analysis by GC-MS, as well as providing information on the mineralisation of these samples. Before the development of residue analysis, phosphate analysis was the major technique used to suggest the presence of faecal material (Ottaway 1984; Sullivan and Kealhofer 2004; Holliday and Gartner 2007). It has been previously shown that coprolites contain a large amount of phosphorus in the form of phosphate, which is thought to be derived from bone fragments within the coprolites as well as the matrix (Allen et al. 2002). The IR absorption band assigned to phosphate around 1023 cm-1 can be partially masked by quartz peaks in the same region, and the distinctive phosphate peaks around 600 cm-1 are often weak in intensity. SEM-EDX was also tested in order to demonstrate the presence or absence of phosphorus in samples where the FT-IR spectra were ambiguous. This research will test the hypothesis:

Experiments were carried out therefore to determine if the elemental composition between different phytolith types varies significantly, as this may be an indictor of the type of soil or environment in which the plant was growing. Moreover, when compared with data on regional soils this could potentially indicate the area in which different plants were growing. The availability of trace elements is dependent on factors such as soil pH and clay content, and so the range of soils in a geographical area may provide unique markers in plants from that region. These experiments were limited by the highly variable assemblages present in midden samples and the difficulty in finding cereal phytoliths amongst a mixed sample under the SEM. Further work is needed to improve this experiment, which is detailed in the discussion chapter. This research will test the hypotheses: 2. Phytoliths from different plant species have distinctive mineralogies and elemental compositions

1. FT-IR can be used as a screening technique to select coprolite samples for GC-MS analysis

3. The mineralogy or elemental composition of phytoliths can be related to the substrate and therefore region where the crops were grown

The second section reports the results of FT-IR and SEMEDX analysis of phytolith samples. An initial use of FTIR in this study was to investigate the mineralogy of phytoliths, in order to better differentiate between similar phytolith types from different species, for example a number of different taxa produce trachied phytoliths, and dicotyledonous species all produce similar amorphous types (Kealhofer and Piperno 1998, Thorn 2004). The aim of this part of the work was to determine whether or

The third section presents results from the analysis of various other components of interest that were encountered during sub sampling and thin section analysis. These include a sequence of ash samples, sequences of bulk sub-samples from selected thin section blocks, and inclusions such as hackberry pericarps and mineral nodules subsequently identified as gypsum. The mineralogy of ash has been shown to vary with the source material (Canti 2003) and under different preservation

80

Table 6.1: Summary of samples whose spectra are presented. The coprolite samples were also analysed by GC-MS, details are given in Chapter 7.

conditions (Albert and Weiner 2001). FT-IR spectra were recorded for a selection of different ash samples from the Çatalhöyük middens to examine variations in the mineralogy of the ash, in order to identify differences in perseveration of ash minerals between middens of different ages, and ashes of potentially different compositions (as indicated by thin section micromorphology and phytolith analysis).

Sample

Calcite

FT-IR and Micro XRD were also used to identify the white mineral nodules that were visible at the macroscale in the field sections and in a number of the middens from the later levels, in particular the samples from the TP area. These were successfully identified as gypsum nodules, likely to be a result of post depositional formation, though, as previously discussed, the origins of the gypsum are unclear. FT-IR of the hackberry sample extracted from a coprolite showed an aragonite composition of the pericarps, confirming the identity as hackberry (Celtis), which is unusual in its production of the biomineral (Cowan et al. 1997). This is shown to be well preserved in many archaeological contexts due to its mineralogy (Wang et al. 1997). These pericarps were found to contain an orange material. This was also subjected to FT-IR analysis, which indicated large amounts of phosphate inside the hackberry seeds. This research will test the hypotheses:

Quartz Kaolinit e Montm orillonit e

5. FT-IR can be used to detect the temperature at which ceramic material has been heated 6. These methods can be integrated to aid in the understanding of midden formation processes

-

Apatite

-

Triticu m husk

-

1542

1

7867/04

7

8932 S3/09 12524 S13 12524 S14 12504 S16 12519 S7 13103 S24 13103 S34

4. FT-IR and XRD can be used to identify and characterise specific midden components

Midde n numb er

Sample type

Reference material Reference material Reference material Reference material Reference material Reference material Hackberry endocarp Gypsum nodule

FTIR

SEMEDX

XR D

SR SIR

Y

N

N

N

Y

N

N

N

Y

N

N

N

Y

N

N

N

Y

Y

N

N

Y

N

N

N

Y

Y

Y

N

Y

N

Y

N

7

Coprolite

N

Y

N

N

2

Coprolite

Y

N

N

N

2

Coprolite

Y

N

N

N

2

Coprolite

Y

N

N

N

2

Coprolite

Y

N

N

N

6

Coprolite

Y

Y

N

N

6

Coprolite

1668/02

1

1668 U3

1

Grass phytolith Phragmites phytolith

Y Y

Y

N

Y

Y

Y

N

Y

Reference materials Following these results there is a section on SRS-IR Microscopy and SRS-Micro XRD carried out at the CCLRC Daresbury laboratory. The major sample type investigated with these techniques was phytoliths, along with the hackberry and mineral nodule samples. Bulk FTIR is useful for large or homogenous samples, however with microscopic samples such as phytoliths a microscope is needed to distinguish between individual cells in a sample. Following the successful recording of spectra of larger mutlicell types of phytoliths at the University of Reading, a successful application to the CCLRC Daresbury laboratory was made to use the Synchrotron Radiation source IR Microscopy (SRS) to analyse the smaller single cell phytoliths. Unfortunately this work was only partially successful as the magnification of the microscope at Daresbury was not high enough to be able to properly identify the individual cells, which are approximately 30 μm in size. Spectra obtained, however, show some differences between individual cells, and there is a great potential for further work in this area. Micro XRD analysis of hackberry and mineral nodule samples confirmed the results obtained through FT-IR.

FT-IR of reference materials A number of reference spectra were taken of authentic samples of likely components to enable peak identification of the spectra obtained from midden samples. Reference materials selected included quartz, calcite and apatite (calcium phosphate) in the form of bone, as well as two representative clay mineral references – kaolin, a kaolinite clay, and montmorillonite, a smectite clay. These spectra were used in combination with published data on these minerals to interpret the sample spectra (Jamieson 1953, Chester and Elderfield 1968, Farmer 1974, Nakamoto 1986, Budd 1986, Loste et al. 2003, Prabakaran et al. 2005). Calcite and quartz are the dominant minerals in many of the midden deposits studied, alongside some clay minerals. The reference spectra for these minerals show a number of characteristic peaks which can be compared to the spectra of samples from the midden deposits in order to identify the major minerals present. Reference data is presented here in the form of spectra and tables. Sample data is presented in the form of spectra. A summary of

81

further characterised by the presence of a band at 910 cmfrom the Al-Al-OH bending from inner OH groups. The band at 540 cm-1 is a Si-O-Al deformation band, and the smaller peaks at 462 cm-1 and 422 cm-1 are Si-O-Si and Si–O deformation bands respectively.

the techniques used for each sample type is presented in Table 6.1.

1

Calcite, apatite and aragonite The spectrum for calcite and aragonite references are compared to a fossil hackberry pericarp in Figure ?? The carbonate anion from calcite shows strong sharp peaks around 1420 cm-1, from the asymmetric stretch (ν3), and an out of plane (v2) vibration near 875 cm-1. The weaker peaks at 2974 cm-1, 2870 cm-1 and 2510 cm-1 are carbonate overtones and combinations. The peak around 710 cm-1 is the carbonate v4 or in plane bend. These peaks match those expected from published spectra (Farmer 1974).

2-

O

Si

Quartz and opaline silica

O

The spectra for quartz and opaline silica are given in Figures 6.2 and 6.3 respectively, with peak assignments being given in Tables 6.3 and 6.4 respectively. Quartz is characterised by a sharp doublet around 779 and 797 cm-1 and the Si–O stretch around 1070 - 1080 cm-1. This Si–O stretch is also a feature of clay mineral spectra, though its position shifts depending on the number and type (i.e. the crystal structure) of Si–O bonds present. The phytolith reference spectra are characterised by a single band at around 795-797 cm-1 rather than the doublet seen in quartz, indicating amorphous opaline silica rather than the highly crystalline quartz. The band of quartz at 1078 cm-1 has a counterpart in the spectrum of opaline silica, though the shoulder at 1160 cm-1 is less intense. The opaline silica spectrum also has a broad OH absorption band around 3450 cm-1.

O

2-

O

2-

2-

O

2-

3+

4+

2-

O

Al O

2-

O

2-

2-

O

2-

O

Figure 6.1: Tetrahedral SiO44- unit (left) and octahedral AlO69- (right).

Clay minerals The FT-IR spectra of clay minerals are more complicated due to the large range and complex structure of clay minerals, which are variations on the same basic structure of aluminosilicate layers arranged in octahedral and tetrahedral sheets. The Si4+ ion can be substituted by Al3+ and other smaller cations in the tetrahedral sheet, whilst medium sized cations such as Mg2+ can substitute for Al3+ in the octahedral sheet (Figure 6.4). The presence of different ions can have an impact on the FT-IR spectra of the minerals. The three main clay groups are kaolinites, smectities and illities.

Figure 6.2: FT-IR spectra of reference kaolinit and montmorillonite

Two major clay minerals were chosen as reference materials, kaolin and montmorillonite. Kaolin is a kaolinite clay with the chemical composition Al2Si2O5(OH)4. The spectrum for this can be seen in Figure 6.5. It has a basic structure of one tetrahedral sheet linked to one octahedral sheet. Kaolinite has mostly Al in its octohedra, and has four absorptions in the OH region, which have the characteristic shape seen in Figure 6.5, around 3690 cm-1 and 3652 cm-1 (Farmer 2000; Madejova 2003). The 3618 cm-1 OH band is produced by inner OH groups between the tetrahedral and octahedral sheets. Like quartz, clays have a broad, distinct Si–O band. In kaolinite this is around 1020 cm-1 and this clay is

Montmorillonite is a smectite clay with the composition (Na,Ca)0.33(Al,Mg)2Si4O10(OH)2.nH2O, and is generally formed as a weathering products of silicate rocks. The spectrum of this clay can be seen in Figure 6.6. Smectites such as montmorillonite are distinguished by the presence of a single band in the OH region. In montmorillonite, which has a high Al content, this is seen around 3620 cm-1 (Farmer 1974). The 3422 cm-1 band arises from the H - O–H vibration of adsorbed water in smectites. The Si–O stretch in montmorillonite is found at around 1030 cm-1. The 912 cm-1 and 884 cm-1 bands are from Al-AlOH and Al-Mg-OH.

82

MS is a time consuming and expensive technique and it was reasoned that using a quicker and cheaper technique such as IR spectroscopy to give a basic indication of the major minerals present in the samples would be a useful screening technique in selecting samples for further analysis by GC-MS. The spectra shown in Figures 6.8 – 6.13 are representative of typical spectra obtained for all of the coprolite samples. All of the samples yield similar spectra, with peaks corresponding to the Si-O stretching bands of quartz and peaks which may be assigned to the carbonate ion in calcite (highlighted in Figure 6.8). The dominance of calcite and quartz within the sample can be seen by the intensity of the peaks from these minerals in all of the coprolites. In regions where there are peaks from two or more components, for example the region between 1020 – 1070 cm-1 where both quartz and phosphate absorb, the peaks overlap and it is sometimes hard to distinguish between them (this can be seen in Figure 6.8 where overlapping peaks are highlighted in red and green). This problem can be resolved to some degree by looking at peaks from other vibrations in quartz and apatite, e.g. the phosphate bending modes in apatite in the 500 – 600 cm-1 region.

Figure 6.3: Reference spectra of opal and quartz

Phosphate peaks are present in the majority of samples, though the intensities of these peaks are variable. In some samples the presence of phosphate was suggested by a shoulder around 1090 cm-1 overlapping the quartz and clay Si – O peaks around 1020-1030 cm-1, and a weak peak around 930 cm-1 (e.g. sample 12524 S13, Figure 6.10) but these were obscured by the dominance of calcite and quartz. To try to further resolve this problem SEM-EDX analysis was used on selected samples (Table 6.6) to determine the amount of phosphorus present in the samples.

The distinctive OH regions can be used to identify the dominant clay minerals in a mixed sample. The bands around 1030 – 1080 cm-1 are more problematic due to the overlap in this region with quartz and other minerals. When interpreting the spectra of experimental samples, comparisons were made between the peak positions obtained and the reference data. A visual comparison is also made of the overall appearance of the spectrum and the shape of the individual bands with the appropriate reference spectra.

Other regions where significant band overlap may occur is around 470 – 600 cm-1, where peaks from phosphate and quartz occur. In this case it may be possible to distinguish the phosphate peaks by looking at the shapes of the peaks at 1020 cm-1 and 600 cm-1. The presence of both of these peaks would strongly suggest the presence of phosphate. The sample which showed the highest organic residue concentrations by GC-MS, sample 7 from the South Area midden 2006 unit 12519, shows the most intense phosphate peaks (highlighted in Figure 6.13).

SEM-EDX of reference materials A sample of bone analysed by FT-IR was also subjected to SEM-EDX analysis to act as a reference for the identification of bone fragments in midden and coprolite samples (Figure 6.7). For comparison, a bone inclusion was taken from sample 8932 S3/09.

It is perhaps useful to describe this spectrum (Figure 6.13) in some detail as an example and to help in interpreting the other spectra which are given. Calcite is a major component in this sample. The peaks at 2922 cm-1, 2848 cm-1 and 2502 cm-1 represent carbonate overtones and combinations from calcite, 1412 cm-1 is a carbonate stretch, and 872 cm-1 is a carbonate bend (see Figure 6.1 for the reference spectrum of calcite).

Results Analysis of coprolites and other samples which potentially contain organic residues FT-IR of coprolites FT-IR spectra were recorded on a selection of samples which potentially contain organic residues (Figures 6.8 – 6.13). GC-MS is the most unambiguous method to characterise and quantify organic residues. However, GC83

The bands at 3416 cm-1 and 1624 cm-1 are stretching and bending modes of water from moisture in the sample. However, the OH stretch could also be from other OH containing components such as hydroxyapatite or clay minerals. The shape of the OH region suggests the presence of a small quantity of smectite type clay in sample 13103 S24. The sharp doublet at 786/774 cm-1 is assigned to quartz. 686 cm-1 and 466 cm-1 are also quartz peaks. The bands at 1024 cm-1 and 602/562 cm-1 represent the stretching and bending modes of PO43respectively, although these are shifted slightly from the expected positions in the reference material (Farmer 1974). SEM-EDX studies of coprolites Because of the slight ambiguities in the FT-IR spectra due to overlapping peaks (e.g. Figure 6.8), a selection of samples was examined by SEM-EDX to determine the concentration of phosphorus. Three coprolite samples which had been analysed using FT-IR and GC-MS were analysed by SEM-EDX – the findings are summarised in Table 6.2. The major elements are O, Si, Ca and C, from calcite and quartz. P is present but is less abundant. There is also a number of trace elements (Figures 6.14 – 6.16). The % w/w of P is very variable between the 3 samples, ranging from 0.5 % in 8932.2/07 (Figure 6.16) to 5.16% in 13103 S34 (Figure 6.15). The relatively low concentration of P would explain the lack of distinct phosphate peaks in the FT-IR spectra. It is clear that while FT-IR has potential as a screening method for identifying coprolites by means of the presence of phosphate, the results may be ambiguous. Where possible IR studies should be backed up by elemental analysis to determine phosphorus concentrations although, of course, this procedure is time consuming.

Figure 6.4: SEM photograph of keystone bulliform phytolith. South Area, Midden 1, 1668/02.

Figure 6.5: SEM photograph of grass stem cells

Figure 6.7: SEM-EDX for 13103 s24. Table 6.2: Summary of coprolite samples analysed with SEM-EDX. Sample Sample Elements Elements Elements type major intermediate (2- trace (10%) 10%)

Figure 6.6: SEM photograph of Phragmites leaf

84

13101 S34

Coprolite

O, C, Ca

P, K, Si, Fe

Na. Mg, Al

13103 S24

Coprolite

O, Si

P, Fe, Al, Ca, K

Mg

8932 S3/09

Coprolite

O, C, Si

Al, Fe, Ca, K

P, Mg, Na

Analysis of phytoliths

Analysis of other midden components of interest

FT-IR of phytoliths

FT-IR and XRD of mineral nodules identified as gypsum

FT-IR of typical phytolith samples are shown in Figures 6.17 to 6.20. The absorptions at 1097 cm−1 and the weak doublet around 790 cm−1 and at 473 cm−1 indicate opaline silica, the mineral component of plant phytoliths (highlighted in Figure 6.17 and 6.18). The spectrum of opaline silica is broadly similar to that of quartz and other silica polymorphs. The crystalline forms of silica tend to have sharper peaks, with amorphous forms showing broader features. A major distinction between crystalline silica and amorphous or opaline silica is the 790 cm−1 doublet. In crystalline forms of quartz this feature is very distinct as being two closely spaced sharp peaks, whereas in reference opal silica it appears as a single peak (see reference spectrum Figure 6.3).

A number of white nodules were visible at the macroscale in the samples from the TP area were analysed by FT-IR and Micro XRD. A photograph of these nodules in the field can be seen in Chapter 4, Figure 4.44. The FT-IR spectrum (Figure 6.26) identifies these nodules as being gypsum, calcium sulphate CaSO4·2H2O. The FT-IR spectrum of gypsum is distinctive due to the presence of bands arising from the stretching and bending vibrations of the sulphate ion (Farmer 1974). Moreover, the distinctive shape of the OH stretching bands in this spectrum between 3600 and 3240 cm-1 confirms the presence of water of hydration, and identifies the mineral as gypsum, rather than anhydrite, or anhydrous calcium sulphate CaSO4. The sulphate bending modes can be seen at 451 cm-1, 605 cm-1, 673 cm-1, the doublet arising from stretching vibrations 1150/1120 cm-1, the 1010 cm-1 shoulder and the relatively intense combinations at 2232 cm-1 and 2112 cm-1.

In the bulk phytolith samples (shown in Figures 6.19 and 6.20) the 790 cm−1 peak has a slight shoulder, suggesting the presence of small quantities of crystalline silica in addition to the amorphous forms. The peaks in the OH stretching region of this sample at 3622 /3400 cm-1 and the small peaks at 530, 462 and 418 cm-1 (corresponding to Si-O, Si-O-Si and Ai-O-Al respectively) also suggests the presence of smectite type clays. In Figure 5.20 peaks around 874 cm-1 and 1450 cm-1 suggest the presence of calcite.

The sample was also analysed by Micro XRD during the beam time at the Daresbury laboratory. The sample spectrum (shown in blue in Figure 6.28) was matched with the gypsum reference standard (shown in pink). FT-IR and XRD of Hackberry samples

SEM-EDX of phytoliths

Hackberries represent a large component of the macroscopic plant record at Çatalhöyük, often being found in clusters within midden deposits (Figure 6.29). This may be due to the good preservation of the hackberry pericarps, which are unusual in that they are composed of biogenic aragonite, a similar material to that found in mollusc shells (Wang and Amundson 1997). FTIR has shown that the seed remains thought to be hackberry pericarps from Çatalhöyük are indeed composed of aragonite, which confirms the visual identification of these as hackberries (Figure 6.31). The hackberries analysed in this research were found embedded within sample number 1542, a suspected coprolite.

In order to support the FT-IR spectroscopy of phytolith samples and to search for trace elements within the samples, SEM-EDX was carried out on individual phytoliths from a selected sample. These are listed in Table 6.3. Phytolith types analysed by SEM-EDX include grass long cells (Figure 6.22 and 6.24) and Phragmites long cells (Figure 6.23 and 6.25). All of the phytolith samples show silicon and oxygen as major elements along with carbon. Trace elements present include Ca, Mg, and Al. interestingly the grass stem long cells show Mg but no Ca, while the Phragmites stem cells show Ca but no Mg. Table 6.3: Summary of phytolith samples analysed by SEM-EDX. Sample Phytolith type Elements Elements Elements major intermediate trace (>10%) (2-10%) (500ºC suggested by the FT-IR data, as shown by experimental studies investigating the characteristics of plant ash (Boardman and Jones 1990). This gives very strong supporting evidence to the interpretation of this midden deposit type, that these extensive repeated in situ burning and ash layers are the result of large high temperature fires on the midden surfaces, for the firing of pottery and/or clay figurines (the excavation data for this unit indicates that 7 clay figurines were found in this layer). The aggregate material examined is thought to be a fragment of clay material used to cover pots during firing. It would be very interesting to investigate any pottery samples from these layers to look for evidence of firing. To test these results, analysis of clays burned at different temperatures was carried out for comparison. Samples of clay fired at 100°C intervals from 100 to 1200°C were available from Professor John Allen (University of Reading) and Dr Wendy Matthews (University of Reading). FT-IR was carried out on these samples to look for shifts in the IR spectra. The result of this experiment can be seen in Figures 6.38, 6.39 and 6.40. Figure 6.38 shows each full spectrum of the heated clay sample from unfired to 1200°C. A noticeable feature is the changing shape of the OH region between 4000 – 2800 cm-1, which becomes broader and loses the sharp peaks at 3600 cm-1 at around 500°C, corresponding with the loss of non H bonded OH groups. This changing pattern in the spectrum can be seen more clearly in Figure 6.39. Another noticeable change in the spectrum is the shape of the peaks between 1400-400 cm-1, with the unfired clay having a distinctly shaped peak closer to 1030 cm-1, compared to the clay heated at 1200°C, where the peak has shifted towards 1100°C as well as becoming broader. This shift in position and shape occurs around 500°C, and can be seen in Figure 6.40.

Figure 6.13: Repeated burning and ash layers in the South Area

The band due to non H bonded OH is not seen in the aggregate sample, suggesting that heating has occurred. Other peaks in the spectrum are explained by the presence of calcite and quartz. The peak at 1444 cm-1 relates to the carbonate v3 mode of calcite. In the reference spectrum in Figure 6.1 this band is located nearer to 1420 cm-1. The shifting of this peak to 1444 cm1 has been observed in previous studies of fired clay (Shoval 2003) and indicate recarbonated calcite, which would suggest a firing temperature between 600 – 700 °C. The 874 and 710 cm-1 are also calcite bands. When carbonates are heated, CO2 is lost, leaving calcium oxide. On cooling, this reacts with atmospheric CO2 to form recarbonated calcium carbonate:

FT-IR of sub sample sequence from thin section blocks 8932, 11016 and sequence of ashes from unit 12524 It was expected that the sub samples from individual layers within the midden deposits would show changes in mineralogy which may help further characterise the deposit types that are observed in thin section. This was tested by subjecting 3 sequences of sub samples from individual layers within micromorphology blocks to FTIR analysis.

88

sample also appears fairly homogenous and it is suggested to be midden material reused as packing material. There are however some differences in the FTIR spectra of the four sub samples taken across the block (Figure 6.43). The uppermost sample for example shows a distinctly different OH region in the FTIR spectrum compared to the other three samples. The OH region of 11016/02 resembles that of gypsum (the red spectrum in Figure 6.43), whereas the other samples resemble smectite type clays. The sharp intense peaks at 1684, 1620, 670 and 598 cm-1 are also from gypsum, and the relatively intense sulphate overtones and combinations at 2232 and 2112 cm-1 can also be seen. This sample has two unusual features – doublets at 1034 / 1112 cm-1 and 1384 / 1352 cm-1. These peaks are not observed in any other samples. Due to the position of these peaks, and the presence of other calcite, quartz and clay peaks, it is suggested that these peaks represent overlaps from the intense sulphate peaks from gypsum and the carbonate and silicate peaks from calcite, quartz and clay. The presence of a large amount of gypsum in this sequence can also be seen in thin section, where the sequence is quite disturbed by post depositional action of gypsum crystals.

Figure 6.14: FT-IR spectra of the 12524 ash sequence

Midden 7, TP Area, sequence from unit 8932 The OH region of the sub-samples in the 8932 sequence suggests smectite type clay minerals, and the presence of clay is supported by the peaks at around 914 cm-1 and the shape of the peaks between 522 - 400 cm-1 (Figure 6.41). However there were some interesting differences between some of the sub samples. Sample 8932/06 in particular shows the definite presence of phosphate indicated by the double peaks 602 and 560 cm-1, and 8932/01 also shows less intense phosphate peaks (Figure 6.42). Comparing this to the laboratory descriptions of the sub samples, these samples were described as orange base layer/possible coprolite and mixed plaster layer (micromorphology description in Chapter 4, section 4.3.1.4). 8932/06 also shows less intense clay peaks, with calcite and quartz being ore dominant, which would support the suggestion that this is a sample containing coprolitic material. Midden 3, 4040 Area, sequence from unit 11016 The block from 11016 appears at the macroscale to be a fairly homogenous sequence, and it was difficult to distinguish individual layers. Micromorphologically the

89

Figure 6.15: FT-IR spectra of experimentally heated clay

Midden 2, South Area, sequence from unit 12524

and multiple peaks in the 400 – 500 region which suggest a lower heating temperature for this deposit (Figure 6.46).

This sequence is a set of bulk samples that do not correspond to a thin section sample. The layers in the field can be seen in Figure 6.44. These were very large and it was possible to sample each of the individual layers in the field. Samples were taken for thin section analysis but the loose nature of the ash deposits meant that this particular sequence was not suitable for thin section sampling, however a thin section was made of the edge of the ash sequence where the layers were thinner, and a similar sequence in the 4040 area was also sampled. This sequence is a set of five samples of repeated burnt and ash layers.

Discussion and summary Analysis of coprolites Despite being a relatively cheap and inexpensive technique, and notwithstanding its usefulness in identifying a range of materials, FT-IR is still an underused method of analysis in archaeology. Although GCMS is the definitive technique for the identification of archaeological faecal material (Bull et al. 1999, Bull et al. 2002, Bull et al. 2003, Bull et al. 2006), the time and cost of sample preparation and analysis mean that limited sample sets can be analysed. Before the development of residue analysis, phosphate analysis was the major technique used to suggest the presence of faecal material (Ottaway 1984, Sullivan and Kealhofer 2004, Holliday and Gartner 2007), and it has been previously shown by FT-IR that coprolites contain a large amount of phosphorus in the form of phosphate, which is thought to be derived from bone fragments within the coprolites as well as the matrix (Allen et al. 2002).

The spectra for this sequence are shown in Figures 6.45, and again contain a mix of clay, calcite and quartz, though the intensities of the peaks are variable. Sample 15 and 16 for example have very weak clay peaks, with no evidence of clay in the Si – O region, which is dominated by the Si-O peak of quartz at 1038 cm-1. The calcite peaks in these spectra are very intense. Samples 17 – 19 have stronger clay peaks, the OH region of 19 in particular having evidence of smectite type OH groups,

90

whether this matches the elemental profile of archaeological plant material. Although modern forensic studies can trace the origins of products using elemental data, these studies are often used to support isotope analysis, and are based on whole plants rather than phytoliths, where the quantities are large enough to use techniques such as ICP-MS for elemental and isotopic analysis (Watling 1998, Kelly et al. 2005). It remains unclear as to whether all of the elements absorbed from the soil are incorporated into phytoliths, and to what extent. A better understanding is needed of how geochemical and isotopic signatures are transferred to plants.

Samples rich in phosphate typically show bands arising from the stretching and bending modes of the phosphate ion around 1030 and 600/560 cm-1 (Nakamoto 1997). The more intense stretching mode may often overlap with other intense bands such as the stretching mode of the silicate ion (Farmer 1979). So it is the presence of a clear doublet at 600/560 cm-1 that provides the best diagnostic test for phosphate in the IR spectrum. Figure 6.13 shows very clear phosphate peaks whilst others such as Figure 6.8 (sample 13103 S34 ) show more indistinct features, which nonetheless probably result from phosphate. To clarify this, SEM-EDX analysis was carried out to confirm the presence of P. For those samples with weak phosphate peaks such as 13103 S24, the presence of phosphate has been confirmed by the use of SEM-EDX analysis (Figure 6.15). The value of infra red spectroscopy as a screening method is revealed by comparisons with GC-MS results. Although some coprolite samples do not show phosphate peaks, these are also not the best samples to select for organic residue analysis.

In conclusion, this research suggests that FT-IR and SEM-EDX analysis of phytoliths from archaeological contexts is of limited use at present, and that further experimental work is necessary. Therefore the hypothesis that phytoliths have distinct mineralogies and elemental compositions that can be related to the region of growing is not supported by the research conducted here.

These results support the hypothesis that FT-IR can be used as a screening technique to select samples for bimolecular analysis of organic residues. FT-IR is therefore proposed as a quick and cheap method of screening archaeological samples before subjecting them to the more expensive and time consuming method of GC-MS. This will eliminate inorganic samples such as clays and ochre from GC-MS analysis, and will screen those samples which are most likely to have a high concentration of preserved organic residues.

Analysis of hackberries and gypsum nodules FT-IR and micro XRD are shown to be useful in the identification of common midden components, specifically hackberries and gypsum nodules. It was found that, for the sample types where the mineralogy was important, the most useful technique was FT-IR, with SEM-EDX being useful in support. Hackberry samples from within coprolites have been identified as having an aragonite pericarp, which confirms the visual identification of these as Celtis. Material contained within the pericarps shows intense phosphate peaks in the IR spectrum, probably from mineralised organic material contained within the endocarp.

Analysis of phytoliths FT-IR analysis in Figures 6.17 and 6.18 shows opaline silica and Figure 6.19 show a mix of opaline silica and quartz. Elemental analysis in Figures 6.24 and 6.25 show Al and Mg as trace elements in addition to Si, O and C. The presence of Al is not surprising, as it has been previously demonstrated that plants absorb this mineral along with Si , and that the two are often co-precipitated (Hodson and Sangster 1993) . However, the presence of this element in aluminosiliacte clays means that we should be cautious when interpreting data. Although great care has been taken to extract a pure phytolith sample, there may be traces of the substrate left. This being said, a large number of the phytolith samples in this work came from pure plant ash deposits, where there would be little or no clay. There has been no previous work on the elemental analysis of phytoliths from archaeological contexts, though some work has been done on paleoecological samples (Carnelli et al. 2002), where the presence of aluminium, and its relative percentage, are used as a supporting diagnostic tool when distinguishing between woody and non woody taxa. It is interesting to note that the Ca and Mg content appear to vary between samples.

Analysis of micromorphology sub-sample sequences Of the sequences of samples studied, the most interesting results relate to sequence 12524 from Midden 2 in the South Area (Figure 6.45) and the clay inclusions found within these ash layers (Figure 6.35). Differences in peaks relating to clay minerals and calcite in these samples suggest differences in the extent of heating of these deposits. FT-IR results from experimental burning of clays (Figure 6.38), in addition to published material on pottery firing (Shoval 2003) and heating of sediments (Berna et al. 2007), supports the suggestion that FT-IR can be used as a technique to detect the extent to which archaeological deposits have been heated. Combined with examination of these ash layers in the field, and phytolith and micromorphology studies, the IR results strongly support the conclusion that these are large outdoor fuel burning areas. This idea is developed further in the discussion chapter. These results support the hypothesis that FT-IR can be used to aid in the understanding of midden formation processes in specific deposits.

Although this method of analysis has potential; a major problem with linking phytolith composition to the region of growth is the elemental characterisation of soils, and 91

Conclusions 







FT-IR is a useful technique for the quick and inexpensive screening of potential coprolite samples before subjecting them to the more expensive and time consuming method of GC-MS. The mineralogy and trace element composition of phytoliths varies between individual phytoliths, but the factors controlling this are poorly understood and need further investigation before they can be related to the growing region of the plants. FT-IR and micro XRD are useful techniques for identifying and characterising specific midden components such as hackberries and post depositional mineral nodules. FT-IR is a useful technique for detecting the extent of heating of midden deposits, and therefore aid in the interpretation of formation processes and activities related to burning.

92

Current methods of identifying faecal material and problems

7: BIOMOLECULAR ANALYSIS OF ORGANIC RESIDUES

Identification of faecal material in the field is still uncertain because of similarities in morphology and structure of faecal material with deposits such as yellow ochre and clay/silt and uncertainties about whether the amorphous material may derive from decayed food remains. It has been argued through the inclusion of larger bone fragments that this material at Çatalhöyük must come from dogs and digested bone fragments averaging two to three cm are often recovered from middens (Russell and Martin 2005 and pers. comm.). Field records of Middens 2 and 6, sampled in 2006, do not include reference to the presence of faecal material (McCann and Brown 2006, Yeomans 2006) despite this being observed as an abundant deposit within the middens (Shillito 2006, Matthews 2005). Material suspected to be of faecal origin has a distinct yelloworange colour in the field, and at Çatalhöyük may contain inclusions such as hackberry seeds and partially digested bone (Chapter 4). These inclusions may suggest faecal material, but identification of species can only be estimated.

Introduction GC-MS and other chromatographic techniques have become established in the analysis of biomolecules preserved in archaeological materials. Many studies have focused on pottery sherds, with the extraction of food residues and other substances to study the use of pottery vessels and dietary practises (Dudd et al. 1999), for example detecting ancient beeswax in Greek pottery (Evershed et al. 2003) and assessing the relationship between form and use of different vessels at Sagalassos, Turkey (Kimpe et al. 2004). Key archaeological studies include investigations into the origins of dairying (Dudd and Evershed 1998, Copley et al. 2003, 2005a, 2005b, 2005c), where bimolecular analysis of organic residues has provided direct evidence of the use of milk products, whereas previously this was restricted to inferences based on analysis of faunal remains (Legge 1981) and the presence of pottery vessels interpreted as “cheese strainers” (Bogucki 1984).

In thin section it has been established that at least some of these amorphous yellow deposits are coprolites (Matthews 2005) and are distinguished, due to the presence of calcareous spherulites which form in the gut through observing reference materials (Courty et al. 1989, Canti 1997, 1998, 1999). But these spherulites are not always present, particularly in omnivore coprolites, meaning that identification of faecal material by field observation and thin section micromorphology alone can be ambiguous. Again there is the suggestion that large bone inclusions indicate dog faeces (Russell and Martin 2005), but some of these coprolites are also seen to contain plant material (Matthews 2005), which seems unusual for dogs. Orange faecal material is also identifiable in thin section and often has inclusions such as bone fragments and phytoliths (Chapter 4). Brownish herbivore faecal material observed in thin section is even more difficult to identify in the field due to poor contrast with other deposits, although it exhibits a distinct appearance in thin section.

Biomolecular analysis has also been used to identify the composition and sources of bitumen and resins in Near Eastern antiquity, for example as mortars in buildings in Mesopotamian sites such as Babylon, and used in mummification in ancient Egypt (Connan et al. 1999) which in turn has enabled a reconstruction of trade routes in the wider region (Connan et al. 1998, Connan and Carter 2007). A high profile example is the analysis of the supposed canopic jars of Ramses II, revealed through biomolecular analysis to have been used to store unguents and embalming packages of an unknown individual, rather than the organs of the famous pharaoh (Charrié-Duhaut et al. 2007). Other studies have included the analysis of relict soils and faecal material as evidence of anthropogenic soil modification (Bull et al. 1999). However, there is still much potential for the technique to be used more widely as a species indicator in coprolite analysis (Bull et al. 2005), especially in conjunction with other techniques such as thin section micromorphology, as in the present study, to understand the depositional context of these deposits and thus their significance.

Advantages of biomolecular analysis Bimolecular analysis of organic residues is the only method that can be used to identify coprolites with any degree of certainty. Identification of faecal residues relies on the presence of sterols and bile acids, the structure and distribution of which are unique to some species. The accurate identification of faecal material as either human or animal is essential in the correct interpretation of archaeological deposits. In particular, the high quantity of this material in middens at Çatalhöyük has implications for health and perceptions of clean and dirty, which depend on establishing whether this is human or animal.

Previously, identification of faecal material at Çatalhöyük and other Near Eastern sites has been problematic in the field, and identification to species has implications for the interpretation of midden deposits containing faecal material. This chapter reviews the analysis of faecal material through bimolecular analysis and the aims and results of this analysis on a set of 29 suspected coprolite samples from Çatalhöyük.

93

Sterols and bile acids The sterols are a subgroup of steroids (characterised by a carbon skeleton of 4 rings in a 6-6-6-5 arrangement) that have a hydroxyl group in position 3 of the A ring. The sterol fraction of faecal residues contains a suite of biomarkers found in the faeces of several species, including cholesterol, coprostanol, and sitosterol. The ratios of these components vary depending on the diet of the animal and between species due to different biochemistries of the gut (Dutka and Elshaarawi 1975, van Faassen et al. 1987, Dabai et al. 1996, Ridlon et al. 2006). The sterol fraction of suspected faecal material is analysed first to distinguish between omnivore or ruminant sources. Figure 7.2: The route of formation and deposition of 5b-sterols and 5astanols formed from cholesterol, campesterol and sitosterol (from Bull et al. 1999).

Coprostanol is the major 5β-stanol of human faeces (Bondzynski and Humnicki 1896, Leeming et al. 1984, Bethell et al. 1994). It is found in other animals at much lower concentrations relative to other sterols and is absent from dog faeces, which do not contain 5β-stanols. Cows and sheep have higher relative abundances of 5βcampestanol and 5β-stigmastanol due to a herbivorous diet and thus the consumption of large amounts of campestanol and sitosterol (Bull et al. 2002). Figure 7.1 shows the structures of the major lipids and bile acids that are detected in faecal material. The structures show the differences between epimers that arise from different microbial transformations, found in soil and in the gut (e.g. Bull et al. 2002, Puglisi et al. 2003) as well as the differences between sterols and bile acids. The 5α epimers are produced by microbial action in the soil rather than the gut (Bethell et al. 1994, Bull et al. 1999) summarised in Figure 7.2. The bile acid fraction is then be analysed to distinguish between different omnivore species as well as ruminants. Whilst the proportions of sterols vary as a result of diet (van Faassen et al. 1987), the types of bile acid present and their relative proportions are highly specific to individual species (Haslewood 1967, Elhmmali et al. 1997, Bull et al. 2003). The major bile acids in human faecal material are deoxycholic acid (DOC) and lithocholic acid (LC) (Hill and Drasar 1968, Thomas et al. 2001, Ridlon et al. 2006). So to distinguish between human and porcine origin of omnivore faeces it is necessary to examine the bile acid content where the presence of hyodeoxycholic acid may be used to infer a porcine faecal source (Elhmmali et al. 1997). If DOC is present in significantly greater quantities than LC, this suggests a ruminant origin. A summary of the criteria used to determine the source of faecal material using multiple biomarkers is given in Figure 7.3.

Figure 7.1: Structures of major lipid and bile acid biomarkers detected. 1. Coprostanol 2. Epicoprostanol 3. 5β-campestanol 4. 5βepicampestanol 5. 5β-stigmastanol 6. 5β-epistigmastanol 7. Cholesterol 8. 5β-cholestanol 9. Campestanol 10. Sitosterol 11. Hyodeoxycholic acid 12. Deoxycholic acid 13. Lithocholic acid 14. Chenodeoxycholic acid 15. Hyocholic acid. Data from Bull et al. (1999).

94

Figure 7.3: A summary of the criteria used to determine the source of faecal material using multiple biomarkers, redrawn from Bull et al. 2002.

range of research questions (Bethell et al. 1994, Evershed and Bethell 1996) focused on studies of manuring and agricultural practises, including analysis of experimental samples at Butser Ancient Farm (Evershed et al. 1997) and Rothamsted Experimental Station (van Bergen et al. 1997, Bull et al. 1998, Bull et al. 2000) to investigate diagenetic impacts on faecal biomarker preservation, as well as archaeological case studies such as a study of anthropogenic soil formation at a Neolithic/Bronze Age site in Orkney (Simpson et al. 1998, Bull et al. 1999a, Bull et al. 1999b), agricultural manuring at a Minoan site in Crete (Bull et al. 1999c, Bull et al. 2002b) and studies of ancient wastewater at a Roman site in Greece (Bull et al. 2003).

Previous studies using sterols and bile acids as faecal biomarkers Methods for the analysis of sterols and bile acids as faecal biomarkers were originally developed for the analysis of water pollution, to monitor human and animal faecal waste inputs (e.g. Walker et al. 1982, Vivian 1986). Their use as biomakers is due to the relative stability of the compounds, and the specificity for different species, which enables the origins of sewage pollution to be determined. Early archaeological studies using combined sterol and bile acid data include a study of 2000 year old coprolites preserved under desiccated conditions in the Nevada Caves, where a dominance of coprostanol, lithocholic acid and deoxycholic acid confirmed these to be human (Lin et al. 1978), and a study of a Roman ditch from Bearsden, Scotland (Knights et al. 1983), interpreted as a cesspit due to the combined evidence of plant debris with sterol ratios matching those in the earlier study by Lin et al. (1978). The biomarkers had persisted in this study despite the poor preservation of distinct coprolites.

Studies specifically on coprolites were carried out on seven samples from Çatalhöyük in 1997 by the University of Bristol Organic Geochemistry Unit, to investigate whether residues would be detectable in samples of this age (Bull et al. 2005). These results showed that the midden deposits contained significant faecal residues, compared to mudbrick control samples, which showed no residues, and indicate that faecal residues are well preserved in these contexts at Çatalhöyük.

Since these early studies the use of sterols and bile acids has been further developed in the analysis of archaeological soils and coprolites to answer a wide

95

Table 7.1: Reference data for sterols showing molecular weight and characteristic fragment ions present in the mass spectra of the methyl ester – trimethylsilyl ether derivatives. Data from Bull et al. (1999, 2002). Molecular weight (TMS ethers)

Compound (in order of elution)

Full name

coprostanol

5β-cholestan-3β-ol

460

epicoprostanol

5β-cholestan - 3α-ol

460

cholesterol

Cholest-5-en-3β-ol

458

5α-cholestanol

5α-cholestan-3β-ol

460

5β-campestanol 5β-epicampestanol campesterol 5α-campestanol 5β-stigmastanol 5β-epistigmastanol sitosterol 5α-stigmastanol

24α-methyl-5β-cholestan-3β-ol 24α-methyl-5β-cholestan-3α-ol 24-methylcholest-5-en-3β-ol 24-methyl-5 -cholestan-3β-ol 24-ethyl-5β-cholestan-3β-ol 24-ethyl-5β-.cholestan-3α-ol 24-ethylcholest-5-en-3β-ol 24-ethyl-5α-cholestan-3β-ol

474 474 472 474 488 488 486 488

Characteristic ions

Major origin

460, 370, 257, 215, 445, 355 370, 355, 257, 215, 445 458, 368, 443, 329 460, 445, 370, 355, 306, 257, 215 384, 369, 257, 215, 459 384, 369, 257, 215, 459 382, 367, 343, 255, 129 384, 369, 257, 215, 459 398, 383, 257, 215 398, 383, 257, 215 396, 381, 357, 255, 129 473, 398, 383, 215

Omnivore Omnivore Omnivore Mammals/soil Ruminant Ruminant Plants Plants/soil Ruminant Ruminant Plants Ruminant

Table 7.2: Reference data for bile acids. Data from Elhmmali et al. (1997). Compound

Full name

Abbreviation

Molecular weight

Deoxycholic acid

3α,12α-dihydroxy-5β-cholanoic

DOC

550

Lithocholic acid

3α-hydroxy-5β-cholanoic

LC

462

Hyodeoxycholic acid

3α,6α-dihydroxy-5β-cholanoic acid 3α, 6α, 7α-trihydroxy-5β-cholanoic acid

HDOC

Hyocholic acid

HC

638

Characteristic ions

Origin

208, 255, 345, 370 215, 257, 357, 372

Human / Ruminant / Dog Human

147, 369, 355, 458

Pig Internal standard

Table 7.3: Summary of samples selected for organic residue analysis. Lab Number sample number

Area

Context

Year of collection

South 4040 North North South South TP North TP TP TP North North North South 4040 South South South -

Infill Midden Burial fill Burial fill Midden 1 Midden Midden 7 Burial fill Midden 7 Midden 7 Midden 7 Burial fill Room infill Burial fill Midden/infill Midden 3 Midden/infill Midden/infill Midden/infill -

1999 2004 1996 1996 2004 1997 2004 1997 2004 2004 2004 1996 1996 1997 1997 2004 1997 1997 1997 -

4040 4040 South South South 4040 4040 South South

Midden 6 Midden 6 Midden 2 Midden 2 Midden 2 Midden 6 Midden 6 Midden 2 Midden 2

2006 2006 2006 2006 2006 2006 2006 2006 2006

Sample set A 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 1 2 3 4 5 6 7 8 9

4477 S7 8864 S4 1380 S1 1494 S6 1668 upper 1 2739 S8b 7867/02 1993 S4 8932 S3 (13) 8932 S3/05 8932 S3 /09 1380 S? 1360 S1 1985 S5 2754 S2 11016 S4 2766 S5 2754 S4 2767 S4 Asikli hoyuk 97.16 Sample set B 13103 S34 13103 S24 12519 S7 12524 S14 12504 S16 13103 S21 13103 S27 12504 S15 12519 S8

96

Analyses were performed using GC and GC-MS. Details of the extraction methods and instrument conditions are given in Chapter 3. The method used to extract faecal biomarkers has been developed to select this range of compounds based on their similar structures and converts sterols to their trimethylsilyl (TMS) ethers for analysis. The addition of the TMS group gives better GC resolution and characteristic fragment ions, enabling easier identification of the compounds. Bile acids are analysed as their methyl esters. 200μl of the internal standards (0.3 μg ml-1), hycholic acid and preg-5-en-3βol, were added to quantify the residues extracted.

Hypotheses and aims of this investigation The bimolecular analysis of organic residues in thisresearch has been carried out to test the hypothesis that the samples are indeed faecal material as identified by the author in the field and that samples collected as coprolites by others during previous excavations (for example from grave contexts) are indeed faecal material, and that these are human, as suggested by micromorphology, rather than animal, as suggested in the field. This work also tests the hypothesis that, through identifying species and looking at the context of the samples in thin section, the origin of the faecal material in the middens can be deduced and that orange material in thin section can be interpreted as “omnivore” or human coprolites rather than herbivore, by directly comparing organic residues with the appearance of coprolites in thin section. These results obtained can then be used in conjunction with micromorphological data to understand deposits in middens containing faecal material. The origin of the faecal material has implications for the interpretation of individual depositional layers as viewed in thin section, and the specific identifications will enable the formation processes of these deposits to be inferred with much greater certainty.

GC-MS results were analysed using Xcalibur software (Thermo Fisher Scientific, Hemel Hempsted, UK). As well as by their characteristic mass spectra, the compounds are identifiable by GC trace by their order of elution. This is related to the mass of the compounds, and the sequence is very specific. The biomarkers of interest are divided into 3 homologous series – C27, C28 and C29 sterols (Christie 2003). The C27 sterols elute first, starting with coprostanol and ending with 5αcholestanol. The traces for the C28 and C29 homologues are superimposed on this series, but with increased retention times. This is shown in Figure 7.5 using sample 15 (2754 S2) as an example. Shaded peaks indicate the first molecule in each of the three homologous series.

Correct identification of faecal material is needed to support other analyses in thisresearch related to diet. The phytolith content of these samples can then be studied and compared with residue data in order to study the plant component of diet. It is possible that changes in diet may be seasonal and related to the differing availability of plant and animal resources throughout the year, which may be determined through the type of phytolith present (see Chapter 5). Sample selection and methods Results obtained for two sets of samples are presented in this chapter. The first set sample set A, comprises a selection of coprolites and soils collected in the 2004 season from Middens 3 and 7, as well as suspected coprolites and soils acquired from storage from the first few years of excavation, from 1996-1999, from contexts including middens and the abdomens of skeletons in graves. This sample set will enable an investigation of whether samples identified as “coprolites” in previous seasons are coprolites. The second sample set, sample set B, was collected in 2006 and analysed 6 months after collection. The suspected coprolites from 2006 are highly targeted in that they can be directly related to their depositional context through comparison with corresponding thin sections (Chapter 4) and are from sequences in Middens 2 and 6. Details of the context of materials analysed are summarised in Table 7.3.

Figure 7.4: GC trace for sample 15 (2754 S2) showing structures of major biomarkers that determine the order of elution. Shaded peaks indicate the first biomarker in each homologous series. 1: coprostanol 2: cholesterol 3: 5α-cholestanol 4: 5βcampestanol 5: 5β-stigmastanol 6: 5α-campestanol 7: sitosterol 8: 5αstigmastanol. Figure courtesy of Dr Ian Bull, University of Bristol.

97

Feature 211) of an adult and child. Ratio 3 for these samples indicates samples 12 and 14 do not contain faecal residues (though 14 does contain some DOC and LC).

In order to identify the likely source of any biomarkers present, three ratios can be calculated: Ratio 1: Coprostanol/(coprostanol + 5α-cholestanol) Ratio 2: Coprostanol + epicoprostanol / (coprostanol + epicoprostanol + 5α-cholestanol)

2004 samples 2.5000

Ratio 3: (Coprostanol+epicoprostanol)/(5β stigmastanol+5β -epistigmastanol)

2.0000

1.5000 Ratio 1

Ratio

It has been proposed that for ratio 1, a value greater than 0.7 is a definite indicator of faecal pollution (Grimalt et al. 1990). Ratio 2 has been proposed by Bull et al. (2002) to account for diagenetic processes leading to the formation of epicoprostanol. Archaeological values are thus adjusted to take into account the further transformation of coprostanol compared to 5αcholestanol. Ratio 3 is used to confirm if the presence of faecal material is from either pig/human, or a ruminant species.

Ratio 2 1.0000 Ratio 3

0.5000

0.0000 1

2

3

4

5

6

7

8

9

10

11

12

13

14

15

16

17

18

19

20

Sample number

Figure 7.5: Ratios for sample set A.

This leaves 13 samples containing significant relative amounts of residues of faecal origin, through observation of the histograms. This is confirmed through calculation of the ratios discussed in the previous section (presented in Figure 7.5) which indicates all 13 of the remaining samples contain faecal residues, with 11 of these being omnivore faeces, 1 being probable ruminant faeces (sample 16), and 1 being a probable mixture of ruminant and omnivore faeces (sample 1). Most samples with faecal residues are from middens and infill, with one (sample 4) from a burial context. The initial study at Çatalhöyük showed a human origin for four of the seven samples studied (Bull et al. 2005), with the ratios (using ratio 3) of the coprolite samples being 0.79 and 0.92, and the midden deposit samples having ratios of 0.83 and just under 1.00. The ratios for the 11 omnivore samples in set A range from 0.81 to 2.34, with the ruminant sample 0.05 and the mixed sample 0.57. Ratio 1 of sample 9 (0.54) suggests this other residues as well as faecal residues.

Results Analysis of sterols Sterol biomarker concentrations for the two sets of samples analysed varied significantly between samples. In sample set A it can be seen that 4 of the 20 samples analysed (samples 2, 3, 7, and 8), contained no residues. Samples 2 and 7 are from middens, whilst 3 and 8 are from burials. A further sample contained only sitosterol and 5α-stigmastanol, from a room infill context, likely to be from decayed plant material. These samples therefore can not be interpreted as coprolites, or containing faecal material. The remaining 15 samples in set A all contain a range of residues of possible faecal origin, with the relative concentrations of the different sterols being very variable. Observation of the relative concentrations of biomarkers indicates sample 12 is not of faecal origin, as the only residues present are cholesterol, campestanol, 5αcampestanol, sitosterol and 5α-stigmastanol. As shown in the flow chart in Figure 7.3, these 5α products are the result of microbial breakdown in the soil rather than the gut. The concentrations of sitosterol and 5α-stigmastanol in this sample are relatively high, at 2.02 and 7.5 μg g-1 respectively. Considering the burial context (Feature 28, Space 110), this sample could be interpreted as decayed plant material deposited in the grave, supporting early suggestions of the deliberate inclusion of plants in graves (Mellaart 1967) as well as more recent phytolith and botanical studies which have found impressions of reed baskets and caches of hackberries, for example in the burial beneath Building 6 in the BACH area (Asouti et al. 1999, Rosen 1999). Sample 14 has a noticeably high concentration of cholesterol at 2.58 μg g-1 compared to 0.02 μg g-1 coprostanol, with other residues of 5αcholestanol (0.06 μg g-1), 5α-campestanol (0.32 μg g-1), sitosterol (0.97 μg g-1 ) and 5α-stigmastanol (2.76 μg g-1). Again this is from a burial fill (Building 1, Space 71,

In sample set B all but two samples (2 and 5) contain significant quantities of sterols including cholesterol, coprostanol and epicoprostanol, ranging from 0.02 μg g-1 in sample 9 to 2.15 μg g-1 in sample 3 for coprostanol. Concentrations of epicoprostanol are relatively high in sample set B, with the highest at 0.38 μg g-1 in sample 3. In sample set A this was only recovered in trace amounts – this could be due the omission of the urea adduction step for sample set B (this step was omitted during processing of the second sample set to try and improve the recovery of residues). Sample 2 contains cholesterol and sitosterol only, excluding a faecal origin, whilst sample 5 contains small quantities of cholesterol, 5βstigmastanol, sitosterol and 5α-stigmastanol. Although this contains a 5β sterol, the low concentration at 0.01 μg g-1 and the lack of any other 5β sterols, suggests this does not have a faecal source, and can be considered as a minor background of extant 5β-stigmastanol. These are presented in Figure 7.6. Ratio 3 of the remaining seven

98

2006 samples 2.0000 1.9000 1.8000 1.7000 1.6000 1.5000 1.4000 1.3000

Ratio 1

1.2000 Ratio

1.1000 Ratio 2

1.0000 0.9000 0.8000

Ratio 3

0.7000 0.6000 0.5000 0.4000 0.3000 0.2000 0.1000 0.0000 1

2

3

4

5 6 Sample number

7

8

9

1

Figure 7.6: Ratios for sample set B.

contain LC or DOC, confirming that these do not contain faeces, whilst the samples with omnivore faecal sterol ratios all contain LC and DOC. This confirms the presence of human faecal material in these samples. Sample 1 (4477 S7), observed to contain a mix of ruminant and omnivore faeces was seen to contain DOC, whilst sample 16 (11016 S4) observed to contain possible ruminant faecal material, did not contain detectable traces of bile acids. Sample 12, interpreted in the previous section as the remains of decayed plant material in a grave, does not contain DOC or LC, further supporting the interpretation of this as decayed plant remains.

samples indicates that these are omnivore coprolites, with ratios ranging from 0.75 to 1.73. Sample 8 has a ratio of 0.62 which suggests a possible ruminant origin. Ratio 1 suggests sample 4 is faecal material mixed with another deposit. The ratios for sample set B are shown in Figure 7.6. Figures 7.7 to 7.16 show GC traces from each of the three context types analysed from sample set A – midden, grave and open area. Figure 7.10 shows sample 11 (8932 S3/09) from Midden 7 in the TP Area. It has a particularly intense coprostanol peak (peak 1). Figure 7.11 shows sample 18 (2754 S4), from an outdoor infill area. Both have intense coprostanol, cholesterol and sitosterol peaks. Figure 7.12 shows sample 4 from a burial, with a smaller relative intensity of coprostanol compared to sitosterol and 5α-stigmastanol. Figures 7.13 and 7.14 show examples of coprolites from Midden 2 (South Area) and Midden 6 (4040 Area), analysed in sample set B. These samples correspond with thin sections analysed and will be compared with microscopic observations of these deposits in the following section.

In sample set B, all samples observed to contain omnivore faecal sterols were found to contain LC and DOC, confirming these as human coprolites. The two samples, 2 and 5, which did not contain sterol residues did not contain bile acid residues either. Sample 8, which was potentially a ruminant sample on the basis of Ratio 3, was found to contain LC and DOC, suggesting that this is human rather than ruminant. The reason for the low Ratio 3 value in this sample is unclear. Figures 7.10, 7.11 and 7.12 show the bile acid traces for samples 11, 18 and 4 from sample set A (the sterol traces for these were shown in Figures 7.7, 7.8 and 7.9). It can be seen that the relative intensity of bile acids is very variable. Samples in set B contain other compounds in addition to the bile acids. Diacids and other hydroxy acids are present in these samples because of the omission of the urea adduction step in the extraction method. Figures 7.15 and 7.16 show the bile acid traces for samples 3 and 7 in sample set B.

Bile acids To distinguish between pig and human for samples found to contain faecal sterols, and to further investigate the two possible ruminant samples, further analysis was carried out to identify the bile acids present. Samples were analysed for the presence of DOC and LC (as summarised in Figure 7.2). The results of this analysis are given in Table 7.4. In sample set A those samples not containing faecal sterols were also observed not to

99

Figure 7.10: GC trace from sample 3 (12519 S7) 1. coprostanol 2. epicoprostanol 3. cholesterol 4. 5α-cholestanol 5. 5β-campestanol 6. 5β-epicampestanol 7. 5β-stigmastanol 8. 5β-epistigmastanol 9. sitosterol 10. 5α-stigmastanol.

Figure 7.7: GC trace for sample 11 (8932 S3/09) 1. coprostanol 2. epicoprostanol 3. cholesterol 4. 5α-cholestanol 5. 5β-campestanol 6. 5β-epicampestanol 7. 5β-stigmastanol 8. 5β-epistigmastanol 9. sitosterol 10. 5α-stigmastanol.

Figure 7.11: GC trace for sample 7 (13103 S27) 1. coprostanol 2. epicoprostanol 3. cholesterol 4. 5α-cholestanol 5. 5β-campestanol 6. 5β-epicampestanol 7. 5β-stigmastanol 8. 5β-epistigmastanol 9. sitosterol 10. 5α-stigmastanol.

Figure 7.8: GC Trace for sample 18 (2754 S4) 1. coprostanol 2. epicoprostanol 3. cholesterol 4. 5α-cholestanol 5. 5β-campestanol 6. 5β-epicampestanol 7. 5β-stigmastanol 8. 5β-epistigmastanol 9. sitosterol 10. 5α-stigmastanol.

Figure 7.9: GC trace for sample 4 (1494 S6) 1. coprostanol 2. epicoprostanol 3. cholesterol 4. 5β-stigmastanol 5. 5β-epistigmastanol 6. sitosterol 7. 5α-stigmastanol.

Figure 7.12: GC trace for sample 11(8932 S3/09) showing the presence of LC and DOC bile acids. HC is the internal standard.

100

Figure 7.16: GC trace for sample 7 (13103 S27) showing the presence of LC and DOC bile acids. HC is the internal standard.

Figure 7.13: GC trace for sample 18 (2754 S4) showing the presence of LC and DOC bile acids. HC is the internal standard.

Discussion Samples containing faecal residues The 22 samples identified as containing faecal residues show significant quantities of 5β-stanols that match the mass spectra of known reference materials (reference mass spectra for faecal sterols can be found in the Appendix, section 8a). There is a dominance of coprostanol as opposed to the C29 5β-stanol and a lack of 5β-stanol epimers. Analysis of the results obtained has enabled identification of these coprolites and deposits as omnivore faecal material, or not containing faecal material. No samples show an unambiguous ruminant origin. 4477 is shown to possibly contain faeces from a ruminant species, with sterol ratio 1 suggesting a mixture of faecal material with another deposit, and ratio 3 suggesting a mix of omnivore and ruminant faeces (coprostanol and cholesterol are found in similar, low quantities at 0.024 and 0.026 μg g-1 respectively). Bile acid data for this sample indicate the presence of DOC. However concentrations of residues in this sample are too low to confirm this as ruminant without ambiguity.

Figure 7.14: GC trace for sample 4 (1494 S6) showing the presence of LC and DOC bile acids. HC is the internal standard.

11016 S4 was seen to possibly contain ruminant faecal material on the basis of ratio 3 at 0.048, but further examination of this data indicate only 0.002 μg g-1 of coprostanol, and no bile acids. To further clarify this sample, comparisons were made with the corresponding thin section and block photographs. Although this thin section is observed to contain faecal material, the sub sample analysed was taken below the coprolite as observed in thin section, and so does not directly correspond. It could be that orange stain as observed in the sample block is an aggregate rather than a coprolite, through the presence of adjacent faecal material in thin section, and low quantities of sterols, could possibly suggest the presence of ruminant faeces.

Figure 7.15: GC trace for sample 3 (12519 S7) showing the presence of LC and DOC bile acids. HC internal standard not shown.

101

to poor preservation, the recovery of high concentrations of faecal residues from other samples suggest that a lack of faecal residues can be used to support the hypothesis that these are not faecal samples, as suggested when the samples were collected. Sample7, 7867/02 has a corresponding thin section (Chapter 4, Table 4.17), and the sub sample is described as dark grey/orange. Examination of the thin section shows this to be quite mixed and homogenous, with no visible faecal material. The orange appearance could therefore be a result of clay aggregates.

Samples containing non-faecal residues These are 1360 S1 from room infill, 13103 S24 from Midden 6 and 12504 S16 from Midden 2. Observation of the sample block for 13103 S24 in the field shows the orange sub sample analysed is embedded within an ash layer and so is likely to be a clay fragment similar to others analysed in this research (Chapter 6). The presence of plant sterols in this sample rather than faecal sterols could also be a result of the presence of plant material as temper, observed in the field and in similar deposits in thin section.

Implications for the Identification of coprolitic deposits in the field

The burial contexts are particularly interesting Asouti et al. (1999) suggest the importance of plants in burials, but also note the lack of charred macrobotanical remains in these contexts. Phytolith analysis by Rosen (1999) has identified reeds in these contexts, and the analysis of deposits associated with skeletons in this research has identified the presence of relatively high concentrations of sterols associated with the death and decay of plant remains.

The presence of faecal residues, non-faecal residues, and a lack of any residues in some samples, can now be used to discuss the implications for identifying coprolites in the field, particularly samples collected from burials, and as non-discreet orange deposits (or “stains”) in the field. The recovery of relatively high concentrations of residues from all samples in set B (apart from 2 and 5, which are explained), suggests identification of coprolites from discrete orange concretions is more reliable.

Table 7.4: Summary of bile acids present in the samples analysed. Sample number Sample set A 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 Sample set B 1 2 3 4 5 6 7 8 9

Deoxycholic acid (DOC)

Lithocholic acid (LC)

√ √ √ √ √ √ √

√ √ √ √

√ √ √ √

√ √

√ √ √

√ √ √

√

√

√ √ √ √ √ √ √

√

Identification of coprolites in burials As previously discussed, only 1 sample collected as a coprolite from a burial has been found to contain faecal residues in this study, and these were found in very low concentrations compared to other residues. Other samples collected as coprolites from burials are found to contain non-faecal residues, as discussed in section 7.5.2. Identification of coprolites in middens and open areas A set of samples which illustrates the importance of organic residue analysis are the deposits in Building 2, Space 117, excavated in 1997. These include samples 2754 S2 and S4, 2766 S5 and 2767 S4. The archive data for this unit debates whether these are yellow ochre or coprolites, with the final tentative interpretation being that these represent animal penning during an intermediate phase between house floors and demolition back fill (Reagan, in Farid 1997). Reagan also notes the presence of large animal bones scattered either over or within the deposit. Faunal records indicate the presence of digested bone, and mention dog faeces based on these inclusions. There are cut marks on some of the bone, and interpretation suggests post consumption discard.

√

√ √ √ √ √

Micromorphological analysis however suggested these were omnivore rather than ruminant coprolites, and were unlikely to be penning areas, due to the lack of sediment compaction (Matthews 2005). Analysis of these samples indicates the faeces present is human not animal, confirmed by both sterol and bile acid residues, and supports Matthews’ hypothesis that this was a latrine area rather briefly used as a waste dumping or toilet area in an abandoned building, before being back filled with building demolition debris. The building debris layers

Samples containing no residues As summarised in section 7.4.1, some samples 2, 3, 7 and 8 in sample set A contained no traces of either faecal or non faecal residues (no sterols and no bile acids). Samples 2 and 7 are from middens, whilst 3 and 8 are from burials. Although it should be considered this is due

102

reported by Reagan (in Farid 1997) that overly the coprolitic layer are interspersed with finer deposits of “midden like” ashy and bone material, which would also suggest some cyclical use of this area as midden.

blocks of Midden 7 (8932 S3, S5, S9 and S13) indicates that these are all human faecal material, confirmed by the presence of faecal sterols and bile acids. Observation of these deposits in thin section shows them to be amorphous organic material with no inclusions that would enable them to be interpreted as coprolites. This illustrates the benefit of organic residue analysis in interpreting the fine organic layers observed in many thin section samples.

Samples collected as coprolites from earlier excavations include 8864 in Space 226, 4040 area, 2739 from the South Area Space 115 (Midden 1, described in the database as lenses of coprolites and phytoliths, with phytolith impressions and hackberries) and 1360 from sub floor packing in Building 1, Space 71. 8864 is described as a coprolite in the database record but is not discussed in the archive report (Stefanova and Dakić 2004). Samples 8864 and 1380 have been shown to contain no faecal residues and illustrates that yellow deposits should not be assumed to be coprolites. 2739 contains human faecal residues, showing that field identification is sometimes correct, particularly when supported by the presence of hackberry inclusions.

A number of coprolites in sample set B have associated thin sections, which enables us to test the hypothesis that orange amorphous material identified in the field by the author is in fact faecal material, and whether or not this is human. This then allows a more accurate interpretation of the fine layers of this material seen in the thin sections samples, and thus midden formation processes and human activity, as detailed in Chapter 1. Both samples analysed from Midden 2 (12519 S7 and S8) contained human faecal residues, and are also observed as amorphous organic material in thin section (Figure 7.18).

Table 7.5: Summary of ratios and which species these indicate for both sample sets. Sample number Lab number Ratio 1 Ratio 3 Sample set A 4477 S7 8864 S4 1380 S1 1494 S6 1668 upper 1 2739 S8b 7867/02 1993 S4 8932 S3 (13) 8932 S3/05 8932 S3 /09 1380 S? 1360 S1 1985 S5 2754 S2 11016 S4 2766 S5 2754 S4 2767 S4 Asikli hoyuk 97.16

1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20

0.5786 0.7270 0.7384 0.8322 0.5390 0.7614 0.8152 0.2268 0.9203 1.0000 0.9943 0.9295 0.8192 0.6180

0.5729 0.9062 1.0942 0.8141 1.1360 1.8842 1.3338 0.9676 0.0472 1.6785 0.9616 1.2758 2.3417

1 2 3 4 5 6 7

0.9645 0.9416 0.5190 0.8462 0.9420

0.7450 1.7319 0.8542 0.8178 1.4033

8 9

0.8797 0.9507

0.6193 0.8368

4 samples were analysed from Midden 6, unit 13103 of these 4 samples, 3 were identified as human (13103 S34, S21, S27). These are seen in thin section to be amorphous organic material. Sample 13103 S24 did not contain faecal residues. The thin section slide for this sample has not yet been prepared, but as discussed earlier, this is likely to be a clay fragment containing plant material as temper (see Chapter 8 for the appearance of this clay material in thin section). One thin section from Midden 2, 12558 S2, which contained an orange coprolite with a large bone fragment and phytoliths has not yet been analysed for faecal residues, though it’s appearance in the field was identical to samples 12519 S7 and S8, identified as human. 8932 S3/09 also contains small bone fragments. It is suggested in this case that larger bone fragments do not necessarily mean that the coprolite is not human, as suggested by Russell and Martin (2005 and pers. comm.).

Sample set B 13103 S34 13103 S24 12519 S7 12524 S14 *13 12504 S16 13103 S21 13103 S27 12504 S15 12519 S8

Implications of faecal residues for the interpretation of midden formation processes and human activity The dominance of human faecal material is surprising considering the large amount of animals present at the site, indicated through analysis of faunal remains (Russell and Martin 2005; Yeomans 2005) and identification of animal pens and faecal spherulites in hearths and middens (Matthews et al. 1996, Matthews 2005). This could suggest that animal faeces were not being deposited in the middens, perhaps because they were used as fuel, evidence of which is presented in this study through the presence of calcareous spherulites in ash deposits. A dominance of human faecal residues have been observed in other prehistoric contexts such as the Neolithic/Bronze Age site of Sanday, Orkney, where they are suggested to have been applied to soils as manure. In this study there was also an absence of cattle or sheep manure, with the suggestion being that these were used preferentially as a fuel source

Figures in bold italic indicate an admixture of faecal material with another deposit Figures in bold indicate faecal material Figures in Roman indicate human/porcine source (given context most likely human) Figure in italic indicative of a mixture of human/porcine and ruminant faeces Figure underlined indicative of ruminant faecal material

Identification of coprolitic material from middens in thin section In sample set A, thin section blocks associated with residue samples are from Midden 7 (Figure 7.17). Analysis of sub samples from the micromorphology

103

Figure 7.17: Block 8932 S3 (Midden 7, TP Area) and organic residue samples 8932 S3/05, 09 and 13. Microscope photographs show the appearance of the coprolites under PPL at x10 magnification. 05 and 09 are human, 13 is human mixed with other organic residues.

Figure 7.18: Block 13103 S26 (Midden 6, 4040 Area) showing location organic residue sample 13103 S27, identified as human. Microscope photographs show the appearance of the coprolite under PPL at x10 (above) and x20 (below) magnification.

104

the plant remains within coprolites, and analysis of bone content within coprolites.

(Simpson et al. 1998). However it must also be noted that this could be due to a sampling bias, as ruminant faeces may be more difficult to identify in the field.

Analysis of diet is an important area of research that is related to questions concerning agriculture and animal management at Çatalhöyük, and a more detailed study of dietary information that could be obtained from coprolite analysis would add greatly to this, particularly analysis of isotopes from faecal material in conjunction with other isotopic analyses on bone and collagen (Richards et al. 2003, Richards and Pearson 2005). So far no isotope work has been carried out on archaeological coprolite material, despite the potential for these deposits in being a rich source of dietary information that can be combined with analysis of bone and phytolith inclusions within the coprolites. The results presented here suggest that this is an area of future work that could be developed further.

Conclusions At Çatalhöyük coprolites are difficult to identify in the field as they often lack a distinct morphology, perhaps due to compression during midden formation. Coprolites with a more distinct morphology have on occasion been mistaken for clay objects (personal observation). Previously any yellowish or orange deposits at Çatalhöyük have been interpreted as either coprolites or yellow ochre, depending on the opinion of the excavator and the context of the material, for example some burials are argued to contain coprolitic material in the pelvic region of skeletons, whereas in other burials this is described as being yellow ochre. Observations of these orange deposits, compared to clays and ochres, suggest the colour and texture of coprolites are distinctive, having an orange colour and being loose and crumb like, compared to clay/silt materials which have a finer texture. Coprolites with a more distinct morphology and bone inclusions recovered during faunal analysis appear to be paler and more cemented (personal observation during 2009 field season).

Due to time limitations only 29 samples were analysed in this study. Since further micromorphological work has been carried out, further examples of orange faecal material containing large bone fragments have been observed which are identical in appearance to samples analysed in this study, which are shown to be human. In addition there are a number of coprolite samples available collected as dog faeces by the faunal team based only on digested bone inclusions. Further work could be carried out to test this hypothesis. This is important, as the presence of digested bone has been used in other studies as evidence of dog domestication (Davis 1987, Horwitz 1990).

The results presented here can be used to test the original hypotheses stated in the introduction. Confirmation of the faecal origin of 7 out of 9 samples collected as coprolites by the author supports the hypothesis that these were indeed coprolites, and that they are largely human in origin. The variable result for faecal residues collected by others in previous seasons, however, indicates that not all material collected as coprolites can be identified as such. This is particularly true of burial contexts. Burial samples described as coprolites from graves include 1494 S6, 1993 S4, 1380 S1 and S?, 1985 S5. Analysis of these samples shows that none of these contain faecal residues, except 1494 S6.

Further comparison with thin sections could help identify deposits which contained plant sterols but no faecal residues, for example sample 12504 S16 and 13103 S24 have associated thin section blocks that have not been analysed in this study, which could be investigated further. It would also be useful to analyse deposits identified as ruminant in thin section, to compare the biomolecular data for these samples.

Further work It could be argued that samples containing higher amounts of sitosterol/stigmastanol (but with bile acids that indicate a human rather than ruminant source) are from herbivores (due to an increase in plant sterols in the diet), though further experimental work is needed to confirm this, as the factors influencing the production of different faecal steroids are complex (Wilson 1961, Wilkins and Hackman 1974, Dabai et al. 1996). It is suggested that this is a potential area that could be developed for future research. Faecal residues are linked to diet. It has been shown here that the combination of sterols and bile acids can narrow identification to species. Further work on the factors governing the concentrations of sterol residues (e.g. preservation and diet) would possibly enable dietary information to be gained from faecal residues. This would be particularly useful in combination with phytolith analysis to examine

105

8: DISCUSSION

Midden formation processes and activities identified

Introduction

Middens are an important source of information, especially at a site like Çatalhöyük, where domestic deposits in other contexts are rare (Matthews et al. 1996). In order to understand midden deposits, it is necessary to investigate midden formation processes i.e. the types of deposits present, and the nature and rate of their accumulation. Previous work on middens at the site has examined large scale patterns such as clusters of bone assemblages and looked at broad patterns in deposition (Yeomans 2005, Martin and Russell 2000), but these studies suggest that examining individual fine layers is not possible, some being less than 1mm thick. In routine excavation and sampling several depositional units have been aggregated together in their analysis, which blurs any cyclical patterns, especially when considering the varying accumulation rates.

This research has contributed to questions concerning early Neolithic society in Anatolia through the case study of Çatalhöyük, and through the approach of studying midden formation processes. Previously middens have only been sampled when specific questions arose, compared to more intensive sampling strategies in primary activity areas. Individual midden layers have been assumed too fine to be able to observe individually. The aims of this research were to use a set of complementary analytical methods to characterise and describe midden components, deposit types and formation processes. By doing this it was hypothesised that sequences of individual domestic and craft activities could be observed, the frequency of which could related to periodic and perhaps seasonal availability of resource use. Specific activities which it was hypothesised may be detectable in middens, based on previous research at Çatalhöyük, were summarised in Table 1.1 (Chapter 1), and included crop processing, hearth rake out, food preparation, food consumption, food waste disposal, fuel use for heating, cleaning of buildings such as sweeping floors, building construction and demolition, crafts (wood working, lithics, basketry, pottery). Many of these activities are related specifically to resource use and diet, and the identification of activities has provided information on these aspects.

This research has tried to overcome this problem through using thin section micromorphology of representative sections of these deposits, to study the fine layers individually and in situ, and through sub sampling these blocks carefully to analyse the variations in phytolith assemblages between each layer, which may be related to specific activities such as crop processing or fuel. Middens have been found in this research to contain deposits from a range of domestic activities which have the potential to inform about frequent and cyclical activities, resource use and diet, as well as the use of space and perceptions of waste in the Neolithic. It was hypothesised in this research that using thin section micromorphology would enable the identification of individual depositional events, and the relative frequencies of different deposit types (Chapter 1, section 1.1, section 1.4.1 and section 1.7, Chapter 4 section 4.1). It was further hypothesised that by analysing sub samples related to individual deposits, the limitations of observing phytoliths and chemical properties in thin section would be reduced.

Chapters 4 to 7 have presented data obtained from thin section micromorphology and phytolith, FT-IR and GCMS analysis of sub samples from these blocks. A total of 21 thin sections have been studied in detail, with over 300 bulk phytolith and chemical analyses. These methods have been used together to characterise and enable the understanding of the microstratigraphy of midden deposits at Çatalhöyük. This has produced a highly detailed dataset which has been summarised through the creation of deposit types and column diagrams indicating the sequence of deposit types in the samples studied. This is a simple visual way of showing the sequence and frequency of different deposit types, the general thickness of each deposit type, and allows an easy comparison between different areas and levels.

Identification of midden deposits from thin section analysis and macro scale observation This work has developed a new way of classifying midden deposits. Previous methods of describing micmorphological features based on attributes such as sorting and orientation of particles (e.g. Bullock et al. 1985, Courty et al. 1989, Stoops 2003) were found to be less useful, being developed largely for naturally deposited sediments, and this research has developed a classification based on major inclusions and deposit types. Deposits in this research have been classified on the basis of inclusion types and microstructure. Observations at the macroscale indicate a complex series of formation processes, with a macroscale pattern being repeated bands of multiple fine lensed deposits interspersed with larger massive ash and mixed deposits, and construction/demolition debris. General midden deposit categories are as follows:

In this discussion these results from the different analytical methods are used in discussing the key themes of this research, that is, midden formation process and activities, cyclicity and seasonality of activities, resource use for these activities, and origins of agriculture and diet. In this discussion it is demonstrated how these integrated results build on previous research on these themes at Çatalhöyük. In addition, current methodological problems are discussed, and ways in which this research has overcome some of these and the final section of this discussion gives an overview of areas which could be developed in future research.

106

1.

2.

3.

4.

Domestic deposits containing multiple fine layers of redeposited domestic type refuse such as ash, charcoal, bone fragments, including deposits with one or two dominant inclusion types (Deposit Types 1,2,3,4,5,9 described in Chapter 4, Table 4.4) such as Midden 1 and Phase 1 of Midden 2, both in the South Area (Chapter 4, section 4.4.1). Demolition debris with multiple periods of large scale aggregate deposition (Deposit Type 6, with type 10 as packing material. May be interspersed with domestic deposit types). Middens that are used for large scale open air burning activities, consisting largely of Deposit Types 3 overlying Deposit Type 1. Large ash layers with underlying charcoal and rubified material from in situ burning such as Midden 2 Phase 2. Deposits that consist of massive redeposited layers, e.g. packing material reused from other middens. These may be entirely mixed or may have concentrations of particular inclusion types (Deposit Types 8 and 10) such as Midden 4 (Chapter 4, section 4.4.2).

the same area. Macroscale observations showed the presence of large lumps of burnt clay with mineralised plant remains or impressions indicating an anthropogenic origin, which were dark orange in appearance and faded on contact with air. Thin section observation of one of these aggregates, sample 13103 S29 from Midden 6 in the 4040 Area, in Figure 8.1, shows the presence of pseudomorphic voids from decayed plant temper, confirming the anthropogenic origin. The presence of plant sterols in a possible aggregate sample also support the use of plant temper (Chapter 7, Figure 7.5), which was discussed in Chapter 7, section 7.5. Previous ideas (Hodder, pers. comm.) of these layers being “sanitary” seems unlikely, as they occur relatively infrequently, and the macroscale morphology shows them to occur as mounds or pits, suggesting an in situ fire rather than spreading of ash.

Each midden may change its major use, for example the category 2 midden in the 4040 area is interspersed with domestic deposits. The sequences of multiple fine layers have been further categorised into deposit types based on their major inclusion type and depositional characteristics. These categories suggest cycles of activities, including building construction and demolition debris and large in situ burning events, suggested as possibly pottery firing events in the deposits studied. Other possibilities for large ash layers include lime burning, and less frequent activities, interspersed with more frequent activities represented by ashy material, plant material and organic material disposal. The fine layers have been classified through thin section observation, which can be seen in Chapter 4, Table 4.4, and are related to more frequent activities.

Figure 8.1: Aggregate in sample 13103 S29 at x4 magnification, showing pseudomorphic voids from decayed plant material (aggregate type 4). From Midden 6 in the 4040 Area.

Phytolith variations in deposits Previous phytolith work on middens at Çatalhöyük has not taken samples systematically from individual layers and has studied the phytolith assemblage without integration with micromorphological analysis (Rosen 2005). Whilst this approach enables comparison of the general phytolith assemblage of middens to other contexts (recognised also by Jenkins 2005), it misses a great deal of the information that the microcontext can provide. Comparison with thin section micromorphology in this research shows that similar phytolith assemblages can derive from very different contexts, such as ash, coprolites or animal dung. These taphonomic considerations have been recognised for macrobotanical remains (Anderson and Ertug-Yaras 1998, Miller and Smart 1984) but have not previously been fully considered for phytoliths. This indicates that for complex finely layered deposits such as middens, looking at phytoliths alone cannot distinguish between different phytolith inputs.

The reuse of midden deposits as packing material, evidenced by cuts removing this material and observations of midden used as packing, for example in Midden 5, as well as the in situ burning activities, for example in Midden 2, suggest that middens were not considered “rubbish” but rather were important resources that were frequently reused in construction, and areas of the site that were also used for in situ activity. Looking at the macroscale to examine thick ash layers (photographs of these layers in the 4040 Area can be seen in Chapter 4, Figure 4.35, and in the South Area in Chapter 6, Figures 6.35 and 6.45), these are seen to be very extensive, suggesting some sort of large scale activity, possibly in situ, for example in Middens 2 and 6, South Area Level VI and 4040 Area Level VI/V respectively. This is suggested as outdoor burning, perhaps for pottery firing, based on the heating temperature of clay inclusions. The layers are repeated, suggesting a similar activity was carried out repeatedly in 107

absolute rate would be interesting, to get an idea of exactly how much time build up they actually represent. Personal observations have suggested that it takes relatively little time to build up large amounts of some waste materials such as ash, but fine layers are less clear. It would be interesting to estimate the time between a sequence of fine layers and a sequence of massive layers to understand the timing of these, for example seasonal versus annual deposition.

Examination of phytoliths from individual layers has shown high variability in the assemblages between different layers (Chapter 5), and has identified concentrations of some phytolith types, such as dendritic phytoliths, which are of potential use as seasonal “marker” deposits, particularly when they occur in well defined context such as coprolites and animal dung. They are seen to be most useful when occurring in these distinct deposit types, due to a general background noise, also mentioned by Rosen (2005), but not fully considered in her interpretations.

The carbon dating sequence for Çatalhöyük (Cessford 2001, Cessford et al. 2005) which uses a number of samples from the Deep Sounding midden (Space 181). Although this is not directly comparable with the samples analysed in this study, the published data has been used to calculate an accumulation rate for the Deep Sounding midden. Using the average dates the deposits span 220 years, however taking into account the minimum and maximum values for the carbon dates this ranges from 120 to 318 years from the top to the bottom of the midden. Estimating the depth of the midden at just over 4 meters, this gives accumulation rate of 1.8, 3 and 1.3 cm per year. However examining the dates of the sequence it seems the difference between some of the dating points is very variable, with some of the earlier deposits having younger dates than later deposits.

The lack of cereal phytoliths in the samples studied is interesting. Considering that cereals such as wheat and barley are found in the charred macrobotanical remains (Fairbairn et al. 2005, Bogaard et al. 2005, 2008), and in previous phytolith analyses (Rosen 2005, Jenkins 2005), it would be expected to see more of these in this research, after the examination of a large number of samples. However, closer examination of previous phytolith data (Rosen 2005) has shown that there are considerable taphonomic issues that have not been considered when interpreting the data, in particular the lack of specific contextual information, and the low numbers of phytoliths that are used to support previous hypotheses. It is suggested both that previous numbers of cereal phytoliths recovered from middens are relatively not as high as is suggested in Rosen’s report, and also that more recent interpretations on the region of cereal growing, based on the size of these phytoliths (Rosen and Roberts 2009), cannot be supported, as discussed in Chapter 5, section 5.1.1 and 5.4.9). Taphonomic and sample processing issues need to be considered more fully.

It would be expected that a slow build up of anthropogenic deposits would be represented by the presence of surface post depositional features within the micro units. Studies of middens at other sites have shown the presence of pedofeatures and wind blown deposits as potential indictors of surface pedogensis, though such features could also be the results of diagenesis within the midden. Even wind blown layers may not indicate a significant period of a lack of midden build up, as such features can be the result of short term events (Simpson and Barrett 1996). No such features were seen in the samples studied.

Midden accumulation rates Determining the time frame of a sequence of deposits is fundamental to interpreting human activity. One way of achieving this is by calculating an accumulation rate for a depositional sequence, through age measurements and deposit thickness measurements (Stein and Deo 2003), which can be used to estimate the quantitative rate of build up. We may estimate a relative deposition time frame through looking at the relative accumulation rate and micromorphology to look for evidence of periods of exposure such as water laid, aeolian deposited layers, or trampling. The lack of any clear naturally laid deposits in thin section suggests a rapid build up, or sheltered deposits. No macroscale evidence has been found of rainfall either (Freya Sadarangani pers. comm.), which is unusual considering the suggestion of a wet seasonal environment.

The dates for the entire Çatalhöyük sequence have recently been revised to take into account methodological improvements at the Oxford radiocarbon laboratory, so whilst the absolute dates for the sequence may be off by 100-300 years (Baylis and Farid 2007). Activities identified from thin section and phytolith analyses Activities identified This detailed analysis of midden deposits has revealed a number of activities at Çatalhöyük that have not previously been clearly identified. The scale of these activities in particular has implications for the social structure at Çatalhöyük and the use of space – it is suggested that midden areas must be considered simultaneously with buildings when assessing the use of space, as the middens are clearly repositories of residues from activity that may be linked to individual households or household areas.

An estimation of the absolute accumulation rate requires a carbon date and depth for at least 2 points within the sequence of interest (Stein and Deo 2003). The thickness in cm is then divided by the time in years. This method assumes a constant rate of build up, and there are problems linked with the dating of the deposit material rather than the actual age of deposition. Another problem is variable compression of the deposits. For such extensive deposits as the Çatalhöyük middens, an 108

Table 8.1: Summary of possible activity types expected and observed at Çatalhöyük, related micromorphological features, and deposit types identified in the samples studied which show these features. Activity

Frequency

Evidence (inclusion types)

Evidence (structure)

Deposit types

Specific examples

Significance

Limitations

Craft – pottery producti on

Cyclical

Midden 2, Midden 6

Evidence for pottery production technology and fuel use

Larger range of samples needed to determine scale and frequency across site

Cyclical

Craft – flints, jeweller y making

Cyclical

Micro artefacts, flake debris

Calcareous spherulites and reed phytoliths embedded in ash layers. Observation of phytoliths as they are preserved in situ, to see size and mode of deposition Concentrations of inclusions in specific layers

1a, 3

Craft – basketry , matting

Massive ash layers containing clay fragments, ash composition reeds with dung Layered articulated phytoliths

-

Not seen in these samples

Food preparat ion

Very frequent

Bone fragments, phytoliths from food plants e.g. cereals

-

Not seen in these samples

Food consum ption

Very frequent

Coprolites identified as human, containing phytoliths

Concentrations of artefacts in specific layers, associations of artefacts Embedded bone and phytolith fragments

Food feasting

Cyclical

Large quantities of animal bones with evidence of butchering and consumption

9

Hearth rake out

Frequent

Food waste disposal Fuel use low tempera ture Fuel use – high tempera ture Cleanin g of building s– sweepin g floors Buildin g construc tion and demoliti on Animal husband ry Redepo sition

Frequent

Mixed ash, charcoal layers, small burnt aggregates Amorphous organic material, bone fragments Mixed ash, charcoal layers Ash with charred flecks and charcoal

Association of animal bones with other material e.g. plant remains Mixed, unorientated inclusions. Embedded inclusions. Unorientated

4a, 2c, 1b, 3b, 3d, 3e

Other possible uses for fuel

Very frequent

2a/2b

One dimensional so difficult to say spatial extent of phytoliths

4c, 5

Evidence for craft activities at specific times of the year

Traces of these activities are likely to become embedded within the midden surface at their time of deposition, either the waste products of the production (smaller debris), or larger broken artefacts Limitation of sampling and sample size may miss artefact concentrations.

Evidence for diet on a short time scale. Implication for health, concepts of “clean”

Larger range of samples more closely linked to micromorphology samples, larger sample sizes for phytolith analysis

Midden 2

Large bone assemblages not seen in thin section.

Frequent, possibly daily activity Frequent cyclical activity

6a, 6b, 2c, 1b, 3c, 8b, 8c, 8d 5

Other possible uses for fuel

Cyclical?

Clean ash with no carbonised material, melted silica

Unorientated

4a, 3a

Use of fuel for specific activities

Frequent

Unburnt rounded aggregates

Mixed, unorientated inclusions.

8e

Small deposits, may not be visible in samples

Cyclical

Concentrations of large unburnt aggregates – bricks and mortar, redeposited midden material as packing

Distinct clusters, large layers at the macroscale

6a, 6c

Very frequent or frequent Cyclical

Animal dung, spherulites, phytoliths

Compacted layers, trampled surfaces Massive homogenous structure, unorientated, mixed

4b, 5

Frequency and extent of animal management, on site or off site

10

Middens as resources

Mixed fragments of charcoal, plaster, ash, organic material

109

Midden 6

Less frequent activity, possible cyclical period marker

Activities not identified

Analysis at the microscale is important as it increases the specificity of the time-signal of materials and it is sensitive enough to detect diverse traces of activity and behaviour (Monks 1981). It is important to recognise that studying deposits at a variety of scales is necessary to fully understand formation processes. Study and interpretation at the excavation or macroscale, is the first and most frequent level of interpretation. This is useful for looking at the overall structure of midden deposits, to understand the spatial extent of deposits and to relate the middens to adjacent features such as buildings. In particular where the units are more than a few cm thick this scale of analysis is useful. However, study at the macroscale does not allow us to observe the information that is present in the deposit boundaries, the precise depositional context of midden inclusions, nor individual depositional layers and inclusions that are too small to be fully resolved at the macroscale. Conversely, whilst study at the microscale gives us highly detailed information on the micromorphology of individual layers and inclusions, by itself it is only a snapshot of midden deposition, and does not provide information on the spatial differences or extent of the individual layers.

Activities not identified are crop processing, lithic crafts, storage and food preparation. Evidence from other studies has been found which indicates at least some of these activities were occurring, for example lithic crafts. Carter et al. (2006, 2007, 2008) have focused largely on obsidian, however large quantities of flint are also found which have not yet been studied in detail (Carter pers. comm.). Storage in the form of cereal bins with charred grains is seen in some of the buildings, and food preparation is seen by butchery marks on animal bones (Russell and Martin 2005), and the presence of clay balls for heating. Evidence for crop processing is less certain, and the phytolith evidence that it was hoped may be present in the phytolith remains (based on previous work indicating particular crop processing assemblages e.g. Harvey and Fuller 2005), was not seen in the samples studied. This could be either because crop processing was not occurring on site, or was occurring in a different part of the site, with waste not being deposited in the middens studied. Limitations are largely due to micromorphology viewing a one dimensional cut – lithics and animal bones for example are present in large quantities, just not in samples selected. This is a difficulty in integrating microscale and macroscale data. The spatial extent of fine layers was also difficult to observe in some cases. Although it was hoped to compare larger inclusions such as macrobotanical remains and bones with the microscale observations, this was not possible due to the different scales at which these materials are analysed. Future work needs to compare the nature of deposition of materials such as animal bones, macrobotanical remains and lithics, so that their relationship with other remains such as ash and coprolites can be better understood. By examining the nature of deposition of these materials, temporal variations in their deposition may be possible that would help resolve the problem of identifying “seasonal” deposits. One way forward would be microexcavation of selected blocks, c. 1m3 of deposits, and comparison of this data with associated thin sections and appropriate microanalyses.

The present research has addressed these issues by combining detailed micromorphological analysis of selected midden sections with information observed at the macroscale. This has been achieved through a sampling strategy (explained in Chapter 2) which can directly link results from several analytical methods, and relating microscale observations to what can be seen in the field. Previous analysis has been largely on bulk samples, and has been of a general, rather than targeted, nature. A previous study of discard and disposal practises through looking at the material assemblages of middens was based on field units (Yeomans 2005) – these units represent broad time periods, and so the information gained from studying the material at this scale only gives us general trends, rather than specific timescales. The study by Yeomans concludes that it is not possible to study the “real” individual units of the middens, as they are too fine to be excavated (Yeomans 2005). The present research has developed this, and shown that a combination of microtechniques is highly effective in studying the formation processes of middens and can be used to examine the individual layers. It is concluded that whilst both approaches have their merits and shortcomings, the microanalytical approach can provide detail at a level which is important in addressing issues such as seasonality, the traces of which occur over relatively short time scales and leave only microscopic traces.

Summary of midden formation processes and activities This research suggests that traditional micromorphological methods for describing and interpreting formation processes do not apply very well to middens. Descriptions focus on structure and orientation characteristics, which tend to be similar throughout midden deposits, as the majority of the material is dumped, and unorientated in the thicker layers, or linear and strongly oriented parallel in thinner layers, particularly of discarded fresh plant remains. Thus the focus on inclusions and deposit types based on these inclusions is proposed as a better way of describing midden deposits. Formation processes can be generally classed as massive dumping of mixed deposits, smaller dumps of a particular material, and in situ activity.

People and environment - Resource use, seasonality and cyclicity Environment In the ash deposits studied, there is no clear change in fuel use over time from the phytolith data. It is suggested that these need further comparison with earlier levels and integration with macrobotanical evidence in order to 110

fully understand the nature of plant resource exploitation, as neither approach is fully comprehensive by itself. Current macrobotanical research has no direct links with specific activities as it is based on flotation units rather than actual units of deposition, and phytolith analysis linked to specific activities misses information from the non-phytolith plant component of middens, particularly wood in the case of fuel, though thin section observations of wood charcoal in thin section indicate that such integration is possible.

full range of midden deposits and components. Components such as animal and bird bones are suggested as particularly useful as their smaller size is easier to link to specific units of deposition, and these also tend to be seasonally present species (O’Connor 1998, 2000). One way to approach this could be through detailed micro-excavation of a midden, as discussed earlier, and analysis of macrobotanical, faunal and lithic remains in as close as possible to their units of deposition, rather than the arbitrary excavation units currently used. Such approaches to analyse faunal material have been utilised in coastal middens, where fish remains have been used as precise seasonal indicators (Leacha 1979), although this study focused only on fish remains rather than integrating different data sets.

The large amount of Phragmites recovered does support the hypothesis of a local wetland environment (Roberts et al. 1999, Boyer et al. 2006) but other evidence such as the presence of bilobes, cereals and dryland weeds (Fairbairn et al. 2005) suggests a more complicated picture of the local environment, perhaps with interspersed drier areas. The observation of phytolith taphonomy in this research questions the hypothesis of dryland cereals on the basis of small multicell cereal size that is used to support the suggestion of cereals being grown many kilometres from the site (Rosen and Roberts 2009), as phytolith size is a result of many depositional and postdepositional factors as well as growing environment and water availability.

Identification of “seasonal” indicators in midden layers Although it was not possible to determine a strictly “seasonal” pattern of activities, cycles of activities were observed, and seasonal “marker” deposits also observed, as discussed in section 8.3.1. Linking this to the previous model of seasonality, shown in Figure 8.8, it could be suggested that specific phytolith and hackberry deposits represent “spring” deposits, whilst hackberry concentrations represent autumn deposits. Increased hearth rake out could be a winter signal (Matthews n.d. Table 8.2).

Seasonality and cyclicity of activities By characterising midden deposits this research has identified deposits relating to specific activities. The scale and frequency of these activities is identified by observing the deposits at the macroscale. An aim of thisresearch was to look for patterns in the frequency of the activities identified, and to investigate whether this could be linked to seasonal “marker” deposits such as crop processing remains, floral phytolith parts, fruit seeds or other remains such as eggshell etc, which are likely to occur only at certain times of the year, or predominately at certain times of the year.

Seasonal indicators include deposits from activities that are likely to have occurred at certain times of the year, such as crop processing after harvest, or from seasonally produced material, such as dendritic floral phytoliths, fresh fruit and egg shell. Environmental evidence from pollen and the KOPAL survey suggests that Çatalhöyük experienced significant seasonal changes in temperature and rainfall (Roberts et al. 1999, Boyer et al. 2000), which is likely to have impacted on resource availability at different times of the year, and thus the timing of subsistence activities (Fairbairn et al. 2005a). Micromorphological seasonal indicators include wind/water laid sediments relating to annual changes in climate and storm events and particular component assemblages which may relate to cyclical activities such as crafts and plastering (Table 8.2). further work examining more extensive sequences many find such naturally laid sediments.

Previous seasonality research at Çatalhöyük has tried to bring together evidence spanning more than 1000 years, from animal bones and plant use for example (Fairbairn et al. 2005a, Table 8.2, Figure 8.3), but without linking these components to their precise depositional context, determining seasonal patterns is difficult. Thisresearch has overcome some of the methodological problems in determining seasonal activities by examining a range of midden components in their precise depositional context. However there are still problems in linking these to a specifically seasonal timescale due to a lack of dates within individual middens on the necessary timescale, and difficulties in pinpointing “seasonal” indicators and deposits.

Hackberry pericarps in particular can be linked to autumn fruit production and seasonal feasting where they occur in concentrations. The presence of a high concentration of hackberries in a midden can link this deposit to a certain time of the year. Concentrations of hackberries can be seen at the macroscale (Figure 8.4), and in thin section. Phytolith analysis of a particularly rich hackberry coprolite deposit shows the phytoliths are also present. An interesting area of further study would be to plot the occurrence of hackberries throughout the middens to investigate patterns of associations with particular deposits. Macrobotanical analysis suggests that hackberries are ubiquitous at the site (Asouti et al. 1999),

In addition, other deposits which could help target “seasonal” deposits, such as egg shell, were not seen in the samples studied. This was discussed briefly in section 8.2.4.2, and it is suggested here that future seasonality studies need to combine the microanalytical approach used in thisresearch, with analysis of larger components in their precise depositional context, to understand the 111

Figure 8.3: A seasonal schedule of activities showing changing environmental conditions and suggested population conditions (Fairbairn et al. 2005a).

however analysis by floatation combines huge volumes of midden deposit, so there is no way of knowing the depositional pattern. This research suggests that hackberries are in fact found in high concentrations in specific locations within middens and can potentially be linked to particular times of the year.

where these phytoliths occur more frequently. Some examples which show an increase in dendritic types compared to the omnipresent smooth single cells are seen below. In the majority of samples the concentration of dendritic phytoliths is relatively low, much lower than the concentration of smooth cell phytoliths, as illustrated in Figure 8.5, which shows sequences of phytoliths where one sample in the set has an increase in dendritic types. Food processing is an important activity, however deposits that could be linked specifically to food processes were difficult to identify in the samples studied. There was no evidence of food processing residues, in the form of cereal chaff. This is unfortunate as this deposit could be linked specifically to harvesting and processing activities that would occur around May/June (Table 8.2). Although establishing a seasonal signal is problematic, cyclical patterns can be seen on a variety of scales, with important differences between the earlier and late levels of the site, as discussed below, as well as repeated patterns of deposit types within middens.

Figure 8.4: Midden 2 (South Area), hackberries in north face in fine layering above large ash layer.

Cycles in midden formation processes

In this research it was hypothesised that midden deposits might contain distinctly seasonal deposit types. This has been suggested in other studies with some deposits containing higher numbers of floral phytolith types than others (Rosen 2005). There are potential problems with the use of dendritic phytoliths as a seasonal indictor due to the problem of storage of cereals. However if cereals were being processed and used throughout the year then it would be expected to see a similar distribution of these types throughout the deposits studied. Analysis of the occurrence of dendritic phytoliths throughout all of the middens studied indicates that there are certain deposits

Cyclical patterns were investigated at the microscale by analysis of the periodicity and frequency of specific deposits, as discussed in section 8.2. These are presented in periodic graphs in Figure 8.6, with the x axis showing deposit types from Chapter 4. Plant rich deposits are to the left of the x axis, with aggregate rich deposits towards the right of the x axis, and large homogenous mixed deposits at the far right of the x axis. Sequences of complex fine layering from South Area midden 2 and 4040 area midden 6 are different – although there are

112

In the large in situ burning layers in Middens 2 and 6, the ash forms the fine material, with articulated phytolith fragments forming part of the coarse fabric, along with a number of small orange aggregate fragments. Some layers do show spherulites under XPL, though these are quite sparse, and the fuel appears to be predominantly plant in origin, with small amounts of mixed dung. However this could be due to spherulites “melting” at high temperatures above 750°C. These repeated layers are the strongest indicator of a repeated cyclical activity in the Çatalhöyük midden deposits. When comparing the thin sections back to the macroscale, it is suggested that these deposits are from a large scale outdoor burning activity, possibly firing pottery. The presence of burnt aggregate inclusions in 2 different parts of the site supports this. These agregates were identified in thin section by the presence of plant pseudomorphic voids, by FT-IR of their clay mineralogy, and GC-MS observations of plant sterols indicating possible plant temper residues.

repetitions of type 6 there is more variability in deposition. The TP samples show cycles of type 6 (aggregate rich deposits) interspersed with other types in the TP midden 7, and the relatively low frequency of fine layering (Figure 8.6 part a). Table 8.2: Expected seasonal indictors (W. Matthews n.d. after Fairbairn et al. 2005a and Hodder ed. 2005). Expected:

Sedimen t

Winter (~JanMar)

?snow cover

Spring (~AprJune)

Water laid

Summer (~JulySept)

Autumn (~Oct-Dec)

Wind blown; oven rake out from cooking on roof Wind and water laid

Animal/ plant remains Increased oven and hearth rake out; smashed marrow for grease extraction; dung in animal pens; green leaf phytoliths Grass flowers, pollen; green leaf phytoliths; eggshell, fish bone, neonate sheep and goats Little or no oven rake out; legumes and cereal wheat and barley husks Reed tubers, hackberry pericarps

Micro artefacts

Wall plasters

Craft debitage: obsidian and flint knapping ; beads; wood shavings; grind stone fragment s

Increased soot

Key macro remains Winterin g bird bone

Problems in determining seasonality In order to pinpoint an actual seasonal distribution of activities it has become clear that an accumulation rate should be calculated for the deposits under investigation, to estimate the timeframe over which they accumulated and thus establish if certain deposit types were occurring with more frequency at a particular time. In section 8.3.1.1 it was attempted to calculate an accumulation rate of middens using existing carbon dating sequences, but this was difficult due to the large range of the carbon dates. Using the available data the rate was calculated at approximately 1-3 cm yr -1.

Summer migrant bird bone

Animal butchery debris from kill off before winter

Also of note are the repeated cycles of in situ burning and massive ash layers, visible in Middens 2 (South Area) and 6 (4040 area), Level VI, and the lack of such deposits in both the earlier levels of Midden 1, Levels VIII-II (and previous studies of the Deep Sounding midden Space 181), and the later levels of Midden 7, Level III-0. Deposits in early Level XIII in the Deep Sounding have large scale lime burning deposits (Matthews 2005), though comparisons with the samples in this study suggest this is a different type of activity. The earlier middens studied (Midden 1 and Phase 1 of Midden 2, Levels VI/VII and VI respectively) are characterised by multiple fine lenses of charcoal rich deposits (Figure 8.6 part d and e). Although these deposits are also found in Middens 2 and 6 (early to mid levels, Levels VI and V), this fine layering is interspersed with the massive deposits from in situ activities, and in the case of Midden 6, massive demolition events which have produced a distinctive sequence of fine layering interspersed with massive aggregates, in which fine constructional layering can be seen. This contrasts with Midden 7 (latest levels of the site, III-0) which has much fewer sequences of fine layering, interspersed with massive redeposited material, with no evidence of in situ burning events.

Although establishing an accumulation rate for each midden is difficult, it was expected that patterns in deposition would be apparent. At Çatalhöyük the empirical evidence suggests refuse disposal was a well established community practice, with the activity of disposal in itself being a repeated and prevalent activity – the nature of the material being deposited however is likely to have varied throughout the year, and this is suggested by results from the fine layering in Middens 2 and 6 in particular. Resource use – fuel, fire and craft activity The activities identified contribute to the knowledge of resource use, fuel and fire at Çatalhöyük. The presence of microcharocal throughout the deposits supports the importance of fire previously suggested by Cessford and Near (2005). The ash deposits that indicate the craft activity of pottery production also give information on the nature of fuel use at Çatalhöyük. Previous studies of fuel use at Çatalhöyük have only considered information from macrobotanical data (e.g. Asouti 2005). Micromorphology and phytolith analysis of ash suggests a large volume of Phragmites reeds were used as fuel, as well as dung.

113

30000

Midden deposits are an important source of information of Neolithic resource use, particularly with regards to vegetation use for fuel and food. An aim of this research was to investigate alternative sources of information on fuel use which had not been previously considered in detail. The investigation of plant material in this research has complemented and enhanced the macrobotanical research carried out at Çatalhöyük (e.g. Asouti 2005, Asouti et al. 1999, Fairbairn et al. 2005b, Bogaard et al. 2008), by investigating in detail how the species and type plant material varies between microlayers, and also the depositional context and associations of the plant material, and how plants were being used for different activities. It is clear from the results that plant material was a major resource for a range of activities, including fuel as well as food consumption.

Long (smooth) Long (dendritic)

25000

n/gm

20000

15000

10000

5000

0 1668/02

1668/03

1668/07

1668 upper 1

1668 upper 2

1668 upper 3

Long cells (smooth) Long cells (dendritic)

60000

50000

Ash and the use of plant resources as fuel - contribution to questions of fuel use

n/gm

40000

30000

Ash deposits represent a significant proportion of midden deposit types, and there is evidence of large scale burning activities producing huge volumes of ash. Analysis of this material gives significant insight into the nature of fuel resource use at Çatalhöyük. Previous studies of plant use as fuel at Çatalhöyük and other Neolithic sites in the region such as Pınarbaşı have concentrated on the macro botanical evidence, and have revealed complex patterns of the use and exploitation of plant resources in the Konya plain during the Holocene, with shifts from the use of local wetland species to use of a wider area including oak, as discussed in Chapter 1, section 1.2.3 (Asouti 2005). The results of the present research clearly show that the burning of reed/grass material was an important fuel source in addition to wood and dung. This raises interesting questions relating to resource use at the site – the inhabitants were clearly making full use of the abundant marsh resources, perhaps an easier or more abundant source of fuel than trees?

20000

10000

0 12524 s15

12524 s16

12524 s17

12524 s18

12524 s19

450000 Long (smooth) Long (dendritic)

400000

350000

300000

250000

200000

150000

100000

n/gm

50000

0 1542

4477

13103 s21

13103 s33

13103 s34

12504 s16

12519 s9

Figure 8.5. Phytoliths are sometimes difficult to see in these thin sections due to their small size and transparency which means they are masked by other components, but they are remarkably well preserved. Detailed spot sampling of the blocks before resin impregnation has given information on the species present and their abundance in numbers per gram. The thin section analysis is essential to give these results context, as well as allowing us to view the degree of heating and articulation of the phytoliths – important information such as orientation and context is lost through analysis of spot samples alone, as the material is removed from its matrix and disaggregated. Spot phytolith analysis does not allow differentiation between phytoliths from mats, dung and plaster stabilisers for example. Micromorphology also enables analysis of articulated phytoliths (e.g. Figures 4.5 – 4.9) and in cases has enabled secure identification of plant species through study of the articulated multi cell form, in contrast to the often single cell phytoliths, or smaller multi cell fragments, in spot samples extracted and disarticulated during routine preparation processes.

The use of this plant in such large quantities suggests it was readily available and abundant, which is supported by paleoecological work at Çatalhöyük and the surrounding region, which suggests that the area was marshy and wet at the time of occupation. Phragmites today is often seen as a weed as it grows rapidly in marshy areas forming large dense reed beds from 2-4 m high. Macrobotanical studies at Çatalhöyük have analysed samples from a range of contexts, including middens, which are acknowledged as one of the richest contexts for plant remains (Asouti 2005). Whilst it is recognised that reed species such as Phragmites were present in large numbers due to the marshy environment surrounding the site, they are not considered in discussing plant resource use due to the poor preservation of these in the macrobotanical record. Wood charcoals from riverine species (Saliceae and Ulmus) in the local alluvial plane are the main assemblages studied which are suggested as fuels, with dryland fruits trees (e.g. Celtis) being suggested as firewood in smaller amounts. 114

firing. Research into pottery production is currently in progress at Çatalhöyük, but methods of production are currently uncertain (Akça et al. 2009). The research in thisresearch can contribute to this by resolving the problem of where pottery was being produced, and the study of burning temperatures achieved, as discussed in section 8.3.3.

Other species are suggested as building timbers (Quercus and Juniperus). Asouti’s suggestion that firewood collection was primarily from the local wetland environment would support the use of reeds as fuel in the earlier levels, identified in this study. It is suggested from the macrobotanical analysis that in later periods a greater catchment area for the collection of firewood was used. Considering the phytolith data, the abundance of Phragmites varies hugely between adjacent layers, so it is difficult to suggest such a general trend from this data. There is a possibility of a seasonal or annual scale pattern here which needs further exploration. A more detailed analysis targeting “fuel” deposit types across a range of levels would be needed, and is suggested as an area for further work. In either case, it can be seen that the high concentration of reeds and stems in the large ash deposits, as well as the identification of Phragmites, is something which needs to be considered alongside the plant macro remains when discussing the use of plants as fuel at Çatalhöyük. The assessment of the current data does not suggest any major differences in reed/grass ash between the earlier and later middens.

Origins of agriculture and diet By studying individual activities and their frequency in middens, this research has contributed evidence to debates on agricultural practises at Çatalhöyük. Examination of coprolites has added a new dimension to the study of diet. Phytolith evidence for cereal consumption in midden deposits The lack of cereal phytoliths and crop processing remains in the midden deposits studied supports the hypothesis that cereal production was not a major part of life at Çatalhöyük. Analysis of phytoliths from coprolites suggests the presence of a C4 food plant, although this is unidentified. There is some suggestion this could be millet (Setaria), described in Jenkins et al. (in press), but this is not seen in the macrobotanical remains.

Herbivore dung is suggested as a fuel through the occurrence of charred seeds in burnt dung fragments (Fairbairn et al. 2005) and spherulites in thin section (Matthews et al. 1996, 2005). This is a suggestion which is supported by the research presented here, which shows dung spherulites in situ in a large scale sequence of burning deposits in Midden 2 and 6, though the concentration of phytoliths may also have originated from a non dung source. Phytolith extraction from human coprolites has shown low numbers of poorly preserved phytoliths, though this would need to be tested for other species. Phytolith analysis of ash has shown a significant presence of tree phytoliths in addition to Phragmites. In addition to macrobotancial work on charred wood this suggests a mix of wood and reeds were used as fuel, perhaps for different activities.

This research has shown a dominance of reeds and wild grass species in midden deposits, with very few cereal husk phytoliths, and no evidence of crop processing activities, for example in the form of glumes, despite the extensive range of samples analysed. This contrasts with previous macrobotanical work at Çatalhöyük (Fairbain et al. 2002) which suggests a larger input of cereal remains, through the presence of charred grain and chaff. In an initial study 61 units were analysed by floatation, producing over 4000 litres of material (since this initial study thousands have now been analysed) – contexts including storage bins and middens have been found to contain seeds from a variety of Triticum species, with Triticum monoccoum and Triticum diccocum being classified as abundant/frequent based on these remains. It is suggested that the large size of the grains indicates favourable growing conditions, although this should also mean normal phytolith production. The charred plant data indicates that cereal grain and chaff were found in 83% of the samples studied from storage bins. Data from midden contexts suggests a considerably more variable abundance, ranging from 17 to 361 individual grains for glume wheat, with an average of 83 grains per sample, with individual samples averaging at 39 litres. This gives an average of 2 grains l-1.

The plant component of ash consists of a mix of microcrystalline calcium carbonate, elongates silica structures, vesicular glassy slag, and very fine crystalline material. Ash is formed when plants are burnt, with the organic components of the plant being released in gaseous form, leaving only the mineral component behind. This mineral component may be altered significantly during the burning process, for example silica in conjunction with alkaline salts may melt to form glassy slag (Canti 2003) Craft activity

There are number of possibilities here a) either the cereals being used were not producing many phytoliths (difficult to assess due to a lack of experimental data, but as phytoliths represent individual cells, we would assume that there would be at least thousands of phytoliths associated with an individual plant) b) cereals were not being used very frequently at all, or c) they were being processed off site. The charred macrobotanical data

Level VI is suggested as being a time of technical change according to lithic technology studies (Connolly 1999). Observation of lithics suggests a household focus to production in this period. The suggestion of outdoor activity areas, possibly for pottery firing, in this research, also represents a change in technology, from lightly fired clay material seen in earlier levels, to large scale open air 115

of faecal spherulites and internal structure (Canti 1999, Courty et al. 1989, Matthews 2005). However, distinguishing between species is very difficult, for example some coprolites are assumed to be dog on the basis of bone inclusions around 20-30 mm (Russell and Martin 2005), and some deposits assumed to be coprolites are actually clay or ochre.

indicates the presence of only dryland weeds in addition to the cereals, which could mean a reduction in phytolith production. Fairbain et al. (2005) suggest that the nearby environment was not being used for agriculture, but rather that the inhabitants of Çatalhöyük were managing and exploiting widely dispersed territories. Considering the macrobotanical and the phytolith data together, a better interpretation could be that the inhabitants were simply not exploiting cereals frequently, either from local or distant areas. In the charred assemblages wild tubers are abundant which also suggests a cultural reliance on the use of wild plants. it is suggested that cereals were just one of many plants exploited from a complex and diverse local environment.

In thin section analysis, where ruminant coprolites are presumed to be the darker brown coloured material with a layered structure and high phytolith content. This shows the importance of chemical analysis for the reliable interpretation of such deposits, and it is suggested that coprolite analysis would benefit from more experimental work to compare the residues, mineralogy and thin section appearance of faecal material from humans and a range of ruminant species.

Evidence for diet from coprolites Previous research on diet at Çatalhöyük has concentrated on inference through plant macro remains (Atalay and Hastorf 2005, 2006) and animal bones (Russell and Martin 2005), and isotopic analysis of skeletal remains (Richards et al. 2003, 2005). Coprolites have not previously been considered as potential sources of dietary information, though they are often used in other archaeological studies (Bryant and Dean 2005, Rhode 2003). Questions of diet have been explored through the analysis of residues and phytoliths in coprolites. The results from organic residue analysis indicate possible variations in the diet of individuals at Çatalhöyük due to different concentrations of sterol types, though further work would be needed to say with any certainty. This is compared and contrasted with the results obtained during this research from the analysis of phytolith assemblages from coprolites, and the evidence for diet obtained in previous research from organic residue analysis (Bull et al. 2005) This analysis is of importance, as the identification of the species from which the coprolites is derived has a significant impact on interpretation, for example, distinguishing between whether it is from human, pig or dog (Bull et al. 1999).

This orange coprolite type is suggested to be of omnivore origin, though the results of thisresearch indicate that the link between species and physical appearance may be more complicated. The orange coprolite types have been identified as largely human. For example Figure 8.2 shows a thin section from Midden 6 in the 4040 area alongside the results from residue analysis of an adjacent sample, the results showing faecal biomarkers suggesting human origin.

Coprolites have great potential as dietary indicators over short timescales, representing a snapshot of diet over only a few days. There is much potential for further work in this area, which is discussed at the end of this section. This discussion uses key results from this research to illustrate different sources of information that can be used to infer diet, including phytolith analysis from extracted coprolite samples, and phytoliths, bone and other inclusions seen in coprolites in thin section. This discussion is predicated on the initial identifications of these coprolites as human by GC-MS, as discussed in Chapter 7.

Figure 8.2: Possible activities at Çatalhöyük and how materials may be deposited within middens

Of the samples studied, there were very different relative concentrations of faecal biomarkers (see Chapter 7, Figure 7.5b). It is suggested that this could be a result of diet, for example human coprolites with increased ratios of plant based sterols could indicate a diet containing a larger amount of plant material. Again, experimental work on the relationship between diet, faecal biomarkers, and the effects of burial and degradation would be useful. From analysis of the samples in this study, there does seem to be an increase in the concentration of biomarkers extracted from the TP samples, Levels III-0, (1st residue

Organic residue analysis of coprolites Chemical residues have the potential to inform about diet as well as reliably identify species. This research has identified a large number of human coprolites as well as a possible ruminant sample. Coprolites in the field are currently identified by a distinct orange colour, and in thin section are identified through their colour, presence 116

surface texture that appear similar to hackberry phytoliths seen in reference photos (Pironon et al. 2001). These are the second most frequent phytolith type in this sample, occurring slightly less frequently than smooth long cells.

sample set) and some of the earlier samples from the South and 4040 Areas, Levels VI/VII (2nd sample set). By using organic residue analysis to target faecal material observed in microlayers, the problem of identifying species of faecal material in thin section has been largely overcome. Conversely, by using micromorphology we can see the context of the faecal material (seen in Figures 8.15 to 8.19, with further examples in Chapter 7, Figures 7.18 to 7.21), which gives much greater detail on the origin of the material, as well as allowing us to observe inclusions within the coprolite which may help interpret diet. This study has shown that the integration of thin section micromorphology when studying organic residues is invaluable in the interpretation of these deposits in middens, and has provided detailed evidence relating to the larger issues of diet at the site, and the use of resources through study of a) contents b) associations and c) depositional and post depositional changes.

Figure 8.7: Polyhedral phytolith in 1542.

The large extent of the deposits, the identification of human faecal material in large quantities, and proximity to human habitation raises important questions about human health, use of space, and perceptions of “clean” and “unclean” in the Neolithic. In addition, by identifying some deposits as containing no residues or non faecal residues, this research has contributed to the understanding of burials, providing evidence for the inclusion of plants in burials through the presence of plant sterols, as discussed in Chapter 7. Phytolith analysis of coprolites from spot sampling and thin section analysis Extraction of phytoliths from coprolites shows a dominance of stem and leaf phytoliths, these have a degraded appearance through digestion in the gut, and it could be that other phytolith types have not survived in the gut. It would be interesting to test pollen analysis of coprolites from Çatalhöyük. The lack of a high concentration of phytoliths (in most cases there were not enough to accurately quantify the number per gram), could suggest a lack of a large amount of plant material in the diet, or at least a lack of plant material that contains phytoliths, such as cereals. In thin section the herbivore coprolites contain a large percentage of phytoliths, which would be expected considering these animals ate a large amount of phytolith producing plants such as grasses and reeds (Matthews 2005). Orange types from Midden 2, suggested to be human, can also be seen to contain large embedded phytoliths (Figures 8.15 and 8.16).

Figure 8.9: An example of a cluster of hackberries in the field, Midden 2, South Area.

Figure 8.12: Husk and dendritic phytoliths from 4477, Midden 1, South Area.

Although it was sometimes difficult to obtain significant quantities of phytoliths from coprolites, some of the samples did yield high numbers, with interesting variations in the type and frequency of phytolith types. Particularly interesting are samples 1542, 4477, 12504 S15 and 12519 S9. Sample 1542 from Midden 1 in the South Area contains a large number of unusual polyhedral shaped phytoliths (Figures 8.7 and 8.8) with

This is particularly interesting as this phytolith is found in the fruit of Celtis. It has been suggested that this may have been stored, but it is also possibly that is was consumed as available – supported by micromorphological and macroscale in situ observations which show distinct clusters rather than general ubiquity.

117

longer be assumed that the presence of digested bone automatically means a dog or carnivore faecal source.

The sample block for these phytoliths showing a high concentration of hackberries can be seen in Chapter 4, Figure 4.18, and the appearance in the field can be seen in Figure 8.9. Sample 12504 S15 (Midden 2, South Area), although low in overall phytoliths, does have a relatively high concentration of bilobe phytoliths, which is unusual (Figure 8.13). Samples 12519 S9 (Midden 2, South Area) and 4477 (Midden 1, South Area) have higher concentrations of dendritic compared to smooth long cells, which could possibly be a seasonal indictor (Figure 8.14), particularly as 4477 is shown by GC-MS to contain mixture of human and ruminant faecal sterols, and bile acids indicate it is likely to be ruminant. 12519 S9 is associated with human faeces. Examples of husk and dendritic phytoliths extracted from 4477 are shown in Figures 8.11 and 8.12.

Figure 8.18: Bone fragment (b) embedded in coprolite sample 8932 S3/05, Midden 7, TP Area.

Figure 8.15: Coprolite with embedded phytoliths in sample 12558 S2, Midden 2, South Area. Figure 8.19: Phytoliths (a) and bone fragments (b) embedded in coprolite, sample 8932 S3/09, Midden 7, TP Area.

Methodological developments Screening of coprolites for GC-MS using FT-IR FT-IR has the potential to be a very useful technique in archaeology, particularly when integrated with other analyses. It is relatively quick and inexpensive, and can provide detailed information on the mineralogy of a range of archaeological materials. FT-IR was also used on the suspected coprolite samples that were selected for organic residue analysis. FT-IR studies have previously been carried out on coprolites from Brean Down, which indicate the presence of inorganic phosphate minerals (hydroxyapatite) (Allen et al. 2002). In this research similar results were obtained, with hydroxyapatite being present in many of the coprolite samples studied and identified using GC-MS, and confirmed by the presence of phosphorus in selected samples by SEM-EDX. This is a useful result and has enabled a distinction to be made between materials which may have a similar macroscopic appearance to coprolites but which may be composed of other material such as ochre. FT-IR therefore has potential to be used as an inexpensive and rapid

Figure 8.17: Bone fragment embedded in coprolite sample 12558 S2, Midden 2, South Area.

Dietary evidence from other inclusions in coprolites Large bone fragments can be seen in samples which are identified as human with residue analysis, for example 12558 S2 (Figure 8.17) and 8932 S3 (Figures 8.18 and 8.19). This has important implications for current work at the site which suggests large fragments of digested bone come from dog (Martin and Russell 2000). It can no

118



screening technique before subjecting samples to the more specific but much more expensive technique of GC-MS analysis.



The importance of specific context for phytolith analysis Phytolith analysis is a relatively new technique in archaeology compared to methods such as pollen analysis. There are major issues related to the taphonomy of phytoliths, and how the phytolith assemblage relates to the original plant assemblage. There are several methodological concerns that have been highlighted throughout this research, particularly the importance of examining the context of phytolith material as well as the assemblage of phytolith types, as this allows a better interpretation of the extracted phytolith assemblage, which in this research has been seen to be similar in different deposit types, seen in Chapter 5, section 5.4.3.

Initially it was hoped to analyse components in situ within the micromorphology slide, and to take small samples from individual layers within blocks for phytolith and organic residue analyses. A problem encountered is the difficulty in sampling very fine layers, and the ability to distinguish individual layers at the macroscale (particularly after oven drying when some of the distinctive colour differences loose their contrast). Although every care was taken to sample from individual layers, some of these were less than 1 mm thick, and in these cases it is not always possible to extract phytoliths because at least a few grams are needed for successful extraction.

Micromorphology and integrated microanalysis This research has highlighted the methodological benefits of combining thin section micromorphology with other analysis to fully characterise individual deposits and allow for a more robust interpretation, particularly in complex, finely layered deposits such as middens. In particular further chemical and phytolith analysis of targeted deposits such as coprolites has enabled a better understanding of both the depositional context and identification of these deposits which is difficult through micromorphology alone, for example as seen in Chapter 7, Figures 7.20 – 7.24. It is suggested that micro sub sampling of micromorphology blocks should be a routine part of micromorphological analysis, so that key features of interest observed under the optical microscope can be further analysed where necessary to identify key components. Where possible further analysis in situ should be conducted on uncoverslipped sections, to remove the possibility of contamination between microlayers – this is suggested as an important area for future research.

It is suggested here that a new method of phytolith extraction could be tested on small sample sizes – a relatively new microwave digestion technique has been developed which would make it much easier to extract phytoliths from smaller sample sizes (Parr 2002, Parr 2006). Also, by analysing thin sections first, phytolith analysis could be prioritised to layers of most interest, which would reduce time constraints of this techniques and the production of phytolith data which does not significantly add to thin section observations. The in situ analysis of samples by FT-IR has been more problematic. A major problem discovered during this research is that many of the components seen in thin section, for example individual phytolith cells, are too small to be analysed successfully with traditional FT-IR microscopy. The size of individual phytoliths is around 20 microns, which is also the limit of traditional FT-IR microscopy and means obtaining a spectrum on a particle this size is difficult. To try and overcome this problem, a number of pilot studies were conducted at the Daresbury laboratory, where the synchrotron radiation source allows analysis of much smaller samples. Whilst overcoming the size problem, the microscope at Daresbury did not allow a detailed visual resolution of the individual phytolith samples, and so targeting and identifying individual cells for infra red analysis was difficult. Hopefully this will be resolved in future studies at the new Diamond facility, which is currently developing its facilities for archaeological studies to include higher powered optical lenses.

Limitations and Future work Suggestions for future work have been given at appropriate points in the results chapters, and also in this discussion, these can be summarised as follows:    

Further integration of thin section micromorphology, microanalysis and other data, through microexcavation. Suggested improvements in phytolith analysis, including extraction methods for small sample sizes.

In situ analysis of micromorphology components by transmittance FT-IR using an IR transparent window. Calculation of accumulation rates using carbon dates associated with thin sections. Experimental heating of clay minerals and comparisons with micromorphological changes in thin section. SEM-EDX and SRS analysis of cereal phytoliths to investigate growing region through trace element inclusions.

The results of this preliminary work show much potential and further experiments in this area are suggested for future work. In particular it would be interesting to study phytoliths from non midden contexts and phytoliths from experimental plant growing, to see if there are differences that can be detected between phytoliths from different species, and under different growing conditions. Further work is also suggested on the burning of

119

anticipated that this research will lead to a greater understanding of formation processes of midden deposits, and the development of resource use proportions of plants that were being used.

phytoliths at different temperatures to examine changes in the infra red spectra which arise as a result of burning. This could be a useful method of identifying burnt phytoliths which have already been extracted (and thus the context as a fuel would be difficult to establish), and there is also potential for analysis of other burnt remains such as burnt bone. Further experimental work of controlled burning at a range of temperatures would provide a useful reference collection for these investigations.

An abundant phytolith type identified in this study has been the leaves and stems of reeds, identified as Phragmites communis. This identification is based on comparisons with reference material (Ollendorf et al. 1988) and discussions with a number of experts in Near Eastern phytolith research (Dr Arlene Rosen and Dr Emma Jenkins). The phytoliths are characterised by abundant stomata, keystone bulliforms and saddles, and a husk-like wave pattern in the stems. It has also been concluded that stacked bulliform cells are likely to have originated from this species. A major distinction between the two species is the presence of bilobate short cells in Arundo donax, whereas studies of Phragmites show it to contain only saddles and tower shaped rondels (Ollendorf et al. 1988).

The technique of FT-IR in this research therefore has been largely supplementary, but has the potential to be developed further, for example at the new Diamond facility, where a combination of high magnification microscope objectives and synchrotron radiation source FT-IR has high potential for the analysis of microscopic material in situ. Although it was hoped to use organic residue analysis to give a more detailed characterisation of the different coprolite morphologies in thin section, type 2 (assumed to be herbivore) was absent for the residue sample set. This is due to a difficulty in identifying this deposit type at the macroscale, as the colour and morphology make it difficult to distinguish within the midden layers, compared to the orange type which has a sharp contrast. With an increased number of samples, this could be overcome in future work through detailed analysis of the thin sections and selection of bulk samples to test for residues, and the study of further comparable samples from animal pens (Bull et al. 2006). It is suggested that in midden deposits this type exists largely as partially or fully burnt deposits due to the use of dung as fuel, which would not contain organic residues.

Some confusion seems to be over the classification of different grass families, for example Phragmites is identified as a C3-Arundinoideae species that produces Chloridoideae types, and Sporobolus, a C4Chloridoideae grass, produces Pooid type short cells. It seems here that the problem is that rondels, saddles and bilobes are not actually specific to each grass subfamily and so cannot be used by themselves to infer environmental conditions. There is confusion also that all three used to be classified as Pooids, which was later split into 3 sub families (Barboni et al. 1999). CONCLUSIONS During this research an integrated methodology has been developed to investigate finely layered midden deposits, with the aim being to understand the individual activities producing these deposits, and possible cyclical or seasonal patterns in human activity (Shillito 2008). This methodology included thin section micromorphology, which has become increasingly important in the study of complex tell deposits, combined with phytolith and chemical analyses to understand the changing nature of plant resource use and diet.

An interesting and very useful further study which was unfortunately not considered during the sampling strategy would be to collect datable material at regular intervals throughout the midden sequences, to compare the accumulation rates of the middens, and within middens between the fine layers and massive depositional events. The variations in accumulation rate between the earliest and latest middens would be particularly interesting. Although a relative rate can be estimated from the thin section micromorphology, an absolute scale cannot be determined without fixed dating points. This would be very useful for pinning down seasonal deposition, and estimating the frequency at which different activities occurred.

Major aims of this research were to examine individual midden deposits and link them to specific human activities which are absent in other contexts at Çatalhöyük, and to look for cyclical/seasonal patterns in deposition and human activity at a range of spatial and temporal scales. Investigation of seasonality is possible through looking at the frequency of specifically “seasonal” indicators such as food processing residues, food remains which are not storable (for example fruits, leaves), wind/water laid sediments relating to annual changes in climate and storm events, and particular component assemblages which may relate to cyclical activities, such as crafts. As well as characterising the sequences of deposits, another aim was to examine components such as ash and coprolites, to elucidate the

Analysis of micro artefacts such as phytoliths is problematic for several reasons. Although it is accepted practise to count c. 300 individual phytoliths (Piperno 2006), it is important to realise that a single plant may contain several thousand phytoliths, and examining only a few samples may not give an accurate general picture. Midden deposits have provided information on the nature of plant resource use at Çatalhöyük, showing a surprisingly limited use of cereals. Results indicate possible cyclical patterns in deposition, but the sample set means this needs to be investigated further. It is 120

of current research at Çatalhöyük (Fairbairn et al. 2005a; Rosen and Roberts 2005), and thisresearch contributes to this by identifying possible seasonal markers in middens, such as concentrations of dendritic phytoliths in specific deposits, and clusters of hackberry pericarps.

changing nature of plant resource use and diet at Çatalhöyük. Analytical developments include the use of FT-IR in characterising midden components (Shillito et al. 2009a, 2009b), which in turn has aided in the understanding of midden formation processes, and the human activities involved in this. The study of midden formation process in particular is important, as middens are a rich source of information, containing a wide range of important deposits relating to activities such as food processing, cooking, diet and discard.

Debates over the use of dung versus wood for fuel are part of the issue of changing resource use – previous studies at Çatalhöyük have focused on the plant macro remains in investigating this issue, and suggest that wood was the major fuel source (Asouti 2005). By studying the context of fuel through micromorphology, and analysing phytoliths from ash deposits, the research in thisresearch has shown a mix of dung and wood ash, along with a significant proportion of reed ash in massive ash layers at Çatalhöyük. This shows that the consideration of microremains is essential in addition to macrobotanical analysis, which misses this information.

Traditionally, the study of middens has focused on the analysis of excavation units and material from flotation, which may mix several depositional units, and destroys the depositional context and associations of midden material (Russell and Martin 2005; Yeomans 2005). In addition, research has been focused on charred plant remains, bones and macro artefacts (Fairbairn, Asouti et al. 2002; Asouti and Austin 2005; Russell and Martin 2005), with little consideration of other important data sources i.e. the sediments themselves, as well as microremains such as phytoliths and coprolites. When the micro-remains are considered, they have been analysed out of context (Madella 2001; Rosen 2005). The context and associations of midden components are essential sources of information, as they enable the identification of exactly how the components were discarded as well as their covariance and context, which are fundamental to the investigation of different activities.

The key findings of this research can be summarised as follows:

Current research at Çatalhöyük debates the importance of cereals as a food source, and the region in which these may have been grown (Rosen and Roberts 2005). By studying phytolith deposits from middens, this research has shown a distinct lack of cereal phytoliths, particularly the analysis of phytoliths from coprolites i.e. direct rather than inferred evidence of plant consumption, which suggests that the idea of Çatalhöyük being a centre of agriculture needs to be reconsidered. Although the Neolithic of Turkey is traditionally considered a period when communities became more reliant on agriculture, isotope and tooth wear research at Çatalhöyük, whilst suggesting a plant based diet, does not support the assumption that cereals played an important role (Richards and Pearson 2005). Thisresearch contributes to the question of diet in using a dual approach – firstly through examining food processing, preparation and cooking residues from middens, and secondly by directly examining plant indicators of diet through extraction of phytoliths from coprolites, in conjunction with analysis of organic residues from coprolites. Key findings include the presence of human faecal material in large quantities in the middens at Çatalhöyük, which has implications for both diet and health. Seasonality of site occupation is an important issue as it gives information on the nature of early settlements and has implications for the timing of sedentary as opposed to nomadic settlement, or in some cases, permanent versus temporary settlement. Seasonality is a main focus 121



Methodological developments highlighting the feasibility and importance of an interdisciplinary approach to the study of midden formation processes from the macro to micro scale, by linking microscopic and chemical analyses to field analyses, and linking micromorphology deposit types with phytolith data from spot sample analysis.



Methodological developments highlighting the range of uses for chemical analyses such as FTIR and GC-MS, and the importance of using these in conjunction with contextual analyses for accurate interpretation.



Complexity of midden formation processes - the integrated micro analyses in this study have contributed considerably towards our understanding of complex midden formation at Çatalhöyük, the range of activities that these represent, and the use of middens for a variety of purposes including large scale in situ burning events such as pottery firing.



Periodicity, seasonality and cyclicity – analysis of formation processes has shown that there are cyclical patterns in deposit types on a variety of scales which vary spatially and temporally.



Plant resource use – this research suggests a lack of reliance of Çatalhöyük inhabitants on domesticated resources for food, or a greater diversity that puts an equal importance on the use of wild resources.



Integrated analysis of coprolites shows variation in inclusions which may be linked to dietary differences.

Atalay, S and Hastorf, C. (2006) Food, Meals, and Daily Activities: The Habitus of Food Practices at Neolithic, Çatalhöyük. American Antiquity 71(2): 283-319. Bailey, G. N. (1975) The role of molluscs in coastal economies: The results of midden analysis in Australia. Journal of Archaeological Science 2(1): 45 - 62. Baird, D. (2005) The History of Settlement and Social Landscapes in the early Holocene in the Çatalhöyük area. Çatalhöyük perspectives: reports from the 1995-1999 seasons. I. Hodder (ed) Cambridge, McDonald Institute for Archaeological Research and the British Institute at Ankara. Balter, M. (1998) Why settle down? The mystery of communities. Science 282(5393): 1442-1445. Barboni, D., Bonnefille, R., Alexandre, A. and Meunier, J. D. (1999) Phytoliths as paleoenvironmental indictors, West Side Middle Awash Valley, Ethiopia. Paleogeography, Paleoclimatology, Paleoecology 152 (1-2): 87-100. Barker, G. (2006) The Agricultural Revolution in Prehistory: Why did Foragers become Farmers? Oxford: Oxford University Press Bayliss, A. and Farid, S. (2007) Re-assessment of the existing dating of the East Mound – a progress report Çatalhöyük Archive Report. Benning, L. G., Phoenix, V. R, Yee, N and Tobin, M. J. (2004). "Molecular characterization of cyanobacterial silicification using synchrotron infra red microscopy." Geochimica et Cosmochimica Acta 68(4): 729-741. Berg, J. M., Tymoczko, J. L. and Stryer, L. (2006). Biochemistry, W. H. Freeman. Berna, F., Behar, A., Shahack-Gross, R., Berg, J., Boaretto, E., Gilboa, A., Sharon, I., Shalev, S., Shilstein, S., Yahalom-Mack, N, Zorn, J. R. and Weiner, S. (2007) Sediments exposed to high temperatures: reconstructing pyrotechnological processes in Late Bronze and Iron Age Strata at Tel Dor (Israel). Journal of Archaeological Science 34: 358-373. Berstan, R., Dudd, S. N., Copley, M. S., Morgan, E. D., Quye, A. and Evershed, R. P. (2004) Characterisation of “bog butter” using a combination of molecular and isotopic techniques. Analyst 129 (3): 270-5. Bethell, P. H., Goad L. J., Evershed R. P. and Ottaway J. (1994) The study of molecular markers of human activity: the use of coprostanol in the soil as an indicator of human faecal material. Journal of Archaeological Science 21: 619-632. Binford, M., A. Kolata, Brenner, M, Janusek, J. W, Seddon, M. T, Abbott, M and Curtis, J. H. (1997) Climate variation and the rise and fall of an Andean civilization. Quaternary Research 47(2): 235-248. Björkhem, I. and Gustafsson J. A. (1971) Mechanism of microbial transformation of cholesterol to coprostanol. European Journal of Biochemistry 21: 428– 432. Boardman, S. and Jones G. (1990) Experiments on the effects of charring on cereal plant components. Journal of Archaeological Science 17: 1–11. Bogaard, A., Charles, M., Ergun, M., Jones, G., Ng, K., Polcyn, M. and Stone, N. (2005). Macro botanical remains. Çatalhöyük Archive Report. Bogaard, A., Charles, M., Ergun, M., Ertuğ, F. and Fillipović, D. (2008) Macrobotanical remains 2008 Çatalhöyük Archive Report 139-146 Bogucki, P. I. (1984) Ceramic sieves of the Linear Pottery Culture and their economic implications, Oxford Journal of Archaeology 3 (1), pp. 15–30. Bondzynski, S. and Humnicki, V. (1896) Ueber das Schicksal des Cholesterins im thierischen Organismus. Zeitschrift für Physiologische Chemie 22: 396-410. Boyer, P., Roberts, N. and Baird, D. (2006) Holocene environment and settlement on the Çarsamba alluvial fan, south-central Turkey: integrating geoarchaeology and archaeological field survey. Geoarchaeology: An International Journal 21(7): 675-698. Bowdery, D., Hart, D. M., Lentfr, C. and Wallis, L. A. (2001). A Universal Phytolith Key. Phytoliths: Applications in Earth Science and Human History. J. D. Meunier and F. Colin (eds) Rotterdam, Balkema 267-278. Bozarth, S. R. and Guderjan T. H. (2004) Biosilicate analysis of residue in Maya dedicatory cache vessels from Blue Creek, Belize. Journal of Archaeological Science 31: 205-215. Bremond, L., Alexandre, A., Wooller, M. J., Hély, C., Williamson, D., Schäfer, P. A., Majule, A. and Guiot, J. (2008) Phytolith indices as proxies of grass subfamilies on East African tropical mountains. Global and Planetary Change 61 (3-4): 209-224.

References

Akça, E., Kapur, S., Özdöl, S., Hodder, I., Poblome, J., Arocena, J., Kelling, G. and Bedestenci, Ç. (2009) Clues of production for the Neolithic Çatalhöyük (central Anatolia) pottery. Scientific Research and Essay 4 (6): 612-625 Akeret, O. and Rentzel, P. (2001) Micromorphology and plant macrofossil analysis of cattle dung from the Neolithic lake shore settlement of Arbon Bleiche 3. Geoarchaeology: An International Journal 16: 687 700. Albert, R. M., Weiner, S., Bar-Yosef, O., and Meignen, L. (2000) Phytoliths in the Middle Palaeolithic Deposits of Kebara Cave, Mt Carmel, Israel: Study of the Plant Materials used for Fuel and Other Purposes. Journal of Archaeological Science 27 (10): 931-947 Albert, R. W. and Weiner, S. (2001) Study of phytoliths in prehistoric ash layers using a quantitative approach. Phytoliths, Applictions in Earth Science and Human History. J. D. Meunier and F. Colin, Balkema Publishers 251-266. Albert, R., Bar-Yosef, O., Meignen, L., and Weiner, S. (2003) Quantitative Phytolith Study of Hearths from the Natufian and Middle Paleolithic Levels of Hayonim Cave (Galilee, Israel). Journal of Archaeological Science 30: 461-480. Albert, R. M., Bamford, M. K., and Cabanes, D. (2006) Taphonomy of phytoliths and macroplants in different soils from Olduvai Gorge (Tanzania) and the application to Plio-Pleistocene palaeoanthropological samples. Quaternary International 148(1): 7894. Albert, R. M, Shahack-Gross, R., Cabanes, D., Gilboa, A., Lev-Yadun, S., Portillo, M., Sharon, I., Boaretto, E., Weiner, S. (2008) Phytolith rich layers from the Late Bronze and Iron Ages at Tel Dor (Israel): mode of formation and archaeological significance. Journal of Archaeological Science 35:57-75 Albert, R. M. and Weiner, S. (2001) Study of phytoliths in prehistoric ash layers using a quantitative approach in Meunier, J.D, Colin, F and Faure Denard, L (eds) Phytoliths: Applications in Earth Sicence and Human History Aix en Provence: CEREGE 251-66 Allen, S. D. M., Almond, M. J., Bell, M. G., Hollins, P., Sonja, M. and Mortimore, J. L. (2002) Infrared Spectroscopy of the mineralogy of coprolites from Brean Down: evidence of past human activities and animal husbandry. Spectrochimica Acta Part A 58: 959-965. Ambrose, S. H. and Norr, L. (1993) Experimental evidence for the relationship of the carbon isotope ratios of whole diet and dietary protein to those of bone collagen and carbonate. In: Lambert JB and Grupe G, editors. Prehistoric human bone: archaeology at the molecular level. Berlin: Springer. 1–37 Amit, R. and Yaalon, D. H (1996) The micromprohlogy of gypsum and halite in reg soils – the Negev Desert, Israel Earth Surface Processes and Landforms 21: 1127-1143. Anderson, S. E. and Ertug-Yaras, F. (1998) Fuel, fodder, and faeces: an ethnographic and botanical study of dung fuel use in Central Anatolia. Environmental Archaeology 1: 99–110. Arpin, T. L., Mallol, C. and Goldberg, P. (2002) Short Contribution: A New Method of Analyzing and Documenting Micromorphological Thin Sections Using Flatbed Scanners: Applications in Geoarchaeological Studies. Geoarchaeology: An International Journal 17(3): 305-313. Asouti, E., Erkal, A., Fairbairn, A., Hadtorf, C., Kennedy, A., Near, J. and Rosen, A. M. (1999) Archaeobotany and Related Plant Studies. Çatalhöyük Archive Report. Asouti, E. (2005) Woodland vegetation and the exploitation of fuel and timber at Neolithic Çatalhöyük: Report on the wood charcoal macro remains. Inhabiting Çatalhöyük: Reports from the 1995-1999 seasons. I. Hodder (ed) London, McDonald Institute for Archaeology/British Institute of Archaeology at Ankara. Asouti, E. and Hather, J. (2001) Charcoal analysis and the reconstruction of ancient woodland vegetation in the Konya basin, south-central Anatolia, Turkey: results from the Neolithic site of Çatalhöyük East Vegetation History and Archaeobotany 10:23-32 Asouti, E. and Austin, P. (2005) Reconstructing woodland vegetation and its exploitation by past societies, based on the analysis and interpretation of archaeological wood charcoal macro-remains. Environmental Archaeology 10(1): 1-18. Atalay, S. and Hastorf, C. A. (2005). Foodways at Çatalhöyük. Çatalhöyük perspectives: reports from the 1995-1999 seasons. I. Hodder (ed) Cambridge, McDonald Institute for Archaeological Research and the British Institute at Ankara.

122

Brochier, J.-L, Jacques E., Villa, P. and Giacomarra, M. (1992) Shepherds and Sediments: geo-ethnoarchaeology of pastoral sites. Journal of Anthropological Archaeology 11`: 47-102. Bronk Ramsey, C., Higham, T., Bowles, A., and Hedges, R. E. M. 2004 Improvements to the pre-treatment of bone at Oxford Radiocarbon, 46, 155-63. Brown, T. (1997) Clearances and Clearings: Deforestation in Mesolithic/Neolithic Britain. Oxford Journal of Archeology 16(2): 133-146. Bryant, V. M and Dean, G. W. (2006) Archaeological coprolite science: The legacy of Eric O. Callen (1912-1970) Palaeogeography, Palaeoclimatology, Palaeoecology 237 (1): 51-66. Budd, D. A. (1988) Aragonite-to-calcite transformation during freshwater diagenesis of carbonates - Insights from pore-water chemistry. Geological Society of America Bulletin 100(8): 1260. Bull, I. D., van Bergen, P. F., Poulton, P. R. and Evershed, R. P. (1998) Organic geochemical studies of soils from the Rothamsted Classical Experiments-II, Soils from the Hoosfield Spring Barley Experiment treated with different quantities of manure. Organic Geochemistry 28: 11-26. Bull, I. D., Simpson, I. A., van Bergen, P. F. and Evershed, R. P. (1999) Muck ‘n’ molecules: organic geochemical methods for detecting ancient manuring. Antiquity 73: 86-96. Bull, I. D., van Bergen, P. F., Nott, C. J., Poulton, P. R. and Evershed, R. P. (2000) Organic geochemical studies of soils from the Rothamsted Classical Experiments-V. The fate of lipids in different long-term experiments. Organic Geochemistry 31: 389408. Bull, I.D., Lockheart, M.J., Elhmmali, M.M., Roberts, D.J. and Evershed R.P. (2002) The origin of faeces by means of biomarker detection. Environment International 27(8): 647-654. Bull, I. D., Elhmmali, M., Roberts, D. J. and Evershed, R. P (2003) The application of steroidal biomarkers to track the abandonment of a Roman wastewater course at the Agora (Athens, Greece). Archaeometry 45(1): 149-161. Bull, I. D., Elhmmali, M. M., Perret, P., Matthews, W., Roberts, D. J. and Evershed, R. P. (2006) Biomarker evidence of faecal deposition in archaeological sediments at Çatalhöyük, Turkey. Inhabiting Çatalhöyük: Reports from the 1995-1999 seasons. I. Hodder (ed) London, McDonald Institute for Archaeology/British Institute of Archaeology at Ankara. Bullock, P, Federoff N., Jongerius, A., Stoops, G. and Tursina, T. (eds). (1985). Handbook for thin section description. WAINE Research Publications. Albrighton, Wolverhampton, U.K. Canti, M. G. (1997) An investigation into microscopic calcareous spherulites from herbivore dungs. Journal of Archaeological Science 24: 219-231. Canti, M. G. (1998) The Micromorphological idenitification of faecal spherulites from archaeological and modern materials. Journal of Archaeological Science 25: 435-444. Canti, M. G. (1999) The Production and Preservation af faecal Spherulites: Animals, Environment and Taphonomy. Journal of Archaeological Science 26: 251-258. Canti, M. G. (2003) Aspects of the chemical and microscopic characteristics of plant ashes found in archaeological soils. CATENA 54(3): 339-361. Canti, M. G. and Linford, N. (2001a) Geophysical evidence for fires in antiquity: preliminary results from an experimental study. Archaeological Prospection 8: 211-225. Canti, M. G. and Linford, N. (2001b) The effects of fire on archaeological soils and sediments: temperature and colour relationships. Proceedings of the Prehistoric Society 66: 385-395. Carter, T., Poupeau, G., Bressy, C. and Pearce N. J.G. (2006) A new programme of obsidian characterization at Çatalhöyük, Turkey. Journal of Archaeological Science 33 (7): 893-909. Carter, T., Dubernet, S., King, R., le Bourdonnec, F-X., Milić, M., Poupeau, G. and Steven Shackley, M. (2008) Eastern Anatolian obsidians at Çatalhöyük and the reconfiguration of regional interaction in the early ceramic Neolithic Antiquity 82: 900-909. Carter, T. and Shackley, M. S. (2007) Sourcing obsidian from Neolithic Çatalhöyük (Turkey) using energy dispersive x-ray fluorescence Archaeometry 49 (3): 437-454. Carnelli, A. L., Madella, M., Theurillat, J-P. and Ammann, B. (2002) Aluminium in the opal silica reticule of phytoliths: a new tool in paleoecological studies. American Journal of Botany 89(2): 346351.

Casadio, F. and Toniolo, L. (2001) The analysis of polychrome works of art: 40 years of infra red spectroscopic investigations. Journal of cultural heritage 2: 71-78. Cessford, C. (2001) A new dating sequence for Çatalhöyük. Antiquity 75: 717-725. Cessford, C., Blumbach, M., Akoglu, G., Higham, T., Kunihom, P. I., Manning, S. W., Newton, M. W., Ozbakan, M. and Ozer, A. M. (2005). Absolute Dating at Çatalhöyük. Changing Materialities at Çatalhöyük: Reports from the 1995 - 1999 Seasons. I. Hodder (ed) Cambridge, McDonald Institute for Archaeological Research and the British Institute of Archaeology at Ankara. Cessford, C. & Near, J. (2005) Fire, Burning and Pyrotechnology at Çatalhöyük in Çatalhöyük perspectives: themes from the 1995-9 seasons, Ian Hodder (ed) Cambridge, McDonald Institute Monographs/British Institute of Archaeology at Ankara Chester, R. and Elderfield, H. (1968) The infrared determination of opal in siliceous deep-sea sediments. Geochimica et Cosmochimica Acta 32(10): 1128-1140. Charrié-Duhaut, A., Connan, J., Rouquette, N., Adam, P., Barbotin, C., de Rozières, M-F., Tchapla, A., and Albrecht, P. (2007) The canopic jars of Ramses II: real use revealed by molecular study of organic residues Journal of Archaeological Science 34 (6): 957967. Charters, S., Evershed, R. P., Quye, A., Blinkhorn, P. W. and Denham, V. (1997) Simulation experiments for determining the use of ancient pottery vessels: the behaviour of epicuticular leaf wax during boiling of a leafy vegetable. Journal of Archaeological Science 24: 1-7 Christie, W. W. (2003) Lipid analysis : isolation, separation, identification and structural analysis of lipids. Bridgwater, The Oily Press. Childe, V. G. (1926) The most ancient East. London, Routledge and Kegan Paul. Ciochon, R. L., Piperno, D. R. and Thompson, R. G. (1990) Opal phytoliths found on the teeth of the extinct ape Gigantopithecus blacki: Implications for paleodietary studies. Proceedings of the National Academy of Science 87: 8120-8124. Claassen, C. (1998) Shells. Cambridge, Cambridge University Press. Connan, J., Evershed, R. P., Biek, L., and Eglinton, G. (1999) Use and trade of bitumen and antiquity and prehistory: molecular archaeology reveals secrets of past civilisations Philosophical Transactions: Biological Sciences 354 (1379): 33-50. Connan, J., Lombard, P., Killick, R., Højlund, F., Salles, J-F. and Khalaf, A. (1998) The archaeological bitumens of Bahrain for the early Dilmun period (c.2200 BC) to the sixteenth century AD: a problem of sources and trade Arabian archaeology and epigraphy 9:141-181. Connan, J. and Carter, R. (2007) A geochemical study of bituminous mixtures from Failaka and Umm an-Namel (Kuwait), from the Early Dilmun to the Early Islamic period Arabian archaeology and epigraphy 18 (2): 139-181. Conolly, J. (1999) Technical strategies and technical change at Neolithic Çatalhöyük, Turkey Antiquity 73: 791-800 Copley, M. S., Berstan, R., Dudd, S. N., Docherty, G., Mukherjee, A. J., Straker, V., Payne, S. and Evershed, R. P. (2003) Direct chemical evidence for widespread dairying in prehistoric Britain. Proceedings of the National Academy of Sciences 100 (4): 1524– 1529. Copley, M. S., Berstan, R., Dudd, S., Straker, V., Payne, S. and Evershed R. P. (2005a) Dairying in Antiquity: I - Evidence from absorbed lipid residues dating to the British Iron Age. Journal of Archaeological Science 32: 485-503. Copley, M. S., Berstan, R., Dudd, S, Straker, V., Payne, S. and Evershed R. P. (2005b) Dairying in Antiquity: II - Evidence from absorbed lipid residues dating to the British Neolithic. Journal of Archaeological Science 32: 523-526. Copley, M. S., Berstan, R., Dudd, S., Straker, V., Payne, S. and Evershed R. P. (2005c) Dairying in Antiquity: III - Evidence from absorbed lipid residues dating to the British Bronze Age. Journal of Archaeological Science 32: 505-521. Corr, L. T., Sealy, J. C., Horton, M. C. and Evershed, R. P. (2005) A novel marine dietary indicator utilising compound-specific bone collagen amino acid δ13C values of ancient humans. Journal of Archaeological Science 32(3): 321-330. Courty, M. A., Goldberg, P. and Macphail, R. (1989) Soils and Micromorphology in Archaeology. Cambridge, Cambridge University Press.

123

Cremeens, D. L. (2005) Micromorphology of Cotiga Mound, West Virginia. Geoarchaeology: An International Journal 20(6): 581597. Crowther, J. (2002) The Experimental Earthwork at Wareham, Dorset after 33 Years: Retention and Leaching of Phosphate Released in the Decomposition of Buried Bone. Journal of Archaeological Science 29 (4): 405-411. Czerniak, L. and Marciniak, A. (2004) Excavations of the TP Area. Çatalhöyük Archive Report. Dabai, F. D., Walker, A. F., Sambrook, I. E., Welch, V. and Owen, R. W. (1996) Comparative effects on blood lipids and faecal steroids of five legume species incorporated into a semi purified, hypercholesterolaemic rat diet. British Journal of Nutrition 75: 557-571. Davidson, D. A. (1976) Processes of Tell Formation and Erosion. Geoarchaeology: Earth Science and the Past. D. A. Davidson and M. L. Shackley (eds) London, Duckworth: 255-266. Davis, S. J. M. (1987) The Archaeology of Animals. Routledge Davidson, S. and Carter, S. P. (1998) Micromorphological Evidence of Past Agricultural Practices in Cultivated Soils: The Impact of a Traditional Agricultural System on Soils in Papa Stour, Shetland. Journal of Archaeological Science 25 (9): 827-838. Delhon, C., A. Alexandre, Berger, J-F., Thiebault, S., Brochier, J-L. and Meunier, J-D. (2003) Phytolith assemblages as a promising tool for reconstructing Mediterranean Holocene vegetation. Quaternary Research 59: 48-60. Driessen, P. M. and de Meester, T. (1969) Soils of the Cumra Area, Turkey. Agricultural Research Reports. Wageningen, Agricultural University, the Netherlands, Department of Tropical Soil Science. Drum, R. W. (1968) Electron microscopy of opaline phytoliths in Phragmites and other Graminae. American Journal of Botany 55: 713. Dudd, S. N. and Evershed, R. P. (1998) Direct Demonstration of Milk as an Element of Archaeological Economies. Science 282 (5393): 1478 – 1481. Dudd, S. N., Evershed R. P. and Gibson, A. M. (1999) Evidence for varying patterns of exploitation of animal products in different prehistoric pottery traditions based on lipids preserved in surface and absorbed residues. Journal of Archaeological Science 26: 1473-1482. Dutka, B. and Elshaarawi, A. (1975) Relationship between various bacterial populations and coprostanol and cholesterol. Canadian Journal of Microbiology 21: 1386– 98. Eastwood, W. J., Roberts D. J. and Boyer, P. (2006). Pollen analysis at Çatalhöyük. Excavations at Çatalhöyük: the 1995-1999 seasons. I. Hodder (ed) Monograph of the McDonald Institute and the British Institute of Archaeology at Ankara (BIAA). Eastwood, W. J., Roberts, N., Lamb, H.F. and Tibby, J.C. (1999) Holocene environmental change in southwest Turkey: a palaeoecological record of lake and catchment-related changes. Quaternary Science Reviews 18: 671-696. Elbaum, R., Weiner, S., Albert, R. M. and Elbaum, M. (2003) Detection of Burning of Plant Materials in the Archaeological Record by Changes in the Refractive Indices of Siliceous Phytoliths. Journal of Archaeological Science 30: 217-226. Elhmmali, M., Roberts, D. J. and Evershed, R. P. (1997) Bile acids as a new class of sewage pollution indicator. Environmental Science and Technology 31: 3663-3668. Epstein, E. (1994) The Anomaly of Silicon in Plant Biology. PNAS 91(1): 11-17. Erickson, C. L. (1999) Neo-environmental determinism and agrarian 'collapse' in Andean prehistory. Antiquity 73(281): 634 - 642. Evershed R. P. and Bethell P. H. (1996) Application of multimolecular biomarker techniques to the identification of faecal material in archaeological soils and sediments. ACS Symposium Series 625:157– 72. Evershed, R. P., Bethell, P. H., Reynolds, P. J. and Walsh, N. J. (1997) 5ß-Stigmastanol and Related 5ß-Stanols as Biomarkers of Manuring: Analysis of Modern Experimental Material and Assessment of the Archaeological Potential. Journal of Archaeological Science 24:485-495 Evershed, R. P., Anderson-Stojanovic, V.R., Dudd S.N. and Gebhard, E.R. (2003) New Chemical Evidence for the Use of Combed Ware Pottery Vessels as Beehives in Ancient Greece. Journal of Archaeological Science 30: 1-12.

Evershed, R. P., Berstan, R., Grew, F., Copley, M. S., Charmant, A. J. H., Barham, H. R. and Brown, G. (2004) Archaeology: Formulation of a Roman cosmetic Nature 432: 35-36. Evershed, R. P., H.R. Mottram, S.N. Dudd, S. Charters, A.W. Stott, G.J. Lawrence, A.M. Gibson, A. Conner, P.W. Blinkhorn and V. Reeves (1997). New Criteria for the Identification of Animal Fats Preserved in Archaeological Pottery. Naturwissenschaften 84(9): 402-406. Evershed R. P, Heron, C. and Goad, L. J. (1990) Analysis of Organic Residues of Archaeological Origin by High-temperature Gas Chromatography and Gas Chomatography-Mass Spectrometry Analyst 115:1339-1342. Evershed, R. P., Heron, C. and Goad, L. J. (1991) Epicuticular wax components preserved in potsherds as chemical indicators of leafy vegetables in ancient diets. Antiquity 65 (248): 540-544. Evershed, R. P., Jerman, K. and Eglinton, G. (1985) Pine wood origin for pitch from the Mary Rose. Nature 314: 528-530. Fairbairn, A., Asouti, E., Near, J. and Martinoli, D. (2002) Macrobotanical evidence for plant use at Neolithic Çatalhöyük southcentral Anatolia, Turkey. Vegetation History and Archaeobotany 11: 41-54. Fairbairn, A., Martinoli D., Butler, A. and Hillman, G. (2007) Wild plant seed storage at Neolithic Çatalhöyük East, Turkey. Vegetation History and Archaeobotany 16: 467-79. Fairbairn, A. (2005) A history of agricultural production at Neolithic Çatalhöyük East, Turkey. World Archaeology 37(2): 197-210. Fairbairn, A., Asouti, E., Russell, N. and Swogger, J. (2005a) Seasonality. I. Hodder (ed.) Çatalhöyük perspectives: Themes from the 1995-9 seasons. McDonald Institute for Archaeological Research/British Institute of Archaeology in Ankara. Fairbairn, A., Near, J., and Martinoli, D. (2005b) "Macrobotanical Investigation of the North, South and KOPAL Area Excavations" in. I. Hodder (ed) Inhabiting Catalhoyuk: reports from the 19951999 seasons. McDonald Institute for Archaeological Research/British Institute of Archaeology in Ankara. Farid, S. (1996). Area Mellaart Summary of results Çatalhöyük Archive Report Farid, S. (1997) Mellaart Area Çatalhöyük Archive Report Farid, S. (2005) Excavation of the South Area – Concluding remarks Çatalhöyük Archive Report Farmer, V. C.(1974) The Infrared Spectra of Minerals. Mineralogical Society Monograph. London, Mineralogical Society. Farmer, V. C. (2000) Transverse and longitudinal crystal modes associated with OH stretching vibrations in single crystals of kaolinite and dickite. Spectrochimica Acta Part A 56(5): 927-930. Geertz, C. (1979) From the native's point of view. On the nature of anthropological understanding. Interpretative social science. P. Rainbow and W. M. Sullivan (eds) Berkeley, University of California Press: 225-241. Gohlke, R. S. and McLaffery, F. W. (1993) Early gas chromatography/mass spectrometry Journal of the American Society for Mass Spectrometry 4 (5): 367-371 Goldberg, P., Weiner, S., Bar-Josef, O., Xud, W. and Liud, J. (2001) Site formation processes at Zhoukoudian, China. Journal of Human Evolution 41(5): 483-530. Goldberg, P. and Byrd, B. F. (1999) The interpretive potential of micromorphological analysis at prehistoric shell midden sites on Camp Pendleton. Pacific coast archaeological society quarterly 35 (4): 1-23. Grave, P. and Kealhofer, L. (1999) Assessing bioturbation in archaeological sediments using soil morphology and phytolith analysis. Journal of Archaeological Science 26: 1239-1248. Grimalt, J. O., Fernandez, P., Bayona, J. M. and Albaiges, J. (1990) Assessment of faecal sterols and ketone as indicators of urban sewage inputs to coastal waters. Environmental Science and Technology 24: 357 - 63. Guttmann, E. B. A., Simpson I. A. and Dockrill, S. J. (2003) Joined-Up Archaeology at Old Scatness, Shetland: Thin Section Analysis of the Site and Hinterland. Environmental Archaeology: The journal of human palaeoecology 8: 17-31. Guttman, E. B. A., Simpson I. A., Neilsen, N. and Dockrill, S. J. (2008) Anthrosols in Iron Age Shetland: Implications for arable and economic activity Geoarchaeology: An International Journal 23 (6): 799 – 823. Gobetz, K. E. and Bozarth S. R. (2001) Implications for Late Pleistocene Mastodon Diet from Opal Phytoliths in Tooth Calculus. Quaternary Research 55(2): 115-122.

124

Hamilton, N. (1996) The figurines and other small finds Çatalhöyük Archive Report http://www.catalhoyuk.com/archive_reports/1996/ar96_14.html Hardy-Smith, T. and Edwards P. C. (2004) The garbage crisis in prehistory: artefact discard patterns at the Early Natufian site of Wadi Hammeh 27 and the origins of household refuse disposal strategies. Journal of Anthropological Archaeology 23: 253–289. Harvey, E. L. and Fuller D. Q. (2005) Investigating crop processing using phytolith analysis: the example of rice and millets. Journal of Archaeological Science 32: 739-752. Hass, M. and Sutherland G. B. B. M. (1956) The infra-red spectrum and crystal structure of gypsum. Proceedings of the Royal Society of London A 236: 427-445. Haslewood, G. A. D. (1967) Bile salt evolution. Journal of Lipid Research 8: 535- 550. Hastorf, C. (2005) Macrobotanical Investigation: field methods and laboratory analysis procedures in. I. Hodder (ed) Inhabiting Catalhoyuk: reports from the 1995-1999 seasons. McDonald Institute for Archaeological Research/British Institute of Archaeology in Ankara. Hibberd, J. M. and Quick, W. P. (2002) Characteristics of C4 photosynthesis in stems and petioles of C3 flowering plants. Nature 415 (6870): 451-4. Hill, M. J. and Drasar B. S. (1968) Degradation of bile salts by human intestinal bacteria. Gut 9: 22-27. Hillman, G. (2000) The potential vegetation under modern climatic conditions in Village on the Euphrates: From Foraging to Farming at Abu Hureyra A M T Moore, G C Hillman and A J Legge (eds) Oxford: Oxford Univesity Press 49-72. Hillman, G. (1984). Interpretation of Archaeological plant remains: Application of ethnographic models from Turkey in Casparie, W. A and van Zeist W (eds) Plants and Ancient Man: studies in Paleoethnobotany. Rotterdam: Balkema 1-41. Hillman, G. (1981) Reconstructing crop husbandry practises from the charred remains of crops in Mercer, R (ed) Farming Practise in British Prehistory Edinburgh: Edinburgh University Press 123-62. Hodder, I. (Ed) (1996). On the Surface: Çatalhöyük 1993-95. Çatalhöyük Project. Cambridge/London, McDonald Institute for Archaeological Research/ British Institute of Archaeology at Ankara. Hodder, I. (1999) The Archaeological Process: An Introduction. WileyBlackman. Hodder, I. (Ed) (2000). Toward Reflexive Method in Archaeology: The Example at Çatalhöyük. British Institute of Archaeology Monograph. Cambridge, McDonald Institute of Archaeology. Hodder, I. (2006) The Leopard's Tale: Revealing the Mysteries of Çatalhöyük. Thames and Hudson. Hodder, I. (2007) Season review Çatalhöyük Archive Report Hodder, I. and Cessford, C. (2004) Daily Practice and Social Memory at Çatalhöyük. American Antiquity 69(1):17-40 Hodson, M. J. and Sangster A. G. (1993) The Interaction between Silicon and Aluminium in Sorghum bicolor (L.) Moench: Growth Analysis and X-Ray Microanalysis. Annals of Botany 72: 389-400. Holliday, V. T. and Gartner W. G. (2007) Methods of soil P analysis in archaeology. Journal of Archaeological Science 34(2): 301-333.

in Triticum durum. Journal of Archaeological Science 36: 24022407. Jenkins, E. (2005) Phytoliths. Çatalhöyük Archive Report. Jenkins, E., Otsaku, M. and Rosen, A. M. (in press) The phytoliths in The last house on the mound. The Berkeley archaeologists at Çatalhöyük Stevanovic, M. and Tringham, R. (eds) The Cotsen Institute, University of California, Los Angeles. Jenkins, E., Jamjoum, K., Nuimat. S., Finlayson. B., Nortcliff. S., and Mithen. S. J. (forthcoming) Further investigations into phytoliths as indicators of water availability: an outline of on-going crop growing experiments and their implications for phytolith research. Proceedings of the 6th International Meeting on Phytolith Research. Karkanas, P., Kyparissi-Apostolika, N., Bar-Yosef, O and Weiner, S. (1999) Mineral Assemblages in Theopetra, Greece: A Framework for Understanding Diagenesis in a Prehistoric Cave. Journal of Archaeological Science 26(9): 1171-1180. Karkanas, P., Rigaud, J.-P., Simek, J. F, Albert, R-M. and Weiner, S. (2002) Ash Bones and Guano: a Study of the Minerals and Phytoliths in the Sediments of Grotte XVI, Dordogne, France. Journal of Archaeological Science 29(7): 721-732. Kealhofer, L. and Piperno D. R. (1998). Opal phytoliths in Southeast Asian flora. Washington D.C, Smithsonian Institution Press. Kelly, S., Heaton K. and Hoogeweff, J. (2005) Tracing the geographical origin of food: The application of multi-element and multi-isotope analysis. Trends in Food Science & Technology 16: 555-567. Kent, S. (1993) Variability in faunal assemblages: The influence of hunting skill, sharing, dogs, and mode of cooking on faunal remains at a sedentary Kalahari community. Journal of Anthropological Archaeology 12: 323-385. Kimpe, K., Drybooms, C., Schrevens, E., Jacobs, P. A., Degeest, R. and Waelkens, M. (2004) Assessing the relationship between form and use of different kinds of pottery from the archaeological site Sagalassos (southwest Turkey) with lipid analysis. Journal of Archaeological Science 31(11): 1503-1510. Koikea, H. (1979) Seasonal dating and the valve-pairing technique in shell-midden analysis. Journal of Archaeological Science 6(1): 63 - 74. Kuzucuoğlu, C. (2002). The environmental frame in central Anatolia from the 9th to the 6th Millenia cal BC. The Neolithic of Central Anatolia: Internal Developments and External Relations during the 9th-6th Millennia cal BC. F. Gerard and L. Thissen. İstanbul, Ege Yayınları: 33-58. Leacha, B. F. (1979) Fish and crayfish from the Washpool Midden site, New Zealand: Their use in determining season of occupation and prehistoric fishing methods. Journal of Archaeological Science 6(2): 109 - 126. Legge, A. J. (1981) Aspects of cattle husbandry. In: R. Mercer (ed) Farming Practice in British Prehistory, Edinburgh University Press, Edinburgh 169–181. Lenain, B. P. (2000) Analytical Raman spectroscopy: a new generation of instruments. Analysis 28: 11-14. Lentfer, C. and Boyd W. E. (1999) An Assessment of techniques for the deflocculation and removal of clays from sediments used in phytolith analysis. Journal of Archaeological Science 26: 31-44. Lin, D. S., Connor, W.E., Napton, L. K. and Heizer, R. F. (1978) The steroids of 2000 year old human coprolites Journal of Lipid Research 19: 215-21. Loste, E., Wilson, R. M., Seshadri, R. and Meldrum, F. C. (2003) The role of magnesium in stabilising amorphous calcium carbonate and controlling calcite morphologies. Journal of crystal growth 254: 206-218. Lux, A., Luxova, M., Hattori, Y., Inanaga, S. and Sugimoto, Y. (2002) Silicification in sorghum (Sorghum bicolor) cultivars with different drought tolerance. Physiologia Plantarum 115(1): 87-92. Lu, H. and K.-B. Liu (2003) Morphological variations of lobate phytoliths from grasses in China and the south-eastern United States. Biodiversity Research 9: 73-87. Lu, H., Zhang, J., Wu, N., Liu, K., Xu, D. and Li, Q. (2009) Phytoliths analysis for the discrimination of foxtail millet (Setaria italica) and common millet (panicum miliaceum) PLoS ONE 4 (2) Macphail, R. I., Cruise, G. M., Allen, M. J. and Reynolds, P. (2004) Archaeological soil and pollen analysis of experimental floor deposits; with special reference to Butser Ancient Farm, Hampshire, UK. Journal of Archaeological Science 31(2): 175191.

Horrocks, M. and Lawlor, I. (2006) Plant micofossil analysis of soils from Polynesian stonefields in South Auckland, New Zealand. Journal of Archaeological Science 33: 200-217. Horwitz, L. K. (1990) The origin of partially digested bones recovered from archaeological sites in Israel. Paleorient 16: 97-106 Houyuan, L., Zhenxia, L., Naiqin, W., Berne, S., Saito, Y., Baozhu, L. and Wang, L. (2002) Rice domestication and climate change: phytolith evidence from East China. Boreas 31: 378-385. Hjulström, B and Isaksson, S. (2009) Identification of activity area signatures in a reconstructed Iron Age house by combining element and lipid analyses of sediments Journal of Archaeological Science 36 (1): 174-183 Inoue, K., Saito, M. and Naruse, T. (1998) Physicochemical, mineralogical, and geochemical characteristics of lacustrine sediments of the Konya Basin, Turkey, and their significance in relation to climatic change, Geomorphology 23 (2-4): 229-243. Jamieson, J. C. (1953) Phase Equilibrium in the System CalciteAragonite. The Journal of Chemical Physics 21(8): 1385-1390. Jenkins, E. (2009) Phytolith taphonomy: a comparison of dry ashing and acid extraction on the breakdown of conjoined phytoliths formed

125

Madejova, J. (2003) FTIR techniques in clay mineral studies. Vibrational Spectroscopy 31: 1-10. Madella, M., Jones, M. K., Echlin, P., Powers-Jones, A. and Moore, M. (2009) Plant water availability and analytical microscopy of phytoliths: Implications for ancient irrigation in arid zones. Quaternary International 193: 32-40. Madella, M., Alexandre, A. and Ball, T. (2005) International code for phytolith nomenclature 1.0. Annals of Botany 96: 253-260. Madella, M. (2001) Understanding archaeological structures by means of phytolith analysis: a test from the Iron Age site of Kilise Tepe – Turkey in J. D. Meunier and F. Colin. (eds) Phytoliths: Applications in Earth Sciences and Human History. A.A Balkema. Marshall L. J., Almond M. J., Cook S. R., Pantos M., Tobin M. J. and Thomas L. A. (2008) Mineralised organic remains from cesspits at the Roman town of Silchester: processes and preservation. Spectrochimica Acta A Molecular and Biomolecular Spectroscopy 71 (3):854-61 Matsulani, A. (1972) Spodographic Analysis of Ash from the Kotosh site. Andes 4: Excavations at Kotosh, Peru, 1963 and 1966. I. Seiichi and T. Kazuo (eds). Tokyo, Kadokawa. Martin, L. and Russell, N. (2000). Trashing Rubbish. Towards reflexive method in archaeology: the example at Çatalhöyük. I. Hodder (ed) Cambridge, McDonald Institute for Archaeological Research. 5769. Matthews, W. (1992). The Micromorphology of Occupational Sequences and the Use of Space in a Sumerian City. PhD thesis. University of Cambridge, Darwin College, Department of Archaeology. Matthews, W., Postgate, J. N., Payne, S., Charles, M. P. and Dobney, K. (1994) The Imprint of living in an early Mesopotamian City: questions and answers. Whither Environmental Archaeology. R. Luff and P. Rowley-Conwy (eds) Oxford, Oxbow Books. Monograph 36: 171-212. Matthews, W. (1995a) Sampling report. Çatalhöyük Archive Report Matthews, W. (1995b). Micromorphological characterisation and interpretation of occupation deposits and microstratigraphic sequences at Abu Salabikh, Iraq. Archaeological Sediments and Soils, Analysis, Interpretation and Management. T. Barham, M. Bates and R. Macphail (eds) London, Archetype books. 41-76. Matthews, W., French, C., Lawrence, T. and Cutler, D. (1996) Multiple surfaces: the micromorphology. In: Hodder, I. 1996. On the Surface Çatalhöyük 1993-95. McDonald Institute for Archaeological Research / British Institute of Archaeology at Ankara Monograph. 301-42 Matthews, W., French, C. I. A., Lawrence, T., Cutler, D. F. and Jones, M. K. (1997). Activities inside the temple: the evidence of the microstratigraphy. The Dilmun Temple at Saar. H. E. W. Crawford, R. Killick and J. Moon (eds) London, Kegan Paul International. Matthews, W., French, C. I. A., Lawrence, T., Cutler, D. F. and Jones, M. K. (1997) Microstratigraphic traces of site formation processes and human activities. World Archaeology 29(2): 281-308. Matthews, W. (2005a) Micromorphological and microstratigraphic traces of uses and concepts of space. Inhabiting Çatalhöyük: Reports from the 1995-1999 seasons. I. Hodder (ed) London, McDonald Institute for Archaeology/British Institute of Archaeology at Ankara. 355-399. Matthews, W. (2005b) Micromorphology and Microstratigraphy: Contextual Studies Inhabiting Çatalhöyük: Reports from the 19951999 seasons. I. Hodder (ed) London, McDonald Institute for Archaeology/British Institute of Archaeology at Ankara. 553-571. Matthews, W. (2005c). Life cycle and life course of buildings. Çatalhöyük Perspectives: Themes from the 1995-99 Seasons. I. Hodder (ed) Cambridge, McDonald Institute for Archaeological Research and British Institute of Archaeology at Ankara. 125-149. Matthews, W., Shillito, L.-M., and Almond, M. J. (2004) Micromorphology: investigation of Neolithic social and ecological strategies at seasonal, annual and life-cycle timescales. Çatalhöyük Archive Report. McCann, S. and Brown, D. (2006) South Area. Çatalhöyük Archive Report. Mellaart, J. (1962) Excavations at Çatal Huyük: First Preliminary Report. Anatolian Studies 12: 43-103. Mellaart, J. (1963) Excavations at Çatal Huyük: Second preliminary Report. Anatolian Studies 13: 43-103. Mellaart, J. (1964) Excavations at Çatal Huyük: Third preliminary report. Anatolian Studies 14: 39-119.

Mellaart, J. (1966) Excavations at Çatal Huyük: Fourth preliminary report. Anatolian Studies 16: 15-191. Mellaart, J. (1967) Çatal Huyük: A Neolithic Town in Anatolia. McGraw-Hill. Miller, N. (1984) The use of dung as fuel: an ethnographic example and an archaeological application. Paleorient 10: 71–79. Miller, N. and Smart, T. (1984) Intentional Burning of Dung as Fuel: A Mechanism for the Incorporation of Charred Seeds into the Archaeological Record. Journal of Ethnobiology 4: 15-28 Mithen, S., Jenkins, E., Jamjoum, K., Nuimat, S., Nortcliff, S. and Finlayson, B. L. (2008) Experimental crop growing in Jordan to develop a methodology for the identification of ancient crop irrigation World Archaeology, 40: 7-25. Molleson, T., Andrews, P. and Boz, B. (2005) Reconstruction of the Neolithic people of Çatalhöyük. In I. Hodder (ed.) Inhabiting Çatalhöyük: reports from the 1995-1999 seasons Cambridge, McDonald Institute for Archaeological Research and British Institute of Archaeology at Ankara. Monje, P. V. and Baran E. J. (2000) First Evidences of the bioaccumulation of alpha-quartz in Cactaceae. Journal of Plant Physiology 157: 457-460. Monks, G. G. (1981) Seasonality Studies. Advances in Archaeological Method and Theory 4: 177-240. Mortimore, J. L., Marshall, L.-J. R., Almond, M. J., Hollins, P. and Matthews, W. (2004) Analysis of red and yellow ochre samples from Clearwell Caves and Çatalhöyük by vibrational spectroscopy and other techniques. Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy 60(5): 1179-1188. Murray, K. K., Boyd, R., Eberlin, M. N., Langley, G. J., Li, L. and Naito, Y. (2006) Standard definition of terms relating to mass spectrometry. IUPAC Analytical Chemistry Division Recommendations. Mulholland, S. C. and Rapp G. J. (1992) A Morphological Classification of Grass Silica-Bodies. Phytolith Systematics: Emerging Issues. G. J. Rapp and S. C. Mulholland. New York/London, Plenum Press. Nakamato, K. (1986) Infrared and Raman Spectra of Inorganic and Coordination Compounds. New York, Wiley. Nunn, P. D. (2003) Revising ideas about environmental determinism: Human-environment relations in the Pacific Islands. Asia Pacific Viewpoint 44: 63-72. O'Connor, T. P. (2004) The Archaeology of Animal Bones. The History Press. O'Connor, T. P. (1998) The Annual Round: an Overview of the AEA Conference 1994 "Seasonality"." Environmental Archaeology 3. Ollendorf, A. L. (1987) Archaeological Implications of a Phytolith Study at Tel Miqne (Ekron), Israel. Journal of Field Archaeology 14: 453-463. Ollendorf, A. L., Mulholland, S. C. and Rapp, G. J. R. (1988) Phytolith analysis as a means of plant identification: Arundo donax and Phragmites communis. Annals of Botany 61: 209-214. Ottaway, J. H. (1984) Persistence of organic phosphates in buried soils. Nature 307: 257-259. Palmer, C. and van der Veen, M. (2002) Archaeobotany and the social context of food. Acta Palaeobotanica 42(4): 195–202. Parmente, G. C. and Folger, D. W. (1974) Eolian biogenic detritus in deep-sea sediment - possible index of equatorial ice age aridity. Science 184: 695. Parr, J. F. (2002) A comparison of heavy liquid floatation and microwave digestion techniques for the extraction of fossil phytoliths from sediments. Review of Palaeobotany and Palynology, 120(3-4): pp 315-336 Parr, J. F. (2006) Microwave extraction of starch. In: R. Torrence and H. Barton (eds) Ancient Starch Research. Left Coast Press, Inc., California Parry, D. W., Hodson, M. J., Sangster, A. G., Jones, W. C. and O’Neill, C. H. (1984) Some recent advances in studies of silicon in higher plants. Philosophical Transactions of the Royal Society of London, Series B 304: 537-549. Patterson, W. A., Edwards K. J. and Maguire, D. J. (1987) Microscopic charcoal as a fossil indicator of fire. Quaternary Science Reviews 6: 3-23. Pearsall, D. M. (1982) Research Reports: Phytolith Analysis: Applications of a New Paleoethnobotanical Technique in Archaeology. American Anthropologist 84: 862 - 871. Pearsall, D. M. and Dinan, E. H. (1992) Developing a Phytolith Classification System. Phytolith Systematics: Emerging Issues. G.

126

J. Rapp and S. C. Mulholland. New York and London, Plenum Press. 65-91. Piperno, D. R. (1984) A comparison and differentiation of phytoliths from maize and wild grasses: use of morphological criteria. American Antiquity 49(2): 361-383. Piperno, D. R. (1988). Phytolith Analysis: An Archaeological and Geological Perspective. New York, Academic Press. Piperno, D. R. (2006). Phytoliths: A Comprehensive Guide for Archaeologists and Paleoecologists, AltaMira Press. Pironon, J., Meunier, J. D., Mathieu, A. A., Mansuy, L., Grosjean, A. and Jardee, E. (2001). Individual Characterisation of phytoliths: experimental approach and consequences on palaeoenvironment understanding. Phytoliths: Applications in Earth Science and Human History. J. D. Meunier and Collins. Powers-Jones, A. H. (1994) The use of phytolith analysis in the interpretation of archaeological deposits: an Outer Hebridean example. Whither environmental archaeology. R. Luff and P. Rowley-Conwy (eds). Oxford, Oxbow. 38: 41-49. Prabakaran, K., Balamurugan, A. and Rajeswari, S. (2005) Development of calcium phosphate based apatite from hen's eggshell. Bulletin of Materials Science 28(2): 115-119. Puglisi, E., Nicelli, M., Capri, E., Trevisan, M. and Del Re, A. A. M. (2003). Cholesterol, ß-Sitosterol, Ergosterol, and Coprostanol in Agricultural Soils Journal of Environmental Quality 32: 466-471. Rey, C., Miquel, J., Facchini, L., Legrand, A. P. and Glimcher, J. (1995) Hydroxyl groups in bone mineral Bone 16 (5): 583-586. Rhee, S. K., Reed, R. G. and Brenna, J. T. (1997) Fatty acid carbon isotope ratios in humans on controlled diets. Lipids 32(12): 12571263. Rhode, D. (2003) Coprolites from Hidden Cave, revisited: evidence for site occupation history, diet and sex of occupants. Journal of Archaeological Science 30 (7):909-922. Richards, M. P. and Pearson, J. A. (2005). Stable-isotope evidence of diet at Çatalhöyük. Inhabiting Çatalhöyük: Reports from the 19951999 seasons. I. Hodder (ed) Cambridge, McDonald Institute for Archaeological Research/British Institute of Archaeology at Ankara. Richards, M. P., Pearson, J. A., Molleson, T. I., Russell, N. and Martin, L. (2003) Stable isotope evidence of diet at neolithic Çatalhöyük. Journal of Archaeological Science 30: 67-76. Richmond, K. E. and Sussman, M. (2003) Got silicon? The nonessential beneficial plant nutrient. Current Opinion in Plant Biology 6(3): 268-272. Ridlon, J. M., Kang, D.-J. and Hylemon, P. B. (2006) Bile salt biotransformations by human intestinal bacteria. Journal of Lipid Research 47(2): 241-259. Roberts, N., Black, S., Boyer, P., Eastwood, W. J., Griffiths, H. I., Lamb, H. F., Leng, M. J., Parish, R., Reed, J. M., Twigg, D. and Yigitbasioglu, H. (1999) Chronology and Stratigraphy of Late Quaternary Sediments in the Konya Basin, Turkey: Results from the KOPAL project. Quaternary Science Reviews 18: 611 - 630. Roberts, N. and Rosen, A. M. (2005). The Nature of Çatalhöyük, People and their Changing Environments on the Konya Plain. Çatalhöyük perspectives: reports from the 1995-1999 seasons. I. Hodder. Cambridge, McDonald Institute for Archaeological Research and the British Institute at Ankara: 39-54. Rosen, A. M. (1989) Ancient town and city sites: a view from the microscope. American Antiquity 54(3): 564-578. Rosen, A. M. (1992) Preliminary Identification of Silica Skeletons from Near Eastern Archaeological Sites: An Anatomical Approach. Phytolith Systematics: Emerging Issues. G. J. Rapp and S. C. Mulholland (eds) New York/London, Plenum Press. 129-47. Rosen, A. M. and Weiner, S. (1994) Identifying Ancient Irrigation: a New Method Using Opaline Phytoliths from Emmer Wheat. Journal of Archaeological Science 21: 125-132. Rosen, A. M., Chang, C. and Grigoriev, F. (2000) Paleoenvironments and economy of Iron Age Sako-Wusu agro-pastoralists in southeastern Kazakhstan. Antiquity 74(285): 611-623. Rosen, A. M. (2001) Phytolith Analysis in Near Eastern Archaeology. The Practical Impact of Science on Near Eastern and Aegean Archaeology. S. Pike and S. Gitin, Weiner Laboratory. 3: 9-15. Rosen, A. M. (2001) Phytolith evidence for agro-pastoral economies in the Scythian period of Southern Kazakhstan. Phytoliths: Applications in Earth Sciences and Human History. J. D. Meunier and F. Colin (eds) Lisse, A.A. Balkema.

Rosen, A. M. (2005) Phytolith Indicators of Plant and Land Use at Çatalhöyük. Inhabiting Çatalhöyük: Reports from the 1995-1999 Seasons. I. Hodder. (ed) Cambridge, McDonald Institute. Rosen, A. M. (1999) Phytolith archive report for 1999 season at catalhoyuk, in Archaeobotany and related plant studies Çatalhöyük Archive Report http://www.catalhoyuk.lan/archive_reports/1999/ar99_07.html Rosen, A. M (1998) Archive report on phytolith studies at Çatalhöyük, in Hastorf, C. Archaeobotanical work 1998 Çatalhöyük Archive Report http://www.catalhoyuk.lan/archive_reports/1998/ar98_08.html Rosen, A and Roberts N. (2009) Diversity and complexity in early farming communities of Southwest Asia: New insights into the economic and environmental basis of Neolithic Çatalhöyük Current Anthropology 50 (3): 393-402. Rovner, I. (1971) Potential of Opal Phytoliths for Use in Paleoecological Reconstruction. Quaternary Research 1(3): 343359. Rowlett, R. M. and Pearsall D. M. (1993) Archaeological age determinations derived from opal phytoliths by thermoluminescence. Current Research in Phytolith Analysis: Applications in archaeology and paleoecology 10. D. M. Pearsall and D. R. Piperno, MASCA: 25-29. Russell, N. (1996) Bone tools. Çatalhöyük Archive Report http://www.catalhoyuk.com/archive_reports/1996/ar96_11.html Russell, N. and Martin, L. (2005). Çatalhöyük Mammal Remains. Inhabiting Çatalhöyük: reports from the 1995-99 seasons. I. Hodder (ed) Cambridge, Macdonal Institute / British Institute of Archaeology at Ankara. Russell, N. and McGowen, K. J. (2005) Çatalhöyük bird bones Inhabiting Çatalhöyük: reports from the 1995-99 seasons. I. Hodder (ed) Cambridge, Macdonal Institute / British Institute of Archaeology at Ankara. Sanderson, D. C. W. and Hunter, V. (1981) Composition and variability in vegetable ash. Science and Archaeology 23: 27-30. Schiegl, S., Goldberg, P., Bar-Yosef, O. and Weiner, S. (1996) Ash deposits in Hayonim and Kebara caves, Israel: Microscopic, microscopic and mineralogical observations, and their archaeological implications. Journal of Archaeological Science 23: 763-781. Schiffer, M. B. (1983) Toward the Identification of Formation Processes. American Antiquity 48(4): 675-706. Schellenberg, H. C. (1908) Wheat and Barley from the North Kurgan, Anau. Explorations in Turkestan. R. Pumpelly. Washington D.C., Carnegie Institute. 3: 471-473. Shahack-Gross, R., Albert, R-M., Gilboa, A., Nagar-Hilman, O., Sharon, I. and Weiner, S. (2005) Geoarchaeology in an urban context: the uses of space in a Phoenician monumental building at Tel Dor (Israel). Journal of Archaeological Science 32: 14171431. Shahack-Gross, R., Berna, F., Karkanas, P. and Weiner, S. (2004) Bat guano and preservation of archaeological remains in cave sites. Journal of Archaeological Science 31(9): 1259-1272. Schlezinger, D. R and Howes, B. L. (2000) Organic Phosphorus and Elemental Ratios as Indicators of Prehistoric Human Occupation. Journal of Archaeological Science 27 (6): 479-492. Schoeninger, M. J. and DeNiro, M. J. (1984) Nitrogen and carbon isotopic composition of bone collagen from marine and terrestrial animals. Geochimica et Cosmochimica Acta 48: 625–639. Shillito, L.-M. (2004). The Importance of Rubbish: Microstratigraphic and phytolith analysis of midden deposits at Neolithic Çatalhöyük as an indicator of seasonality. Unpublished MSc thesis. University of Reading, Department of Archaeology. Shillito, L-M. (2006) Micromorphology, microanalysis and organic residues of middens. Çatalhöyük Archive Report. Shillito, L.-M., Matthews, W. and Almond, M. J. (2008) Investigating midden formation processes and cultural activities at Neolithic Çatalhöyük, Turkey Antiquity 82 (317) project gallery. Shoval, S. (2003) Using FT-IR spectroscopy for study of calcareous ancient ceramics. Optical Materials 24: 117-122. Sillar, B. (2000) Dung by preference: the choice of fuel as an example of how Andean pottery production is embedded within wider technical, social and economic practises. Archaeometry 42: 43-60. Simpson, I. A., van Bergen, P. F., Perret, V., Elhmmali, M. M., Roberts, D. J. and Evershed, R. P. (1999) Lipid biomarkers of manuring practice in relict anthropogenic soils. The Holocene 9(2): 223– 229.

127

Simpson, I. A. and Barrett, J. H. (1996) Interpretation of Midden Formation Processes at Robert's Haven, Caithness, Scotland using Thin Section Micromorphology. Journal of Archaeological Science 23(4): 543-556. Simpson, I. A., Dockrill, S. J., Bull, I. D. and Evershed, R. P. (1998) Early anthropogenic soil formation at Tofts Ness, Sanday, Orkey. Journal of Archaeological Science 25: 729-746. Simpson, I. A., Vesteinsson, O., Adderley, W. P., and McGovern, T. H. (2003) Fuel resource utilisation in landscapes of settlement. Journal of Archaeological Science 30 (11): 1401-1420. Smith, G. D. and Clark, R. J. H. (2004) Raman Spectroscopy in archaeological science. Journal of Archaeological Science 31: 1137-1160. Spangenberg, J. E., Jacomet, S. and Schibler, J. (2006) Chemical analyses of organic residues in archaeological pottery from Arbon Bleiche 3, Switzerland - evidence for dairying in the late Neolithic. Journal of Archaeological Science 33: 1-13. Stefanova, T. and Dakić, P. (2004) Excavation of the 4040 Area Spaces 226 and 243. Çatalhöyük Archive Report. Stein, J. K. (1992). Deciphering a Shell Midden, Academic Press. Stein, J. K. and Deo, J. N. (2003) Big Sites - Short Time: Accumulation rates in archaeological sites. Journal of Archaeological Science 30: 297-316. Steiner, M. C., Kuhn, S. L., Surovell, T. A, Goldberg, P., Meignen, L., Weiner, S. and Bar-Yosef, O. (2001) Bone Preservation in Hayonim Cave (Israel): a Macroscopic and Mineralogical Study. Journal of Archaeological Science 28(6): 643-659. Stoops, G. (ed) (2003) Guidelines for Analysis and Descriptions of Soil and Regolith Thin Sections. American Society of Agronomy Sullivan, K. A. and Kealhofer, L. (2004) Identifying activity areas in archaeological soils from a colonial Virginia house lot using phytolith analysis and soil chemistry. Journal of Archaeological Science 31: 1659-1673. Tebo, B. M., Johnson, H. A., McCarthy, J. K. and Templeton, A. (2005). Geomicrobiology of manganese(II) oxidation. Trends in Microbiology 13(9): 421-428. Terry, R. E., Fernandez, F. G. , Parnella, J. J. and Inomata, T. (2004). "The story in the floors: chemical signatures of ancient and modern Maya activities at Aguateca, Guatemala." Journal of Archaeological Science 31: 1237-1250. Thorn, V. C. (2004) Phytoliths from subantarctic Campbell Island: plant production and soil surface spectra. Review of Palaeobotany and Palynology 132(1-2): 37-59. Thomas, L. A., Veysey, M. J., French, G., Hylemon, P., Murphy, G. and Dowling, R. (2001) Bile acid metabolism by fresh human colonic contents: a comparison of caecal versus faecal samples. Gut 49: 835-842. Trombold, C. D. and Israde-Alcantara, I. (2005) Paleoenvironment and plant cultivation on terraces at La Quemada, Zacatecas, Mexico: the pollen, phytolith and diatom evidence. Journal of Archaeological Science 32: 341-353. Twigger, E. (2004) Excavations of the 4040 Area Spaces 229, 230, 241, 242 and 244. Çatalhöyük Archive Report. Twiss, P. C. (1969) Morphological Classification of Grass Phytoliths. Soil Science Society of America Proceedings 33: 109-115. Twiss, P. C. (1992) Predicted World Distribution of C3 and C4 Grass Phytoliths. Phytolith Systematics - Emerging Issues. S. C. Mulholland and G. J. Rapp (eds) New York and London, Plenum Press: 113-129. Umbanhower, C. E. and McGrath, M. J. (1998) Experimental production and analysis of microscopic charcoal from wood, leaves and grasses. The Holocene 8(3): 341-346. Vagenas, N. V., Gatsouli, A. and Kontoynnis, C. G. (2003) Quantitative analysis of synthetic calcium carbonate polymorphs using FT-IR spectroscopy. Talanta 59(4): 831-836. van Bergen, P. F., Bull, I. D., Poulton, P. R. and Evershed, R. P. (1997) Organic geochemical studies of soils from the Rothamsted Classical Experiments-I. Total lipid extracts, solvent insoluble residues and humic acids from Broadbalk Wilderness. Organic Geochemistry 26: 117-135. van Faassen, A., Bol, J., van Dokkum, W., Pikaar, N. A., Ockhuizen, T. and Hermus, R. J. (1987) Bile acids, neutral steroids, and bacteria in feces as affected by a mixed, a lacto-ovovegetarian, and a vegan diet. American Journal of Clinical Nutrition 46: 962-967. van der Merwe, N. J. and Vogel J. C. (1978) 13C content of human collagen as a measure of prehistoric diet in Woodland North America. Nature 276: 815–816.

Van der Veen, M. (2007) Formation processes of desiccated and carbonized plant remains – the identification of routine practice. Journal of Archaeological Science 34(6): 968-990 Vivian, C. M. G. (1986) Tracers of sewage sludge in the marine environment: a review Science of the Total Environment 53:5–40. Walker R. W. , Wun C. K. and Litsky, W. (1982) Coprostanol as an indicator of fecal pollution CRC Critical Reviews in Environmental Control 12:91 – 112. Wallis, L. A. (2003) An overview of leaf phytolith production patterns in selected northwest Australian flora. Review of Palaeobotany and Palynology 125: 201-248. Wang, Y., Jahren, A. H. and Amundson, R. (1997) Potential for 14C Dating of Biogenic Carbonate in Hackberry (Celtis) Endocarps. Quaternary Research 47(3): 337-343. Watling, J. R. (1998) Sourcing the provenance of cannabis crops using inter-element association patterns ‘fingerprinting’ and laser ablation inductively coupled plasma mass spectrometry. Journal of Analytical Atomic Spectrometry 13: 917-926. Wattez, J. and Courty, M. A. (1987). Morphology of ash of some plant materials. N. Fedoroff, L. M. Bresson and M. A. Courty (eds) Soil Micromorphology Paris. 677–683. Weiner, S., Goldberg, P. and Bar-Yosef, O. (2002) Three-dimensional Distribution of Minerals in the Sediments of Hayonim Cave, Israel: Diagenetic Processes and Archaeological Implications. Journal of Archaeological Science 29(11): 1289-1308. Wilding, L. P., Smeck, N. E. and Drees, I. (1989) Silica in soils: quartz, crystabolite, tridymite and disordered silica polymorphs. Minerals in Soil Environments. J. B. Dixon and S. B. Weed (eds) Madison, Wisconsin, Soil Science Society of America. 1: 913-974. Wiles, J. (2009) An analysis of plaster sequences from the Neolithic site of Çatalhöyük (Turkey) by microspectroscopic techniques. Unpublished PhD thesis, University of Reading, Department of Chemistry. Wilkins, T. D. and Hackman, A. S. (1974) Two patterns of neutral steroid conversion in the feces of normal North Americans. Cancer Research 34: 2250-2254. Wilson, J. D. (1961) The effect of dietary fatty acids on coprostanol excretion by the rat. Journal of Lipid Research 2(4): 350-356. Wright, H. E. (1993) Environmental Determinism in Near Eastern Prehistory. Current Anthropology 34(4): 458-469. Wüst, R. A. J. and Bustin, R. M. (2003) Opaline and Al-Si phytoliths from a tropical mire system of West Malaysia: abundance, habit, elemental composition, preservation and significance. Chemical Geology 200: 267-292. Yalman, N. (2006) Pottery report Çatalhöyük Archive Report 181-225 Yeomans, L. (2005). Discard and Disposal Practises at Çatalhöyük: a study through the characteristation of the faunal remains. Inhabiting Çatalhöyük: Reports from the 1995-1999 seasons. I. Hodder (ed) London, McDonald Institute for Archaeology/British Institute of Archaeology at Ankara. Yeomans, L. (2006) Neolithic sequence - central midden area sealing earlier buildings. Çatalhöyük Archive Report. Zhao, Z. and Pearsall, D. M. (1998) Experiments for improving phytolith extraction from soils. Journal of Archaeological Science 25: 587-598.

128