The Effect of Various Synthetic Detergents on Cotton, Viscose, Cellulose Acetate, Nylon, and Wool Fabrics as Determined by Soil Removal and Degradation

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P U R D U E U N IV E R SIT Y

THIS IS TO CERTIFY THAT THE THESIS PREPARED UNDER MY SUPERVISION

BY

R u t h Marie Le^g

ENHTLEDThg Effect of Various SynthatjLc DetergBn_t3__on Cotton, Viscose, C ellulose Acetate, Nylon, and Wool Fabrics as D et ermined b y S o il Removal

and D e g r adation._________

COMPLIES WITH THE UNIVERSITY REGULATIONS ON GRADUATION THESES

AND IS APPROVED BY M E AS FULFILLING THIS PART OF THE REQUIREMENTS

FOR THE DEGREE OF

Doc t or of P h il o so ph y

P ro fessor in

C h a r g e o f T h e s is

( V H ) - a d o f S c h o o l or D e p a r t m e n t

TO THE LIBRARIAN:-IS THIS THESIS IS NOT TO BE REGARDED AS CONFIDENTIAL.

GKAD.

SC HO OL FO RM 9 —3 - 4 9—1M

THE EFÎECT OF VARIOUS SIMHETIC DETERGENTS ON COTTON, VISCOSE, CELLULOSE ACETATE, NYLON, AND WOOL FABRICS AS DETERMINED BY SOIL REMOVAL AND DEGRADATION

A Thesis

Submitted to the Faculty

of

Purdue University by Ruth Marie Legg In Partial Fulfillment of the

Requirements for the Degree of

Doctor of Philosophy

June, 1950

ProQuest Number: 27712257

All rights reserved INFORMATION TO ALL USERS The quality of this reproduction is d e p e n d e n t upon the quality of the copy subm itted. In the unlikely e v e n t that the a u thor did not send a c o m p le te m anuscript and there are missing pages, these will be noted. Also, if m aterial had to be rem oved, a n o te will ind ica te the deletion.

uest ProQuest 27712257 Published by ProQuest LLC (2019). C opyright of the Dissertation is held by the Author. All rights reserved. This work is protected against unauthorized copying under Title 17, United States C o d e M icroform Edition © ProQuest LLC. ProQuest LLC. 789 East Eisenhower Parkway P.O. Box 1346 Ann Arbor, Ml 48106 - 1346

AŒKWWIÆDGÆENT S

The writer is deeply indebted to Dr. Elizabeth D. Roseberry, with­ out whose help and guidance this thesis could not have been written. She also wishes to acknowledge the help of Dr. H. W. Galbraith, Dr. Karl Meissner, Mrs. Barbara McKee, and Mr. and Mrs. Robert Cantrell.

TABLE OF CONTENTS Page ABSTRACT......................................................... INTRODUCTION........................................................1 A SURVEY OF THE LITERATURE.......................................... 3 PROCEDURE.........................................................13 The Removal of Soil by Synthetic Detergents in the LaunderO m e t e r ...................................................13 The Removal of Soil by Synthetic Detergents in the Washing Machine............... ...

17

Fabric Degradation during theWashing Process.................. 19 DISCUSSION OF RESULTS AND CONCLUSIONS............................. 23 The Removal of Soil by Synthetic Detergents in the LaunderO m e t e r ...................................................23 The Removal of Soil by Synthetic Detergents in the Washing Machine...................................................44Fabric Degradation during theWashing Process.................. $8 SUMMARY OF RESULTS AND CONCLUSIONS................................. 74 BIBLIOGRAPHY.......................................................77 VITA.............................................................. 80

TABLES Table

Page

1. The Percentage of Soil Removed from Cotton Fabrics Washed in the Launder-Omete n ....................................24 2. The Percentage of Soil Removed from Viscose Fabrics Washed in the Launder-Omete r ....................................25 3. The Percentage of Soil Removed from Cellulose Acetate Fabrics Washed in the Laund er-Omet e r ............... 26 4. The Percentage of Soil Removed from Nylon Fabrics Washed in the Laund er-Omet er .................................

27

5. The Percentage of Soil Removed from Wool Fabrics Washed in the Laund er-Omet e r .............

28

6 . The Percentage of Soil Removed and Whiteness Retained on Cotton Fabrics Washed in the Washing Machine.............. 45 7. The Percentage of Soil Removed and Whiteness Retained on Viscose Fabrics Washed in the Washing M a c h i n e ............ Ijo

8. The Percentage of Soil Removed and Whiteness Retained on Cellulose Acetate Fabrics Washed in the Washing Machine . 47 9. The percentage of Soil Removed and Whiteness Retained on Spun Nylon Fabrics Washed in the Washing Machine.......... 48 10.

The percentage of Soil Removed and Whiteness Retained on Wool Fabrics Washed in the Washing Machine................ 49

11.

The percentage of Oil Removed from Cotton, Viscose, Spun Cellulose Acetate, Nylon, and Wool Fabrics during one Wash in the Washing Machine ............................ 55

12.

The pH*s of Sixteen Synthetic Detergents as Determined in a 0.15 Per Cent Solution in Zeolite-Softened Water. . . . .

57

The Percentage of Loss in the Breaking Strength of Cotton Fabrics during Fifty Washes . . . . ....................

59

The percentage of Loss in the Breaking Strength of Viscose Fabrics during Fifty Washes ............................

60

The Percentage of Loss in the Breaking Strength of Filament Cellulose Acetate Fabrics during Fifty Washes ..........

6l

The Percentage of Loss in the Breaking Strength of Spun Cellulose Acetate Fabrics during Fifty Washes ........

62

13-

14.

15.

16.

.

TABLES CONT'D. Table

Page

17. The Percentage of Loss in the Breaking Strength of Filament Nylon Fabrics during Fifty Washes......................... 63 18. The Percentage of Loss in the Breaking Strength of Spun Nylon Fabrics during Fifty Washes. .....................

64

19. The Percentage of Loss in Cellulose Viscosity after Ten and Fifty Washes

.............

69

20. The percentage of Wool Shrinkage during Fifty Washes when Washed with Various Synthetic Detergents ................ 71

FIGURES Figure

Page

1. The Effect of Detergent Concentration, Type cf Detergent, and Hardness of Water on Soil Removal from Cotton Fabrics Washed in the Launder-Ometer.......................

30

2. The Effect of Detergent Concentration, Type of Detergent, and Hardness of Water on Soil Removal from Viscose Fabrics Washed in the Launder-Ometer...................

31

3. The Effect of Detergent Concentration, Type of Detergent, and Hardness of Water on Soil Removal from Cellulose Acetate Fabrics Washed in the Launder-Ometer...........

32

4. The Effect of Detergent Concentration, Type of Detergent, and Hardness of Water on Soil Removal from Nylon Fabrics Washed in the Launder-Ometer. . . . . .... ....

33

5. The Effect of Detergent Concentration, Type of Detergent, and Hardness of Water on Soil Removal from Wool Fabrics Washed in the Launder-Ometer...........................

34

6. The Effect of Detergent Concentration, Builder, and Hardness of "Water on Soil Removal from Cotton Fabrics Washed in the Launder-Ometer.................

37

7. The Effect of Detergent Concentration, Builder, and Hardness of Water on Soil Removal from Viscose Fabrics Washed in the Launder-Ometer........................

38

8. The Effect of Detergent Concentration, Builder, and Hardness of Water on Soil Removal from Cellulose Acetate Fabrics Washed in the Launder-Ometer. .......................

39

9* The Effect of Detergent Concentration, Builder, and Hardness of Water on Soil Removal from Nylon Fabrics Washed in the Launder-Ometer. . . . . . . . . ................... . . .

40

10. The Effect of Detergent Concentration, Builder, and Hardness of Water on Soil Removal from Wool Fabrics Washed in the Launder-Ometer. ..................... 11. The Effect of Type cf Detergent and Builder on the Soil Re­ moved from Cotton and Viscose in One "Washing in the "Washing M a c h i n e .......... ....................... * . . 12. The Effect of Type of Detergent and Builder on the Soil Removed from Cellulose Acetate and Nylon Fabrics in One Washing in the Washing Machine. ...............

41

50

51

FIGURES CÛNT'Û. Figure

Page

13. The Effect of Type of Detergent and Builder on the Soil Removed from Wool Fabrics in One Washing in the Washing Machine...............................................

52

14. The Effect of Type of Detergent and Builder on the Percentage of Loss in the Warp Breaking Strength of Cotton and Viscose Fabrics after Fifty Washes •

65

15. The Effect of Type of Detergent and Builder on the Percentage of Loss in the Warp Breaking Strength of Spun and Filament Cellulose Acetate Fabrics after Fifty Washes ♦ 66 16. The Effect of Type of Detergent and Builder on the Percentage of Loss in the Warp Breaking Strength of Spun and Filament Nylon Fabrics after Fifty Washes .............. . . . . 67 17• The Effect of the Number of Washes and Type of Detergent on .............................. Wool Shrinkage (Warp).

72

ABSTRACT In the first two sections of this study sixteen synthetic deter­ gents, some of which contained a builder and some which did not, were tested for their ability to remove an artificial soil containing Oildag, hydrogenated vegetable oil, and carbon tetrachloride from five different types of fabrics, cotton, spun viscose, spun cellulose acetate, spun nylon, and wool.

Six different chemical classifications were represented.

These were the alkyl sulfates, the alkyl aryl sulfonates, the sulfonated esters, the sulfonated amides, the non-ionics, and an alkylated aryl polyether sulfonate. In the first part of the study the ability of the detergents

in

0 .075» 0 .15, 0.30, 0.45, and O .60 per cent concentrations to remove soil from the various fabrics was determined in the Launder-Ometer in both distilled water and water containing 300 p.p.m. calcium carbonate. Samples of soiled fabrics were washed for twenty minutes at 120°F.

The

amount of soil removed from the fabrics was determined by reading the light reflectances of the fabrics with a Hunter reflectometer, both be­ fore and after washing. For the second part of the study soiled and original white samples of each of the five fabrics plus enough cotton muslin pieces to make a seven pound load were washed in a 0.15 per cent solution of each deter­ gent in a conventional washing machine, using zeolite-softened water for ten minutes at 120°F.

These samples were given five successive washings

and their light reflectances were measured between each wash.

In addition,

extra sets of samples were washed once in each detergent go determine the amount of oil removed from the fabric during the washing process.

A Beckman pH meter was used to determine the pH of each of the de­ tergents in a 0.15 per cent solution in zeolite-softened water. In the third part of this study each of the five fabrics plus sam­ ples of a filament nylon fabric and of a filament cellulose acetate fab­ ric were washed in a 0.15 per cent solution of eleven of the original sixteen detergents in zeolite-softened water.

In addition a twelfth

group of samples was washed in water containing no detergent in order to determine the amount of mechanical degradation of the fabrics during the washing process.

The washing machine, the length of the wash cycle, and

the washing temperature were all the same as the ones in the second part of the study.

The samples were washed for 10, 20, 30, 40, and 50 washes.

The washing load was maintained at seven pounds by the addition of cotton muslin load pieces as needed. The amount of degradation of the fabrics was determined by: 1. The loss in the wet breaking strengths after 10,'20, 30, 40, and

50 washes for all of the fabrics except wool. 2. The loss in viscosity at 25°C. of the cupriethylene diamine solutions of the cotton and viscose samples after ten and fifty washes. 3. The amount of shrinkage of the wool samples after 5, 10, 20, 30, 40, and 50 washes. 4. Tests for oxidation of the wool and also for alkali damage to the wool. In both the soil removal and the degradation studies, there were very few statistically significant differences between the results ob­ tained with the various types of detergents.

In the soil removal study

a liquid non-ionic detergent removed more soil than did any other

detergent in the study. in low concentrations.

This detergent was especially good when used Conversely, far less soil was removed by the

alkylated aryl polyether sulfonate than by any other detergent in this study. There was a slight loss in the ability to remove soil when hard water was used to make the detergent solutions of low concentrations. The built detergents lost a little more of their effectiveness in hard water than did the unbuilt detergents.

The alkyl aryl sulfonate deter­

gents were especially poor in their stability to hard water. The optimum amount of soil removal was obtained at a detergent con­ centration of 0.30 per cent.

There was a sharp rise in the amount of

soil removed when the detergent concentration was raised from 0.075 to 0.30 per cent.

After this point the increase of soil removal with in­

creasing concentration was much slower. The presence of builder in the detergent assisted in removing the soil from the nylon and wool fabrics, but had little effect on the soil removal from the other types of fabrics.

The built detergents caused a

greater loss of breaking strength with every fabric than did the unbuilt detergents.

This loss was especially pronounced with the acetate and

filament nylon fabrics.

However, the builder did not seem to affect

the amount of wool shrinkage or the loss in viscosity of the viscose samples. There was a small but significant correlation between the amounts of soil removed by the various detergents in the Launder-Ometer and in the washing machine.

There were no significant correlations between

the amounts of oil removed and the amounts of soil removed from the various fabrics or between the pH of the detergent solutions and the amount of oil removed or the amount of wool shrinkage.

There was an almost per­

fect linear correlation between the time of agitation and the amount of wool shrinkage when that shrinkage was between 10 and 30 per cent. Washing the fabrics without a detergent caused as much or nearly as much degradation as did washing than in detergent solutions on all fabrics except nylon and wool.

There was definitely more shrinkage when the

wool fabrics were washed in the detergent solutions than when they were washed without a detergent.

In so far as this study was able to deter­

mine, there was no chemical degradation of the wool fabrics.

THE EFFECT OF VARIOUS SYNTHETIC DETERGENTS ON COTTON, VISCOSE, CELLULOSE ACETATE, NYLON, AND WOOL FABRICS AS DETERMINED BY SOIL REMOVAL AND DEGRADATION INTRODUCTION

For the past fifteen years there has been an ever increasing num­ ber of synthetic detergents placed on the market, not only for use in industry but also for use in the home.

Industrial concerns have been

able to evaluate the detergents objectively and to select the best for their purposes.

But the consumer in the home is confronted with a be­

wildering array of boxes on the grocers shelves and bombarded continu­ ally with advertising concerning the merits of this or that cleansing agent.

In many cases, the detergents have not been adequately tested

before placing them on the market. Furthermore, there has been very little clearly written material which could help the housewife in her attempt to wash her clothes in the best way possible.

This has not been

entirely the fault of either the manufacturing firms or the educational sources, but rather has been the effect of the confusion resulting from the extremely rapid growth of the industry* There have been many studies made in order to develop an adequate method for testing detergents in the laboratory.

At this time, however,

the results from these studies do not correlate very well with the re­ sults obtained in actual use tests.

Some studies have been made on the

efficacy of the various detergents in their removal of soil. most of these studies have been done on cotton alone. from other fibers has received very little study.

However,

The soil removal

And neither have very

many studies been made on the degradation of the fabrics during the washing process.

2

It was the aim of this study to determine the effect of sixteen synthetic detergents of six different chemical types, both built and un­ built, on five different types of fibers, cotton, viscose, cellulose acetate, nylon, and wool.

The ability of these detergents to remove an

artificial soil from the five types of fabrics was to be determined in the Launder-Ometer in both hard and distilled water at 120°F.

Each de­

tergent was to be tested at five concentrations, 0.075» 0*15, 0.30, 0.45, and 0.60 per cent. Next, all sixteen of the detergents were to be tested for their ability to remove soil from each of the five fabrics in the washing machine at 120°F.

In this study, only one concentration, that of 0.15

per cent, was to be studied. practical for most detergents pacity of the washing machine.

A concentration higher than this is not produce suds too voluminous for the ca­ The ability of the detergents to remove

oil from all of the fabrics under these conditions was also to be determined.

It was hoped that there would be a correlation between the

results obtained when the fabrics were washed in the Launder-Ometer and those obtained when they were washed in the washing machine. The third part of the research was to be a study of the degradation of the fabrics by eleven of the original sixteen detergents during the washing process.

In addition, the mechanical degradation of the fabrics

during the washing process was to be determined by washing the fabrics without a detergent, holding all other variables constant.

This de­

gradation was to be determined by the losses in breaking strength, the losses in cellulose viscosity using cupriethylene diamine as the solvent, the amount of wool shrinkage, and by various chemical tests for wool degradation.

3

A SÜRVÏùY OF THE LITERATURE

It seems incredible that an industry which manufactured 600 million pounds of detergents and surface active agents in 1947 (26) was almost completely unknown in the 1930's. troduced to the American market.

In the early 1930fs Gardinol was in­ In spite of its high price (much higher

than that of the soaps which had been the important cleansing agents for hundreds of years prior to this discovery) it found an immediate accep­ tance in the industrial market.

Soon after this, Dreft appeared on the

market for use in dishwashing and the washing of fine fabrics. The main reasons for this rapid growth of a new industry are three­ fold.

The first is the relative stability of the synthetic detergents

to hard water, that is water containing calcium and magnesium ions.

It

is a well-known fact that the calcium and magnesium salts of the fatty acids used in soaps are insoluble in water,

These lime soaps, as they

are called, not only reduce the cleansing efficiency of the soap solutions, thereby making the use of soaps uneconomical in hard water, but they also tend to precipitate onto the fabric, causing stiffness and color when the fabric is ironed.

The stability of the synthetic detergents in hard

water is a great boon to housewives in hard water areas, especially the Midwest, for the installation of water-softening equipment is expensive. The second reason is the stability of many of these synthetic de­ tergents in acid solutions.

Mille this is of little importance to the

housewife, it is extremely important to textile mill men, since many textile operations which require a surface active agent are carried out in acid solutions. The third reason is the greater efficiency of many of the synthetic

4

detergents, especially the newer non-ionics, in scouring wool. The im­ proved efficiency of the non-ionics on wool has been explained by Schwartz and. Perry (3)•

They claim that since these detergents do not ionize in

water solutions, they are not adsorbed by the ionizable amino acids in the wool as are the ionic detergents.

When such adsorption takes place,

the detergent concentration is lowered, thereby reducing the cleaning efficiency and also the ability to suspend solid soil (14)* After it became apparent that the synthetic detergents had definite uses in which they were superior to soap and other cleansing agents, the market expanded rapidly.

Although the myriad number of detergents and

their different tradenames is highly confusing, order can be restored by grouping these detergents into six main chemical classifications.

The

first four of these groups are anionic detergents, while the fifth and sixth are cationic and non-ionic respectively. 1. The alkyl sulfates. veloped.

The six groups are:

These were the first detergents to be de­

They are stable in acid, alkaline, and hard water solutions.

Their production probably accounts for 20 per cent of the total produc­ tion of synthetic detergents (26). 2. The alkyl aryl sulfonates.

These detergents are the cheapest to

produce and, therefore, account for about $0 per cent of the total pro­ duction of synthetic detergents (26).

Their stability in hard water and

their power to suspend solid soil are not as good as those of the alkyl sulfate detergents.

The suspending power of these detergents can be

increased by the addition of sodium carboxymethyl cellulose. 3* The sulfonated and sulfated amides.

These detergents are not only

stable in acid, alkali, and hard water, but they are also superior in their soil removing abilities.

5

4» The sulfonated and sulfated esters.

These compounds, although

unaffected by hard water, lack stability in strong acid or alkaline solutions. 5. Cationic detergents. cleansing agents.

These compounds have very little value as

Their main use is in textile finishing operations.

6. Non-ionic detergents.

These compounds posset excellent soil

removal and grease émulsification properties.

Since they are usually

ethers, they are extremely stable in acid and alkaline solutions.

They

are compatible with both the anionic and cationic types of detergents. It has been reported that if a mixed detergent, containing both anionic and non-ionic compounds, is used the soil removal will be greater than that obtained with either type alone. In addition to the organic detergents, there are many alkaline salts, such as the phosphates, carbonates, and metasilicates, which are often added to these detergents,

when these compounds are used in such

a way, they are termed builders.

Their functions, as outlined by tes­

terling (2?) are: 1. To neutralize the slightly acid reaction of soiled fabric in water. 2. To soften hard water. 3. To prevent the hydrolysis of the detergent which sometimes occurs at high temperatures, especially when the detergent concentration is low. 4. To improve the efficiency in removing soil. The removal of soil from a fabric is far from being a simple, straightforward process. For example, the properties which a detergent

6

must have in order to be able to remove soil effectively have been listed by Dr. Malcolm Dole (14.) as follows: 1. The surface tension of the water must be lowered.

This has been

shown to be quite important. 2. The solid particles must be wetted by the detergent solution. 3. The detergent solution must be able to penetrate into the ca­ pillary pores of the solid particle.

Penetration is important, whether

it is into the fabric or into the dirt. 4. The dispersion or the émulsification of the grease or other hy­ drophobic solids in the detergent solution.

That is, after the soap

solution has penetrated into the fabric, it is necessary to emulsify the grease that holds the dirt to the fabric; or if it is just dirt without grease, it is necessary to disperse or deflocculate the dirt. 5« The detachment of the grease from the fabric. Sisley has not only listed the preceding properties which a deter­ gent must have, but has also listed other variables (30) such as: 1. The power to protect against redeposition of soil. 2. The resistance to lime salts (hard water). He also states that the efficacy of any one detergent will depend upon: 1. Its chemical composition 2. Its concentration 3. The temperature of the washing solution 4» The nature of the mechanical treatment applied. Both Sisley and Dole agree that the penetration of the fabric is of extreme importance.

Since the soil lies within the fabric as well as

on the surface, the detergent must penetrate into the capillaries in

7

order to remove this soil.

The lowering of the surface tension, wetting,

and émulsification of the grease are important in removing the soil from the fabric.

The actual removal of the soil from the fabric is accom­

plished because the detergents have a hydrophobic part of the molecule which has a stronger attraction for the soil than does the fabric.

In

addition, all detergents must have a hydrophilic group in the molecule in order that they may be soluble in water, Untermohlen (36) has not agreed that soil is removed from a fabric by the émulsification of the grease binding that soil to the fabric, since fabrics which were run through a soiling solution containing more oil were not cleansed as efficiently as fabrics which were soiled with little or no oil in the soiling solution.

At this time, no other work

has corroborated his theory. After the soil has been removed from the fabric, it must still be held in suspension in the detergent solution.

If the soil is allowed

to redeposit on the fabric, then we have the familiar "tattle-tale gray" wash.

This suspending power can be changed by concentration, presence

of alkali, and washing time (14).

In all three cases the curves showing

the suspending power of a detergent rise to a maximum with an increase in the variable (such as time or concentration), and then drop off as the variable is increased still further. Since the number of detergents increased so rapidly, it was obvious­ ly an impossible task to determine the effectiveness of each one in an actual use test.

For this reason, the development of a rapid laboratory

test for determining the amount of soil removed by a detergent became mandatory.

The first attempts were extremely discouraging, not only

8

from the point of reproducibility, but also in their lack of agreement with the results of actual use tests.

Gradually the methods have been

improved (8) (9) (11) (13) (16) (1?) (22) (23) (35) (40), although there is still no standard method which has been accepted by the American Association of Textile Chemists and Colorists. In general, these methods consist of soiling a white cotton fabric, usually Indian Head, in a soiling mixture consisting of carbon, oil, fat, and a solvent.

The most accepted soiling solution seems to be

one containing Oildag (graphite suspended in lubricating oil), a hydro­ genated vegetable oil or a mineral oil, and carbon tetrachloride.

Hy­

drogenated vegetable oil was substituted for beef tallow which was first used because its rate of oxidation is much slower than that of the tallow.

This oxidation of the oil in the soiling mixture tends to bind

the soil more firmly to the fabric, making it much more difficult to wash out. Even so, most methods require that the soiled fabric be used within 90 days of the time that it was soiled. Usually the soil is applied by drawing the fabric through the soiling mixture and then through a wringer which serves to impregnate the soil in the fabric and to remove the excess soiling solution. After the fabrics are soiled, the degree of soiling is measured by determining the light reflectance of the samples.

Many people (8)

(35) have agreed that the change in light reflectance of the samples is not a linear function of the amount of soil removed during the washing process.

Bacon and Smith (8) have developed a formula for use with a

Lange reflectometer which they claim will give the actual per cent of soil removed.

However, for most comparative purposes, soil removal is

9

still calculated as a linear function of the change in light reflectance of the samples.

There are many types of refhectometers in use for

measuring light reflectance.

One of the most common, although not the

easiest to use, is the Hunter Reflectometer.

It is based on the null

principle, in which a monochromatic beam of light is split, one-half going to a standard gloss plate and then to a photoelectric cell, while the second strikes the sample and is reflected into a second photoelec­ tric cell.

This second cell is movable, so that the amount of light

going into it can be varied to exactly match that going into the standard cell.

After washihg the samples are again measured for their light

reflectance* The usual means of agitating the samples is in the standard Launder-Ometer, although many tests are run under actual use conditions■ While the problem of reproducibility has been greatly reduced, the prob­ lem of the correlation of the Laund er-Omet er tests with the actual use tests is still largely unsolved. Almost all of the soil removal studies, which have been repor­ ted in the literature, have been done on cotton.

The soil removal from

wool has been studied to a slight extent (11) (17)> but has received far less attention than has the soil removal from cottoh, while the soil removal from the synthetic fibers has been left virtually unstudied (11)• One of the most recent studies on the soil removal from both wool and cotton (17) has shown that the alkyl sulfate, one sulfonated ester, and the non-ionic detergents removed the most soil from cotton while the built non-ionics were the most efficient in their soil removal from wool.

The results of this study also showed that the unbuilt non-ionic

10

detergents were the least effective in their soil removal from wool fabrics. In addition to determining the effect of these detergents upon the removal of soil from a fabric, it has also been deemed necessary to study their effect on the fabrics during the washing process (15) (18). The damaging effects of the washing process have been determined in many ways.

Among the more important are:

1. The breaking strengths of the fabrics.

Since the degradation

seems to be more apparent in the wet strengths (15) , the ravel strips are usually broken wet in this test.

Standard methods for this test

are available in many places (1) (4) (6). 2. The viscosities of solutions of the fibers.

These viscosities

are a measure of the chain length of the molecules of the fibers.

Any­

thing which reduces this chain length will also reduce the viscosity of the solution of the fiber.

A reduction in the viscosity of the solution

usually correlates very well with a reduction in the tenacity of a fila­ ment yarn or of a fiber.

The most important are the cellulose viscosi­

ties using cuprammonium solution as the solvent.

Recently, the use of

cupriethylene diamine as the solvent has been increasing since these solutions are much more stable to light and air than are the cuprammonium solutions (1) (25) (33) (34)»

This use of the more stable solutions

has increased the reproducibility of the results obtainable from such a measurement.

Various types of viscometers can be used for the test, but

the most common are the pipette and the Ostwald-Cannon-lfenske capillary tubes (1) (34)*

11

3* Shrinkage of the fabric.

This test is especially valuable for

wool, since it tends to shrink and felt to a great extent in the presence of heat, mechanical action, and moisture. 4* Other tests for wool damage. damage devised.

There have been many tests for wool

Among the more important are the tests for oxidation de­

veloped by Harris and his co-workers (19) (28), the test for alkali damage (6), and the test for total sulfur content (6) (15).

The Pauly

test for damage to the scales has been widely publicized (4) (5) (6), but without any reference to its reliability. Very few actual studies have been made on damage to fabrics other than wool during the washing process.

In those that have been done (15)

(18) the damage seemed to be caused by mechanical agitation of the fab­ rics while they were wet.

This was shown by the fact that the fabrics

were degraded as much when they were washed without a detergent as they were when they were washed with a detergent.

In one study that has

been made which compared the relative losses in breaking strength of the different fibers (15), the percentages of the original wet breaking strengths which were lost after fifty washes were: 1. Cellulose acetate

8

2. Cotton

15

3. Viscose

25

4. Linen

50

The mechanism of wool shrinkage has been studied by many people. The work which is most pertinent to this study has been reported by Creely and LeOompte (12), Ester (15)» and Harris (20).

Ester reported

that wool fabrics which were washed with an aryl sulfonate detergent

12

shrank more than did those washed in water alone, while those washed in soap solutions shrank even less than did those washed in water alone. This action was partially explained by Creely and LeCam.pte when they found that the lubricating property of the detergent solution had a pronounced effect on the shrinkage of wool.

That is, as the lubrication

of the wool increased, so did the shrinkage* The reports on the effect of the pH of the washing solution on the degree of wool shrinkage are conflicting*

Creely and LeCompte report that

increasing the pH between 8.0 and 10*30 resulted in increasing the shrinkage of the wool fabrics*

However, Ester (15) reported no corre­

lation between the pH of the washing solutions and the amount of wool shrinkage.

13

PROCEDURE Part I The Removal of Soil by Synthetic Detergents in the Launder-Ometer

Fabric.

In this study five different types of fabrics were used.

These were cotton Indian Head, spun viscose, spun cellulose acetate, spun nylon, and wool crepe. parable weights.

An effort was made to have fabrics of com­

However, the nylon, a chafer duck, was slightly heavier

per square yard than were the other fabrics.

All fabrics were woven with

a plain weave. Soiling.

All fabrics were soiled with a soiling solution consisting

of:

l6o grams of hydrogenated vegetable oil 100 grams of Oildag 8 liters of carbon tetrachloride After cutting the fabrics into strips one yard long and eight inches wide, the strips were run through the soiling solution and then through a wringer in order to remove the excess solution.

They were then re­

versed end for end and top for bottom and the padding operation was repeated.

An attempt was made to soil the fabrics just enough to give

an original light reflectance reading of .200— .225 Hunter Units.

Be­

cause the spun nylon accepted the soil so readily, it was run through only once.

Even so, it was soiled more heavily (since its average light

reflectance was .175 Hunter Units) than were any of the other fabrics. After the solvent had evaporated, the fabrics were brushed to remove loose soil, cut into four by four inch squares, and numbered. ples were washed before they were three months old.

All sam­

u

Light reflectance. The light reflectance of each sample was read on both the front and back before the sample was washed and then again after the sample was washed.

The backings for these readings were made

of the same soiled fabrics as were the samples being read. After wash­ ing readings were made using the duplicate washed sample as a backing. A Hunter Multi-Purpose Reflectometer was used for these readings.

Stan­

dard 45° reflectances were read using green light for illumination. Washing.

Both distilled water and water containing 300 p.p.m.

hardness calculated as calcium carbonate were used for the washing so­ lutions.

The general procedure which was used for preparing the hard

water was as follows : Two parts of magnesium carbonate to one part of calcium carbonate were used— calculating the hardness on the basis of calcium carbonate.

The carbonates were dissolved in hydrochloric acid,

and all free acid evaporated.

The chloride salts were then dissolved in

water and made into a stock solution of the desired hardness. The samples were washed by placing two in a pint Launder-Qmeter jar with 200 ml. of detergent solution and ten one-quarter inch steel balls. The washing temperature was 120°F.

Five different detergent

concentrations (0.075» 0 .15 » 0 .30, 0.45> and 0.60 per cent) were used. These concentrations were calculated on the weight of the detergent as delivered, irrespective of the per cent of active ingredient present. Samples were rinsed in beakers containing water of the same hardness as that used in making the detergent solutions and at a temperature of 120°F. VJhen the samples were spread out to dry, an effort was made to smooth out the wrinkles.

Each test was repeated as a check.

The amount of soil

removed was calculated from a total of eight reflectometer readings.

15

The amount of soil removed by sixteen synthetic detergents was de­ termined in this part of the study.

The synthetic detergents can be

subdivided into the following chemical classifications: 1. Sodium alkyl sulfates a. No builder added b. Builder added

2 1

2. Alkyl aryl sulfonates a. No builder added b. Builder added

5 2

3. Sulfonated esters a. No builder added

2

Sulfonated amide a. No builder added

1

5. Non-ionic a. No builder added b. Builder added

1 1

6. Alkylated aryl polyether sulfonate a. No builder added 1 This group included all (nine) of the synthetic detergents generally available for use in the home laundry at the time that the study was started.

This explains the large number of alkyl aryl sulfonate deter­

gents which were studied.

Besides these there were seven industrial de­

tergents which are nomally used in textile finishing processes. Calculation of results.

The percentage of soil removal was calcu­

lated using the following formula: Per Cent Soil Removal =

vil—S

X 100

where R equals the reflectance of the washed soiled samples S equals the reflectance of the unwashed soiled samples W equals the reflectance of the

original white, unsoiled samples.

The results were calculated for statistically significant differences, using the standard t-p test for statistical significance of the difference.

16

When correlation coefficients were calculated, z transformations were applied in order to determine whether they were significant or not.

17

Part II The Removal of Soil by Synthetic Detergents in a Washing Machine

The fabrics, the soiling procedure, and the procedure for determin­ ing the light reflectance are the same for this part of the study as they were for the Launder-Omet er study. Test bundles.

Test bundles were made by sewing together a four by

eight inch piece of each of the soiled and original white fabrics.

In

order that the test bundles would not be too long, the cotton, viscose, and wool samples were sewn into one strip while the cellulose acetate and nylon samples were sewn into another. Washing. The samples were washed in a centrally agitated, non­ automatic washing machine which contained 14.8 gallons of water*

Enough

detergent (84 grams) was added to give a detergent concentration of 0.15 per cent.

All of the water used in this test was softened by passing

through a zeolite water softener.

The grains of hardness did not exceed

four per gallon or about 70 p.p.m. hardness. washed in each load.

Two test bundles were

In addition enough cotton muslin pieces were added

to bring the total load up to seven pounds.

These load pieces had an

area of one square yard. The samples were washed in the detergent solutions for ten minutes and then were given two three minute rinses.

Between the wash and the

rinse, and between the rinses, the fabrics were run through a wringer to remove excess water.

The temperature of both the wash and rinse waters

was 1 2 0 The test bundles were washed five times.

Between each wash,

however, they were dried and the light reflectances of the samples were read.

All sixteen of the detergents were tested.

18

pH.

In addition the pH of each of the sixteen detergents was de­

termined in a solution containing 0.15 per cent by weight of detergent in zeolite-softened water.

A Beckman pH meter was used for these

d et ermi nat i ons. Oil extraction. After an extra set of samples had been washed once with each detergent, the oil from the soiled samples was extracted with carbon tetrachloride in Soxhlet extractors. to siphon twelve times.

The Soxhlets were allowed

Samples of the original soiled fabrics were also

extracted in order to determine the amount of oil which was deposited on the different types of fabrics. Calculation of results.

The formula used for the per cent soil

removed during the first wash and also after the five washes was the same as that used in the Launder-0meter study.

Other formulas which were

used in the calculation of results are: Per Cent Soil Removed during 2nd Wash =

w -S-j_

x 100

where Rg equals the reflectance of the soiled samples after the second wash S^ equals the reflectance of the soiled samples after the first wash W

equals the reflectance of the original, white samples.

Per Cent Whiteness Retention =

A ,X 100 W

where A equals the light reflectance of the washed white samples W equals the light reflectance of the original, white samples.

Per Cent Oil Removed during Washing -

X 100

where 0 equals the oil present in the soiled samples before washing B equals the oil present in the soiled samples after washing.

19

Part III Fabric Degradation during the Washing Process

Fabrics.

The five kinds of fabrics used during the two preceding

parts of the study were used again in this study.

In addition, a fila­

ment nylon fabric of the type commonly used for uniforms and a filament cellulose acetate fabric were tested.

Both of these fabrics were also

of plain weave constructions. Washing.

The test samples of each original white fabric were twen­

ty-four by eighteen inches* washed at one time.

Five samples of each type of fabric were

In addition, enough muslin load pieces were used to

obtain a seven pound load.

One sample of each type of fabric was removed

from the washing load after 10, 20, 30, 40, and 50 washes.

As the test

samples were removed enough load pieces were added to maintain the seven pound load. Only eleven of the original sixteen detergents were used in this study.

These consisted of an unbuilt commercial detergent, and unbuilt

household laundry detergent, and a built household laundry detergent for both the alkyl sulfate and alkyl aryl sulfonate detergents.

Both of

the sulfonated esters were included in this study as were the two non­ ionics , and the sulfonated amide*

Besides these, a control set was

washed without a detergent. As in the previous part of the study, the washing temperature was 120°F. and the detergent concentration was 0.15 per cent.

The washing

and rinsing times were also identical with those used in the previous washing machine study.

Likewise, the water was zeolite-softened.

20

Measurement of degradation.

Various methods for the determination

of degradation were used depending upon the type of fabric being tested. These were as follows: 1. Breaking strength.

The wet ravel strip breaking strengths were

determined on both warp and filling yarns on all fabrics except wool (1). Wet breaking strengths were used because a conditioning room was not available and also because it was hoped that any degradation would be more pronounced in the wet breaking strengths than it would be in the dry strengths.

Although the temperature could be kept fairly constant,

dessicator humidification was not feasible for the 8,000 breaking strength strips which were broken for this study.

The wool breaking strengths

were not done because it was felt that the shrinkage of the wool would invalidate any results which were obtained. The cotton and nylon fabrics were tested on a Model J Scott Tester while the viscose and acetate fabrics were tested on a Scott IP-4..

The

IP-4 was used for these fabrics since their wet breaking strengths were so low that the percentage of experimental error which would be obtained . on the Model J would have been excessive. 2. Cellulose viscosities.

The viscosities of the cotton and viscose

samples were determined at 25°C. using 0.500 M. cupriethylene diamine as the solvent.

Since a grinder was not available, the samples were

ravelled out and the yarns cut as small as was possible in order that the pieces might approach the size required by the standard method (1). The Cannon-Fenske modification of the Ostwald viscometer was used for measuring the viscosities of the solutions.

These viscometers were cali­

brated against standard viscosity oils supplied by the National Bureau

21

of Standards.

The solutions were made according to the procedure given

in the A.S.T.M. Standards on Textile Materials, October, 194-8 (!)• 3. Wool shrinkage.

A ten inch square was marked with marking ink

on the fabrics before washing.

After the first five washes all five

samples were measured in four places in both the warp and filling direc­ tions.

This gave a total of twenty measurements in each direction for

each detergent.

Bach sample was measured again in both warp and filling

after its required number of washes.

This gave a total of four measure­

ments in each direction for each detergent for each of the 10, 20, 30,

40 , and 50 wash values. 4. Chemical tests for wool damage.

The Rutherford and Harris quali­

tative method for determining wool oxidation (28) was applied to the samples which had been washed fifty times.

This method is based on the

fact that oxidized wool will oxidize the ferrous ion to the ferric ion, which gives a deep cherry red color when in the presence of the thiocyanate ion.

The Smith and Harris quantitative method for the determi­

nation of wool oxidation (19) which depends upon the solubility of the wool in 0.1 N. sodium hydroxide was also used in an attempt to detect damage to the fabrics. The stannous chloride test (6) for alkali damage was also tried. This test depends upon the formation of stannous sulfide on the fabric which gives a brown color if the cystine linkages have been broken by the alkali.

Apparently the sulfur in these linkages is reduced to a

form which acts like a sulfide when the linkages are attacked by alkali. 5. Abrasion resistance.

Measurement of the abrasion resistance of

these fabrics was attempted using a Taber Abraser with vacuum attachment.

22

However, it was discontinued because of extremely erratic results. Calculation of results# Three percentages were calculated. were: Per Cent Loss in Breaking Strength =

Prffl .X 100

where 0 equals the original wet strength W equals the wet strength after washing.

Per Cent Loss in Viscosity - ■P.t X .X 100 where 0 equals the original viscosity V equals the viscosity after washing.

Per Cent Wool Shrinkage - ..Prf..X 100 where 0 equals the original size S equals the size after washing*

These

23

DISCUSSION OF RESULTS AND CONCLUSIONS Part I The Removal of Soil by Synthetic Detergents in the Launder-Ometer

The results of the Launder-Ometer study are given in Tables 1 through 5.

The same system of numbering of the detergents that is used in Table

I will be used in all succeeding tables contained in the Discussion of Results.

The letter I after the detergent*s number denotes an industrial

detergent, while the letter H denotes a household laundry detergent. The letter B denotes that the detergent has had a builder added, while the letter U denotes that no builder has been added.

Since these

tables contain so much data. Table I will be considered in detail, and then these factors will be studied separately in this order:

the effect

of type of detergent, the effect of builder, the effect of hardness of water, and the effect of detergent concentration. In Table I it may be seen that an increase in the concentration of the detergent solutions increases the per cent of soil removed from the fabric.

The chemical type of the detergent seems to have very little

effect on the amount of soil removed from cotton, although one deter­ gent, No. 14, a liquid non-ionic, removes much more soil than does any other detergent.

Conversely, number 16, an alkylated aryl polyether

sulfonate, removes much less soil than does any other detergent.

The

presence of builder in the detergent does not increase the soil removal from cotton in this test.

Hard water causes a loss of soil removal ef­

ficiency, especially in detergent solutions of low concentrations.

The

exception to the preceding statement is the sulfonated amide, which showed no loss of efficiency in soil removal from cotton in hard water.

24

Table 1 The Percentage of Soil Removed from Cotton /Fabrics Washed in the Launder-Ometer Hard Water

Distilled Water Detergent

Concentration in Per Cent 0.075 0.15 0.30 0.45 0.60 0.075 0.15 0.30 0.45 0.60

âlkyl Sulfates 1 XU 2 HR 3 HB

4.3 1.8 4.6

7.2 12.5 13.2 12.8 5.5 9.2 11.3 12.5 3.9 8.5 13.7 14.3

3.1 1.4 0.4

9.1 11.1 12.3 12.1 6.1 11.3 9.1 12.9 1.3 10.2 15.7 13.4

Avge

3.6

5.5 10.1 12.4 13.2

1.6

5.5 10.9 12.3 12.8

0.9 4.9 5.0 2.8 3.4 3.2 3.0

2.6 9.4 8.6 8.4 7.6 7.7 6.9 11.1 3.6 5.2 8.6 10.4 5*0 12.9 12.8 14.3 4.8 9.8 10.6 10.9 6.4 10.1 11.3 11.9 5.0 7.0 10.4 9.6

0.1 0.0 0.0 0.8 1.7 0.3 4.1

0.4 2.7 2.5 2.8 3.9 1.7 2.6

1.9 3.4 8.0 6.5 5.7 4.7 4.6 5.6 7.6 3.0 9.4 10.1 8.7 12.1 12.9 8.4 8.8 11.3 9.3 10.8 10.1

3.3

5.0

9.9 10.9

1.0

2.4

6.1

5.9 3.8

8.2 10.2 11.4 11.1 5.7 8.4 10.1 9.3

2.9 2.6

5.5 12.0 15.3 14.4 4.4 7.3 7.6 10.5

4.8

7.0

9.3 10.8 10.2

2.8

5.0

4.4

6.4

8.8 10.0 10.3

4.6

6.6 10.2 13.5 15.0

Alkyl Aryl Sulfonates 4 IU 5 IU 6 HU 7 HU 8 HU 9 HB 10 HB Avg. Sulfonated Esters 11 IU 12 HU Avg. Sulfonated Amide 13 IU Non-Ionics 14 IU 15 HB Avg.

8.8

8.0

9.2

9.6 11.4 12.4

15.7 21.8 27.6 27.8 25.6 4.9 7.3 10.4 9.3 8.2

12.8 18.6 17.3 16.7 16.4 3.4 4.6 7.5 8.7 8.6

10.3 14.6 19.0 18.6 16.9

8.1 11.6 12.4 12.7 12.5

Miscellaneous 16 IU

1.8

2.6

3.1

1.5

0.2

0.0

1.2

3.6

Avg. of all Unbuilt

4.5

6.8 10.3 11.2 11.7

2.7

5.2

7.9

8.3

9.3

Avg. of all Built

3.9

5.6

9.0 11.2 11.0

2.0

2.6

8.8 11.0 10.8

2.1

2.6

25

Table 2

The Percentage of Soil Removed from Viscose Fabrics Washed in the Launder-Ometer Hard Water

Distilled Water Detergent

Concentration in Per Cent 0.075 0.15 0.30 0.45 0.60

0.075 0.15 0.30 0.45 0. 60

Alkyl Sulfates 1 IU 2 HU 3 HB

16.0 19.3 23.4 23.7 22.6 15.9 19.9 25.7 26.1 26.4 17.0 21.1 24.8 24.9 24.0

15.2 20.4 20.4 20.8 22.4 12.2 17.4 18.3 20.3 16.6 4.6 14.4 22.3 24.0 25.2

Avg.

16.3 20.1 24.6 24.9 24.3

10.7 17.4 20.3 21.7 21.4

5.2 14.8 8.8 6.9 11.7 15.0 10.6

0.0 3.7 3.3 2.0 11.1 2.8 3.5

Alkyl Aryl Sulfonates 4 IU 5 IU 6 HU 7 HU 8 HU 9 HB 10 HB Avg.

16.5 13.9 15.2 10.1 17.7 20.6 21.0

23.2 17.4 16.8 18.3 20.3 20.4 23.1

22.8 19.0 16.0 20.2 21.8 21.4 25.6

23.0 20.5 15.8 19.0 17.9 21.9 24.8

7.8 12.4 10.1 11.6 19.2 14.8 13.3

14.0 14.6 12.2 16.6 21.9 20.6 18.6

16.3 16.4 16.6 19.5 19.0 21.8 18.9

15.8 17.8 17.9 18.9 19.2 20.0 19.8

10.4 16.4 19.9 21.0 20.4

3.8 12.7 16.9 18.4 18.5

16.6 19.8 20.4 22.2 23.1 22.2 18.6 20.2 20.3 20.7

11.6 16.0 20.6 21.9 20.9 9.3 14.5 18.1 19.6 20.7

19.4 19.2 20.3 21.2 21.9

10.4 15.2 19.4 20.8 20.8

Sulfonated .Amide 13 IU

17.1 16.2 17.9 19.2 20.0

11.8 15.5 17.4 18.2 17.4

Non-Ionics 14 IU 15 HB

21.2 24.6 26.9 26.0 23.8 12.4 18.0 19.9 20.5 18.8

15.2 17.6 19.4 18.1 17.5 5.6 13.8 15.2 16.5 17.5

17.6 21.3 23.4 22.8 21.3

10.4 15.7 17.3 17.3 17.5

Sulfonated Esters 11 IU 12 HU Avg.

Avg. Miscellaneous 16 IU

8.6

6.7

8.2 13.7 15.0

0.2

0.7

7.5 12.6 16.2

Avg. of all Unbuilt

13.7 16.5 19.9 20.9 20. 6

8.0 13.6 16.8 18.3 18.4

Avg. of all Built

13.8 20.2 22.1 23.2 22.4

4.1 14.1 19.2 20.3 20.6

26

Table 3 The Percentage of Soil Removed from Cellulose Acetate Fabrics Washed in the Launder-Ometer Hard 'Water

Distilled Water Detergent

Concentration in Per Cent 0.075 0.15 0.30 0.45 0.60

0.075 0.15 0.30 0.45 0.60

âlkyl Sulfates 1 IU 2 HU 3 HB

19.6 29.2 32.7 31.6 31.1 23.5 32.6 34.9 32.2 28.0 23.4 26.7 32.6 35.0 33.2

25.0 27.8 30.8 28.3 29.3 21.9 22.0 25.5 26.2 25.3 3.6 22.8 26.4 27.8 27.5

Avg.

22.2 29.4 33.4 32.9 30.8

16.8 24.2 27.6 27.4 27.4

âlkyl Aryl Sulfonates 4 IU 5 IU 6 HU 7 HU 8 HU 9 HB 10 HB

12.9 18.1 17.6 16.7 17.9 20.1 16.1

31.3 24.8 25.6 27.4 23.6 31.1 28.6

33.4 27.1 23.4 29.5 28.4 32.2 30.6

28.9 25.7 24.9 27.3 28.7 30.7 32.2

30.9 24.9 25.9 26.8 25.1 31.5 34.4

2.1 1.9 0.8 1.4 12.8 1.4 3.4

6.2 21.9 3.2 1.8 20.6 16.2 18.8

26.3 18.2 17.8 24.5 20.5 23.4 32.2

27.2 16.0 17.0 25.2 24.6 24.8 30. 6

25.7 15.8 20.1 23.4 23.6 26.8 32.6

17.1 27.5 29.2 28.3 28.5

3.4 12.7 23.3 23.6 24.0

29.8 31.1 33.2 33.7 35.1 18.9 23.0 27.4 24.3 25.8

14.9 21.1 28.6 30. 5 29.9 17.4 26.0 25.9 28.0 27.3

24.4 27.1 30.3 29.0 30.4

16.2 23.6 27.2 29.2 28.6

Sulfonated Amide 13 IU

27.7 25.9 29.3 28.9 28.7

16.2 20.0 22.7 24.2 25.2

Non-Ionics 14 IU 15 HB

26.5 30.1 30.7 31.5 29.0 18.9 19.8 20.1 20.8 21.9

20.9 24.6 24.6 24.4 25.9 7.0 16.2 21.2 21.3 21.4

22.6 24.9 25.4 26.2 25.4

14.0 20.4 23.0 22.9 23.7

Avg. Sulfonated Esters 11 IU 12 HU Avg.

Avg. Miscellaneous 16 IU

11.3 14.8 16.7 20.1 22.3

Avg. of all Unbuilt

20.0 26.6 28.9 28.2 27.8

11.7 16.9 23.2 25.0 24.9

Avg. of all Built

19.6 2 6.6 28.8 29.6 30.2

3.8 18.5 25.3 26.2 27.1

5. 6

7.3 12.8 27.4 26.8

27

Table 4 The Percentage of Soil Removed from Rylon Fabrics Washed in the Launder-Omet er Hard Water

Distilled Water Detergent

Concentration in Per Cent 0.075 0.15 0.30 0.45 0.60

0.075 0.15 0.30 0.45 0.60

àlkyl Sulfates 1 IU 2 HU 3 HB

0.1 16.1 29.4 29.8 28.3 0.0 7.2 28.2 31.0 29.5 6.3 24.6 27.6 27.3 30.4

0.5 17.9 25.2 25.4 27.8 0.0 4.7 16.8 22.2 23.5 0.0 0.7 23.3 23.6 25.5

Avg.

2.1 16.0 28.4 29.4 29.4

0.2

7.8 21.8 23.7 25.6

0.0 2.9 25.8 0.0 5.7 24.0 0.0 3.2 22.8 0.0 1.7 23.4 0.0 5.2 22.0 1.2 25.0 22.6 0.7 9.2 24.8

26.4 24.8 24.0 25.6 20.0 25.8 28.0

0.0 0.0 0.0 0.0 0.7 0.0 0.0

0.0 0.2 0.0 0.0 9.0 0.9 0.0

7.6 23.6 23.8 25.0

0.1

1.4 15.1 18.4 19.4

AJkyl Aryl Sulfonates 4 IU 5 IU 6 HU 7 HU 8 HU 9 HB 10 HB Avg. Sulfonated Esters 11 IU 12 HU Avg. Sulfonated Amide 13 IU Non-Ionics 14 IU 15 KB Avg.

0.3

27.6 18.3 22.8 25.4 22.1 24.9 25.4

14.2 15.4 13.5 9.2 15.6 24.2 13.4

18.5 16.5 15.1 17.0 17.4 24.8 19.3

16.3 18.5 18.0 19.9 18.2 23.3 21.8

6.3 14.6 19.4 22.0 20.7 0.0 0.5 10.1 13.7 16.3

5.0 12.2 19.9 24.8 26.2 0.3 4.1 11.0 15.2 12.8

3.1

2.6

7.6 14.8 17.8 18.5

8.2 15.9 20.5 19.5

8.1 21.2 24.0 23.5 22.9

6.4 14.2 16.6 18.0 22.4

18.6 27.0 27.6 29.1 29.1 1.9 8.3 16.2 16.2 16.2

21.6 25.3 21.8 22.8 23.9 0.0 0.0 2.0 5.9 9.8

10.2 17.6 21.9 22.6 22.6

10.8 12.6 11.9 14.4 16.8

Miscellaneous 16 IU

0.0

0.0

0.9

0.0

0.0

Avg. of all Unbuilt

2.8

8.8 21.4 22.1 22.4

2.9

7.3 15.0 18.3 20.6

Avg. of all Built '

2.5 16.8 22.8 23.4 25.1

0.0

0.4 15.8 18.4 20.1

0.0

0.4

1.1

7.2 19.3

23

Table 5 The Percentage of Soil Removed from 'Tool Fabrics Washed in the Launder-Ometer Hard Water

Distilled Water Detergent

Concentration ir Per Cent 0.075 0.15 0.30 0.45 0.60

0.075 0.15 0.30 0.45 0.60

Alkyl Sulfates 1 IU 2 HU 3 HB

3.9 21.6 56.6 66.9 71.0 2.3 12.5 22.8 35.9 46.3 4.3 13.3 42.6 48.8 59.7

3.9 13.9 51.7 59.6 61.6 0.0 6.8 38.6 56.0 61.6 0.6 5.7 52.4 69.8 72.0

Avg.

3.5 15.8 40.7 50. 5 59.0

1.5

8.8 47.6 61.8 65.1

0.0 0.1 0.3 0.3 0.0 1.0 0.6

44.4 52.6 48.1 58.1 35.4 60.9 49.4

0.0 0.0 0.0 0.0 0.0 0.5 0.1

0.0 4.7 3.9 0.8 1.8 8.5 4.6

0.3 10.9 35.7 45.1 49.8

0.1

3.5 35.7 48.8 53.9

8.3 25.2 45.9 51.2 58.3 0.0 1.0 10.0 21.3 29.7

9.8 23.8 46.6 55.0 59.3 0.0 9.8 32.6 45.5 55.1

4.2 13.1 28.0 36.2 44.0

4.9 16.8 39.6 50.2 57.2

6.7 15.3 26.7 32.7

6.4 23.8 41.2 46.6 53.4

26.2 15.4 13.2 15.1 12.3 10.1 49.6 63.2 60.3 62.3

18.7 20.4 20.6 13. 1 23.2 5.0 24.8 54.3 59.3 58.3

18.6 32.5 38.2 38.0 37.6

11.8 22.6 37.7 58.7 40.8

Alkyl Aryl Sulfonates 4 IU 5 IU 6 HU 7 HU 8 HU 9 HB 10 HB Avg. Sulfonated Esters 11 IU 12 HU Avg. Sulfonated Amide 13 IU Non-Ionics 14 IU 15 HB Avg.

1.1

2.9 12.7 12.3 12.5 1.0 19.7 15.0

27.8 39.8 34.1 46.5 11.4 44.4 45.9

39.6 50.2 43.4 56.0 24.7 53.5 48.4

16.4 40.5 38.0 27.6 20.6 58.4 48.2

41.9 47.3 37.8 43.7 42.2 63.4 65.2

48.4 50.2 46.3 48.2 52.3 67.2 64.4

Miscellaneous 16 IU

0.0

2.1

0.0

0.0

Avg. of all Unbuilt

3.5 10.3 27.0 37.0 40.9

3.2

9.2 31.2 42.1 48.1

Avg. of all Built

4.0 24.4 49.1 52.9 58.2

1.6 10.9 53.4 54.4 65.5

0.0

0.0

0.1

0.0 12.0 16.8

29

The effect of type of detergent on soil removal.

In addition to

Tables 1 through 5, these results are shown in Figures 1 through

In

this study there was one detergent, number 14, which was excellent and another, number 16, which was quite poor in soil removal.

It is es­

pecially interesting to note that the liquid non-ionic detergent, 14, is quite effective at low concentrations, probably because of its high concentration of active ingredient. This is important since the concen­ trations usually used by housewives in laundering fall in the range of 0.075 to 0.15 per cent.

Between these two extremes in ability to remove

soil the differences were very small among the various detergents.

In

this connection, it must be ran embered that in general a difference of between five and seven per cent is needed in order to have a statistic­ ally significant difference.

However, if the total soil removal is be­

low five per cent, then a two per cent difference is sufficient. The results obtained in washing cotton are shown in Table 1 and Figure 1.

On cotton the best soil removal in distilled water was ob­

tained when the non-ionic detergents were used.

The poorest soil re­

moval was obtained when the samples were washed in the alkylated aryl polyether sulfonate, number 16.

There were no significant differences

among any of the other types of detergents.

In general, however, the

industrial detergents in each class seemed to remove slightly more soil than did the household laundry detergents.

This is probably explained

by the higher concentration of active ingredient present in the indus­ trial detergents. On viscose, as shown in Table 2 and Figure 2, number 16 again removed less soil than did any of the other types of detergents.

At the 0.075

30

m — ott

If ât.Qi3

LegenÛ;

Cent

31

in Pejr

32

of B eteri i

o f WiSirgr

o b r3 o jx 3 -

^9mpya4 from

Legend;

yl Sulfates k y l A ry l Bu.. f ouates Ss

dlfeuated ;Ara^ 4-

Distilled Water

Q*d75

0, 15

0

.

0,^5

Detergent Goncent[ratioDJ in Petr Cent

33

Pig. 4:

The E^tlect of Detergent Concentration, Type of Peter-

_________ gent, and Hardness of Water on Soil Removal from Hylon Fabrics Washed in "the Launder-Ometer Hard Water

2e

10 Per Gent Soil Removal

—

Legend : . Alkyl Sulfates X Ab-kyl Aryl Sulfonates

Distilled Water

© Splfonated Amide ® Non-Ionics 3.1

10

20

30

2.0

6.0

4.4

2.0 +3.5 >4.0

Alkyl Sulfates 1 IU 2 HU 3 HB

14.1 11.7 14.8 14.8 17.2 4.6 3.9 5.4 15.6 18.0 6.2 20.8 11.7 29.3 30.5

Avg.

8.3 12.1 10.6 19.9 21.9

Alkyl Aryl Sulfonates 4 IU 7.8 6.2 7.0 11.3 12.1 7 HU *2.4 >1.6 5.4 10.4 11.7 10 HB 10.9 16.8 17.2 29.6 16.8 Avg. Sulfonated Esters 11 IU 12 HU Avg.

5.4

7.1

9.9 17.1 13.5

40

50

50

>2.3 >9.8 3.6 2.4 4.4 +6.0 >6.2 >2.0 1.6 2.0 3.1 4.4 11.2 21.6 18.3 4.3

8.5

8.2

1.2 2.8 +3.5 +2.0 +0.8 2.4 0.0 3.6 5.2

0.8 1.6 6.0

2.0 3.1 6.4

>0.3

2.8

3.8

4.0 6.8 6.8 10.3

3.2 7.6

5.4

5.4

>1.7 +3.9

1.9

>2.3 12.5 13.7 14.8 18.4 9.4 12.1 15.6 20.7 22.6

>3.2 +2.0 4.0 1.2

3.6 12.3 14.6 17.8 20.5

0.4 >0.4

1.4

8.8

Sulfonated Amide 13 IU

+ 5.1 +2.3 +1.2

2.7

+7.2 +6.4 +4.3 +2.8 >2.0

Non-Ionics 14 IU 15 HB

+6.2 +1.2 2.7 3.9 6.3 7.8 21.1 27.7 40.6 37.8

>6.4 +8.8 +4.0 +2.8 +2.0 2.4 8.4 19.1 21. 1 21.1

Avg.

0.8

0.8 10.0 15.2 22.2 22.0

Avg. of all Unbuilt

1.3

Avg. of all Built

8.3 19.6 18.9 33.2 28.3

5.2

7.9 11.5 13.6

+ 2.0 +0.2

7.6

9.2

9.6

+ 2.7 >3.5

0.3

2.3

2.3

1.3

5.5

11.8 16.2 15.3

64

Table 18 The Percentag 3 Of Loss in the Breaking Strength of Spun Nylon Fabrics During Fifty Washes Filling

tfarp Detergent

Number of Washes 10

20

30

40

50

10

0.7

0.0

0.7

4.2

0.0

2.0 +0.7

Alkyl Sulfates 1 IU 2 HU '3 HB

10.6 8.5 10.6 12.0 11.3 9.9 14.9 12.0 12.8 12.8 7.8 9.2 9.2 11.3 9.2

13.1 7.8 9.7 10.3 4.1 2.8

Avg*

9.4 10.9 10.6 12.0 11.1

No Detergent

Alkyl Aryl Sulfonates 4 IU 9.9 6.4 12,8 12.8 11.4 7 HU 14.9 11.4 13.5 13.5 11.4 10 HB 25.6 26.9 23.4 25.6 25.6 Avg. Sulfonated Esters 11 IU 12 HU Avg. Sulfonated Amide 13 IU Non-Ionics 14 IU 15 HB Avg. Avg. of all Unbuilt Avg. of all Built

16.8 14.9 16.6 17.3 16.1

9.0

20

7.0

30

40

50

4.1

4.1

0.0

6.2 5.5 6.2 8.3 10.3 11.7 8.3 4.8 9.8 7.6

6.9

9.2

2.8 2.8 6.9 6.9 5.5 5.5 6.2 9.0 11.7 9.6 19.3 18.6 20.7 19.3 18.6 9.2

9.2 12.2 12.6 11.2

8.5 18.5 19.8 27.6 25.5 7.8 6.4 7.8 7.1 8.5

8.3 12.4 19.3 19.3 24.1 4.8 +0.7 5.5 1.4 8.3

8.2 12.4 13.8 17.4 17.0

6.6

5.8 12.4 10.4 16.2

6.4

9.2 12.8

4.1

3.4

5.5

6.2

7.1 12.7 7.1 5.7 8.5 10.6

6.2 6.9

2.1 9.0

4.1 6.9

3.4 5.5 7.6 13.1

6.4 10.6

8.8

6.6

5.6

5.5

5.5

9.3

9.8 10.6 11.1 12.3 11.0

6.8

5.5

8.1

8.1

9.3

5.6

10.2 12.7 5.0 8.5 7.6 10.6

5.0

12.8 14.9 12.8 15.1 15.1

3.4

10.1 10.1 12.0 10.6 13.8

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[ I

i i i I I ' M ! r.-j..!.. 4 X I i i 11 i I - 14 i 11 ; I 1 1 i I-

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—j—U-i—1— —J— : -.1- -- 1-- J-- L '

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23

31 of Washai

4-

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---------

73

no effect on the amount of shrinkage.

Likewise, no significant corre­

lation was found between the pH of the detergent solutions (see Part II, Table 12) and the per cent shrinkage, although the correlation coefficient was found to be a plus 0.51 after being corrected for the small number of samples.

When a z transformation was applied, however, this was

found to be insignificant because of the small sample size.

If a larger

number of samples were taken, it would probably be possible to find a significant correlation between pH and the amount of shrinkage. Chemical degradation of wool.

In no case was a positive test for

degradation of wool obtained with any of the tests used.

Prom these re­

sults, it can be concluded that the damage to the wool fabrics is caused by mechanical agitation in the presence of water and a detergent*

74

SUMMARY OF RESULTS AND CONCLUSIONS

An attempt was made to determine the effects of sixteen synthetic detergents of six chemical classifications on five different types of fabrics, cotton, viscose, cellulose acetate, nylon, and wool.

The effect

of these detergents was determined by measuring the amount of soil which they removed in both the Launder-Ometer and the washing machine.

In

addition, the degradation of the fabrics during the washing process was determined with eleven of the original detergents and also with water alone. The following conclusions can be drawn from the results of the Launder-Ometer study: 1. The liquid non-ionic detergent removed more soil than did any other detergent in the study.

The alkylated aryl polyether sulfonate

removed less soil than did any other detergent.

Other than these two

cases, there were few significant differences between the amounts of soil removed from the fabrics by the various types of detergents. 2. The non-ionic detergents were especially effective in removing the soil from nylon and wool fabrics. 3. The ability of the detergent solutions of low concentrations, especially when the detergents contained a builder, to remove soil from the fabrics was impaired to a slight extent when calcium and magnesium ions were present in the water.

This was especially noticeable when

the detergents were of the alkyl aryl sulfonate type. 4. The presence of builders in the detergents helped to remove soil from nylon and wool, but had little effect on the soil removal from the other types of fabrics.

75

5» An increase in the concentration of the detergent in the solution increased the amount of soil removed from the cloth.

An optimum amount

of soil removal was attained at about 0.30 per cent detergent concentration* The data on soil removal by the detergents in the washing machine confirmed conclusions one, two, and four of the Launder-Ometer study. Other conclusions which can be drawn are: 1. When repeated washings are made on a soiled sample the greatest amount of the removable soil is removed in the first two washes. 2. Although the correlation coefficients were not high, there was a significant correlation between the amount of soil removed in the washing machine test and that removed in the Launder-Ometer tests. 3. There was no significant correlation between the amount of oil removed and the amount of soil removed from the various fabrics. The results of the fabric degradation study can be summarized as follows : 1. Washing the fabrics without a detergent caused as much or nearly as much loss in breaking strength as did washing them with a detergent. The one exception was nylon, which lost no strength when washed fifty times without a detergent. 2. There wer few, if any, significant differences between the losses of breaking strength caused by the various types of detergents. 3. The built detergents did cause a slightly greater loss in break­ ing strength than did the unbuilt detergents.

This effect was especial­

ly noticeable on the cellulose acetate and filament nylon fabrics. 4. The losses in cellulose viscosity were greater for cotton than they were for viscose.

Here again there were no significant differences

76

between the losses caused by the various types of detergents* 5* Washing wool in the presence of a synthetic detergent caused more shrinkage than did washing it without a detergent. 6. There was a perfect linear correlation between the time of agi­ tation and the amount of shrinkage when that shrinkage was between 10 and 30 per cent* 7. There was no significant correlation in this study between the pH of the detergent solution and the amount of wool shrinkage*

77

BIBLIOGRAPHY. Books 1. American Society for Testing Materials, Standards on Textile Materials, Philadelphia, 1948• 2. Matthew, J. M , , Textile Fibers, New York, John Wiley and Sons, 1947* 3* Schwartz, A. M« and Perry, J. W., Surface Active Agents » New York, Interscience Publishers, Inc., 1949# 4. Skinkle, J. H . , Textile Testing, New York, Chemical Publishing Co., 1940 • 3. Trotman, S. R. and Trotman, B. R., The Bleaching, Dyeing, and Chemical Technology of Textile Fibers, London, Charles Griffin, 1948. 6. Trotman, S. R. and Trotman, B. R., Textile Analysis, London, Charles Griffin, 1948. Articles 7. Bacon, L. R . , Hensley, J. W., and Vaughn, T. H . , "Properties of De­ tergent Solution, " Industrial and .Engineering Chemistry, Vol. 35» ' 1943, pp. 1286-9. 8. Bacon, 0. C. and Smith, J. B . , "Detergent Action", Industrial and Engineering Chemi stry, Vol. 40, 1948, pp• 2361-70. 9. Bacon, 0. C., "A Practical Laboratory Test for Evaluating Scouring Agents for Cotton, " Bulletin of the Technical Laboratory of du Pont. 10. Barker, G. E.,"Nonionic Detergents," Soap and Sanitary Chemicals, Vol. 24, 1948, pp. 46-8, 65. 11. Clark, J. R. and Holland, V. B., "Studies in Soiling and Detergency," American Dyestuff Reporter, Vol. 36, 1947» PP• 734-47# 12. Creely, J. W. and LeCompte, G., "Factors Influencing Wool Felting," American Dyestuff Reporter, Vol. 29, 1940, pp. 292-4. 13. Crowe, J. B., "Cooperative Studies on Laboratory Methods for Evalu­ ating Synthetic Detergents," American Dyestuff Reporter, Vol. 32, 1943, pp. 237-41# 14. Dole, M . , "Physical Chemistry of the Newer Detergent Processes," American Dyestuff Reporter, Vol. 29, 1940, pp. 314-22.

73

15. Sster, V. and Others, "Comparison of an Aryl Sulfonate and Soap for Washing in Hard Water," American Dyestuff Reporter, Toi. 32, 1943» pp. 121—2 , 135—41• 16. Furry, M. S., McLendon, T* I*, and Alder, M. E . , "An Evaluation of Soaps and Synthetic Detergents," American Dyestuff Reporter, Toi. 37» 1948, pp. 751-80. 17. Furry, M. S. and McLendon, T. I . , "Effectiveness^of Detergents in Removing Soil from a Cotton and A Wool Fabric," American Dyestuff Reporter, Toi. 39, 1950, pp. 209-12. 18. Graydon, M. H . , Lindsiey, D. M . , and Brodie, J. B., "Mechanical Degra­ dation of Rayon Fabrics in Domestic Laundry Procedures," American Dyestuff Reporter, Toi. 36, 1947» pp. 397-9. 19. Harris, M. and Smith, A., "An Alkali Solubility Test for Determining the Extent of Wool Oxidation," American Dyestuff Reporter, Toi. 25 » 1936, pp. 542-4 . 20. Harris, M . , "Some Factors Contributing to the Felting of ’ Wool," American Dyestuff Reporter, Toi. 34» 1945> PP• 72-5• 21. Hetzer, J., "Fundamentals of Wetting and Detergent Compounds," Petro­ leum Refiner, Toi. 24, 1945» pp. 199-200. 22. Holland, B. T. and Petrea, A., "Proposed Method for Evaluation of Detergents," American Dyestuff Reporter, Toi. 34» 1943» PP* 534-7* 23. Kelly, A. J. and Gunther, D. H . , "A Simple Laboratory Method for Evaluation of Detergency," Ameri can Dyestuff Reporter, Toi. 38, 1947 » PP. 455-8. 24. Kuentzel, L. E., Hensley, J. W., and Bacon, L. R., "Properties of Detergent Solutions," Industrial and Engineering Chemistry, Toi. 35» 1943, pp. 1286-9. 25. Levy, R. M. and Muffat, P., "The Mature of the Cupriethylene diamine Cellulose Solvent," Paper Trade Journal, Toi. 118, 1944. 26. McCutcheon, J. W., "Synthetic Detergents," Chemical Industries, Toi. 61, 1947, PP. 811-24.

27. Oesterling, J. F. , "Additive Effect of Builders in Detergency," American Dyestuff Reporter, Toi. 27, 1938, pp. 617-20. 28. Rutherford, and Harris, M . , "The Detection of Oxidation in Wool," Journal of Research of National Bureau of Standards, Toi. 20, 1938.

29. Schwartz, A. M . , "New Concepts and Trends in the Detergent Field," Soap and Sanitary Chemicals, Toi. 24, 1948, pp. 51-3» 181, 183.

79

30• Sisley, J. P., "Studies on Detergent Power," American Dyestuff Reporter, Vol. 36, 1947, pp. 457-65. 31. Snell, P. D . , "Some Factors in Detergency,” Paper Trade Journal, Vol. 116, 1943, pp. 128-30. 32. Snell, F. D . , "Surface Active Agents," Industrial and Engineering Chemistry, Vol. 35, 1943, p. 107. 33* Straus, P. L. and Levy, R. M . , "Cupriethylene Diamine Disperse Vis­ cosity of Cellulose," Paper Trade Journal, Vol. 115, 1942. 34. Technical Association of the Pulp and Paper Industry, "Cupriethylene Diamine Disperse Viscosity of Pulp," 1946. 35* Unt ermohlen, ¥• P., Jr., and Wallace, S. L., "Detergency Studies," Textile Research Journal, Vol. 17, 1947, pp. 670-88. 36. Dhtermohlen, W. P., Jr. and Others, "Detergency Studies," Textile Research Journal, Vol. 19, 1949, pp. 489-96. 37# Van Antwerpen, P. J., "Surface Active Agents," Industrial and Engi­ neering Chemistry, Vol. 33, 1941, pp. 16-22.

38. Van Antwerpen. P. J., "Surface Active Agents," Industrial and Engi­ neering Chemistry, Vol. 35, 1943, pp. 126-30. 39* Vaughn, T. H. and Vittone, A., Jr., "Properties of Detergent Solutions," Industrial and Engineering Chemistry, Vol. 35, 1943, pp. 1094-8. 40. Vaughn, T. H. and Vittone, A., Jr., "Properties of Detergent Solutions," Industrial and Engineering Chemistry, Vol. 33, 1941, pp. 1011-9. 41. Wilson, J. L., Measurement of Detergency," Industrial and Engineering Chemistry (Analytical Edition), Vol. 16, 1944, pp. 251-4*

80

VITA

Ruth Marie Legg was born in Lecompte, Louisiana on November 5» 1923• After obtaining the Bachelor of Science Degree in Home Economics from Purdue University in February, 1945» she worked as a chemist for the Acetate Research Section of E. I. DuPont de Nemours and Co. from March, 1945 to August, 1946. From September, 194& to August, 1947 she was textile chemist for the Appliance Testing Laboratories of the General Electric Co., leaving to re-enter Purdue University where she served both as a graduate teach­ ing assistant and a research fellow. She is a member of Alpha Lambda Delta, Sigma Delta Epsilon, Omicron Nu, Sigma Xi (Associate) and of the American Association of Textile Chemists and Colorists.