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Particle size studies: The influence of a synthetic tanning material on quebracho infusions

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UNIVERSITY OF CINCINNATI

I hereby recommend th at the thesis prepared under m y supervision b y - ^ E t f ^entitled

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F orm 668— G. S. and Ed.— 1M— 7-37

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Reproduced with permission of the copyright owner. Further reproduction prohibited without permission.

PARTICLE SIZE STUDIES THE INFLUENCE Of A SYNTHETIC TANNING MATERIAL ON QUEBRACHO INFUSIONS

A d i s s e r t a t i o n s u b m itte d t o t h e G ra d u a te S c h o o l o f A r t s an d S e i e n e e s ©f t h e U n i v e r s i t y o f C i n c i n n a t i i n p a r t i a l f u l f i l l m e n t ©f t h e r e q u i r e m e n ts f o r th e d e g re e ©f DOCTOR 01 PHILOSOPHY

1 11 Dee gom pton Ch* I . U n i v e r s i t y o f C i n c i n n a t i 1939 M* S . U n i v e r s i t y o f C i n c i n n a t i 1940

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UMI Number: DP15700

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I n g r a t e f u l a ck n o w le d g em en t o f th e g u id a n c e a n d a i d w h ic h h e r e c e i v e d fro m D o c to r F r e d o * F l a h e r t y and D o c to r B . M. D o l l a r , t h e a u th o r e x p r e s s e s h i s s i n ­ c e re th a n k s .

And t o t h e M o n san to C h e m ica l Company f o r

t h e F e llo w s h ip w hich made t h i s w ork p o s s i b l e , he e x ­ p r e s s e s h is s in c e r e a p p re c ia tio n *

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ABSTRACT

The e f f e c t o f t a n n i n c o n c e n t r a t i o n a n d t h e ad* d i t i o n o f s y n t h e t i c t a n n i n g m a t e r i a l on t h e p a r t i c l e s i z e o f o r d i n a r y q u e b ra c h o t a n n i n *• m a te r i n f u s i o n s , w as s t u ­ d ie d .

The s t u d y w as made b y u l t r a f i l t r a t i o n .

The r e ­

s u l t s show no a p p a r e n t ch an g e i n p a r t i c l e s i z e e i t h e r w i t h e h an g e i n t a n n i n c o n c e n t r a t i o n o r a d d i t i o n o f s y n ­ t h e t i c ta n n in g m a t e r i a l, w ith in th e l i m i t s o f c o n c e n tra ­ tio n s tu d ie d .

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Table of Contents

S ubject

Page

In tro d u c tio n

1

P u rp o se

1

H is te r i e a l

2

P ro c e d u re

4

E x p e r im e n ta l l e s u i t s

9

D is c u s s io n o f

R e s u lts

20

C o n c lu s io n s

2S

B i b li o g r a p h y

23

k S '42

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L is t o f Tables Subject

T a b le Number

U l t r a f i l t r a t i o n o f O r d in a r y Q ueb raelio I n f u s i o n ( 5 . 0 g . q u e b ra c h o e x t r a c t per l i t e r

I

U l t r a f i l t r a t i o n o f O r d in a r y Q u e b rac h o S y n t h e t i c T an n in g M a t e r i a l I n f u s i o n ( 5 . 0 g . q u e b ra c h o e x t r a c t p l u s 2 .0 g . s y n th e tic ta n n in g m a t e r i a l p e r l i t e r )

II

U l t r a f i l t r a t i o n o f o r d i n a r y Q u e b rac h o S y n t h e t i c T a n n in g M a t e r i a l I n f u s i o n ( 5 . 0 g . q u e b ra c h o e x t r a c t p l u s 1 .0 g . s y n th e tic ta n n in g m a t e r i a l p e r l i t e r )

III

U l t r a f i l t r a t i o n o f O rd in a ry Q u e b rac h o S y n t h e t i c T an n in g M a t e r i a l I n f u s i o n ( 5 .0 g . q u e b ra c h o e x t r a c t p l u s 0 .5 g . s y n th e tic ta n n in g m a te r ia l p e r l i t e r )

IV

U l t r a f i l t r a t i o n o f O r d in a ry Q u eb rach o I n f u s i o n ( 1 0 .0 g . q u e b ra c h o e x t r a c t per lite r ) U l t r a f i l t r a t i o n o f O r d in a r y Q u e b rac h o S y n t h e t i c T a n n in g M a t e r i a l I n f u s i o n (1 O .0 g . q u e b ra c h o e x t r a c t p l u s 4 .0 g . s y n t h e t i c ta n n in g m a t e r i a l p e r l i t e r ) U l t r a f i l t r a t i o n o f O rd in a ry Q u eb rach o I n f u s i o n ( 2 0 .0 g . q u e b ra c h o e x t r a c t per lite r ) U l t r a f i l t r a t i o n o f O r d in a r y Q u eb rach o S y n t h e t i c T a n n in g M a t e r i a l I n f u s i o n ( 2 0 .0 g . q u e b ra c h o e x t r a c t p l u s 8 .0 g . s y n t h e t i c ta n n in g m a t e r i a l p e r l i t e r )

V

VI

V II

V III

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L is t o f I l l u s tr a ti o n s

Subject

Figure Number

U l t r a f i l t r a t i o n o f in f u s io n s c o n ta in in g 5 .0 g . o f q u e b ra c h o e x t r a c t p e r l i t e r

I

U l t r a f i l t r a t i o n o f in f u s io n s c o n ta in in g 1 0 .0 g . o f q u e b ra c h o e x t r a c t p e r l i t e r

II

U l t r a f i l t r a t i o n o f in f u s io n s c o n ta in in g 2 0 .0 g . of q u e b ra c h o e x t r a c t p e r l i t e r

III

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- 1 -

In tro d u c tio n

Two o f t h e m o st i n t e r e s t i n g and im p o r t a n t p h e n ­ omena in d u c e d by t h e a d d i t i o n o f a s y n t h e t i c t a n n i n g m a t­ e r i a l t o a v e g e t a b l e t a n n i n i n f u s i o n a r e th e s o l u b l i z a t i o n o f p h lo b a p h e n e s and s t a b i l i z a t i o n o f t h e i n f u s i o n a g a in s t e le c tr o ly te s .

As h a s b e e n p r e v i o u s l y p o i n t e d o u t

(3 ) t h e s o l v e n t a c t i o n o f a s y n t h e t i c t a n n i n g m a t e r i a l m ay be e x p l a i n e d b y o n e , o r a c o m b in a tio n o f tw o o r m o re , o f th e

f o l lo w in g h y p o th e s e s : 1.

t h e a c t i o n o f th e s y n t h e t i c t a n n i n g m a t­

e r i a l i s p r i m a r i l y d i s p e r s i v e , fo rm in g s m a l l e r p a r t i c l e s o f t a n n i n w h ic h a r e m ore e a s i l y d i s s o l v e d i n th e 2.

s o lv e n t.

t h e s y n t h e t i c t a n n i n g m a t e r i a l u n i t e s chem­

i c a l l y w ith th e v e g e t a b l e t a n n i n t o fo rm a m ore l y o p h i l i e c o llo id . 3.

th e s y n t h e t i c ta n n i n g m a t e r i a l i s a d s o r b e d

on th e v e g e t a b l e t a n n i n p a r t i c l e s and th e r e s u l t a n t p a r ­ t i c l e s a r e m ore l y o p h i l i e t h a n th e o r i g i n a l v e g e t a b l e t a n ­ n in p a r t i c l e s . The s t a b i l i z a t i o n o f v e g e t a b l e t a n n i n i n f u s i o n s a g a i n s t e l e c t r o l y t e s may a l s o be e x p l a i n e d b y t h e s e h y p o ­ th e s e s ( 4 ) . P u rp o s e I n t h i s s tu d y u l t r a f i l t r a t i o n

i s u sed to i n v e s ti -

Reproduced with permission of the copyright owner. Further reproduction prohibited without permission.

2

•*

g a t e t h e s i z e o f th e p a r t i e l e s i n o r d i n a r y q u e b ra c h o i n ­ f u s i o n s a t v a r i o u s c o n c e n t r a t i o n s a n d i n o r d i n a r y q u e­ b ra c h o - s y n th e tic ta n n in g m a te r i a l in f u s i o n s . H is to ric a l T h e re h a s b e e n much d i s c u s s i o n a s to th e m ech­ a n is m b y w h ic h s y n t h e t i c t a n n i n g m a t e r i a l s s o l u b l i z e v e g ­ e ta b le ta n n in s .

On th e

a d d itio n o f a s y n th e tic ta n n in g

m a t e r i a l to a v e g e t a b l e t a n n i n l i q u o r c o n t a i n i n g p h lo b a ­ p h e n e s i t c a n b e e a s i l y s e e n t h a t t h e l a r g e p h lo b a p h e n e p a r t i e l e s a re re d u c e d in s i z e .

P o l i a k (9 ) s t a t e s t h a t

t h i s i s t h e o n ly i n f l u e n c e e x e r t e d b y th e

s y n th e tic ta n ­

n in g m a t e r i a l - t h a t i t h a s no e f f e c t on th e s o l u b l e r n a t u r a l ta n n in s .

H ow ever, S t i a s n y a n d O r th (1 1 ) s t a t e t h a t

th e s y n t h e t i c ta n n in g m a t e r i a l d i s p e r s e s n o t o n ly t h e c o a r s e ( s l i g h t l y s o l u b l e , r e l a t i v e l y l y o p h o b ic , p h lo b a ­ p h en e - l i k e ) p a r t i c l e s , b u t a l s o d i s p e r s e s t h e s m a l l e r p a r t i c l e s # i i e h do n o t s e t t l e o u t o f t h e i s p e rm itte d to s ta n d .

i n f u s i o n w hen i t

They a l s o s t a t e t h a t th e s y n t h e t i c

t a n n i n g m a t e r i a l d o e s n o t com bine c h e m i c a l l y w i t h t h e v e g ­ e t a b l e t a n n i n b u t m e r e ly r e d u c e s th e p a r t i c l e

s iz e .

S tia s n y

an d O r th b a s e d t h e i r c o n c l u s i o n s o n t h e e x p e r i m e n t a l s t u d y o f t h e i n f l u e n c e o f G e r b s t o f f I o n t a n n i n f i x e d b y h id e pow der fro m v e g e t a b l e t a n n i n i n f u s i o n s , u p o n t h e d e c r e a s e o f i n s o l u b l e s , a n d th e s t a b i l i z a t i o n o f th e i n f u s i o n a g a i n s t so d iu m c h l o r i d e .

S t a t h e r and L o c h n e r ( 1 0 ) , s t u d y ­

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in g a number o f s y n t h e t i c t a n n i n g m a t e r i a l s , u s i n g t h e t e c h n iq u e em ployed b y S t i a s n y and O r th ( 1 1 ) , drew th e sam e c o n c lu s io n s .

Thuau a n d Hough (1 2 ) d i f f e r w ith S t i a s n y an d

G rth i n t h a t t h e y b e l i e v e t h a t th e

s y n t h e t i c t a n n i n g m a t­

e r i a l c o m b in es c h e m i c a l l y w i t h th e

t a n n i n o f th e e x t r a c t

t o fo rm a m ore com plex t a n n i n .

As s u p p o r t f o r t h i s c o n ­

c l u s i o n T huau a n d Hough c i t e th e c o l o r c h a n g e o b s e r v e d when s y n t h e t i c t a n n i n g m a t e r i a l i s a d d e d t o a v e g e t a b l e ta n n in .

A f u r th e r in d ic a tio n o f a p o s s ib le r e a c tio n b e­

tw e e n t h e s y n t h e t i c t a n n i n g m a t e r i a l a n d t h e v e g e t a b l e t a n n i n i s show n b y th e m ark e d i n f l u e n c e o f a s y n t h e t i c t a n ­ n in g m a t e r i a l on t h e " re ta in e d * * a n d " a s s o c i a t e d " w a t e r s i n v e g e t a b l e ta n n e d l e a t h e r ( 1 ) . The b e s t e v id e n c e f o r th e d i s p e r s i v e a c t i o n o f a s y n th e tic ta n n in g m a te r ia l i s t h a t re p o rte d by S tia s n y a n d O r th ( 1 1 ) , a n d c o n firm e d b y S t a t h e r a n d L o c h n e r (1 G ). H ow ever, t h e i r m eth o d i s b a s e d on t h e a s s u m p tio n t h a t an i n c r e a s e i n t h e s t a b i l i t y o f a c o l l o i d a l s y s te m to w a rd e l e c t r o l y t e s i s due to a d e c r e a s e i n t h e i c l e s o f thB d i s p e r s e p h a s e .

s i z e o f th e p a r t ­

As h a s b e e n p o i n t e d o u t p r e ­

v i o u s l y , t h i s a s s u m p tio n i s n o t n e c e s s a r i l y t r u e .

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4 4-

P ro c e d u re s The u l t r a f t i t r a t i o n p r o c e d u r e s , a p p a r a t u s , a n d m em brane p r e p a r a t i o n and. c a l i b r a t i o n b a r e b e e n d e s c r ib e d , i n a p re v io u s p u b lic a tio n ( 2 ) ,

The m em branes u s e d a r e

p r e p a r e d fro m a n e t h y l a l c o h o l - e t h e r - a c e t o n e - a m y l a l c o h o l s o lu tio n o f P a rlo d io n .

The A v e rag e P o re D ia m e te r i s c o n ­

t r o l l e d b y th e a d d i t i o n o f g l a c i a l a c e t i c a c i d o r w a t e r . T h ese m em branes a r e c a l i b r a t e d b y an a p p l i c a t i o n o f P o i s e u i l l e f s Law.

I n th e u l t r a f i l t r a t i o n o f ta n n in i n ­

f u s i o n s s u c c e s s i v e sa m p le s o f th e u l t r a f i l t r a t e

fro m th e

mem brane u n d e r c o n s i d e r a t i o n a r e a n a ly z e d f o r t a n n i n . The maximum am ount o f t a n n i n i n th e f i l t r a t e c o rd e d .

i s th e n r e ­

T h ese m axim a, p l o t t e d a g a i n s t th e A v e rag e P o re

D ia m e te r s o f th e m em branes u s e d , l e a d s t o th e

d e te r m in a ­

t i o n o f th e L im i ti n g P o r e D i a m e te r s , w h ic h i s p r o p o r t i o n ­ a l t o th e a v e r a g e p a r t i c l e d i a m e t e r . The l i q u o r s w e re p r e p a r e d f o r u l t r a f i l t r a t i o n b y d i s s o l v i n g th e d e s i r e d am ount o f o r d i n a r y q u e b ra c h o e x ­ t r a c t i n 900 m l. o f d i s t i l l e d w a te r a t 8 5 ° G. t h e t i c t a n n i n g m a t e r i a l w as a d d e d i n th e w a t e r .

The s y n ­ The q u e ­

b r a c h o - s y n t h e t i c t a n n i n g m a t e r i a l - w a te r m ix tu r e w as h e a te d in a w a te r - b a th u n t i l th e d is s o lv e d .

e x t r a c t w a s c o m p le te ly

The i n f u s i o n w as p e r m i t t e d to s t a n d a t room

t e m p e r a tu r e o v e r n i g h t , made up t o one l i t e r , a n d t h e n f i l ­ t e r e d w ith t h e a i d o f k a o l i n .

T h is f i l t e r e d i n f u s i o n w as

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th e n u se d in th e u l t r a f i l t e r s . S in c e t h e u l t r a f i l t r a t i o n p r o c e d u r e r e q u i r e s t h e a n a l y s i s o f s m a ll q u a n t i t i e s o f f i l t r a t e ,

fre q u e n tly

w ith v e r y low t a n n i n c o n c e n t r a t i o n s , a s e n s i t i v e m eth o d o f ta n n in e s tim a tio n i s r e q u ir e d .

As a m eans o f t a n n i n

e s t i m a t i o n we u s e d a t u r b i d i m e t r i c m eth o d b a s e d on t h e n e p h lo m e tr ie m eth o d d e v e lo p e d b y G ra ssm a n n , C hu, an d S e h e lz ( S ) . The t a n n i n c o n t e n t o f th e

s o l u t i o n s a n a ly z e d b y

t h i s m eth o d s h o u ld be b e tw e e n 0 . 5 and 5 .5 mg. o f t a n n i n p e r 100 m l.

A n a ly s e s o f s o l u t i o n s c o n t a i n i n g m ore t h a n

3 .5 mg. o f t a n n i n p e r 100 m l. a r e s u b j e c t t o c o n s i d e r a b l e e rro r.

I n e x tre m e c a s e s s o l u t i o n s c o n t a i n i n g l e s s th a n

0 . 5 mg. t a n n i n p e r 100 m l. c a n b e a n a ly z e d w ith r e a s o n a ­ b le a c c u ra c y .

The n o n - t a n n i n f r a c t i o n fro m A .L .C .A . O f­

f i c i a l A n a l y s i s show s some t a n n i n b y t h i s m e th o d , b u t t h i s c o r r e c t i o n i s so s l i g h t t h a t i t c o u ld be n e g l e c t e d i n t h i s s tu d y .

In th e

c o n c e n tr a tio n s u se d in th e s tu d y th e sy n ­

t h e t i c t a n n i n g m a t e r i a l h a d no a p p a r e n t e f f e c t on t h e a n ­ a ly s e s .

H ow ever, a t r e l a t i v e l y h ig h c o n c e n t r a t i o n s t h e

s y n t h e t i c t a n n i n g m a t e r i a l e a u s e d an a p p a r e n t i n c r e a s e i n t h e am ount o f t a n n i n p r e s e n t i n a s o l u t i o n o f known co n ­ c e n tra tio n . The f o l l o w i n g s o l u t i o n s a r e u s e d i n t h e t u r b i d i ­ m e t r i c m eth o d o f t a n n i n e s t i m a t i o n :

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1*

C lo u d r e a g e n t

2.

ft/2 so d iu m a c e t a t e

I.

N /2 a c e t i c a c i d

4.

S ta n d a r d t a n n i n s o l u t i o n s

5.

Unknown t a n n i n s o l u t i o n s

The s t a n d a r d t a n n i n s o l u t i o n s a r e p r e p a r e d fro m a t a n n i n e x t r a c t o f known t a n n i n c o n t e n t , t h e a n a l y s i s b e ­ i n g made h y th e O f f i c i a l A .L .C .A . m e th o d .

T h is p r im a r y

s t a n d a r d m u st b e t h e same k i n d o f t a n n i n a s t h a t b e in g s t u ­ d ie d .

The p r im a r y s t a n d a r d s o l u t i o n i s p r e p a r e d b y d i s s o l v

in g a p o r t i o n o f th e e x t r a c t c o n t a i n i n g 1 .0 0 g . o f t a n n i n i n 900 m l. o f d i s t i l l e d w a te r a t 85® 0 .

The s o l u t i o n i s

p e r m i t t e d t o c o o l and i s h e l d a t room te m p e r a t u r e o v e r n i g h t I t i s th e n

made up to one l i t e r w ith d i s t i l l e d

s ta n d a rd s o lu tio n s

w a te r.

f o r th e d e t e r m i n a t i o n a r e p r e p a r e d

The fro m

t h e p r im a r y s t a n d a r d s o l u t i o n b y m aking th e p r o p e r d i l u ­ tio n s . T hese m a t e r i a l s a r e u s e d i n t h e p r e p a r a t i o n o f t h e c lo u d r e a g e n t : 30 g .

1.

u rea

2.

4 0 $ fo rm a ld e h y d e

375 ml

3.

d i s t i l l e d w a te r

125 m l

4.

ft. h y d r o c h l o r i c a c i d

5.

ft. so d iu m h y d r o x id e

5 ml —

sal

The c lo u d r e a g e n t i s p r e p a r e d a s f o l l o w s :

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TJbe w a te r a n d fo rm a ld e h y d e a r e a d d e d to th e u r e a I n a one l i t e r , r o u n d b o tto m e d f l a s k , e q u ip p e d w ith a s t i r ­ r e r , and a r e f lu x c o n d en se r. o i l b a th .

The f l a s k

i s h e a te d in an

A f t e r t h e u r e a h a s d i s s o l v e d i n t h e fo rm a ld e h y d e

s o l u t i o n t h e h y d r o c h l o r i c a c i d i s a d d ed w ith s t i r r i n g . s o l u t i o n i s s t i r r e d 10 m in u te s i n th e

c o ld .

The

H eat i s th e n

a p p l i e d so t h a t t h e te m p e r a t u r e o f th e b a t h i s r a i s e d t o 1 2 0 ° 0 . i n one h o u r .

When th e r e a c t i o n m ix t u r e b o i l s

( b . p . 98® C .) t h e te m p e r a t u r e o f th e b a t h i s p e r m i t t e d t o f a l l t o 115° C. a n d i s m a i n t a i n e d a t t h i s t e m p e r a t u r e f o r 2 h o u r s w ith c o n tin u o u s s t i r r i n g .

The w h i t e s l u r r y w h ic h

a p p e a r s d u r i n g t h e r e a c t i o n s h o u l d c o m p le te ly d i s a p p e a r b e f o r e t h e en d o f th e h e a t i n g p e r i o d .

The r e a c t i o n p r o ­

d u c t i s p e r m i t t e d t o c o o l s l o w l y a n d i s s t o r e d a t room tem ­ p e r a t u r e f o r one w eek .

At t h e e n d o f t h i s a g in g p e r i o d ,

t h e pH o f th e p r o d u c t i s a d j u s t e d to a p p r o x i m a t e ly 10 w i t h N so d iu m h y d r o x i d e .

The c lo u d r e a g e n t i s t h e n r e a d y f o r

u se. l o r th e e s t i m a t i o n o f t a n n i n , b u f f e r e d c lo u d r e ­ a g e n t i s f r e s h l y p r e p a r e d ( a t m o st t h i s s o l u t i o n s h o u ld n o t b e m ore th a n 30 m in u te s o l d ) .

T h is b u f f e r e d c lo u d r e a g e n t

i s p r e p a r e d b y m ix in g 25 m l. o f th e c lo u d r e a g e n t , 50 m l. o f N /2 a c e t i e a c i d , and 50 m l. o f H /2 so d iu m a c e t a t e i n a 250 m l. v o l u m e t r i c f l a s k .

The f l a s k

i s th e n f i l l e d t o t h e

m ark w i t h d i s t i l l e d w a t e r , s h a k e n t h o r o u g h l y , a n d th e b u f ­

Reproduced with permission o f the copyright owner. Further reproduction prohibited without permission.

8

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f e r e d c lo u d r e a g e n t i s r e a d y f o r u s e . A K l e t t - S u m e r s o n P h o t o e l e c t r i c C o lo r im e te r e q u ip p e d w ith a N o. 281 f i l t e r tio n .

i s u s e d f o r th e d e te r m in a ­

The i n s t r u m e n t i s s t a n d a r d i z e d a g a i n s t d i s t i l l e d

w a te r. The a n a l y s e s a r e c a r r i e d o u t a s f o l l o w s : A tw e n ty m l. a l i q u o t o f th e

ta n n in s o lu tio n i s

p l a c e d i n a 50 ml* b e a k e r , t h e n a 20 m l. a l i q u o t o f th e b u f f e r e d c lo u d r e a g e n t , f r e s h l y p r e p a r e d , i s a d d e d w i t h s tirrin g .

The m ix tu r e i s t h e n s t i r r e d o c c a s i o n a l l y d u r i n g

a 40 m in u te a g in g p e r i o d .

A t t h e en d o f t h i s

t u r b i d i t y i s d e te r m in e d b y m eans o f th e

p e r i o d th e

c o lo rim e te r.

The

a g in g p e r i o d m u st b e tim e d f a i r l y a c c u r a t e l y , w i t h 0 .5 m in u t e . The c o l o r i m e t e r r e a d i n g s o b t a i n e d w ith th e v a r i o u s s o l u t i o n s o f known t a n n i n c o n t e n t a r e p l o t t e d a g a i n s t t h e ta n n in c o n te n t.

The t a n n i n c o n t e n t o f th e unknown s o l u ­

t i o n s a r e t h e n r e a d fro m t h i s

c a lib r a tio n c u rv e .

A new

c a l i b r a t i o n c u rv e s h o u ld b e d e te r m in e d f b r e a c h l o t o f b u f ­ f e r e d c lo u d r e a g e n t . I n f u s i o n s c o n t a i n i n g 5 , 10 a n d 20 gram s o f o r d ­ i n a r y q u e b ra c h o e x t r a c t p e r l i t e r w e re u s e d i n t h e s t u d y . The s y n t h e t i c t a n n i n g m a t e r i a l - q u e b ra c h o e x t r a c t r a t i © v a r i e d fro m 0 .1 t o 0 . 4 g . o f s y n t h e t i c t a n n i n g m a t e r i a l p e r gram o f q u e b ra c h o e x t r a c t .

The h i g h e r s y n t h e t i c t a n n i n g

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m a t e r i a l - q u e b ra c h o e x t r a c t r a t i o a p p r o x im a te s t h a t r a t i o a t itfhich t h e s y n t h e t i c ta n n in g m a t e r i a l h a s m a x i­ mum s o l v e n t a c t i o n on q u e b ra e h o e x t r a c t ( 3 ) . E x p e r im e n ta l R e s u l t s The t a n n i n r e p o r t e d i n th e e x p e r i m e n t a l r e s u l t s i s th e t a n n i n c o n t r i b u t e d b y t h e q u e b ra e h o e x t r a c t o n l y , s in c e th e t u r b id im e tr ie a n a l y s i s u se d i n t h i s s tu d y does n o t r e s p o n d t o th e

s y n t h e t i c ta n n in g m a t e r i a l .

The " p e r c e n t o r i g i n a l t a n n i n i n f i l t r a t e "

is

c a l c u l a t e d fro m t h e maximum am ount o f t a n n i n fo u n d i n a s e r i e s o f s a m p le s ta k e n d u r in g th e u l t r a f i l t r a t i o n o p e r a ­ tio n (2 ). T a b le s 1 , 2 , 3 an d 4 and f i g u r e I ,

show t h e r e ­

s u l t s o b t a i n e d on t h e u l t r a f i l t r a t i o n o f i n f u s i o n s c o n ­ t a i n i n g §.© g . o f o r d i n a r y q u e b ra e h o e x t r a e t a n d v a r y in g a m o u n ts o f s y n t h e t i c ta n n in g m a t e r i a l p e r l i t e r . The r e s u l t s t a b u l a t e d i n t h e s e p a r a t e d i v i s i o n s o f th e t a b l e s a r e r e s u l t s o b t a i n e d w ith a g iv e n i n f u s i o n , t h e t a n n i n a n a l y s i s o f w h ic h i s g iv e n a b o v e th e s e c t i o n . The L im i t i n g P o r e D ia m e te r , a s d e te r m in e d fro m t h e p l o t o f th e d a t a i n t h e t a b l e , i s g i v e n a t t h e b o tto m of the table.

Reproduced with permission of the copyright owner. Further reproduction prohibited without permission.

Reproduced with permission of the copyright owner. Further reproduction prohibited without permission.

TABLE I ULTRAFILTRATION OF ORDINARY QUEBRACHO INFUSION § • 0 g . Qua b r a oho E x t r a c t P e r L i t e r . 0«S 75 g. t a n n i n /1 0 O m l* A v e rag e $ O rig in a l P o re T a n n in i n D ia m e te r F iltra te 1 4 .3 1 1 .0 1 0 .6 8 .7

33*6 1 9 .8 1 3 .1 8 .4

1 4 .1 S 8 .0 1 .1 7 3 .0

© .3 0 3 g . t a n n i n / 1 0 0 m l. A v e rag e $ O rig in a l P o re T a n n in i n D ia m e te r F iltra te 2 6 .8 1 3 .3 1 1 .2 9 .3

3 7 .0 3 .1 4 7 .0 6 4 .0

0 .3 1 9 g . t a n n i n /1 0 0 m l. A verage io O r i g i n a l P o re T a n n in i n D ia m e te r F iltra te 7 0 .0 4 0 .1 4 .6 4 8 .7

0 .3 0 4 g . t a n n i n /1Q 0 m l. A verage $ O rig in a l P o re T a n n in i n D ia m e te r F iltra te 2 6 .8 1 8 .2 1 3 .1 1 0 .0

8 .9 4 3 .0 9 1 .0 7 5 .0

0 .3 0 0 g . t a n n i n /1 0 0 m l A v e ra g e O rig in a l P o re T a n n in i n D ia m e te r F iltra te 3 5 .0 2 6 .3 1 8 .2 8 .6

1 8 .7 1 0 .4 6 .9 0 .1

0 .2 9 9 g . t a n n i n /10O m l A v e ra g e io O r i g i n a l P o re T a n n in i n D ia m e te r F iltra te 3 3 .6 1 9 .8 1 3 .1 9 .7

L im i t i n g P o re D ia m e te r 9 - I S m i l l i m i c r o n s

1 4 .0 1 4 .6 7 5 .0 1 7 .0

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T a b le s 7 a n d 7 1 a n d F ig u r e 2 show th e r e s u l t s o b t a i n e d on t h e u l t r a f i l t r a t i o n o f i n f u s i o n s e o n t a i n i n g 10*0 g . o f o r d i n a r y q u e b ra e h o e x t r a c t , w i t h a n d w ith o u t 4*0 g . s y n t b e t i e t a n n i n g m a t e r i a l , p e r l i t e r .

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