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WOOL

WOOL

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Published by: api-3733260 on Nov 25, 2009
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Infrared Study ofth e E ffecto f H eat onW ool
M .A . M OHARRAM ,N ational Research Centre,Cairo,E gypt,T .Z .
A B D E L -R E H IM ,A l-A zhar U niuersity, Cairo,E gypt, a n dS .M . R A B IE ,
M id d le E a s te r n R e g io n a l C e n tr e , C a ir o , E g y p t
S y n o p s is
T he infrared spectra of w ool heated in vacuum and in air to differenttem peraturesranging from
1 2 0t o 2 5 0 \u00b0 C were investigated. Itwasfound thatcertainabsorptionbandsdisappearwhen wool
ish e a t e d in v a c u u mt o1 8 0 \u00b0 C a n d in a irt o 120O C fo r2 h r .
A lso ,th e resu lts sh o w ed th a t th e in te n sitie s
of th eC
4stretching band a t1 6 6 0 cm -',N -H
stretching band at3 3 2 5 cm -I and th e C -H

s tr e tc h in g band at2940cm -I decrease w hen w ooli s heated in vacuumt o 180\u00b0C and in airt o 120\u00b0C .T h e sp ectra of the sam ples heated in vacuum to 25O O C and in air to 2 2 5 \u00b0 Ce x h ib ite d s tr o n g a b s o r p tio n b a n d s belonging to the carboxyl and sulfonate groups.

IN T R O D U C T IO N
T h e s tu d y of h e a t e ffe c ts o n w o o l h a s b o th fu n d a m e n ta l a n d a p p lie d in te re s t.
I tis w ell know n th at the physical properties of w ool are influenced by therm al
p re tre a tm e n ts .

Indeed,the specific changes produced w hen wool is subjected to heat have been show n to depend not only on tem perature b u ta ls o on th e tim e of treatm ent an d other conditions of heating such as th e presence of oxygen.

S e v e ra l r e ~ e a r c h e r s l - ~
have show n that in the low er tem perature range the
o n ly im p o rta n t c h a n g e in w ool is d ry in g ; th is d o m in a te s to a b o u t 120\u00b0C .
O th e r
w orkerss7 have found th at in the range1 4 0 -1 7 0 \u00b0 C

th e c o n c e n tra tio n of a c id a n d base groups both decrease,leading to the notion that am ide crosslinks are form ed b e tw e e n th e m .

A sthe tem perature is raised above170"C , the solubility of w ool
in s o d iu m b is u lfite b e g in s to in c re a s e in d ic a tin g a m o re g e n e ra l th e r m a l b re a k -
dow n.
A thigher tem peratures, how ever, w ool undergoes as o r t of m elting w hich
has been put at240\u00b0C .

T h e p re s e n t s tu d y is u n d e rta k e n to in v e s tig a te th e e ffe c t of th e rm a l tre a tm e n ts u n d e r v a rio u s c o n d itio n s (in v a c u u m a n d in a ir ) o n th e m o le c u la r s tr u c tu r e of w o o l.

T h e c h a n g e s in th e m o le c u la r s tru c tu re w e re d e te rm in e d b y s tu d y in g th e
corresponding changes in th e infrared spectra of th e treated sam ples.
E X P E R IM E N T A L
W o o l fib e rs fro m fo u r b re e d s s u c h a s M e rin o , B a rk i, O sim i, a n d R a h m a n i w e re
u s e d .
T h e sheep are of nearly the sam e age( - 2
years) and are grazed on the
s a m e la n d u n d e r t h e w e a th e rin g c o n d itio n s of E g y p t.

T h e R a h m a n i w o o l is c h a ra c te riz e d b y its b ro w n is h c o lo r, th e O s im i is w h ite -c re a m , a n d b o th M e rin o a n d B a r k i w o o ls a r e w h ite .

Scouring of raw woolwas carried outb y u sin g th e m e th o d of F in c h a m .8
F irst,
th e fib e rs w e re rin s e d in w a te r a n d e x tra c te d in s o x h le t a p p a ra tu s w ith e th e r fo r
2 4 h r , th e n w ith e th a n o l fo r th e s a m e p e rio d .
Second, th e fibers w ere w ashed
J o u r n a l o f A p p lie d P o ly m e r S c ie n c e ,V o l. 2 6 ,9 2 1 -9 3 2
(1 9 8 1 )
0
1 9 8 1 J o h n W ile y& S o n s , I n c .
C C C 0 0 2 1 -8 9 5 /8 1 /0 3 0 9 2 1 -1 2 $ 0 1 .2 0
9 2 2
M OHARRAM
E T
A L .
w ith distilled w ater an d left to dry in open air.
F in a lly , th e y w e re w a s h e d w ith
3g llite r s o lu tio n o f n o n io n ic d e te rg e n t H o s tip a l C V (H o e c h s ta g ) fo r 1hr at2 5 \u00b0 C
a n d th e n b y d is tille d w a te r u n til fre e fro m d e te rg e n t.
T he fibers w ere subse-
q u e n tly d rie d in a n e le c tro n ic o v e n a t 7 0 \u00b0 C fo r a b o u t2 4 h r.
In m easuring wool fineness,the air flow m ethod was used.
A lso th e gravi-
m e tric m e th o d 9 w asused for m easuring th e m oisture contents.
T h e a s h i n g m e t h o d u s e d i s t h a t o f A S T M .'O

In this m ethod5g of th e w ool s a m p le s w e re in itia lly c h a rre d in a c ru c ib le u n til n o m o re v o la tile m a tte r w a s p ro d u c e d ; th is w a s fo llo w e d b y ig n itio n in a m u ffle fu rn a c e a t 6 5 0 \u00b0 C fo r6 h r u n til carbon had been burned off. A fter ashing had taken place th e ash sam ples w ere c o o le d in a d e s ic c a to r fo r4hr or m ore.

S am ple w eight w as determ ined using
a m acrobalance.
T h e extensively dried fibers w ere cu t into sm all pieces an d ground in a hard-
e n e d s te e l v ia l c o n ta in in g tw o s te e l b a lls .
T h e vial w as fitted to a S pex-m ixer
m ill w hich w as ro tated for sh o rt periods.

T h e grinding process w as carried out several tim es for short periods in order to avoid th e oxidation of th e sam ples.ll T h e pow der w as then served to a particle size of a fraction of diam eter ranging fro m0 .0 5 3t o 0 .2 9 7m m .

Ap art of th e pow der w as heated in sealed evacuated glass tubes(
to rr)
in a w e ll-c a lib ra te d e le c tric fu rn a c e .
A n o th e r p a r t w a s h e a te d in a ir.
Aw eight of the pow derw as w eighed accurately into a sm allpolystyrene tube.

T h is w e ig h t w a s th o ro u g h ly m ix e d w ith K B r to g iv e c o n c e n tra tio n of s a m p le t o K B r of 1 .5 % .T h e tu b e w a s th e n c la m p e d in t h e h o ld e r o f t h e W ig -I-B u g m ix e r fo r a b o u t2m in .

Aw eight of2 0 0 m g of th e K B r sam ple m ixture w as pressed
under vacuum into transparent disks.
T h e infrared sp ectra (IR ) w ere recorded
on th e B eckm anI R4 2 2 0 in fra re d s p e c tra p h o to m e te r.
I tseem s very im portant to m ention here th at th e obtained intensities of th e
in fra re d a b s o rp tio n b a n d s a re th e a v e ra g e s of th re e re p lic a te ru n s .
T h e accuracy
of th e m easured values w as found to be 2% .
RESULTS AND
D IS C U S S IO N
T h e infrared spectra of w ool sam ples from th e different breeds of sheep are
sh o w n in F ig u re1 .
I tcould be seen from th is figure th a t th e in ten sities of th e
a b s o rp tio n b a n d s v a ry fro m

breed to breed, and th e m ost intense absorption bands are show n in the spectrum of M erino w ool,w hile the less intense bands are show n in the spectrum of R ahm ani w ool.

B o th O s im i a n dB a r k iw o o ls e x h ib it
a b s o rp tio n b a n d s of in te rm e d ia te in te n s itie s .
Abrief sum m ary of th e structuralassignm ents for th e characteristic absorption
b a n d s fo u n d in th e lite ra tu re w ill b e g iv e n .
T h e tw o b a n d s a t3 3 2 5 and 3075 cm -l w ere assigned as N -H
s tre tc h in g v i-
b ra tio n ~ .~ ~ -~ ~

T h e th re e a b s o rp tio n b a n d s a t 2 9 6 0 ,2 9 4 0 , a n d2 8 7 5 c m -l w e re assigned to the asym m etric and sym m etric CH3 and CH2 stretching vibra- tio n ~ .~ ~ -~ ~

The bands at1 6 0 0 and
1 5 2 5 cm -'
w ere assigned
to the C-0
s t r e t c h i n g v i b r a t i o n a n d N -H
b e n d in g v ib ra tio n s , re s p e c tiv e ly .
T he three bands at1 4 5 0 ,1 4 0 0 ,a n d 1 2 4 0 cm -' seem to have been recognized
a s c h a ra c te ris tic p ro te in b a n d s .
T h e first b an d is usually assigned to th e w ell-
know n characteristic deform ation frequency of CH2 and CH 3 groups.
T he band
a t1 4 0 0cm -l w as assigned to th e low erC O O - absorption frequency.15
T he1 2 4 0
c m - l b a n d w a s a s s i g n e d a s N -H
deform ation frequency.12-17
E F F E C T
O F
H E A T
O N
W OOL
9 2 3
L
500
1 0 0 0
1 5 0 0
Z O a ,
2 5 0 0
3000
3500
4000
W AVE
N U M B E R
C m -1
Fig.1 . IR spectrao f R ahm ani (R ),O sim i(0 ),B arki (B ),an d M erino (M )w o o ls .
T h e rem aining bands a t 1340 and 1075 cm -l w ere assigned as N-H
d e fo r-
m a tio n l8 a n dR -S O 2 H
v ib ra tio n s , re s p e c tiv e ly .

P re v io u s in v e s tig a tio n s of th eI R spectra of oxidized keratin have revealed th a t a llth e oxidized species absorb a t 1040 cm -l and in som e cases an absorption band a t 1175 cm -l also appears.

T his led to th e conclusion th at th e presence
o fth e 1 1 7 5 c m -l
b a n d in d ic a te s th e fo rm a tio n of s u lfo n a te o r s u lfo n ic a c id
a n d
the occurrence of the band
at 1040 cm -l
w a s in d ic a tiv e of s u lfo x id e

H o w e v e r, H a rv e y a n d B it-A lk h a s lg s ta te d t h a t th e p rin c ip a l c h a n g e in th eI R spectra caused by th e oxidation of hair is th e appearance of new bands a t 1175 and 1040cm-1.

T h is s ta te m e n t is in a g re e m e n t w ith th e in fo rm a tio n re p o rte d by R obbind7 w ho observed these tw o bands at1 0 4 0and 1175cm -l in theI R s p e c tr a of o x id iz e d k e r a tin a n d c o n c lu d e d t h a t th e o x id a tio no f d is u lfid e t o s u l- fonate is a m ajor transform ation in this reaction.

H ow ever,these results do not
g ro ~ p .1 4 -1 7 ,1 9
T A B L E
I
In te n s ityo f th e C -0
Band at1660\u00b0C forW ool
B reed
lo gId 1
A V IIZ
( c m - ')
lo g1 0 1 1X
A u ilz
R ahm ani
0 .1 8 1
0 .1 3 5
2 4 .4 3
O sim i
0 .2 1 1
0 .1 2 5
2 6 .3 7 5
B arki
0 .2 0 8
0 .1 4 0
2 9 .1 2
M erino
0 .2 8 4
0 .1 1 0
3 1 .2 4

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