Dongare, M B

Pawar, S T

English

IACS Institutional Repository

juni J- Phys. 76A (5). 481 -483 (2002)U P  Aan in te rn a tio n a l jo u rn a lX-ray diffraction studies on jaggery samplesS T  P a w a r  an d  M  B  Dongare*'^D e p a rtm e n t o f P hys ics , S h iv a ji U n iv e rs ity , K o lh a p u r -4 1 6  0 0 4 , M a h a ra s h tra , In d iaE -m a il m bd o n p a rc (p )h o tm a il comH c i t t v e d  2 1  M a y  2 0 0 2 .  c u i e p i t ' d  5  J u n e  2 0 0 2\ | ) s ir i i i  l T h e  to ta l s u g a rc a n e  p ro d u c t io n  in  In d ia  is 227  06  la k h to n n c s  O u t o f  th is  su ga rcane  43 5%  is used lo i  ja g p e iy  and kh a iid sa riB a  ( 2 0 (H ))] T h e  Ja g g e ry  in d u s try  is an ii i ip o r ta n t  a g ro -p ro ce s s in g  in d u s try  in ru ra l In d ia  In present fia p c r we have u n d e ita ke n  X -ra y  (iiiiK uuo ii s tud ies on  ja g g e ry  and th e re b y  s tu d ie d  s tru c tu ra l aspects o f  ja g g e ryw o ld s  Ja g g e ry  sa m p le . X - ra y  d if f ra c t io n .r \ (  S N os. 61 10 N z , 61 4 3  H r\  i.i\ i l i l l r a c t io n  is th e  m o s t e x te n s iv e ly  used  te c h n iq u e  to  nil, iii ih  ihc c ry s la ll in e  p h a s e  o f  s o lid  a n d  to  d c tc rn iin c  its c ry s ta l siiuLiinc 1 I j .  H e r e ,  th is  m e th o d  has b e e n  u sed  to  id e n t ify  th esi! 11^, lin e  o f  ja g g e ry .\  L’ I v e il s u b s ta n c e  a l w a y s  p r o d u c e s  a c h a r a c t e r is t i c  d il lu c iiu n  p a tte rn , w h e th e r  th a t  s u b s ta n c e  is p re s e n t in  the  puu siaic o r as o n e  c o n s t itu e n t  o f  a m ix tu r e  o f  s u b stan ces . T h is  l iu  is ihc basts fo r  th e  d i f f r a c t io n  m e th o d  o f  c h e m ic a l a n a ly s is , n iu liia iiv e  an d  q u a n t ita t iv e  a n a ly s is  a re  a ls o  p o s s ib le , becau se  ihv iiiic iis iiie s  o f  th e  d i f f r a c t io n  lin e s  d u e  to  o n e  p h a se  o f  a niivturc d e p en d  o n  th e  p ro p o r t io n  o f  th a t p h a se  in the  s p e c im e n , bciailed tre a tm e n t o f  c h e m ic a l a n a ly s is  b y  X - r a y  d if f r a c t io n  are  h\ se ve ra l w o rk e rs  [ 1 - 3 ] .H ie c ry s ta l lo g ra p h ic  fe a tu re s  a re  s tu d ie d  b y  u s in g  X R D .  Hie XKi:> te c h n iq u e  b a s e d  o n  m o n o c h r o m a t ic  ra d ia t io n  is yencuilly m o re  im p o r ta n t  b e c a u s e  th e  s p a c in g  o f  th e  p la n e s  spacing) ca n  b e  d e d u c e d  f r o m  th e  o b s e rv e d  d i f f r a c t io n  fh e  p h e n o m e n o n  o f  X - r a y  d if f r a c t io n  can  be c o n s id e re d  a ivl lection  o f  X - r a y s  f r o m  th e  c ry s ta l lo g ra p h ic  p la n e s  o f  the  lal and is g o v e rn e d  b y  B ra g g *s  e q u a tio n .h l s i n e ^ n X  (1 )^'hcMc (1 is th e  la t t ic e  s p a c in g , X  is th e  w a v e le n g th  o f'^^•''Pmuling A u th o rm o n o c h ro m a tic  X -r a y s  , n is th e  o rd e r.o l d if lra c t io n  and 0  is the  d if f ra c t io n  a n g le . F o r  th in  an d  th ic k  f i lm s , the p o w d e r  tec h n iq u e  in  c o n ju n c tio n  w ith  d if f r a c to m e te r  is m o s t c o m m o n ly  used. In  th is  in s tru m e n t the d if fra c te d  ra d ia tio n  is d e tected  by the c o u n te r  tu b e , w h ic h  m o v e s  a lo n g  th e  a n g u la r  ra n g e  re llc c t io n s . T h e  in te n s itie s  arc  re c o rd e d  on a c o m p u te r  system  T h e  cJ va lu e s  are  c a lc u la te d  u s in g  re la t io n  (1 )  fo r  k n o w n  v a lu e s  o f  X  . 0  and  n,  ? T h e  X - r a y s  d if f r a c t io n  d a ta  thus o b ta in e d  is p r in te d  in  ta b u la r  fo rm  on  p a p e r an d  c o m p a re d  w ith  J C P D S  (J o in t c o m m itte e  on  p o w d e r  d if f r a c t io n  s ta n d a rd s ) d a ta c a rd  to  id e n tify  the u n k n o w n  m a te r ia l .  T h is  X - r a y s  d i f f r a c t io n  d a ta  ca n  a ls o  be used to  d e te rm in e  d im e n s io n s  o f  the u n it  c e l l ,  c ry s ta l s tru c tu re  and  c ry s ta llin ity  1 4 .5\ ,T h e  X R D  s p e c tru m  w a s  re c o rd e d  on  P h il ip s  P W  3 7 1 0  d if fra c to m e te r  a ttached  to a d ig ita l c o m p u te r a lo n g w iih  g rap h ica l a s s e m b ly  in  w h ic h  CuK^^ ra d ia t io n  so u rce  co n n e c te d  w ith  the  tu b e  C u - N i  2 5 k V /2 0  m A  w as used.T h e  X - r a y  d if f ra c to g ra m  o f  ja g g e ry  sa m p le  reco rd s  n in e tee n  re llc c tio n s  b e tw e en  IQ ’ and 70 " (2  0 )  w ith  m a x im a  at 2 0  = 2 4 .5 6 "  c o rre s p o n d in g  to  a v a lu e  o f  d  =  3 .6 2  A " . T h e re  is no  A S 7 M  (A m e r ic a n  S o c ie ty  fo r  T e s tin g  an d  M a te r ia ls )  d a ta  a v a ila b le  fo r  ja g g e ry . H e n c e , the  in d e x in g  o f  th e  s p e c tro g ra m  w ith  res p ec t to  th e  p e aks  h a v e  b e en  c a rr ie d  o u t b y  u s in g  c o m p u te r  s o ftw a re  an d  tr ia l an d  e r ro r  m e th o d  t i l l  a g o o d  f i t  c o u ld  be o b ta in e d©20021ACST ab le  1. P ow der  X -ray  d if fraclion  daia  oT laggeiy  sample482 S T Pawar and M 8 Dori^arePeak No 2 Q deg 2 Q deg  d obsA"456 7 910 I 1 12 I  ^IS  10 17 19Obs J 1.51 12 90  16 54  18 .63  19 3719 4920  10 21 8824  5025 103 0  7631 70  38 33 ^9 08  4 0  10 50  6 0Cal 1 1 5 1  12 9 6  16 5418 7 019 2719 5720  1921 9424 0 025 123 0  7031 7238 3239 7 34 0  19so 687 6 8 2  6  82 3  5 354  4 7 5 9  4  57 9  4 55 1 4 399  4 05 8  3 622  3 S45 2 90 4  2 815  2 U6  2 2 6 9  2 24 3  1 80 2d cal A"7 6 8 2  6  8 2 3  5 35 4  4 7 4 2  4 601 4 5 ^ 2  4 395  4 0 4 8  3 6 1 6  3 54 3  2 9 0 4  2 8 1 9  2 34 7  2 267  2 24 2  1 8 0 0hkl1 2 02 1 0 1 0 1 3 0  1 1 2 1 2 0 1 2 1 1 2 2 12  3 1 0  4  13 5 0 2 5 10 7 15 4  16 1 11 0 1R1%20  30  20  6 0  6 0  5 0  20 20 100  6 0  20 30  4 0  2 0 20  10t =0 .9  A  B c o s OT ab le  2. Data  for g rain  size and hom o g en e i tyNo.ik B inradian X20ObsDeg0deg cos 0 sin t)X1(J1 1 .60 1 1.51 5 7 5 0 . 9 9 5 0  100 1 v jn ,2 3 . 2 0 1 2 .9 6 6 . 4 8 0 9 9 3 6 0  1 13 3 17‘)<,3 2 4 0 1 6 .5 4 8 .2 7 0  9 8 9 6 0 1444 2 . 4 0 2 0  16 10  08 0  9 8 4 5 0 175 25 4 . 0 0 21 8 8 10 9 4 0 9 8 1 8 0 1896 3 20 2 4  56 12  28 0 .9 7 7 1 0 213 ' Uf,'7 1 6 0 25  10 12  55 0 .9 7 6 1 0 .217 1 SM-;8 1 6 0 3 0  7 6 15 .3 8 0 .9 6 4 1 0 265 19 1 6 0 38 33 19 16 0  9 4 4 6 0 32810 4 . 8 0 4 0  16 2 0  08 0 9 3 9 2 0  :i43 '1 1 ()>,.'Average -  jT h e  n a tu re  an d  b e h a v io r  o f  th es e  v a lu e s  fo r  th e  present sanipk arc  s h o w n  g r a p h ic a l ly  in  F ig u re  1. \Graph of Bcos 0 versus sin 6b e tw e e n  th e  o b s e rv e d  a n d  c a lc u la te d  2  6  an d  d  v a lu e s . T h e  m e th o d  a ls o  y ie ld e d  in  g iv in g  h k l  ( M i l l e r  in d ic e s )  v a lu e s .  C o m p a r is o n  o f  th e  v a lu e s  o f  J  an d  2 6 / (T a b le  1) re v e a ls  a g o o d  a g re e m e n t b e tw e e n  th e  c a lc u la te d  an d  o b s e rv e d  v a lu e s  o f  2 0  an d  d  on  th e  b a s is  o f  a s s u m p tio n s  o f  o r th o r h o m b ic  c ry s ta l s t r u c tu r e ,  g i v i n g  u n i t  c e l l  p a r a m e te r s  a  =  1 4 .7 4 5 9  A “ , h  =  1 7 .9 9 8 5  A “ , C  =  5 .7 4 5 6  an d  V =  1 5 2 4 .9 2  A “ . In  c o n ju c t io n  w ith  su ch  c e ll p a ra m e te rs  th e  c o n d it io n  su ch  as a - p - y -  9CV' an d  a  c  , r e q u ire d  fo r  th e  s a m p le  to  b e  o r th o rh o m b ic  is fo u n d  to  be s a t is fa c to ry  16 ). H e n c e , it  is c o n c lu d e d  th a t the  s tru c tu re  o f  p re s e n t s a m p le  is fo u n d  to  be o r th o rh o m b ic  [7 ] .  T h e  g ra m  s ize  o f  the s a m p le  w a s  d e te n m n e d  b y  u s in g  S c h e rre rs  e q u a tio n  [8 ]8ffiw h e re , /  is g ra in  s ize  o f  th e  s a m p le , A is w a v e le n g th  o f  X - r a y  r a d ia t io n ,  8  is th e  e x c e s s  o f  l in e  w id th  o f  r a d ia t io n  o f  th e  d if f r a c l io n  p e a k  a n d  9  is B ra g g 's  a n g le . F o r  th e  d e te rm in a t io n  o f  g ra in  s iz e , th e  c o rre s p o n d in g  p e a k  w a s  e n la rg e d  fo r  b e tte r  a c c u ra c y  in  m e a s u r in g  th e  h a l f  w id th  a t m a x im u m  in te n s ity  .T h is  p a ra m e te rs  ca n  d is t in g u is h  b e tw e e n  n a tu ra l g ra in  s ize  a n d  g ra in  s iz e  d u e  to  b ro a d e n in g  e f fe c t  w h ic h  w a s  d o n e  b y  c a lc u la t in g  fu l l  w id th  a t h a l f  m a x im u m  ( B )  c o rre s p o n d in g  to  its  B r a g g ’s a n g le  6  a n d  th e re b y  c o m p u t in g  cos a n d  s in  v a lu e s .0.1 0.113 0.144 0.175 0.189 0.213 0.217 0.265 0 328 0 3-J3sin 0F i g u r e  1. G rap h  lo d e te r m in e  h o m o g e n e i ty  0 9AG iam  .size r = = 539.756 A .B cos 0where A = I 54056 AI t  is  c o n c lu d e d  th a t th e  s tru c tu re  o f  p re s e n t sam ple is louiul to  be o r th o r h o m b ic .A  p lo t  o f  ^ c o s f l  v e r s u s  sin  6  is not sinuiihi lin e  in d ic a t in g  a p re s e n c e  o f  f lu c tu a t io n s . H e n c e , present sample se em s lo  b e  n o n -h o m o g e n e o u s  w i t h  re s p e c t lo  the particle si/c d is to r t io n .AcknowledgmentO n e  o f  th e  a u th o rs  S h r i S .T .P a w a r  is  th a n k fu l to theG ra n ts  C o m m is s io n  fo r  providing th e  te a c h e r  fe llow sh ip  ufiFTP.X-ray diffraction studies on jaggery samples 483Rffcrt-nces,1 H P  K*'*? ^  ^  Alexander X-ray Diffraction Procedure,!'''' ^ d l l ,  (New York : W iley) (1974)|2| L Zwell and A W  Danko Appl. Spectivsc Rev. 9 167 (1975)Ml M Neiiadic, A S d iaries and J D Cortile D e v e l o p m e n t  in A p p l i e d  S f H 'L t r o s c o p y .  vol.9 (1971) p343-41 K W Janies The Optical Principle.s of Diffraction of the X-Ray.s ' (]vjew York : Macmilan) (1948)(5] G L Clark A p p l i e d  X ' t a v  4'^ edn (New York , McGraw-Hill)(1955)[61 H S Pciser, H P Roukshy X - r a \  D i f f r a t t i o n  h y  P o l y a y s t u l l i n e  M a t e r i a l  (ed) A J C W ilson, (Insiiiutc of Physics, London)(1956)17] R T  Pallar, K R Choukimalh and V G Tulsigm I n d i a n  J  Ph ys.  73A 343 (1999)18) B D Cullily E le m e n t s  o f  X - i a y  D i f f r u i  turn  (Massachusetts Addison Wesley) (1956)

X-Ray Diffraction Studies on Jaggery Samples

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X-Ray Diffraction Studies on Jaggery Samples

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