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SPECTROSCOPIC STUDY OF GROWTH
AND CHARACTERISATION OF L-
VALINE FUMARIC ACID CRYSTAL




               PROJECT HANDLER
               V.REVATHIAMBIKA
INTRODUCTION
 MATTER
 • SOLID
 • LIGUID
 • GAS

 PHASE TRANSFORMATION
 • Solid to solid
 • Liquid to Liquid
 • Gas to gas

 CRYSTALLINE SOLIDS
 • Single crystal
 • polycrystalline
Spectroscopic study of growth and characterisation of l valine
Spectroscopic study of growth and characterisation of l valine
NUCLEATION
1.   Development of super saturation

2.   Generational of embryo

3.   Growth of the embryo from the
     unstable critical state to stable state.

4.   Relaxation process where the texture
     of the newly born nucleus alters.
Spectroscopic study of growth and characterisation of l valine
SLOW EVAPORATION
METHOD
   Ex
        40g of solute in 100 ml of solvent is
    considered as saturated at 50 C. Now the
    solution is reduced to some lower level
    say 70 ml then 40gms in 70 ml at 50 C is
    super saturated solution.
L-VALINE & FUMARIC ACID
   L-VALINE                       FUMARIC ACID
Formula : C5H11No2              Formula : C4H4O4
Molecular Weight :117.15        Molecular Weight : 116.07
Melting Point : 295-3000C       Melting Point : 2870C
Solubility : Soluble in water   Solubility : Soluble in water
Spectroscopic study of growth and characterisation of l valine
GROWTH OF LVF CRYSTALS
   1.952 gms of L- valine is dissolved in 100 ml of water then 1.934 gms
    of fumaric acid is dissolved in 100 ml of water.

   These two solutions were mixed and these solutions may contain
    impurities such as solid dust particles. So it was filtered.

   This solution is covered with polythene paper and for slow
    evaporation few holes are made in the polythene paper and the
    solution is undisturbed.

   It shows the slow evaporation of water the excess of solute atoms join
    together to form cluster. The cluster is grown which resulted in the
    formation of crystals in a few weeks.
SOLUTION PREPARATION
L- Valine and fumaric acid in the molar ratio 1:1
 following the reaction




Optically transparent
Free from visible
Colourless crystals
15- 20 days.
Spectroscopic study of growth and characterisation of l valine
Spectroscopic study of growth and characterisation of l valine
SINGLE CRYSTAL X-RAY DIFFRACTION

   X- ray differaction studies using a CAD- 4 MACH 3 MOK
     = 0.71073 A . X- ray diffractometer to determine the unit
    cell dimensions of LVF are


 A= 22.350 A                  = 90
 B= 7.301 A                    = 91
 C= 5.343 A                   = 90

 Volume is 871.5 A ˆ3.
 It belongs to monoclinic.
UV-Vis- NIR Spectral analysis
ACIC
                                      St.Jo sep h's Colle ge (Auton omo us), Trich y-2


                                                                                               UV Result
                                                                                               Dat e: 9/18/2 008


              Spe ctru m Na me: NO-1 .SP
 100.0

     95

     90                               383.01,99.553

     85                   381.04,99.493                                                        1062.0,99.616
     80

     75

     70

     65

     60

     55

     50
%T
     45

     40

     35

     30

     25

     20

     15

     10            223.78,0.065091

      5

     0.0
      190.0        300               400              500   600        700       800     900       1000            1100.0
                                                                  nm

              Instrument Model: Lambda 35
ANALYSIS OF INFRARED SPECTUM OF LVF CRYSTALS

   It gives sufficient information about the structure of
    compound.

   The absorption of IR radiations causes the various bands in
    molecules to stretch and bend with respect to one another.

   The vibrational spectrum used in the identification of
    ligands or ions in a molecule.



   The absorption of the Infrared and Raman radiation can be
    expressed either in terms of wavelength or wave number
FT-IR STUDIES OF L-VALINE FUMARATE
S.NO   L-Valine Fumarate   Assignment
       cm-1
1.     3084                NH+ asymmetric stretching
2.     2935                CH2 asymmetric stretching
3.     2602                NH---O stretching
4.     1619, 1513          NH3+ asymmetric bending
5.     1452                NH3+ symmetric bending
6.     1413                COO- symmetric stretching
7.     1361,1303           C-C stretching
8.     1151                C-N stretching
9.     1012                C-C stretching
10.    918                 C-CH bending
11.    773                 C-C skeletal stretching
12.    646                 COO- bending
13.    540                 C-C=O wagging
14.    413                 COO- rocking
ACIC
                                      St. Josep h's Colleg e ( Autonomo us )
                                                      T rich y-2



                                                                                                                   FT IR S PECT RUM
                                                                                                                   Date: 9/18/20 08
           Sp ectrum Name: Sam =N0 -1. sp
 100.0
                                                                                                                                     412.81


     90


     80


     70                                                                                                              792.71



     60

                                                                                                            931.29                     477.26

     50                                                                                                                 748.58
%T
                                                  2047.92                                                            835.99   677.38
                                                                                                                                 588.17
     40                                                                                                                              518.22

                                        2658.96                                                                885.63
     30                                                                              1358.30
                                   2740.95


                                                                                               1160.19
     20
                                                                                                         1003.10


                                                                                                     1066.90
     10
                            2972.27                                             1425.85          1111.57
                                                                                      1291.51
                        3073.03                                     1637.72
     0.0                                                                    1502.99
      4000.0               3000                     2000                      1500                       1000                             400.0
                                                                   cm -1
       Sam =N0 -1. pk

       SAM_ N0 ~2. SP   3 601     400 0. 00   400. 00   6. 89   10 0. 00   4. 00 % T      3 0 .8 0

       REF 4 000 98 .1 6 2000 5 3. 55 600
       30 73. 03 10. 14  2972 .2 7 1 2. 84 2 740. 95 41 .3 5 26 58. 96 41. 31   204 7. 92 51. 96
       16 37. 72 10. 16  1502 .9 9 6 .8 9  142 5. 85 17. 10  1358 .3 0 1 9. 55 1 291. 51 11 .1 5
       11 60. 19 19. 85  1111 .5 7 1 5. 22 1 066. 90 17 .7 4 10 03. 10 24. 74   931 .2 9 43 .2 4
       88 5. 63 43 .3 6 83 5. 99 5 0. 20 7 92. 71   59. 55 7 48. 58   54. 94  677. 38   54. 12
       58 8. 17 48 .6 4 51 8. 22 4 9. 56 4 77. 26   62. 06 4 12. 81   83. 85
Spectroscopic study of growth and characterisation of l valine
Spectroscopic study of growth and characterisation of l valine
Spectroscopic study of growth and characterisation of l valine
CONCLUSION
   Single crystals of LVF - grown by slow evaporation technique at room
    temperature.

   Unit cell parameters have been evaluated by single crystal X-ray
    diffraction technique.
                                A≠B ≠ C
                              = = 90       ≠ 90
                           Volume is 871.5 A ˆ3

   LVF belongs to monoclinic structure.
CONTINUE….
   The good optical transmittance in the entire 300-1100 nm region
    makes the crystal, a potential candidate for optoelectric applications.

   The functional groups present in the grown crystal have been
    conformed by FT-IR spectral analysis.

   It is also evident from spectral studies that binding of Valine with
    fumaric acid occurs through Nitrogen.
Spectroscopic study of growth and characterisation of l valine
REFERENCE
♣   Gupta, Kumar, Solid State Physics, K. Nath & Co., Publication (2003)
♣   K. Nakamoto, Infrared & Raman Spectra of Inorganic & Co-ordinate
    compounds, Willey New York) 1978)
♣   N. Prasad, David, J. Williams, Introduction to Non Linear Effects is
    Molecules and polymers (willey – Interscience publications, New York
    (1991).
♣   P.S. Dharmambal, M.Phil Thesis, Gel growth and characterization      of
    pure and doper and mixer KDP crystals (Bharathidasan University,
    Thiruchirapalli).
♣   C. Ramachandra Raja, PhD Thesis, Growth and characterization of
    Potassium Penta Borate and Beta Barium Borate Crystals (Anna University,
    Chennai, 1993).
♣   I. John David Ebenezar, M.Phil. Thesis, Growth and characterization of
    KDP crystals, (Bharathidasan University, Thichirapalli, 1995).
Spectroscopic study of growth and characterisation of l valine
Spectroscopic study of growth and characterisation of l valine

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Spectroscopic study of growth and characterisation of l valine

  • 1. SPECTROSCOPIC STUDY OF GROWTH AND CHARACTERISATION OF L- VALINE FUMARIC ACID CRYSTAL PROJECT HANDLER V.REVATHIAMBIKA
  • 2. INTRODUCTION MATTER • SOLID • LIGUID • GAS PHASE TRANSFORMATION • Solid to solid • Liquid to Liquid • Gas to gas CRYSTALLINE SOLIDS • Single crystal • polycrystalline
  • 5. NUCLEATION 1. Development of super saturation 2. Generational of embryo 3. Growth of the embryo from the unstable critical state to stable state. 4. Relaxation process where the texture of the newly born nucleus alters.
  • 7. SLOW EVAPORATION METHOD  Ex 40g of solute in 100 ml of solvent is considered as saturated at 50 C. Now the solution is reduced to some lower level say 70 ml then 40gms in 70 ml at 50 C is super saturated solution.
  • 8. L-VALINE & FUMARIC ACID  L-VALINE  FUMARIC ACID Formula : C5H11No2 Formula : C4H4O4 Molecular Weight :117.15 Molecular Weight : 116.07 Melting Point : 295-3000C Melting Point : 2870C Solubility : Soluble in water Solubility : Soluble in water
  • 10. GROWTH OF LVF CRYSTALS  1.952 gms of L- valine is dissolved in 100 ml of water then 1.934 gms of fumaric acid is dissolved in 100 ml of water.  These two solutions were mixed and these solutions may contain impurities such as solid dust particles. So it was filtered.  This solution is covered with polythene paper and for slow evaporation few holes are made in the polythene paper and the solution is undisturbed.  It shows the slow evaporation of water the excess of solute atoms join together to form cluster. The cluster is grown which resulted in the formation of crystals in a few weeks.
  • 11. SOLUTION PREPARATION L- Valine and fumaric acid in the molar ratio 1:1 following the reaction Optically transparent Free from visible Colourless crystals 15- 20 days.
  • 14. SINGLE CRYSTAL X-RAY DIFFRACTION  X- ray differaction studies using a CAD- 4 MACH 3 MOK = 0.71073 A . X- ray diffractometer to determine the unit cell dimensions of LVF are  A= 22.350 A = 90  B= 7.301 A = 91  C= 5.343 A = 90  Volume is 871.5 A ˆ3.  It belongs to monoclinic.
  • 16. ACIC St.Jo sep h's Colle ge (Auton omo us), Trich y-2 UV Result Dat e: 9/18/2 008 Spe ctru m Na me: NO-1 .SP 100.0 95 90 383.01,99.553 85 381.04,99.493 1062.0,99.616 80 75 70 65 60 55 50 %T 45 40 35 30 25 20 15 10 223.78,0.065091 5 0.0 190.0 300 400 500 600 700 800 900 1000 1100.0 nm Instrument Model: Lambda 35
  • 17. ANALYSIS OF INFRARED SPECTUM OF LVF CRYSTALS  It gives sufficient information about the structure of compound.  The absorption of IR radiations causes the various bands in molecules to stretch and bend with respect to one another.  The vibrational spectrum used in the identification of ligands or ions in a molecule.  The absorption of the Infrared and Raman radiation can be expressed either in terms of wavelength or wave number
  • 18. FT-IR STUDIES OF L-VALINE FUMARATE S.NO L-Valine Fumarate Assignment cm-1 1. 3084 NH+ asymmetric stretching 2. 2935 CH2 asymmetric stretching 3. 2602 NH---O stretching 4. 1619, 1513 NH3+ asymmetric bending 5. 1452 NH3+ symmetric bending 6. 1413 COO- symmetric stretching 7. 1361,1303 C-C stretching 8. 1151 C-N stretching 9. 1012 C-C stretching 10. 918 C-CH bending 11. 773 C-C skeletal stretching 12. 646 COO- bending 13. 540 C-C=O wagging 14. 413 COO- rocking
  • 19. ACIC St. Josep h's Colleg e ( Autonomo us ) T rich y-2 FT IR S PECT RUM Date: 9/18/20 08 Sp ectrum Name: Sam =N0 -1. sp 100.0 412.81 90 80 70 792.71 60 931.29 477.26 50 748.58 %T 2047.92 835.99 677.38 588.17 40 518.22 2658.96 885.63 30 1358.30 2740.95 1160.19 20 1003.10 1066.90 10 2972.27 1425.85 1111.57 1291.51 3073.03 1637.72 0.0 1502.99 4000.0 3000 2000 1500 1000 400.0 cm -1 Sam =N0 -1. pk SAM_ N0 ~2. SP 3 601 400 0. 00 400. 00 6. 89 10 0. 00 4. 00 % T 3 0 .8 0 REF 4 000 98 .1 6 2000 5 3. 55 600 30 73. 03 10. 14 2972 .2 7 1 2. 84 2 740. 95 41 .3 5 26 58. 96 41. 31 204 7. 92 51. 96 16 37. 72 10. 16 1502 .9 9 6 .8 9 142 5. 85 17. 10 1358 .3 0 1 9. 55 1 291. 51 11 .1 5 11 60. 19 19. 85 1111 .5 7 1 5. 22 1 066. 90 17 .7 4 10 03. 10 24. 74 931 .2 9 43 .2 4 88 5. 63 43 .3 6 83 5. 99 5 0. 20 7 92. 71 59. 55 7 48. 58 54. 94 677. 38 54. 12 58 8. 17 48 .6 4 51 8. 22 4 9. 56 4 77. 26 62. 06 4 12. 81 83. 85
  • 23. CONCLUSION  Single crystals of LVF - grown by slow evaporation technique at room temperature.  Unit cell parameters have been evaluated by single crystal X-ray diffraction technique. A≠B ≠ C = = 90 ≠ 90 Volume is 871.5 A ˆ3  LVF belongs to monoclinic structure.
  • 24. CONTINUE….  The good optical transmittance in the entire 300-1100 nm region makes the crystal, a potential candidate for optoelectric applications.  The functional groups present in the grown crystal have been conformed by FT-IR spectral analysis.  It is also evident from spectral studies that binding of Valine with fumaric acid occurs through Nitrogen.
  • 26. REFERENCE ♣ Gupta, Kumar, Solid State Physics, K. Nath & Co., Publication (2003) ♣ K. Nakamoto, Infrared & Raman Spectra of Inorganic & Co-ordinate compounds, Willey New York) 1978) ♣ N. Prasad, David, J. Williams, Introduction to Non Linear Effects is Molecules and polymers (willey – Interscience publications, New York (1991). ♣ P.S. Dharmambal, M.Phil Thesis, Gel growth and characterization of pure and doper and mixer KDP crystals (Bharathidasan University, Thiruchirapalli). ♣ C. Ramachandra Raja, PhD Thesis, Growth and characterization of Potassium Penta Borate and Beta Barium Borate Crystals (Anna University, Chennai, 1993). ♣ I. John David Ebenezar, M.Phil. Thesis, Growth and characterization of KDP crystals, (Bharathidasan University, Thichirapalli, 1995).