basic concept of crystal, introduction crystal, fundamental study of spectro, L-valine fumaric acid crystal, single crystal

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.

15. UV-Vis- NIR Spectral analysis

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).