Spectroscopic study of growth and characterisation of l valine
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SPECTROSCOPIC STUDY OF GROWTH AND CHARACTERISATION OF L- VALINE FUMARIC ACID CRYSTAL PROJECT HANDLER V.REVATHIAMBIKA
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basic concept of crystal, introduction crystal, fundamental study of spectro, L-valine fumaric acid crystal, single crystal
Transcript of Spectroscopic study of growth and characterisation of l valine
SPECTROSCOPIC STUDY OF GROWTH AND CHARACTERISATION OF L-VALINE FUMARIC ACID CRYSTAL
PROJECT HANDLERV.REVATHIAMBIKA
INTRODUCTIONMATTER•SOLID•LIGUID•GASPHASE TRANSFORMATION•Solid to solid•Liquid to Liquid•Gas to gas
CRYSTALLINE SOLIDS•Single crystal•polycrystalline
NUCLEATION
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.
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 ACIDL-VALINEFormula : C5H11No2
Molecular Weight :117.15
Melting Point : 295-3000C
Solubility : Soluble in water
FUMARIC ACIDFormula : C4H4O4
Molecular Weight :116.07
Melting Point : 2870CSolubility : Soluble in
water
GROWTH OF LVF CRYSTALS1.952 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
H3C-CH-CH2-COOH +COOH-CH H3C-CH-CH2-NH3+....._OOC-CH
CH3NH2 COOH-CH CH3COOH COOH-CH
Optically transparentFree from visible Colourless crystals15- 20 days.
SINGLE CRYSTAL X-RAY DIFFRACTION
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 = 90B= 7.301 A = 91C= 5.343 A = 90
Volume is 871.5 A ˆ3.It belongs to monoclinic.
UV-Vis- NIR Spectral analysis
ACICSt.Joseph's College (Autonomous), Trichy-2
UV Result
Spectrum Name: NO-1.SP
Instrument Model: Lambda 35
Date: 9/18/2008
190.0 300 400 500 600 700 800 900 1000 1100.0
0.0
5
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85
90
95
100.0
nm
%T
1062.0,99.616
383.01,99.553
381.04,99.493
223.78,0.065091
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
cm-1
Assignment
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
FTIR SPECTRUM
ACIC
St.Joseph's College ( Autonomous )Trichy-2
Spectrum Name: Sam =N0-1.sp Date: 9/18/2008
Sam =N0-1.pk
SAM_N0~2.SP 3601 4000.00 400.00 6.89 100.00 4.00 %T 3 0.80
REF 4000 98.16 2000 53.55 6003073.03 10.14 2972.27 12.84 2740.95 41.35 2658.96 41.31 2047.92 51.96 1637.72 10.16 1502.99 6.89 1425.85 17.10 1358.30 19.55 1291.51 11.15 1160.19 19.85 1111.57 15.22 1066.90 17.74 1003.10 24.74 931.29 43.24 885.63 43.36 835.99 50.20 792.71 59.55 748.58 54.94 677.38 54.12 588.17 48.64 518.22 49.56 477.26 62.06 412.81 83.85
4000.0 3000 2000 1500 1000 400.0
0.0
10
20
30
40
50
60
70
80
90
100.0
cm-1
%T
3073.03
2972.27
2740.95
2658.96
2047.92
1637.72
1502.99
1425.85
1358.30
1291.51
1160.19
1111.57
1066.90
1003.10
931.29
885.63
835.99
792.71
748.58
677.38588.17
518.22
477.26
412.81
CONCLUSIONSingle 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.
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).
