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).