Spectroscopic study of growth and characterisation of l valine

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

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Spectroscopic study of growth and characterisation of l valine

  1. 1. SPECTROSCOPIC STUDY OF GROWTHAND CHARACTERISATION OF L-VALINE FUMARIC ACID CRYSTAL PROJECT HANDLER V.REVATHIAMBIKA
  2. 2. INTRODUCTION MATTER • SOLID • LIGUID • GAS PHASE TRANSFORMATION • Solid to solid • Liquid to Liquid • Gas to gas CRYSTALLINE SOLIDS • Single crystal • polycrystalline
  3. 3. NUCLEATION1. Development of super saturation2. Generational of embryo3. Growth of the embryo from the unstable critical state to stable state.4. Relaxation process where the texture of the newly born nucleus alters.
  4. 4. SLOW EVAPORATIONMETHOD 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.
  5. 5. L-VALINE & FUMARIC ACID L-VALINE  FUMARIC ACIDFormula : C5H11No2 Formula : C4H4O4Molecular Weight :117.15 Molecular Weight : 116.07Melting Point : 295-3000C Melting Point : 2870CSolubility : Soluble in water Solubility : Soluble in water
  6. 6. 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.
  7. 7. SOLUTION PREPARATIONL- Valine and fumaric acid in the molar ratio 1:1 following the reactionOptically transparentFree from visibleColourless crystals15- 20 days.
  8. 8. 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.
  9. 9. UV-Vis- NIR Spectral analysis
  10. 10. ACIC St.Jo sep hs 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
  11. 11. 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
  12. 12. FT-IR STUDIES OF L-VALINE FUMARATES.NO L-Valine Fumarate Assignment cm-11. 3084 NH+ asymmetric stretching2. 2935 CH2 asymmetric stretching3. 2602 NH---O stretching4. 1619, 1513 NH3+ asymmetric bending5. 1452 NH3+ symmetric bending6. 1413 COO- symmetric stretching7. 1361,1303 C-C stretching8. 1151 C-N stretching9. 1012 C-C stretching10. 918 C-CH bending11. 773 C-C skeletal stretching12. 646 COO- bending13. 540 C-C=O wagging14. 413 COO- rocking
  13. 13. ACIC St. Josep hs 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
  14. 14. 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.
  15. 15. 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.
  16. 16. 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).

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