Spectroscopic study of growth and characterisation of l valine
SPECTROSCOPIC STUDY OF GROWTHAND 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
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.
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.
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
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 PREPARATIONL- Valine and fumaric acid in the molar ratio 1:1 following the reactionOptically transparentFree from visibleColourless crystals15- 20 days.
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.
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
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.
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).