Synthesis, Growth and Characterization Studies on Leucine and Β-Alanine Mixed (La) single Crystal by Slow Evaporation Method

 

M. Santhi1*, A. Rathinavelu1, M. Sathya2, S. Ananthakumar3

1Assistant Professor of Chemistry, Erode ARTS and Science College, Erode-638 009, T.N. India.

2Assistant Professor of Chemistry, Nandha College of Technology, Erode-638052, T.N. India.

3M. Phil. Research Scholar, Erode Arts and Science College, Erode-638 009, T.N. India.

*Corresponding Author E-mail: santhisendil@gmail.com

 

ABSTRACT:

The synthesis of Leucine and β-alanine mixed (LA) single crystals done under low temperature slow evaporation solution growth method. The synthesized crystals characters are studied using XRD, FT-IR, SEM, and UV-VISIBLE Processes. XRD studies are used to carry out the crystallographic analysis. FT-IR studies are used to observe the functional groups of leucine and β-alanine mixed crystals. SEM studies are used to study the morphological identification. UV-VISIBLE studies are used to study the optical absorbance analysis.

 

KEYWORDS: Growth from solution, Single crystal, XRD, FT-IR, SEM, and UV-VISIBLE.

 

 


INTRODUCTION:

A crystal or crystalline solid is a solid material whose constituent atoms, molecules, or ions are arranged in an orderly, repeating pattern extending in all three spatial dimensions. In addition to their microscopic structure, large crystals are usually identifiable by their macroscopic geometrical shape, consisting of flat faces with specific, characteristic orientations. The scientific study of crystals and crystal formation is known as crystallography. The process of crystal formation via mechanisms of crystal growth is called crystallization or solidification. The word crystal is derived from the Ancient Greek word krustallos, meaning both “ice” and “rock crystal”, from kruos, "icy cold, and frost"[1-2]. A single crystal or monocrystalline solid is a material in which the crystal lattice of the entire example is continuous and unbroken to the edges of the sample, with no grain boundaries. The absence of the defects associated with grain boundaries can give monocrystals unique properties.

 

 

Particularly mechanical, optical and electrical, which can also be anisotropic depending on the type of crystallographic structure. These properties, in addition to making them precious in some gems are industrially used in technological applications, especially in optics and electronics. The strong influence of single crystals in the present day technology is evident from the recent developments in the above mentioned fields. Hence, in order to achieve performance from the device, good quality single crystals are needed. Crysatlline structure is more likely used in many applications compare to the non-crystalline structure[3]. Amino acids are molecules containing an amine group, a carboxylic acid group and a side chain that varies between different amino acids. Recent studies indicate the Leucine favorably forms several salts with organic or inorganic acids. In this paper, the method of crysatl growth with emphasis on low temperature solution growth technique was described. The synthesized crystals characters are studied using XRD, FT-IR, SEM, and UV-VISIBLE Processes.

 

GROWTH OF CRYSTALS:

Synthesis Leucine And Β-Alanine Mixed (LA) Single Crystals:

The synthesis of mixed crystals are done under low temperature slow evaporation method. 5g of each Leucine and β–alanine is weighed accurately and dissolved in 50ml of double distilled water and stirred it vigorously at 280c for 15 minutes. Then, the saturated solution was decanted into the 100ml beaker. The remaining solute was dissolved in 5ml of distilled water; the solution is stirred continuously for 15 minutes. The above process is continued until the solute is fully saturated. After the saturation, the solution was taken in a 100ml beaker which was tightly closed with the filter paper, so that the rate of evaporation could be minimized. Good transparent mixed (LA) crystals are obtained after 4 weeks. The grown crystals are shown in Figure1. Then, the synthesized crystals are characterized using XRD, SEM, FT-IR, UV-VISIBLE studies.

 

 

Fig.1: Leucine and β–alanine mixed (LA) Single Crystals

 

CHARACTERIZATION METHODS:

XRD ANALYSIS:

X-ray powder diffractograms were recorded for Leucine and β-alanine mixed (LA) single crystals at room temperature. The sample for the powder X-ray diffraction was prepared by crushing a small piece of a crystal into fine powder. The fine calcined particles were characterized for crystal phase identification by powder x-ray diffraction (XRD) using a XRD-6000 (Shimadzu, Japan). The powder was then spread over a glass plate with uniform thickness. Methanol was used as a binder to spread the powder on the glass plate with uniform thickness. The radiation used was Ni filtered Cu Kα (λ=1.5418Ĺ). The scan speed was 10°/minute and the scan range was 4.0000°-90.0000°.

 

FT-IR SPECTRAL ANALYSIS:

Fourier Transmission Infrared (FT-IR) spectra of the Leucine and β–alanine mixed (LA) single crystals (as pellets in KBr ) were recorded using IR Affinity-1 Fourier Transmission Infrared spectrometer (Shimadzu, Japan) in the range of 4000-400 cm-1 with a resolution of 1cm-1.

 

 

 

 

SEM ANALYSIS:

The particle size and external morphology of the fine calcined powders were characterized by scanning electron microscopy Jsm-6390 (Shimadzu, Japan).

 

UV-VISIBLE SPECTRUM:

The optical Absorption spectra was studied using UV–1700 Pharma spectrophotometer (Shimadzu, Japan) in the range of 200–800 nm.

 

RESULTS AND DISCUSSION:

XRD SPECTRUM:

The powder XRD patterns of Leucine(C6H13NO2) and β–alanine (C3H7NO2) mixed crystals are shown in figures a=4.01, b=2.68, c=1.24 and a=14.234 b=11.052, c=5.860 and the data’s are the lattice parameters and the crystal system are presented. The data indicates that (LA) single crystal crystallizes in orthorhombic structure [4]. To confirm the XRD data, powder XRD studies were also carried out for the sample. The grown crystals of (LA) were crushed into fine powder and powder X-ray diffraction analysis has been carried out using a powder X-ray diffractometer. The recorded pattern is shown in Figure 2. The sharp peaks of XRD pattern indicate high degree of crystalline structure of grown crystal. The observed diffraction pattern has been indexed and Miller indices were estimated by Indexing software package.

 

 

Fig.2: XRD diffraction Leucine and β- alanine mixed (LA) single crystals

 

FT-IR SPECTRAL ANALYSIS:

The presence of N-O stretching asymmetric is indicated by a sharp absorption peak at 1520.11cm-1. The sharp absorption peak’s observed at 1101.15 cm-1 respond to CO2 symmetric stretching. The sharp absorption peak observed at 1750.01 cm-1. The absorption peak observed at 1200.07cm-1 respond to C=O asymmetric stretching of Acid group. Stretching of N-O linkage produces very strong and broad peak at 676.11cm-1 is attributed to Nitrate group. The sharp absorption observed at longer wavelength near 402.09cm-1 likely result from NO2 bending vibration.

 

 

Fig.3: FT-IR spectrum of Leucine and β-alanine mixed (LA) single crystals

 

Table.1. Vibrational Assignments for (LA) Crystal

FREQUENCY CM-1

ASSIGNMENT

3850.10

OH – Stretching

1520.11

N-O stretching asymmetric

1101.15

CO2 symmetric stretching

1750.01

sharp absorption

1200.07

C=O asymmetric stretching of Sulphate group

676.11

N-O linkage of Nitrate group

402.09

NO2 bending vibration

 

SEM ANALYSIS:

Typical SEM micrographs for powder synthesised at different magnifications are shown in Figure 4. it is evident from the photograph that the background of the surface was crystalline and morphology crystalline Leucine mixed crystals the size of the particle determined from the SEM image are 5-100 µm.

 

 

Fig.4: Scanning Electron Micro Graph of Leucine and β- Alanine mixed (LA) single crystals

 

 

UV-VISIBLE ABSORBANCE:

The lower cut-off the weak concentration of Leucine and β–alanine mixed crystals (LA) single is around strong absorbance 1.253 in the mid range uv-302 nm and high concentration of Leucine and β –alanine mixed (LA) single crystals is around strong absorbance 3.010 in the mid range uv-301 nm. The mixed crystals of Leucine and β – alanine mixed (LA) single crystals are used in the field of medical phototherapy and dermatological, solar experimentation.

 

A) WEAK CONCENTRATION

 

Fig.5a: UV-visible absorption spectrum of Leucine and β-alanine mixed (LA) single crystals

 

No.

p/v

Wavelength

Abs.

1

302.00

1.253

2

 

263.00

0.297

 

B) HIGH CONCENTRATION:

 

Fig.5b: UV-visible absorption spectrum of Leucine and β-alanine mixed (LA) single crystals

 

No.

p/v

Wavelength

Abs.

1

301.00

3.010

2

262.50

0.696

 

CONCLUSION:

A Leucine doesn’t have NLO application because that compound having centro symmetry nature and NLO application of Leucine and β –alanine mixed (LA) single crystals have non centro symmetry nature crystals were successfully grown at low temperature slow evaporation method.The grown crystals have been subjected to various characterization studies such as XRD, FT-IR, SEM, analysis, UV-VIS-Spectrum. The mixed crystals of X-Ray Diffraction (XRD) analysis confirms that the Leucine and β –alanine mixed (LA) single crystals is Orthorhombic in structure with space group Cmc1. The molecular structure of the synthesis compound was confirmed by FT-IR analysis. The background of scanning electron microscope (SEM) shows the formation of microparticles. The weak concentration of Leucine and β –alanine mixed (LA) single crystals is around strong absorbance 1.253 in the mid range uv-302 nm and high concentration of Leucine and β – alanine mixed (LA) single crystals is around strong absorbance 3.010 in the mid range uv-301 nm. So the present study of mixed (LA) single crystals are greater role in chemical industries and biological studies.

 

REFERENCES:

1.       Krassmann. Thomas. "The Giant Crystal Project". (2005–2008).

2.       Teaching Pamphlets". Commission on Crystallographic Teaching. (2007).

3.       Santhi M. Rathinavelu A. Sathya M. Jayalakshmi S. Ananthakumar S. Synthesis, Growth and Characterization Studies on Butylamine, Ascarbic Acid and Leucine (BAL) Mixed Single Crystal By Slow Evaporation Method. IOSR Journal of Applied Physics (IOSR-JAP). 2018; 10 [2]: 60-64.

4.       Madhavan J. Aruna S. Thomas P C. Vimalan M. Rajasekar SA. Sagayaraj P. Crystal Research and Technology. 2007; 42:59-64.

 

 

 

 

 

Received on 15.05.2018           Modified on 13.06.2018

Accepted on 07.07.2018           ©AJRC All right reserved

Asian J. Research Chem. 2018; 11(4):751-754.

DOI: 10.5958/0974-4150.2018.00132.3