Analytical Reagent Grade Research Articles

Removal of REE and Th from solution by co-precipitation with Pb-phosphates

The supply of technologically important rare earth elements (REE) is a concern in Europe, hence the recovery of REE from alternative sources has recently become widely investigated. One of the problems is the lack of cost-effective technologies for REE recovery from leaching solutions. The present work investigated the potential for recovering REE and Th from leaching solutions by co-precipitation with Pb phosphates. A set of four experiments were conducted using analytical reagent grade chemicals to analyze the effects of Pb and different pH on the efficiency of REE and Th removal from aqueous solutions. After selecting the best conditions, two additional experiments were performed using solutions obtained from leaching REE-rich apatite mine waste.The precipitates resulting from the experiments as well as the solutions before and after precipitation were analyzed. It was found that the formation of a crystalline mixture of REE- and Th- enriched pyromorphite, Pb5(PO4)3Cl, and Pb-phosphates, about which little has been known so far, was responsible for complete (>99%) removal of REE and Th from aqueous solutions at pH 4 and 6. At lower pH, the removal is incomplete except for Sc and Th, which probably form a distinct phases. Besides that, no fractionation of LREE and HREE was observed. The experiments included the study of solutions resulting from the leaching of REE-rich apatite waste, which may contribute to the development of new technologies for REE recovery from wastes.

Short-process simultaneously recycling cobalt and manganese from environment-hazardous di-methyl-dithiocarbamate chelate slag as lithium-ion battery cathode material

An efficient and high recovery rate short-process environment-hazardous chelate recycling method is utilized to prepare nickel–cobalt-manganese layered oxide which simultaneously recovers cobalt and manganese and not includes solvent extraction. The recovery rate of cobalt and manganese can achieve 97.68% and 96.74% respectively. The X-ray diffraction spectrum of the recycling sample shows a well-ordered layered structure, and no impurity phase is observed. The sample uses chelate slag has the same purity level and approximate electrochemical performance as the sample prepared by analytical-grade reagents. The recycling sample exhibits a high discharge capacity at 10 C rate, average capacity excesses 105 mAh·g-1compared to 90 mAh·g−1 of the sample prepared by analytical-grade reagents. The capacity retention rate at 0.5 C and 1 C of the recycling sample is 82.86% and 73.14%, compared to 86.71% and 88.95% of the sample prepared by analytical-grade reagents. The capacity at 0.2 C of the recycling sample is 169.58 mAh·g-1compared to 159.86 mAh·g−1 of the sample prepared by analytical-grade reagents. This article first-time reports the recycling method of chelate slag which shows a high feasibility and utilization prospect that can efficiently recycle the valuable metal elements simultaneously prepare valuable production from environment-hazardous chelate slag and alleviate the shortage of cobalt resources.

Concentrations of Total Petroleum Hydrocarbons N-Alkanes in Surface Seawater from The Red Sea Coast of Hodeidah City, Yemen

Field work has been carried out to identify the occurrence of oil and oil by- product pollution from the Red Sea coast of Hodeidah city, was evaluated from December, 2021 to June, 2022. Surface seawater samples were collected from four stations and extracted using standard methods. The extracts were subsequently analyzed by gas chromatography-flame ionization detection. EPH aliphatic hydrocarbon standard 14 components (C9 – C36), high performance liquid chromatographic (HPLC) grade solvents and analytical grade reagents used for this work. The total concentration of aliphatic hydrocarbons n-alkanes (TPH) in surface seawater samples ranged from 9400.5 μg /l at Hodeidah harbor to 2409.7 μg /l at Hodeidah Power Plant in winter and from 4880.9 μg /l at Hodeidah Harbor to 1109.1 μg /l at Hodeida Power Plant in summer. This pollution is a consequence of localized oil operation and /or heavy ship traffic. The investigations in These locations can serve as a reference for future evaluations and studies.

Development of the spectrophotometric method for the determination of metoprolol in tablets by using bromophenol blue

The aim of the work was to develop a simple, economical and eco-friendly spectrophotometric method for determining metoprolol tartrate in tablets based on the reaction with bromophenol blue (BPB).
 Material and methods: A double–beam Shimadzu UV-Visible spectrophotometer, with a spectral bandwidth of 1 nm wavelength accuracy ±0.5 nm, Model –UV 1800 (Japan), Software UV-Probe 2.62, and a pair of 1 cm matched quartz cells, was used to measure the absorbance of the resulting solution. All the chemicals were used in analytical reagent grade. Pharmacopeial standard samples of metoprolol tartrate and bromophenol blue (BPB) were provided by Sigma-Aldrich (≥ 98%, HPLC). The used dosage forms of metoprolol tartrate are tablets of Metoprolol 50 mg and 100 mg.
 Results and discussion: The method of spectrophotometric determination of the quantitative content of metoprolol tartrate based on its reaction with BPB in a methanol solution has been developed. The stoichiometric ratios of the reactive components as 1:1 were obtained by the methods of continuous changes and the saturation method. The developed method of quantitative determination of metoprolol tartrate was validated. The linearity regression equation was y = 0.0373x + 0.0038, and the obtained correlation coefficient was R2=0.9984. A linear relationship was found between absorbance at λmax and concentration of metoprolol tartrate in the range of 9.56-15.02 µg/mL. The LOD and LOQ values were calculated to be 0.81 µg/mL and 2.67 µg/mL.
 Conclusions. A simple, economical and eco-friendly spectrophotometric method has been developed for the quantitative determination of metoprolol tartrate in tablets based on the reaction with BPB. The developed method of quantitative determination of metoprolol tartrate was validated in accordance with the requirements of SPhU. We suggest our work with offered detailed and successful solutions for the mentioned aim with less sophisticated equipment for QC lab for routine manufacturing control

Development and characterization of hydralazine mouth dissolving tablet

Tablet dosage form is the most popular among all existing conventional dosage forms because of its convenience of self-administration, compactness and easy manufacturing. Many patients find it difficult to swallow tablets and capsules. The difficulty is experienced in particular by pediatric and geriatric patients, but it also applies to people who are ill on bed and to those active working patients who are busy or traveling, especially those who have no access to water. The drug hydralazine HCl were used. The amount of drug was 35 mg. the different super disintegrates was used to make a suitable mouth dissolving tablet. All the other reagents which is used in analytical grade reagents. In the present study mouth dissolving tablets of hydralazine HCl were designed, prepared and evaluated. These tablets can disintegrate or dissolve rapidly once placed into the oral cavity. The feofenadine was analyzed for its organoleptic, physicochemical and spectral (IR, UV) properties. The obtained hydralazine HCl was concordant with reference specifications. A complex of hydralazine HCl was successfully formulated. The volunteers rated the resinate as tasteless and agreeable complex.

Developing the analytical methods for the assay of anthelmintics (Albendazole) and anti- tuberculosis agents (Ethionamide) by utilizing two CT reagents - iodine and picric acid

Introduction - Rifampin, isoniazid, pyrazinamide, and ethambutol are antitubercular drugs that have been licenced by the FDA for the treatment of Mycobacterium tuberculosis infections. Antitubercular medicines are drugs that are used to treat tuberculosis. The term "anthelmintic" refers to a medicine used to treat parasitic worm infestations in animals. This comprises both flat and round worms, such as flukes (trematodes) and tapeworms (cestodes) (nematodes). Aim of this study - The primary aim of this research is to develop and validate simple, fast, reliable, robustness and ruggedness analytical procedures for anthelmintics (ALB) and antitubercular (ETH) medicines. Material and Methods - Two CT reagents, iodine and picric acid, were used to produce two simple and somewhat sensitive Albendazole (ALB) and Ethionamide (ETN) techniques. The CT complex with the placebo blank had almost the same absorbance as the reagent blank, indicating that there was no interference by using Systronics model 166 digital spectrophotometer tools. Organic solvents were employed to dissolve all of the chemicals, which were of analytical reagent grade.

Cs2 CO3 -Promoted C-O Coupling Protocol Enables Solventless (Hetero)aryl Ether Synthesis under Air Atmosphere.

In this work, a Cs2 CO3 -promoted synthetic approach was identified for (hetero)aryl ether synthesis via the C-O coupling of various (hetero)aryl chlorides and alcohols/phenol. To our delight, the reactions could be carried out under transition-metal-free and solvent-free conditions. Moreover, analytical-grade reagents and air atmosphere were readily tolerated. To showcase the practical usefulness of the present protocol, the assembly of a bioactive molecule was facilely realized and the gram-scale production of selected ether products was also efficiently accomplished. In addition, density functional theory (DFT) studies, along with a few mechanistic experiments, were conducted to elucidate a proposed reaction pathway and rationalize the pivotal role of Cs2 CO3 in promoting this process. Hopefully, this work could provide useful information for researchers who are engaging in C-O cross-coupling reactions.

Study of Effect of Substrate Temperature on Structure, Morphology and optical Properties of Spray Deposited Cu2ZnSnS4 Nano Thin films.

Cu2ZnSnS4 (CZTS) films for different substrate temperatures were deposited by using simple chemical spray technique. Analytical reagent Grade; Copper chloride (CuCl2), Zinc chloride (ZnCl2), Tin chloride (SnCl4.5H2O) and thiourea (SC(NH2)2) were used as Cu+, Zn+, and Sn+ and ion sources respectively. A set of five CZTS films was deposited using five different substrate temperatures (175, 200, 250, 275, and 300 ). The structure, Morphology, Elemental analysis and optical properties of these films were studied using X-ray diffratometer (XRD), Scanning Electron Microscopy (SEM), Energy Dispersive X-ray Analysis (EDX) and UV-Visible spectroscopy techniques respectively. The XRD spectra showed that all films are polycrystalline and exhibit kesterite tetragonal crystal structure with preferential orientation along (112) direction. The crstallinity was found increased with substrate temperature. The calculated crystallite size was increased with increase in substrate temperature. The surface morphology of CZTS films was improved with increase in substrate temperature. The film sample deposited for 275 represent excellent spherical granules CZTS crystals of increasing size from 640 nm to 1.8 μm arranged in regular fashion with some void spaces. The purity of the composition was investigated using Elemental analysis of the deposited films. The optical band gap was estimated using Tauc plots. The band gap obtained was to be in the range of 1.4 to 1.6 eV.

Recycling of dredged sediment as a raw material for the manufacture of Portland cement – Numerical modeling of the hydration of synthesized cement using the CEMHYD3D code

Around 56 million m3 of sediments are dredged in France per year to maintain the access to ports and waterways. Sediments are considered as waste according regulations and cause environmental, ecological and economic issues. This paper aims to use dredged sediments as raw material to replace traditional materials in Portland cement production. Two cements were produced at the laboratory: a reference cement made from analytical grade reagents of CaCO3, SiO2, Al2O3 and Fe2O3 and a second cement made from sediment as a partial substitution for traditional materials. The components proportions in the raw meal were adjusted using the cementitious modulus values (LSF, SR and AR). The produced clinkers/cements were characterized by X-ray diffraction; X-ray fluorescence and scanning electron microscopy (SEM-EDS) in order to study their mineralogical and chemical composition as well as their microstructure. The reactivity of the cements was measured by isothermal calorimetry, and by the determination of the degree of hydration and the compressive strength. The CEMHYD3D code was used to numerically model the hydration of cement paste in order to follow the evolution of all phases and to predict the properties of hydrated cements.The results demonstrate that sediments can be used as a raw material in the cement production at a high rate (31 wt%) without affecting the phase assemblage and the hydration behavior.

Liquid chromatography-mass spectrometric methods for trace quantification of potential genotoxic impurities in ivacaftor and lumacaftor

The objective of the current study was to develop and validate the sensitive LC-MS methods for trace analysis of genotoxic impurities in Ivacaftor and Lumacaftor. The first method is for the trace analysis of 2,4-di-tert-butyl-5-nitrophenol in ivacaftor and the second method is for the trace analysis of 1-(2,2-difluoro-1,3-benzodioxol-5yl)-cyclopropane carboxylic acid and 3-carboxyphenyl boronic acid in lumacaftor.High pure analytical grade solvents and reagents were used for this study. The chromatographic separation was performed on Luna C18 (250×4.6mm, 5.0μm) at a column temperature of 25°C using eluent consisting of acetonitrile and 0.1% v/v formic acid in water in a gradient elution mode. The eluent was run at a flow of 1.0mL/min and injection volume of 20μL.The linearity, precision and accuracy of the developed methods was validated over the concentration range of 0.35-15.0ppm for 2,4-di-tert-butyl-5-nitrophenol, 0.30-15.0ppm for 1-(2,2-difluoro-1,3-benzodioxol-5yl)-cyclopropane carboxylic acid and 0.23-15.0ppm for 3-carboxyphenyl boronic acid. In both methods, interference was not observed at the retention time of analyte peaks. All the analytes were found to be stable in solution for a period of 48h.The proposed methods are reliable, sensitive, precise, accurate, and robust for the trace level quantification of genotoxic impurities in Ivacaftor and Lumacaftor. These methods can be successfully implemented in the quality control lab for routine analysis.

Application of approach for development of hptlc identification and quantification methods for determination of phenolic compounds and terpenoids of several Thymus L. species

The aim of this work was to improve the approaches for standardization of Thymus L. species by development of HPTLC identification of phenolic compounds (flavonoids and phenylpropanoids) and terpenoids (essential oils and triterpenoids) and quantitative determination of rosmarinic acid and flavonoids for six Thymus L. species of Ukraine flora, as well as determination of chromatographic profiles of Thymus L. species’ extracts obtained using different extraction methods.
 Materials and methods. Objects were: samples of dry herb of Th.serpyllum, Th.vulgaris, Th.Marschallianus, Th.Pallasianus, Th.calcareus, and Th.moldavicus of Ukraine origin collected in 2019-2021 years or acquired commercially on Ukraine market. Instruments: CAMAG HPTLC Herbal System, visionCats 2.5. The analytical grade reagents were used. Reference substances were purchased from Extrasynthese, Sigma Aldrich. Chromatography was performed on HPTLC plates Si 60 F254, Merck according to the developed methods.
 Results. A new approach for quality control of different Thymus L. species of Ukraine flora included the development of HPTLC methods for identification of main groups of bioactive substances of these species, such as flavonoids and phenylpropanoids, essential oils, triterpenoids; development of quantification method of rosmarinic acid and assay of total flavonoids, expressed as luteolin-7-O-glucoside. The characteristic HPTLC fingerprints of six Thymus L. species in three mobile phases of different polarities that cover a wide range of bioactive substances were established. The content of rosmarinic acid in different Thymus L. species samples was in the range of 0,11-0,72 %: Th.moldavicus – 0,11 %; Th.Marschallianus – 0,19-0,27 %; Th.serpyllum – 0,38 %; Th.vulgaris – 0,51 %; Th.calcareus – 0,56 %; T.Pallasianus – 0,72 %. The total flavonoids content, expressed as luteolin-7-O-glucoside, was in the range of 0,8-2,72 %: Th.moldavicus – 0,8 %; Th.serpyllum – 0,87 %; Th.vulgaris – 1,06 %; Th.Pallasianus – 1,28 %; Th.Marschallianus – 1,89 %; Th.calcareus – 2,72 %.
 Conclusions. The proposed scientific approach for quality evaluation of Thymus L. species using HPTLC allows to determine comprehensive information of chemical composition and content of active substances of multiple samples in parallel, in a cost and time-efficient manner

The relatively higher concentrations of trace elements to arsenic may have influenced on methylation process of inorg- As in humans

The relatively higher concentrations of trace elements to arsenic may have influenced on methylation process of inorg- As in humans

Effect of thiourea on structure, morphology and optical properties of spray deposited CZTS thin films for solar cell applications

<p>Cu2ZnSnS4 (CZTS) films of different Thiorea (SC (NH2)2) molarity were deposited by using simple chemical spray technique at substrate temperature 275°C. Analytical reagent Grade Copper chloride (CuCl2), Zinc chloride (ZnCl2), Tin chloride (SnCl4.5H2O) were used as Cu+ , Zn+ , and Sn+ ion sources respectively and thiourea (SC(NH2)2) (0.02, 0.04 0.06 0.08, and 0.1 M) was used as a Sion source. A set of five CZTS films was deposited using five different molarity of thiourea. The structure, Morphology, Elemental analysis and optical properties of these films were studied using X-ray diffratometer (XRD), Scanning Electron Microscopy (SEM) Energy Dispersive X-ray Analysis (EDX) and UV-Visible spectroscopy techniques respectively. The XRD spectra showed that all films are polycrystalline tetragonal structure with preferential orientation along (112) plane. The calculated crystallite size was increased with increase in thiourea concentration. Variations of optical band gap with thiourea molarity have been investigated using Tauc plots. SEM micrographs exhibits CZTS spherical granules regularly arranged with some void spaces. Purity of deposited films was investigated using EDX analysis. All the CZTS films exhibits higher absorption coefficient (𝛼 > 104) cm-1 and band gap in the reported range (1.2-1.53 eV) can be used as an absorber layer in solar cells.</p>

A dual responsive probe based on bromo substituted salicylhydrazone moiety for the colorimetric detection of Cd2+ ions and fluorometric detection of F‒ ions: Applications in live cell imaging

A dual responsive probe based on bromo substituted salicylhydrazone moiety for the colorimetric detection of Cd2+ ions and fluorometric detection of F‒ ions: Applications in live cell imaging

Role of cerium as a promoter and process optimization studies for dehydration of glycerol to acetol over copper chromite catalyst

Cerium-promoted silica supported copper chromite catalyst was synthesized from acid hydrolysis of sodium silicate by sol–gel method. The catalyst was characterized by Brunauer–Emmett–Teller (BET) method, field-emission scanning electron microscopy (FESEM), X-ray diffraction (XRD), H2-temperature programmed reduction (H2-TPR), NH3-temperature programmed desorption (NH3-TPD) and pyridine adsorbed Fourier transform infrared spectroscopy (Py-FTIR). Among cerium doped catalysts, 5 wt% of Ce promoted copper chromite supported by 40 wt% of silica (SiCuCr40–Ce5) shows the largest BET surface area. XRD analysis of the reduced form of the catalyst shows both CeO2/Ce2O3 redox system and CuO/Cu2O/Cu redox system. Py-FTIR shows the maximum number of Lewis acid sites for SiCuCr40–Ce5 than others. The highest acetol selectivity with analytical reagent (AR) grade glycerol conversion is observed for SiCuCr40–Ce5 at 200 °C for 3 h in a batch reactor at atmospheric pressure. Cerium promotion lowers the reaction temperature with enhanced glycerol conversion and increased acetol selectivity. Though the above catalyst shows higher conversion for laboratory reagent (LR) grade glycerol but it reduces acetol selectivity. The addition of glucose into the LR grade glycerol further reduces glycerol conversion and decreases the acetol selectivity to zero. This may be due to the presence of iron as impurity in LR grade glycerol. XRD analysis of spent catalyst shows the absence of redox catalytic system and the pore volume reduces identified by BET analysis. Raman analysis of the spent catalyst shows graphite-like carbon deposition in the spent catalyst.

Studies of molar refraction and polarizability constant of 6-(4-chlorophenyl)-1,2,3,4-tetrahydro-2, 4-dioxopyrimidine-5-carbonitrile in 60% DMSO in the temperature range 298 to 313 K

Objectives: The main purpose of this study is to investigate the impact of 6-(4-chlorophenyl)-1, 2, 3, 4-tetrahydro-2, 4-dioxopyrimidine-5-carbonitrile in binary solution at different concentrations and valuable information on electronic polarizability and molecular interactions in the solution. Methods: 6-(4-chlorophenyl)-1, 2, 3, 4-tetrahydro-2, 4-dioxopyrimidine-5-carbonitrile was synthesized and purified by recrystallization technique in laboratory(1). DMSO used is of analytical reagent grade (AR) of minimum assay of 99.9%. Stock solutions of 0.02 (mol L-1) of compound were prepared by dissolving calculated amounts in 60% dimethyl sulphoxide solution. Solutions in various concentration ranges from 0.002 to 0.010(mol L-1). The pycknometer was calibrated by measuring the densities of triple distilled water. The densities of distilled organic liquids like acetone, toluene and carbon tetrachloride were evaluated with respect to density of water. Refractive index were measured by Abbe’s Refractometer (AR-56, COSLAB) having range 1.3000 to 1.7100. The desired temperature was maintained by circulating water through refractometer. Findings: In the present work we found that density, refractive index, molar refraction and polarizability constant increases the increase in concentration due to decrease in angle of refraction or increase in angle of incidence. The decrease in density with increase in temperature is due to increase in molar volume of solvent. However, the decrease in refractive index is due to the fact that the solute-solute and solute-solvent interactions weaken with increase in temperature. This can be correlated that change in these properties changes the intermolecular attraction between solute and solvent. With increase in temperature the interaction between solute and solvent weakens and hence molar refraction and polarizability decreases. Novelty: The work incorporated with the study of molar refraction and molar polarizability of 6-(4-chlorophenyl)-1, 2, 3, 4-tetrahydro-2, 4-dioxopyrimidine-5-carbonitrilehas been not studied until now. So we wish to present the systematic measurement of refractive index of 6-(4-chlorophenyl)-1, 2, 3, 4-tetrahydro-2, 4-dioxopyrimidine-5-carbonitrile in 60% DMSO in the temperature range 298 to 313 K at different concentration. From refractive index we have calculated molar refraction and molar polarizability which has provided important information regarding interactions between solute and solvent. Keywords: 6-(4-chlorophenyl)-1; 2; 3; 4-tetrahydro-2; 4-dioxopyrimidine-5-carbonitrile; refractive index; molar refraction; molar polarizability

Adsorption of Orange II Onto Zn2Al–Layered Double Hydroxide Prepared From Zinc Ash

The dye industry is one of the largest water consuming industries, and at the same time generates large quantities of wastewaters. The resulting wastewaters require proper treatment before discharge, because the dye contents have a negative effect on the water body and organisms present in it. The most efficient treatment method for water containing dyes is represented by adsorption processes. The challenge with these adsorption processes is to develop new, efficient, viable, and economic adsorbent materials. Therefore, in the present paper, the performance of Zn2Al-layered double hydroxide, prepared from an industrial waste (zinc ash) as a zinc source, was investigated in the Orange II dye adsorption process. The Zn2Al-layered double hydroxide prepared from secondary sources presents similar morphological and structural characteristics as those prepared from analytical grade reagents. The influence of initial dye concentration, adsorption time, solid:liquid ratio, pH, and temperature was evaluated in order to confirm the benefit of this waste valorization. A comparison with the reference Zn2Al-layered double hydroxide prepared from analytical grade reagents was performed and the results show that due to the small presence of impurities, the material prepared from zinc ash shows better adsorption capacities (qmax,exp = 42.5 mg/g at 293 K) than the material prepared from reagents (qmax,exp = 36.9 mg/g at 293 K), justifying the utilization of secondary sources for layered double hydroxides preparation. The proposed treatment process presents advantages from both economic and environmental protection point of view.

New approach to removal of hazardous Bypass Cement Dust (BCD) from the environment: 20Na2O-20BaCl2-(60-x)B2O3-(x)BCD glass system and Optical, mechanical, structural and nuclear radiation shielding competences

In the present work, aiming to collaborate in the removal of Bypass Cement Dust (BCD) from the environment, we studied a system consisting of three glasses prepared from analytical reagent grade chemicals with the following composition: 20Na2O-20BaCl2-(60-x)B2O3-xBCD, where (x = 0, 10, and 20 %). BCD is an important contributor of many respiratory human health issues. In this work we investigate their optical, physical and gamma-ray shielding properties. The experimental results of mass attenuation coefficients are contrasted with the FLUKA Monte Carlo code and the XCOM database at 0.081, 0.356, 0.662, 1.173, and 1.332 MeV photon energies. Additionally, the mechanical, structural, and optical properties of these glasses were measured. A rising peak with an increase of BCD concentration in the region from 450 cm-1 to 480 cm-1 was observed. The results show that shielding properties such as the mass attenuation coefficient (μm), the effective atomic number (Zeff), and the effective electron density (Nel) increase as BCD fraction increases. The half value layer (HVL), the tenth value layer (TVL), and the mean free path (MFP) decrease as the BCD content increases. It is noticed that 20Na2O-20BaCl2-(60-x)B2O3-xBCD, where (x = 0, 10, and 20 %), has the highest optical conductivity value at x = 20%. It was found that the gradual addition of BCD content increases the hardness of the studied glasses.

A REPORT ABOUT BENZOXAZINONE MATERIAL

In this study, the objective was to investigate the Benzoxazinone material using the uncorrected and open capillary method for conducting and reporting the melting points. Laboratory grade and analytical grade reagents were used for conducting the synthesis and analytical studies based on with or without modification appropriately as and were required. Results showed that First of all the Synthesis of 2H-1, 4- benzoxazin-3(4H)-one was carried out by reacting 2- amino phenol with chloro acetyl chloride in dichloromethane in presence of triethylamine and then the bromo substitution was done by reacting with dibromoethane. Piperazine substituents were prepared in laboratory and then the title compounds were synthesized. One additional benzoyl substitution was also done. The entire synthesized compounds were primarily characterized by running T.L.C. and melting point analysis.

Structure, morphology and optical parameters of spray deposited CZTS thin films for solar cell applications

Objectives: To develop simple method for Cu2ZnSnS4 (CZTS) thin film deposition suitable for solar cell device application. Method: Cu2ZnSnS4 (CZTS) thin film was deposited by using simple chemical spray pyrolysis technique for substrate temperature (270±5) ◦C. Analytical reagent Grade 0.025 M Copper chloride (CuCl2), 0.0125 M zinc chloride (ZnCl2), 0.0125 M Tin chloride (SnCl4.5H2O) and 0.05 M Thiourea (SC (NH2)2) were used as sources of copper (cu+ ), zinc (Zn+), tin (Sn+ ) and sulfur (S- ) ions respectively. The structure, morphology and optical band gap of the film were investigated by using X-ray Diffractometer (XRD), Scanning Electron Micrograph (SEM) and UV-Visible spectroscopy respectively. Energy dispersive X-ray Analysis (EDX) was used for elemental analysis of deposited CZTS film. Findings: The XRD spectra showed that CZTS film exhibit polycrystalline tetragonal crystal structure with preferential orientation along (112) plane. The crystallite size calculated using full width at half maximum (FWHM) of (112) peak was to be 36.82 nm. SEM image revealed that film composed of regular arrangement of spherical granules of average size 1.61 µm. The purity of the CZTS phase was confirmed by elemental analysis. The calculated energy band gap (Eg) by using Tauc\'s plot was about 1.62 eV. The dc resistvity estimated by using IV characteristics of the CZTS film was to be 2.3× 10-2 Ω-cm. It is concluded that CZTS film prepared using present deposition technique can be used for solar cell device applications. Keywords: Chemical spray technique; CZTS Thin Films; band gap; structure of CZTS; electrical resistivity; elemental analysis