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  • Author or Editor: S. K. Sharma x
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Abstract  

Effect of various doses of gamma radiation on the ion-exchange capacity, distribution coefficient values, elution behaviour, pH titration and infrared spectra of some thermally stable inorganic ion exchangers has been studied systematically. No change has been observed in the ion-exchange capacity, elution behaviour and the infrared spectra of the materials irradiated up to a total dose of 3·108 rad, while, a change has been observed in their pH-titration and distribution behaviour.

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Abstract

A number of silicon-based inorganic ion exchangers were synthesized under different conditions of preparation. The original and regenerated ion exchange capacities (IECs) were determined. Thermal stability of these materials was investigated in the temperature range of 40–800 °C. The gain/loss of IEC was studied as a function of temperature. These exchangers show a higher IEC and its retention to a considerable extent at elevated temperatures when compared to that of corresponding ion exchangers which do not contain silica. The thermogravimetric curve shows greater percent mass loss in H+ form of the exchanger than in K+ form. Dehydration studies seem to throw some light on the state of water molecules present in various samples. The empirical formula and the tentative structure for stannic arseno silicate have also been proposed.

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Abstract  

The dissolution of UO2 in carbonate-bicarbonate solutions containing sodium hypochlorite as an oxidant has been investigated. The effect of temperature, sodium hypochlorite concentration and stirring speed was examined. In the temperature range of 303 to 318 K, the leaching reaction displayed linear kinetics. Apparent activation energy obtained from the differential approach was found to be 57 kJ mol–1. This relatively high activation energy value indicates a chemically controlled behavior of UO2 dissolution. The order of reaction with respect to sodium hypochlorite concentration was found to be unity.

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Abstract

The phase diagram of 1,4-dibromobenzene (DBB) with pyrogallol (PG) shows the formation of a monotectic and a eutectic alloys at 0.12 and 0.99 mol fractions of DBB, respectively. The phase equilibrium shows the large miscibility gap region with the upper consolute temperature 159.0 °C at 0.55 mol fraction of DBB. Growth kinetics of pure compounds and their monotectic and eutectic at different undercooling (ΔT) obey Hillig–Turnbull's equation: v = uT)n. Thermodynamic parameters such as enthalpy of mixing, entropy of fusion, interfacial energy, roughness parameters and excess thermodynamic functions were computed based on enthalpy of fusion values obtained from DSC studies. The Cahn wetting condition is applicable for monotectic alloy. The optical microphotographs of binary alloys show lamellar and dendritic features.

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Abstract  

Extraction behavior of U(VI) and Th(IV) from nitric acid medium is investigated using organo-phosphorous extractant, tri(butoxyethyl) phosphate in n-paraffin at room temperature (27 ± 1 °C). The effect of diluents, nitric acid concentration as well as extractant concentration on extraction of U(VI) and Th(IV) are evaluated. Extraction of U(VI) and Th(IV) from nitric acid medium proceeds via solvation mechanism. Slope analysis technique showed the formation of neutral complexes of the type of UO2(NO3)2·2TBEP and Th(NO3)4·3TBEP with U(VI) and Th(IV) respectively in the organic phase. The FTIR data showed shifting of P=O stretching frequency from 1,282 to 1,217 cm−1 indicating the strong complexation of P=O group with UO2 2+ ions in the organic phase. Effect of stripping agents, other metal ions and their separation with respect to U(VI) extraction has also been investigated.

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Abstract  

Solvent extraction of U(VI) with di-isodecyl phosphoric acid (DIDPA)/dodecane from nitric acid medium has been investigated for a wide range of experimental conditions. Effect of various parameters including nitric acid concentration, DIDPA concentration, temperature, stripping agents, and other impurities like rear earths, transition metal ion, boron, aluminum ion on U(VI) extraction has been studied. The species extracted in the organic phase is found to be UO2(NO3)(HA2)·H2A2 at lower acidity (<3.0 M HNO3). Increase in temperature lead to the decrease in extraction with the enthalpy change by ∆H = −16.27 kJ/mol. Enhancement in extraction of U(VI) from nitric acid medium was observed with the mixture of DIDPA and tri butyl phosphate (TBP). The stripping of U(VI) from organic phase (DIDPA–U(VI)/dodecane) with various reagents followed the order: 4 M H2SO4 > 5% (NH4)2CO3 > 8 M HCl > 8 M HNO3 > Water. High separation factors between U(VI) and impurities suggested that the use of DIDPA for purification of uranium from multi elements bearing solution.

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Abstract  

Radiotracers are extensively used in many industries for trouble shooting and optimization of process parameters leading to considerable savings in time and huge economic benefits. In chemical and petrochemical industries different gases and vapours flowing in the conversion reactors play a major role in the final production. Gaseous radiotracers are ideal to study hydrodynamics of gas phases in process vessels. 41Ar and 79Kr are the preferred gaseous radiotracers for such studies. Owing to the increase in demand from Indian industries for gas phase radiotracers, efforts have been made to produce 41Ar and 79Kr indigenously by irradiation of 40Ar and enriched 78Kr gaseous targets in research reactors. Prequalification of the containers used, safety aspects concerning accidental rupture and mandatory tests necessary for irradiation of gaseous targets in the reactors have been studied. The paper describes some of the important safety aspects involved and the results of trial irradiations on the production of 41Ar and 79Kr radiotracers. Standardization of suitable assay protocols for their regular production and supply for applications in industries is also described.

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Abstract  

Knowledge of the dynamics of HTO in leafy plant–soil system is required to verify models, such as the NORMTRI code, which predict environmental tritium following its release. Tritium concentrations in plants has been evaluated using the code NORMTRI and experimentally by collection of samples of different plants and their soils samples. In the present study, major seasonal crop plants i.e. wheat, mustard, sugar cane, coriander, spinach, potato, were collected beyond Narora Atomic Power Station site boundary and gular, arandi, neem, ashok, amaltas, csuarina leaf samples within NAPS site boundary for analysis of HTO content. Data analysis indicated that HTO in leaf is strongly influenced by atmospheric relative humidity and type of the plant.

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Summary

A simple, rapid, and specific thin layer chromatographic (TLC) method has been developed and validated for the simultaneous estimation of icariin and l-arginine from commercial polyherbal formulations for sexual dysfunction. The separation of the methanol extract of these formulations was achieved on silica gel 60 F254 aluminum backed TLC plates by using ethyl acetate-acetone-glacial acetic acid-formic acid-water 12:2:1:2:2 (υ/υ) as mobile phase. Densitometric analysis of icariin and l-arginine was monitored in absorbance mode at 270 and 195 nm, respectively. The linear regression analysis data for the calibration plots for icariin and l-arginine showed good linear relationship with r 2 = 0.9984 +- 0.01 and 0.9968 +- 0.02, in the concentration ranges of 250–750 and 500–1500 ng/spot, respectively. The method was validated for precision, robustness, and recovery. The average percentage recovery was found to be 98.26% for icariin and 99.63% for l-arginine. The limits of detection and quantitation were 72, 116 and 238, 383 ng/spot, respectively, for icariin and l-arginine. Statistical analysis proves that the method is repeatable and selective for the estimation of the targeted drugs. Since the proposed mobile phase effectively resolves the icariin and l-arginine, this method can be applied for the identification and quantitation of these components in herbal extracts and marketed formulations.

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Summary

In this paper we describe a sensitive and reproducible reversed-phase high-performance liquid chromatography (HPLC) method with photodiode-array detection for isolation and quantification of the bioactive hydrophilic constituent 7-(1-O-β-d-galacturonide-4′-(1-O-β-d-glucopyranosyl)-3′,4′,5,7-tetrahydroxyflavone, 1, from the seeds of Cuminum cyminum. Compound 1 was separated isocratically on a C18 preparative column, in high purity, after removal of solvents. The purity and identity of the compound were established by use of LC-mass spectrometry and by spectroscopic techniques (1H and 13C NMR). The purity of 1 was also confirmed by HPTLC.

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