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Some studies on thallium oxalates — IV

Thermal decomposition of rubidiumbis-oxalato diaquo thallate(III) dihydrate

Journal of Thermal Analysis and Calorimetry
Authors: S. R. Sagi, Karri V. Ramana, and M. S. Prasada Rao

Thallium(III) was precipitated with oxalic acid in the presence of 0.025M RbNO3 (or 0.0125M Rb2SO4) in 0.1M HNO3 (or 0.05M H2SO4). Chemical analysis of the solid obtained corresponds to the formula Rb[TlIII(C2O4)2]·4 H2O. Thermal studies (TG, DTG and DTA) indicated the dehydration and redox decomposition of the thallic salt to the thallous salt, and finally to a mixture of rubidium carbonate and oxides of thallium(I) and thallium(III). Infrared absorption spectra, microscopic observations and X-ray diffraction data were used to characterize the original salt, as well as the intermediates formed during the thermal decomposition of the salt. On the basis of these results, the salt may be represented as: Rb[TlIII(C2O4)2(H2O)2]·2 H2O.

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A new chelating solid extractant prepared by the chemical immobilization of xanthate on silica gel was characterized by Fourier transform infra red spectrometry (FTIR), thermogravimetric analysis (TGA) and microanalysis and used for the preconcentration and separation of uranyl ion prior to its determination by Arsenazo-III. The effect of pH, weight of the solid extractant, volume of the aqueous phase and the interference of neutral electrolytes, cations and anions on the determination of uranium, have been studied in detail to optimize the conditions for trace determination of uranium(VI). The accuracy of the developed procedure was tested by analyzing marine sediment (MESS-3) and soil (IAEA-SOIL-7) reference materials. The results obtained on analysis of soil and sediment samples are comparable to standard ICP-MS values.

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Journal of Thermal Analysis and Calorimetry
Authors: B. S. Maruthiprasad, M. N. Sastri, S. Rajagopal, K. Seshan, K. R. Krishnamurthy, and T. S. R. Prasada Rao

Thermal analysis of alumina precursors prepared by two different PFHS (precipitation from homogeneous solution) methods and a conventional method is described. All three precursors exhibit distinct thermal behaviour patterns, marked by multiple phase transformations, to yieldγ-Al2O3 ultimately. Thermal analysis studies, coupled with XRD, IR and elemental analysis data, indicate that the precursors obtained by the PFHS methods are monophasic in nature, and hence yield relatively small, uniform microspheroidal alumina in comparison with the alumina obtained by the conventional method.

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