A simple spectrophotometric method has been developed for the determination of phosphate dissolved in soil and water. The method is based on the formation of phosphomolybdate with added ammonium molybdate followed by reduction with hydrazine in acidic medium. Orthophosphate and molybdate ions condense in acidic solution to give molybdophosphoric (phosphomolybdic) acid, which upon selective reduction (perhaps with hydrazinium sulphate) produces a blue colour, due to molybdenum blue of uncertain composition. The intensity of blue colour is proportional to the amount of phosphate. If the acidity at the time of reduction is 0.5 M in sulphuric acid and hydrazinium sulphate is the reductant, the resulting blue complex exhibits maximum absorption at 830 nm. The system obeys Lambert-Beer's law at 830 nm in the concentration range of 0.5-5 μg/mL of phosphate with a relative standard deviation (RSD) of 0.1% and correlation coefficient of 0.99. Molar absorptivity was determined to be 2.9 × 10⁴ L mol⁻¹ cm⁻¹ at 830 nm. The method is also applicable for the determination of phosphate in nuclear reprocessing plants, medical science, clinical science, agriculture, metallurgy and environmental science.

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Tri-n-butyl phosphate (TBP) in diluent is generally used as a solvent for the extraction of fissile materials in the reprocessing of spent fuels by the PUREX process. The mutual solubility of TBP and water leads to the transfer of some finite amount of TBP into the aqueous phase. The distribution study of TBP between normal paraffin hydrocarbon (NPH) and nitric acid has been studied. Equilibrium curves have been generated for TBP in different concentrations of nitric acid and NPH. The distribution coefficient (K d ) is also calculated by measuring the concentration of associated TBP in the aqueous and organic phase. The effect of an inert diluent on the solubility of TBP in nitric acid is also studied. It has been found that the distribution coefficient value varies with the concentration of TBP, nitric acid, and NPH. Nitric acid partitioning between TBP and water has also been studied. The concentration of nitric acid in both phases was determined by the titration method. It has also been proven that the concentration of nitric acid varies during this equilibrium study due to 1:1 complex formation with TBP by hydrogen bonding. The equilibrium study of this TBP-NPH-nitric acid system will aid in finding out the amount of TBP in different concentrations of nitric acid in the presence of a diluent. This study will be useful in nuclear waste management generated by spent fuels of reprocessing origin.

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