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  • Author or Editor: Y. Sayi x
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Abstract  

Detailed investigations have been carried out on the well-known method of spectrophotometric determination of boron particularly in uranium compounds as boron-curcumin complex after extraction into 2-ethyl hexane 1,3-diol (EHD) to understand a number of parameters, which have not been addressed earlier in the literature. These include (i) effect of different acid media on analytical results of boron which are employed for dissolution of nuclear fuel samples, (ii) effect of diluents namely ethyl alcohol and N,N-dimethyl formamide on sensitivity of method which are employed for final dilution, and (iii) studies on loss of boron, if any, during conversion of uranium compounds to U3O8. Based on the present studies, the existing procedure has been suitably modified to improve the sensitivity in the measurements. In addition, this paper also describes about interference studies with Al, Cr, Mg, Ca, Fe, Mn, Mo, F and W and amount of EHD on modified method. Absolute detection limit was found to be 10 ng. The precision and accuracy of the method, is 3% at level 100 ng·g−1 of boron.

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Abstract  

Boron concentration has been determined in groundwater samples, collected from Khuchch, Gujarat, India, by prompt gamma neutron activation analysis (PGNAA) after selective separation and pre-concentration by solvent extraction with 10% 2-ethyl hexane 1,3-diol in CHCl3. Solvent extraction separation helped to eliminate the interfering elements in PGNAA determination of boron. The sensitivity of PGNAA is found to be 18.83 cps/mg B based on the slope of a calibration plot obtained by carrying out measurements on synthetic boric acid samples containing boron in the range of 30–150 μg. Detection limit of the method is 0.2 μg/g counted for 35,000 seconds at a sample size of 15 gram. The precision (relative standard deviation at 1σ level) and accuracy of the method is 5%. The analytical results of the present method agreed well with well-established spectrophotometric determination of boron as boron-curcumin complex and inductively coupled plasma atomic emission spectroscopy (ICP-AES).

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Abstract  

A simple and rapid method has been developed for the separation and purification of plutonium from solid analytical waste (containing uranium, plutonium, nickel and graphite) generated during the analysis of the nuclear fuels for their oxygen and nitrogen contents by inert gas fusion technique. The method is based on crushing the graphite crucibles, electromagnetic separation of plutonium-nickel alloy, dissolution in nitric acid and ion exchange purification of plutonium. Recovery of plutonium is better than 98%. The method may be extendable for the recovery of any other valuable materials from such analytical waste.

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Abstract  

A hot vacuum extraction technique for the determination of hydrogen in metal and alloy samples has been standardised. After measuring the total pressure of the evolved gases, individual hydrogen and deuterium intensities are measured using an on-line quadrupole mass spectrometer. Synthetic mixtures of H2 and D2, in known concentrations, have been analysed by QMS and an analytical expression correlating the measured [D2]/[HD] intensity ratio with the mole fraction of deuterium in the synthetic mixture has been arrived at. The precision and accuracy in the measurement of hydrogen is about 10% at 50 ppmw level.

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