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Abstract  

A differential spectrophotometric method has been developed for plutonium in hexavalent state using a double beam spectrophotometer. The absorbance measurements were made at 835 nm in 4M sulfuric acid using a 5 cm cell. In the method developed the absorbance of six Pu(VI) standards, taken in the sample cell, were recorded against a molybdenum blue solution of appropriate intensity in the reference cell. A least-squares fit of data on absorbance and concentration of plutonium standards gave slope F and intercept Co which were used to determine the unknown concentrations using the relationship, C=C0+F·Ar where Ar is the absorbance of a plutonium solution of unknown concentration C mg/g. Various parameters like choice of acid and acidity, slit width, oxidant etc. were studied and the conditions optimized. Plutonium in the concentration range of 0.1–0.3 mg/g could be determined with a precision of ±0.5%. Uranium does not interfere. The method is useful for the analysis of a large number of samples on a routine basis.

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Abstract  

A differential spectrophotometric method has been developed for uranium in presence of plutonium by making absorbance measurements at 420 nm in 4M H2SO4 using 5 cm cells. The absorbance measurements are made with two independent sets of standards: (1) having uranium only and (2) having uranium and plutonium in a fixed ratio R, against a uranium solution of high absorbance (1A) in the reference beam. A least-squares fit of data on absorbance and uranium concentration in the two cases gave two slopes m1 and m2, which were used to determine the concentration of uranium using the relationship CU=C0+m1·[AT-(1/m2–1/m1) R·CPu] where AT is the relative absorbance of uranium and plutonium at 420 nm and C0 is the intercept corresponding to slope m1 for pure uranium standards and m2 is the slope for mixed uranium and plutonium standards. A knowledge of CPu, the plutonium concentration, is essential and is obtained by differential spectrophotometric measurements at 835 nm by oxidizing plutonium to its hexavalent state. In the same aliquot, plutonium could be determined with a precision of better than ±0.5% and uranium with a precision of better than ±1.0%.

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Abstract  

A reverse isotope dilution alpha spectrometric /R-IDAS/ method using239Pu as a spike is described for the determination of plutonium concentration in high burn-up fuel samples wth238Pu/(239Pu+240Pu) alpha activity ratio >0.5, without resorting to any purification from241Am and a bulk of other impurities. It involves the addition of a pre-clibrated spike solution to a known aliquot of the plutonium sample solution followed by source preparation using TEG as a spreading agent. The results obtained on a number of plutonium samples containing 20–80% of241Am /alpha activity wise/ using this method are compared with those achieved by R-IDAS using purification with TTA, with respect to precision and accuracy. Precision and accuracy of 0.5% are demonstrated. This method eliminates the need of any separation and purification of plutonium from241Am and a bulk of other impurities like uranium.

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Abstract  

A method is described for the determination of plutonium concentration in the presence of a bulk of other impurities by isotope dilution mass spectrometry /IDMS/ using239Pu as a spike. The method involves the addition of239Pu spike / 90 atom%/ to samples with239Pu / 70 atom%/ and vice versa. After ensuring chemical exchange between the sample and the spike isotopes, plutonium is purified by conventional anion exchange procedure in 7M HNO3 medium.239Pu/240Pu atom ratio in the purified spiked sample is determined with high precision /better than 0.1%/ using a thermal ionization mass spectrometer. Concentration of plutonium in the sample is calculated from the changes in239Pu/240Pu atom ratio in the spiked mixture. Results obtained on different plutonium samples using239Pu as a spike are compared with those obtained by the use of242Pu spike. Precision and accuracy comparable to those achieved by using242Pu are demonstrated. The method provides an alternative in the event of non-availability of enriched242Pu or244Pu required in IDMS of plutonium and at the same time, offers certain advantages over the use of242Pu or244Pu spike.

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Abstract  

A direct evaporation method is described for the preparation of sources using stainless steel as the backing material and tetraethylene glycol (TEG) as a spreading agent in the presence of large amounts of uranium. It is shown that FWHM and tail contribution at the low energy peak due to energy degradation of the high energy peak can be optimized by heating the source under controlled conditions in a furnace at 500–600°C for about 15 min. An accuracy of 0.5–1% is demonstrated for the determination of238Pu/(239Pu+240Pu) alpha activity ratio in the U/Pu range of 10 to 1500 generally encountered in dissolver solution of irradiated fuel.

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Journal of Radioanalytical and Nuclear Chemistry
Authors: S. Aggarwal, A. Almaula, P. Khodade, A. Parab, R. Duggal, C. Singh, A. Rawat, G. Chourasiya, S. Chitambar, and H. Jain

Abstract  

K-factors (= certified isotope ratio/observed isotope ratio) are determined for the isotope abundance measurements of uranium and plutonium by thermal ionisation mass spectrometry. An mdf of 0.07% and 0.18% per mass unit differing by a factor of about 3, is obtained for uranium and plutonium, respectively, employing double rhenium filament assembly in the ion source and Faraday cup as the detector using the presently available isotopic reference materials of uranium and plutonium.

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