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- Author or Editor: M. Mahajan x
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Abstract
A method based on the back-extraction of Th(IV) from its TTA complex in benzene by aqueous F– followed by spectrophotometric measurement of Th(IV), for the determination of fluoride has been developed. The coefficients of variation obtained are 2.4% and 1.4% in 11 determinations at F– concentration levels of 1.0 
g ml–1, respectively.
Abstract
An improved method for the determination of plutonium in an aliquot using cerium/IV/ as an oxidant is reported. Plutonium is oxidized quantitatively to plutonium/VI/ in nitric acid medium by cerium/IV/, the excess of which is chemically destroyed in a single step by hydrochloric acid. Plutonium/VI/ is then reduced to plutonium/IV/ with a known amount of Fe/II/, the excess of which is back titrated potentiometrically with standard dichromate. Results of analysis of 3–5 mg amounts of plutonium in aliquots containing standard plutonium nitrate solution are reliable within 0.2%. Effect of the presence of some relevant foreign ions has been studied. The application of the method for the analysis of mixtures containing various amounts of uranium and plutonium has been examined.
Abstract
Determination of fluoride at trace level is important for the specification analysis of nuclear fuel samples. This is generally accomplished by pyrohydrolytic separation followed by ion selective electrode potentiometry. In the present work, a method has been developed for the determination of fluoride by radiometric assay of181Hf back-extracted from thenoyltrifluoracetone (HTTA) in benzene.181Hf back-extracted is proportional to the concentration of fluoride.
Abstract
Stability constants of the fluoride complexes of Pu(III), Sm(III) and Bi(III) in 1.0M NaClO4/HClO4 medium at 23±1°C have been determined by potentiometry using a fluoride ion-selective electrode. Plutonium was reduced to the trivalent state using quinhydrone with an excess to serve as holding reductant. The log values of concentration stability constants log 
1, log
2, and log
3 are 3.58, 6.40 and 12.61 for Pu(III), 3.23, 5.81 and 10.54 for Sm(III) and 3.69, 6.13 and 11.04 for Bi(III), respectively. The log
2 values in all these cases have very large deviation and may be taken only as rough estimates.
Abstract
A rapid method for simultaneous determination of fluorine and chlorine in radioactive liquid wastes with ion chromatography after pyrohydrolysis separation was proposed for routine analysis. The elements were separated from radioactive liquid wastes by pyrohydrolysis and were subsequently determined with ion chromatograpy. Total time taken to determine these elements is about 45 min including 30 min for the pyrohydrolysis and 15 min for ion chromatography. The results of recovery tests ranged 95% or above. The limits of detection for F and Cl are 0.5 and 0.8 mg kg−1, respectively.
Abstract
A quartz pyrohydrolysis apparatus designed for the safe handling of pyrophoric carbide nuclear fuel samples while separating C1 and F trace impurities for quality control analysis is described. It has several advantages over the commonly used pyrohydrolysis apparatus. Performance of the apparatus during routine analysis of a large number of nuclear fuel samples has been found to be quite satisfactory.
Abstract
The liquid-liquid extraction behavior of plutonium(IV) from aqueous nitric acid media into n-dodecane by di(2-ethylhexyl)sulfoxide (DEHSO) was investigated over a wide range of conditions. Optimum-parameters such as the aqueous phase acidity, reagent and metal concentrations, etc., were established for efficient extraction-separation of tracer as well as macro levels of plutonium. It was found that the extraction increased with increasing nitric acid concentration up to 6M HNO3 and then decreased. Extraction also increased with increasing extractant concentration. After loading of the organic phase with 2 to 50 mg/ml of U(VI), extractability of Pu(IV) became considerably lower. Recovery of Pu(IV) from the organic phase was accomplished using dilute uranium(IV) nitrate as the strippant.
