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  • Author or Editor: H. Jain x
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Abstract  

Half-life of241Pu is of great importance in nuclear technology. In view of large variation in the values (13–15 y) reported till 1974 in literature, efforts have been made in different laboratories to determine this half-life with high precision and accuracy. In our laboratory, it has been determined by different methods which may be classified in two categories, viz. (1) parent decay method, and (2) daughter growth method. In the parent decay method, change in isotope ratios241Pu/239Pu,241Pu/240Pu and241Pu/242Pu was studied periodically by a thermal ionization mass spectrometer. Single as well as double ratio method was used to calculate the half-life. In the daughter growth method, the half-life was obtained in four independent ways. These were (1) alpha spectrometry taking239Pu and242Pu separately as reference isotopes and studying periodically the increase in alpha activity ratio, (2) alpha proportional counting for observing periodically the change in total alpha activity, (3) isotope dilution alpha spectrometry using243Am as a spike, (4) isotope dilution mass spectrometry using243Am as a spike. In all these methods, synthetic mixtures were prepared for achieving high precision and accuracy in different measurements. Based on the results obtained in this laboratory and the values reported by other laboratories, a half-life value of 14.4±0.1 y is recommended. The paper reviews the past history, puts forth the present status, highlights the current trends for studying the effect of chemical composition of plutonium on the half-life of241Pu and presents the future requirements for achieving higher accuracy in the half-life of241Pu.

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Abstract  

Relative activity method offers the potentiality of providing half-life values over a wide range in a short time for different -emitting transactinium isotopes. The method involves the preparation of a synthetic mixture using another isotope of the same element followed by the determination of atom ratio and -activity ratio by thermal ionization mass spectrometry and -spectrometry, respectively. A double dilution technique is described which helps in maintaining the atom ratios as well as -activity ratios close to unity so that these could be determined with high precision and accuracy. Results obtained on the half-lives of232U,238Pu,242Pu and243Am using double dilution technique in relative activity method are summarized. Requirements, advantages and applications of this technique for determining the half-lives of other transactinium isotopes are presented.

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Abstract  

A method based on the geometric progression decrease of the counts in the far tail of the alpha spectrum is described for the simultaneous determination of plutonium, americium and curium by alpha spectrometry. For evaluating the precision and accuracy, synthetic mixtures were prepared from solutions of enriched isotopes and sources were prepared by direct evaporation method using tetraethylene glycol /TEG/ as a spreading agent and electropolished stainless steel discs as the backing material. Precision and accuracy of about 1% is demonstrated in the determination of244Cm/239Pu,241Am/239Pu,244Cm/233U,241Am/233U and239Pu/233U alpha activity ratios using a 450 mm2 silicon surface barrier detector.

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Abstract  

Determination of actinides in the environmental and bioassay samples is important in view of the following factors: increasing energy production by nuclear reactors; environmental contamination due to fallout from nuclear weapons testing and burn up of nuclear-powered satellites; the growing emphasis on the desirability of a cleaner environment; and public concern over the potential hazards associated with nuclear reactors. Among the various actinides, plutonium is one of the most important due to the large amounts produced in the nuclear fuel cycle. Further, the extremely low levels of plutonium in the different biological and environmental samples demand the development of precise, accurate, and sensitive methods to arrive at meaningful conclusions from the results obtained in various studies. In addition to various other techniques available, alpha spectrometry is commonly used.

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Abstract  

Extraction of plutonium from analytical waste solutions containing phosphoric acid using a solution of monooctylphenylphosphoric acid (MOPPA) is described. Effect of reagent concentration, presence of uranium, plutonium loading and back extraction of plutonium from the organic phase are described. Using a solution of 0.05 F MOPPA in xylene, more than 90% plutonium could be extracted in one cycle.

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Abstract  

Experimental evaluation on the use of239Pu spike in Isotope Dilution-Thermal Ionization Mass Spectrometry (ID-TIMS),238Pu spike in Isotope Dilution Alpha Spectrometry (IDAS) and233U as a Non-Isotopic Diluent in Alpha Spectrometry (N-IDAS), for determing plutonium concentration in samples with burn-up values in the range of 1,000–10,000 MWD/TU is done. Precision is determined by analyzing replicate aliquots from different samples using each of the three spikes. Accuracy is established by comparing the results with those obtained by using well recognized spike242Pu in ID-TIMS. It is shown that the use of239Pu spike with the latest generation thermal ionization mass spectrometers gives the best precision (0.2%), whereas the precision values of 0.5 and 1% can be obtained by using238Pu and233U spikes, respectively, on a routine basis. Reasons for the difference in the precision values are discussed, along with the merits and drawbacks on the use of different spike isotopes.

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Abstract  

An experimental evaluation of the recently available passivated ion-implanted detectors, which appear promising for high resolution -spectrometry, is presented in terms of % tail contribution per unit -activity ratio, peak to valley ratio, and resolution /FWHM/. The two IPE detectors with areas of 20 mm2 and 450 mm2 were used for comparing these parameters. It is seen that the smaller area detector provides a better resolution for single nuclide sources, but there is no significant difference for sources containing nuclides with close lying -energies, e.g.,239Pu,240Pu. Further, the large area detector gives less tail contribution and should be preferred to minimize the error in -activity ratio determinations. However, the small area detector offers a possibility of qualitative or semiquantitative determination of nuclides with close lying -energies.

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Abstract  

Investigations have been carried out for the electrodeposition of milligram amounts of uranium on electropolished stainless steel disks with an objective of preparing good quality sources for -spectrometric studies on uranium. The parameters studied include the variation of electrodeposition yield as a function of voltage, time, distance between the cathode and anode, and the volume of 0.2M ammonium oxalate solution. The conditions selected for preparing good quality sources with nearly 100% yield were: electrodeposition voltage 25 V, time of deposition 15 min, volume of 0.2M ammonium oxalate solution in the cell 4 ml and a distance of 2 cm between the cathode and anode. The sources prepared using this method have been used successfully for the -spectrometric determination of234U/238U ratios in uranium samples.

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Abstract  

A biamperometric method for the determination of sulfate has been developed. Its application to the determination of sulfate content in rubidium uranium trisulfate is discussed. Sulfate is determined by titration with lead nitrate in aqueous ethanolic medium using ferrocyanide-ferricyanide redox system as biamperometric indicator. Initially, the method has been tested for standard. K2SO4 solutions. In case of Rb2 U(SO4)3, since uranium interferes, it is precipitated as ammonium diuranate and excess ammonia is removed prior to the titration. Precision of better than 0.3% was achieved with no significant bias.

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Abstract  

A method for the sequential determination of thorium and uranium has been developed. In the sample solution containing thorium and uranium, thorium is first determined by complexometric titration with ethylenediaminetetraacetic acid (EDTA) and then in the same solution uranium is determined by redox titration employing potentiometry. As EDTA interferes in uranium determination giving positive bias, it is destroyed by fuming with HClO4 prior to the determination of uranium. A precision and accuracy of better than ±0.15% is obtained for thorium at 10mg level and uranium ranging from 5 mg to 20 mg in the aliquot.

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