Separation of trace impurities of131I from99Mo obtained by extraction from fission products of uranium

The radioisotope⁹⁹Mo was separated from a mixture of²³⁵U fission products in the presence of Hg²⁺ by sorption on a chromatographic column filled with Al₂O₃ and elution with 1M NH₄OH. Trace impurities of¹³¹I in the molybdenum fraction were eliminated by selective sorption on silver iodide or by repeated sorption of⁹⁹Mo on Al₂O₃.     

Separation of fission and corrosion products from boric acid solutions by solvent extraction

Extractive purification of boric acid from radioactive corrosion and fission products dissolved in aqueous solutions modelling nuclear reactor coolants has been studied. Aliphatic 1,3-diols containing 8 and 9 carbon atoms per molecule were used as extractants fro boric acid. The behaviour of some representative corrosion and fission products as well as various factors affecting their distribution between the organic and aqueous phases have been investigated under the conditions of boric acid extraction. Conditions for the effective separation of boric acid from most of the radioactive contaminants are presented.     

Separation of uranium from other metals by partition chromatography

Uranium(VI) can be separated quantitatively from most other metal ions by partition chromatography on a silica-gel column. The column is treated with aqueous 6M nitric acid; after sorption of the sample, uranium(VI) is selectively and rapidly eluted by methyl isobutyl ketone. In addition to the separation of macro quantities of metal ions, the method has been used successfully for the isolation of trace amounts of metal ions from uranium(VI).     

Separation and determination of uranium and thorium in zircon sands by extraction chromatography

An extraction chromatography method with a column of microporous polyethylene supporting tri-n-octylamine /TNOA/ was used to separate uranium and thorium from zircon sands. The two elements were determined both by physical-chemical techniques /fluorimetry and colorimetry/ and by radiometric techniques /alpha spectrometry/ after electrodeposition: their respective contents agreed well; furthermore, uranium and thorium isotopes resulted in secular equilibrium in the analyzed material.     

Separation of tin from some metals by extraction chromatography

Much attention has been devoted to Sn (IV) strongly retained on the TBP-Daiflon column from 2M HCl in extraction chromatography. The separations of Sn?Cu, Zn, As, Cd, Sb, Pb,¹¹³Sn-¹²⁵Sb,¹¹³Sn-^113mIn (^113mIn milking) and Sn?Hg?Fe were successfully achieved without any contamination. In the separations, except for the last, only tin was retained separately on the column upon passing the mixed solution. The daughter indium was eluted with 0.5M HCl. In the last separation, iron was eluted with 0.5 M HCl, tin with 0.1M HCl and mercury with 2M HNO₃, for these metals retained on the column. Radioactive tracers for tin, iron, mercury and antimony were used.     

Radiochemical determination of fission products of uranium

An analysis has been elaborated to determine the long-living γ-emitting fission products of uranium. It consists of a sodium bisulphate melt of the fission product solution or the U-fuel, followed by liquid-liquid extractions. Afterwards the isotopes are absolutely counted with a standardized 3″×3″ NaI crystal. The total γ-spectrum of the original fission product solution, taken with a NaI crystal or a Ge−Li detector, is also analyzed mathematically by mixed γ-spectrometry. From a short post-irradiation of the fission product solution the concentrations of both²³⁵U and²³⁸U are determined. The absolute amount of fission products related to the U-concentration allows the calculation of the percent atomic burn-up, the irradiation time, the cooling period, the flux of the reactor and the original degree of enrichment of the uranium. Research associate of the I. I. K. W.     

Extraction-chromatographic separation of uranium from long-lived fission products using tributyl phosphate

Extraction-chromatographic separation of uranium from fission products was performed using undiluted tributyl phosphate sorbed on Chromosorb W as a stationary phase, and nitric acid (1: 3) as a mobile phase. Most of the fission products that contributed greatly to the radiation level of the sample passed through the column; this effected considerable decontamination. Uranium retained on the column was quantitatively recovered by elution with water.     

Separation of uranium from different uranium oxide matrices employing supercritical carbon dioxide extraction

Uranium from different uranium oxide matrices was extracted with tri-n-butyl phosphate–nitric acid (TBP–HNO₃) adduct using supercritical carbon dioxide (SC CO₂). While 30 min dissolution time at 323 K was sufficient for U₃O₈ and UO₂ powder, UO₂ granule (at 333 K) and crushed green pellet (at 353 K) required 40 min. Crushed sintered pellet required 60 min at 353 K for complete dissolution. Influence of various experimental parameters such as temperature, pressure, volume of TBP–HNO₃ adduct, acidity of nitric acid used for preparing TBP–HNO₃ adduct and extraction time on uranium extraction efficiency was also investigated. For UO₂ powder, temperature of 323 K, pressure of 15.2 MPa, 1 mL TBP–HNO₃ adduct, 10 M nitric acid and 30 min extraction time was found to be optimum. ~70% uranium extraction efficiency was obtained on extraction with SC CO₂ alone which increased to 90% with the addition of 2.5% TBP in SC CO₂ stream. Extraction efficiency was found to vary linearly with TBP percentage and nearly complete uranium extraction (~99%) was observed with 20% TBP. Nearly complete extraction was also achieved with addition of 2.5% thenoyltrifluoroacetylacetone (TTA) in methanol. The optimized procedure was extended to remove uranium from simulated tissue paper waste matrix smeared with uranium oxide solids.     

Trace quantities of uranium in some Indian chewing tobaccos as determined by fission track analysis

The sandwiched pellet technique using Makrofol-E plastic track detectors has been employed to determine trace quantities of uranium in nine brands of flavored chewing tobaccos consumed by the Indian population. In this technique the nuclear reaction,²³⁵U(n,f), is used for the quantitative estimation of uranium. The maximum value of uranium (1.88 ppm) has been found in raw tobacco leaves (Surti), while the minimum (0.13 ppm) in Tulsi (Double Zero brand). Other seven brands showed intermediate values of U-contents which are also reported in this paper. These values are compared with the U-contents reported in the literature for other forms of tobaccos.     

Separation of rare earth elements from uranium by solvent extraction and ion exchange

The detection limit of⁹⁹Tc in (,) radio-activation analysis was determined in the presence of molybdenum and compared with that of⁹⁹Tc in pure materials in the previous paper. The isotopic ratio of molybdenum in a⁹⁹Mo–^99mTc generator column could be simultaneously determined by photon activation analysis.     

Separation of bismuth from gram amounts of thallium and silver by cation-exchange chromatography in nitric acid

Traces and small amounts of bismuth can be separated from gram amounts of thallium and silver by successively eluting these elements with 0.3M and 0.6M nitric acid from a column containing 13 ml (3 g) of AG50W-X4, a cation-exchanger (100-200 mesh particle size) with low cross-linking. Bismuth is retained and can be eluted with 0.2M hydrobromic acid containing 20% v/v acetone, leaving many other trace elements absorbed. Elution of thallium is quite sharp, but silver shows a small amount of tailing (less than 1 gmg/ml silver in the eluate) when gram amounts are present, between 20 and 80 mug of silver appearing in the bismuth fraction. Relevant elution curves and results for the analysis of synthetic mixtures containing between 50 mug and 10 mg of bismuth and up to more than 1 g of thallium and silver are presented, as well as results for bismuth in a sample of thallium metal and in Merck thallium(I) carbonate. As little as 0.01 ppm of bismuth can be determined when the separation is combined with electrothermal atomic-absorption spectrometry.     

Determination of radiocerium in fission products by extraction chromatography using di-(2-ethylhexyl)phosphoric acid

An extraction chromatographic method is described for the determination of cerium in a fission product mixture. Cerium(IV) is separated on a column of siliconized kieselguhr saturated with di-(2-ethylhexyl)phosphoric acid (HDEHPA). After washing the column with a mixture of sodium bromate and nitric acid, cerium is eluted by a mixture of 5M HNO₃ and 0.1M ascorbic acid. The optimum conditions for the quantitative sorption and elution of cerium were found, and the reproducibility of the yield was verified. The influence of other fission and corrosion products (Mg, Fe, Al, U) on the sorption and elution of cerium was studied. The method has been successfully applied for the determination of cerium in artificial and natural mixtures of fission products.     

Separation and determination of uranium and radium-226 in phosphorites and their industrial derivatives by extraction chromatography

An extraction chromatographic method based on microporous polyethylene (Microthene) supporting tri-n-octylphosphine oxide (TOPO) was used to separate uranium and²²⁶Ra from phosphorites and their industrial derivatives. Uranium was then determined by fluorimetry and by alpha-spectrometry after electroplating, and radium by precipitation as Ba(Ra)SO₄ and alpha counting with a ZnS(Ag) alpha detector. The method was checked by using an IAEA phosphorite sample having a certified uranium concentration. Some phosphorite, phosphoric acid and plaster samples supplied by an Italian industrial plant were analyzed; uranium isotopes always resulted in radioactive secular equilibrium.     

Gas-chromatographic technique for rapid isolation of uranium fission products

Summary A gas-chromatographic technique for a rapid separation of fission iodine or bromine from the other elements formed in nuclear fission was developed. Recoil-formed, volatile methyl bromide and methyl iodide were isolated within 1 min after the end of irradiation. An extension of this technique to other elements and to other nuclear reactions should be possible.The -ray spectra of both halogen fractions were measured. A dominating -ray at 0.79 MeV and a weaker -ray at 0.51 MeV were assigned to ⁸⁸Br (half life 16 sec). No -ray could be unambiguously attributed to ¹³⁷I (24 sec), a fact which makes unlikely the presence of highly intensive peaks in the -ray spectrum of this isotope. Further details of the spectra are discussed.

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Zusammenfassung Eine gaschromatographische Methode zur schnellen Isolierung von Spaltjod oder Spaltbrom aus dem Gemisch der bei der Kernspaltung entstehenden Elemente wurde entwickelt. Mittels Spaltrückstoß gebildetes, flüchtiges Methylbromid oder Methyljodid wurde innerhalb 1 min nach Bestrahlungsende isoliert. Die Methode sollte auf andere Elemente und andere Kernreaktionen übertragbar sein.-Spektren der beiden Halogenfraktionen wurden gemessen und ergaben für ⁸⁸Br (Halbwertszeit 16 sec) eine dominierende Linie bei 0,79 MeV und eine schwache Linie bei 0,51 MeV. In der Jodfraktion wurde keine -Linie beobachtet, die man eindeutig ¹³⁷J (24 sec) hätte zuordnen können, was sehr intensive Peaks im Spektrum dieses Isotops unwahrscheinlich macht. Weitere Einzelheiten der Spektren werden diskutiert.

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Dedicated to Prof. Dr. F. Strassmann on his 65th birthday.     

The determination of fission products in irradiated uranium by electrophoretic focussing of ions

Electrophoretic focussing of ions was applied to the separation of fission products present in solutions of nuclear uranium fuel irradiated in various European reactors. By combining two separation methods, all the long-lived fission products could be determined individually and quantitatively by counting with a NaI(T1) and a GM detector of known detection efficiency. Radiography and autoradiography were used for semi-quantitative purposes. The concentrations of²³⁵U and²³⁸U were determined from a short post-irradiation of the fuel solution and counting of¹⁴⁰Ba−¹⁴⁰La and²³⁹Np, respectively. An iterative calculus method is presented which allows calculation of the irradiation history of the fuel solution from the above analyses. without any a priori knowledge.     

Solvent extraction of technetium(VII) by 4-(5-nonyl)pyridine and its separation from uranium and some fission products

The extraction of technetium (VII) by 4-(5-nonyl)pyridine has been investigated from different aqueous solutions. Separation from uranium and some fission products has been achieved in nitrate media. From the results of partition experiments, attempts have been made to deduce the nature of the extracted species.