Simultaneous Plutonium and Uranium Isotopic Analysis from a Single Resin Bead - A Simplified Chemical Technique for Assaying Spent Reactor Fuels

Abstract

The method uses basic anion resin to adsorb plutonium and uranium from 7–8 M HNO₃ solutions containing dissolved spent reactor fuels. After equilibrating the resin with the solution, a single bead is used to determine the isotopic composition of plutonium and uranium on sample sizes as small as 10^?9 to 10^?10 g of each element per bead. Isotopic measurements are essentially free of isobaric interferences and fission product contamination in the mass spectrometer is eliminated. A very small aliquot of dissolver solution containing 10^?6 g of U and 10^?8 g of Pu is sufficient sample for chemically preparing several resin beads. A single prepared bead is loaded onto a rhenium filament and analyzed in a two-stage mass spectrometer using pulse counting for ion detection to obtain the high sensitivity required. Total quantity of the elements, in addition to isotopic abundances, can be determined by isotope dilution. Other areas where the method may be useful are: in plutonium production, isotope separations, and for trace detection of contamination on reactor parts.     

A Bulk Resin Bead Procedure To Obtain Uranium And Plutonium From Radioactive Solutions For Mass Spectrometric Analysis

Abstract

A method is described for extracting representative uranium and plutonium samples from highly radioactive solutions for isotopic mass spectrometric analysis. Anion resin beads in the nitrate form are used to effect separation from fission products and other actinides. Conditions required to achieve separation are proper adjustment of the uranium and nitric acid concentrations. Once uranium and plutonium are adsorbed, each bead serves as a sample for mass spectrometric analysis, with plutonium and uranium being run sequentially from the same bead. Quantitative determination of the two elements is effected through the technique of isotopic dilution.     

Analysis of Resin-Bead Loaded U And PU Samples with a Single-Stage Mass Spectrometer

Abstract

The resin bead sample loading technique has been applied to a conventional single-stage mass spectrometer equipped with pulse counting. Isotopic data obtained for U and Pu are comparable to those obtainable from similar instruments using conventional techniques.     

A Rapid Tandem Mass Spectrometric Assay for Determination of Ursolic Acid – Application to Analysis of Ursolic Acid in Four Species of Staphylea L. and Leaves of Staphylea Pinnata L. Gathered During Ontogenesis

Plant extracts of Staphylea L. exhibit a number of biological activities which are presumably attributed to ursolic acid. A rapid and specific tandem mass spectrometric (MS-MS) assay for the quantification of ursolic acid in the leaves of four species of Staphylea L. (Bladdernut) and in the leaves of S. pinnata L. during ontogenesis, was developed and validated. The samples were analyzed by flow injection analysis without chromatographic separation using a transport liquid of methanol/water/formic acid (80:20:0.1 v/v/v) at a flow-rate of 0.2 mL min⁻¹. The run cycle time was ~2-3 min injection-to-injection. Quantification was achieved using multiple reaction monitoring at MRM transition m/z 439 > 203. Calibration curves were linear over the concentration range of 2–20 μg mL⁻¹ with a lower limit of quantification of 2 μg mL⁻¹ (1.8 ± 0.297, RSD: 0.165). Validation data showed that the RSD% values were in the range of 1.8 to 6.8%, whereas the % DEVs ranged from −18 to −2% indicating reasonable and acceptable precision and accuracy, respectively. A recovery percent of 106.8 ± 10.3 of ursolic acid from spiked extracts samples, indicated the specificity and reliability of tandem mass procedure for determination of ursolic acid in the plant extracts. The derived data of sample analysis showed different contents of ursolic acid among various Staphylea species. The highest content of ursolic acid was found in the leaves extract of S. pinnata L. Additionally, the highest amount of ursolic acid accumulated in the leaves of S. pinnata L. was in the August /September period of the year. Smaller amounts of ursolic acid were found in samples collected before and after that time. The results obtained serve as a justification of determining the most appropriate time for collecting plant material as a source of ursolic acid.