Reliability of using 238U/235U and 234U/238U ratios from alpha spectrometry as qualitative indicators of enriched uranium contamination.

Alpha spectrometry is a commonly used technique for the measurement of uranium isotopes in environmental samples because it is widely available at a relatively low cost. For natural uranium the (234)U to (238)U activity ratio should be 1 and the (238)U to (235)U activity ratio should be 21.7. However, a lower (238)U to (235)U ratio is usually observed in alpha spectrometric analysis of environmental soil samples. This observation has led to the conclusion that soils from nuclear weapons facilities were contaminated with highly enriched uranium. This study was undertaken to test the reliability of using activity ratios from alpha spectrometry to infer the presence of highly enriched uranium in soil samples. The results of these experiments indicate that the (238)U to (235)U activity ratio is not a reliable indicator, but that the (234)U to (238)U activity ratio can be used to qualitatively indicate the presence of highly enriched uranium at concentrations near 10 ng g(-1) and above.

Analysis of perchlorate in water and soil by electrospray LC/MS/MS.

A method has been developed for the determination of perchlorate in water and soil matrixes using electrospray liquid chromatography/mass spectrometry/mass spectrometry. Perchlorate is quantitated by monitoring the ion signal from mass 83, which is formed by a loss of an oxygen atom from the perchlorate molecular ion. The method was developed to be effective and economical in production laboratory analysis of perchlorate in environmental water and soil samples. Data were gathered to define method sensitivity, performance, selectivity, and robustness. Analyte stability, method susceptibility to interferences, and the reliability of the chlorine isotope ratio as an identification tool were examined. The aqueous method detection limit (MDL) is 0.05 microg/L and was determined using an actual groundwater matrix. The soil MDL is 0.5 microg/kg and was determined using Ottawa sand. The stability study was performed by spiking water samples at 0.25, 10, and 20 microg/L and analyzing them 50 days later. Acceptable recoveries were obtained for all samples. The relative standard deviation (RSD) for the replicate analyses in the stability study indicates that the method is capable of RSD values less than 5% in a relatively clean groundwater matrix. The ionization suppression study was performed by spiking water samples containing 1000 mg/L carbonate, chloride, and sulfate with 0.05 and 0.5 microg/L perchlorate and then measuring the recovery of the spike. The results indicate that the procedure does not have significant suppression effects at the high salt levels tested. Calibration, quality control sample, field sample, and suppression study data were combined to examine isotope ratio reliability. The results of that work show that chlorine isotope ratios can be used to define statistical process control limits for use as an additional analyte identification tool.