The kinetic phosphorlmeiric determination of uranyl Ion in aqueous solutions at room temperature yielded a detection limit for UOz2+ of 1 ng/L. The response to uranlum Is linear from the detection ilmH up to 5 mg/L. The method Is fast and accurate, with no separative pretreatment needed for most of the real samples investlgated. I n the anaiysls of bloioglcai samples, wet-ashlng with HNO3/HzO2 Is requlred for measurements near the detection ilmlt. Samples with uranium concentrations hlgher than 0.1 pg/L gave relatlve standard devlations typically below 5 %. Factors affecting the quantum yield of the uranyl Ion phosphorescence, e.g. quenchlng from specles present In the matrix, are accounted for in the klnetlc analysis of the uranyl phosphorescence.

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This study was undertaken to investigate the possibility of measuring total body water in human subjects to better than +/-0.5%. Accurate serial estimates of total body water were required to complement densitometric and anthropometric measurements used to monitor body compositional changes in obese patients undergoing dietary or surgical weight reduction therapy. The method required the oral administration of 1-2 g of deuterium oxide and the analysis of pre-dose and respective equilibrated samples of urine, plasma or saliva. The sample size required for analysis was 5 microliter and the conversion of gaseous phase was accomplished using a uranium reduction furnace. Isotopic enrichment of samples was measured using a mass spectrometer incorporating several features designed to cope with problems inherent in H2/H2H isotopic analysis. Reproducibility of sample preparation and accuracy of the mass spectrometer were tested using international standards and shown to give an overall sensitivity of 2 parts in 10(7) for the determination of deuterium in H2O/H2HO mixtures. This precision has enabled us to demonstrate that isotopic fractionation of deuterium with respect to hydrogen occurs within the body and expands the potential use of this isotope for quantitative biochemical studies in the human subject.

Oxy anions in complex nuclear process-waste materials are being determined by laser Raman spectrometry (LRS). The double internal-standard technique developed by A. L. Marston [Nucl. Techno/., 25,576 (l975)] is applied to the simultaneous determination of up to six anions in alkaline solutions. The method of A. L. Marston has been extended to solutions prepared from the solids formed in nuclear waste storage tanks. As many as six anions, aluminate, chromate, nitrate, nitrite, phosphate, and sulfate, are slmultaneousiy determined in about 1 h. Carbonate may also be determined, but In the presence of the prevalent nitrate, a chemical separation is required. Individual methods have been relegated to a secondary status because of the many advantages of LRS. The typical precidon obtained for analytes In high concentration is around 5 % RSD at the 95% confidence level.The chemical processing of irradiated nuclear fuels has resulted in large quantities of nuclear wastes which occur in three general types: concentrated aqueous liquor, water soluble salt cake, and sludge of insoluble salts and hydroxides. T h e major species, other than water, are sodium salts of oxy anions and the hydroxides of aluminum and iron. The analyses of these nuclear waste materials present a difficult task because of the concentrations and complexity of the samples. Table I shows a likely composition of waste samples.Compositions may vary widely and many other species may be present in trace amounts. Knowledge of anion concentrations is important to monitoring the integrity of the nuclear waste storage, t o research in developing nuclear waste solidification methods, and to current processes for reducing waste liquors to salt cake. The methods used in the past have largely been trace methods for speed, dilution of the matrix, and freedom from interference. Examples are specific ion electrode and spectrophotometric methods.T h e quantitative analytical characteristics of Raman spectroscopy have been reviewed and discussed by Irish and Chen ( I ) . More recently, Ozeki and Ishii (2) have described the principles of determining anions by laser Raman spectroscopy (LRS). Other analytical investigations include the detection limits of inorganic oxy anions in water (3) and the determination of sulfate in sodium nitrate (4). A. L. Marston of the US. Energy Research and Development Administration's Savannah River nuclear plant has applied LRS to the determination of oxy anions in the Savannah River Plant's waste supernate liquors (5). Of the above, only Cunningham et al. (3) addressed themselves to carbonate. Because of the spectral interference of nitrate, Marston did not determine COS2-. The work described here includes the application of modifications of Marston's method to three types of Hanford nuclear waste materials: waste liquor, salt cake, and sludge.

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