13 research outputs found
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Long-term retention of radium in female former dial workers
The results of measurements of radium contents in 13 women made over 20 years or more were used to measure radium retention. The women were all employed at different studios of the same Illinois plant as luminous dial workers for up to 4 years. The data for each woman were fitted to an exponential function of time, yielding a biological half-life of approximately 30 to 60 years. There was a strong negative correlation between elimination rate and body content, suggesting an effect of radiation of bone resorption or remodelling. A strong negative correlation was observed between the elimination rate and the reduced x-ray score, a measure of bone damage observed radiographically in the same subjects. Age at first exposure and duration of exposure were not significantly correlated with the elimination rate. The concentration of radium in soft tissues from eight other subjects, expressed as a percentage of the terminal radium content, decreased with increasing body content, providing further evidence that radiation was affecting the elimination rate. An effect of radiation on the late retention of radium has been demonstrated. 10 references, 4 figures, 2 tables
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Analytical chemistry of aluminum salt cake
Component phases of Al salt cake or products from processing salt cake, resist dissolution, a key first step in most analysis procedures. In this work (analysis support to a study of conversion of salt cake fines to value-added oxide products), analysis methods were adapted or devised for determining leachable salt, total halides (Cl and F), Al metal, and elemental composition. Leaching of salt cake fines was by ultrasonic agitation with deionized water. The leachate was analyzed for anions by ion chromatography and for cations by ICP-atomic emission spectroscopy. Only chloride could be measured in the anions, and charge balances between cations and chloride were near unity, indicating that all major dissolved species were chloride salts. For total halides, the chloride and fluorides components were first decomposed by KOH fusion, and the dissolved chloride and fluoride were measured by ion chromatography. Al metal in the fines was determined by a hydrogen evolution procedure adapted for submilligram quantities of metallic Al: the Al was reacted with HCl in a closed system containing a measured amount of high-purity He. After reaction, the H/He ratio was measured by mass spectroscopy. Recoveries of Al metal standards (about 30mg) averaged 93%. Comparison of the acid evolution with caustic reaction of the Al metal showed virtually identical results, but reaction was faster in the acid medium. Decomposition of the salt cake with mineral acids left residues that had to be dissolved by fusion with Na carbonate. Better dissolution was obtained by fusing the salt cake with Li tetraborate; the resulting solution could be used for accurate Al assay of salt cake materials by classical 8-hydroxyquinolate gravimetry
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Isotopic anomalies in high Z elements: Uranium
Uranium in terrestrial volcanic ejecta from mantle-related sources has been analyzed mass spectrometrically. The objective was to seek supporting evidence for or refutation isotopic variations reported by Fried et al. (1985) for some such samples. The possibility that terrestrial U is not of constant isotopic composition is extraordinary. If true, mechanisms for creating the variation must be sought and the lack of homogenization within the earth addressed. Samples of 100 grams or more were processed in order to minimize reagent and environmental (laboratory) blank interference and to permit isolation of large amounts (several to tens of ..mu..g) of U for the mass spectrometer (MS) measurements, which utilizes aliquots of /approximately/1 ..mu..g. Aliquants from four volcanic samples gave data which indicate enrichments of /sub 235/U ranging from 0.2% to 5.9% in the 235/238 ratio relative normal uranium ratios. These relative enrichments are consistent with, and in some cases, higher than the 0.18% enrichment reported by Fried et al. (1985) for two volcanic lava samples. However, we were not able to reproduce their results on the Kilauea lava for which they report 0.18% /sup 235/U enrichment. The relative error in our MS ratios is 0.05% -- 0.07%. 1 tab
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Determination of labile copper, cobalt, and chromium in textile mill wastewater
Copper, chromium, and cobalt species present in filtered wastewater effluent were separated by cation exchange and reverse phase chromatography. Three sample fractions were obtained: one containing metal cations (i.e., trivalent Cr, divalent Cu, and divalent Co), one containing organic species (including metallized dyes), and one containing other unretained species. The metal content of each fraction was determined by inductively coupled plasma atomic emission spectroscopy (ICP-AES). The sum of the corrected data was compared to the metal content of a filtered effluent aliquot digested totally with fuming sulfuric acid. Other aliquots of the filtered effluent were spiked with the metals of interest and digested to confirm chemical yield and accuracy. Method detection limits were consistently below 20 {mu}g L{sup -1} for Cu, 30 {mu}g L{sup -1} for Co, and 10 {mu}g L{sup -1} for Cr. Spike recoveries for undifferentiated Cu and Cr were statistically indistinguishable from unity; although Co spike recoveries were slightly low ({approximately}95%), its chemical yield was 98%. Copper retention on the sodium sulfonate cation exchange resin was closely correlated with the [EDTA]/[Cu] ratio, suggesting that metals retained upon the cation exchange column were assignable to labile metal species; however, mass balances for all three elements, though reasonable ({approximately}90%), were significantly different from unity. Mechanical factors may have contributed to the material loss, but other data suggest that some metal species reacted irreversibly with the reverse phase column. 3 refs., 2 figs., 4 tabs
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Preparation of waste oil for analysis to determine hazardous metals
Two methods for preparing waste-oil samples to permit measurement of their metals content were evaluated. For this evaluation, metals-in-oil standard reference materials were prepared by each method and the resulting solutions were analyzed for 20 metals, including those (As, Ba, Cd, Cr, Pb, Hg, Se, and Ag) regulated as hazardous under the Resource Conservation and Recovery Act. One preparation method involved combustion of the waste oil under oxygen at 25 atm pressure, as described in the American Society for Testing and Materials test method E926-88. As we applied it, this method gave recoveries well under 90% for most of the metals that we examined and, hence, proved unsatisfactory for routine application to waste-oil analysis. With the other method, nitric acid decomposition in a sealed vessel heated with microwave energy (analogous to US Environmental Protection Agency Method 3051), recoveries of all 20 metal contaminants were within 90 to 110% of the certified values. This microwave digestion procedure was also more efficient since it allowed six samples to be prepared together, whereas the oxygen combustion approach allowed processing of only one sample at a time
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Argonne National Laboratory Reports
Uranium in terrestrial volcanic ejecta from mantle-related sources has been analyzed mass spectrometrically. The objective was to seek supporting evidence for or refutation isotopic variations reported by Fried et al. (1985) for some such samples. The possibility that terrestrial U is not of constant isotopic composition is extraordinary. If true, mechanisms for creating the variation must be sought and the lack of homogenization within the earth addressed. Samples of 100 grams or more were processed in order to minimize reagent and environmental (laboratory) blank interference and to permit isolation of large amounts (several to tens of .mu.g) of U for the mass spectrometer (MS) measurements, which utilizes aliquots of (approximately)1 .mu.g. Aliquants from four volcanic samples gave data which indicate enrichments of ₂₃₅U ranging from 0.2% to 5.9% in the 235/238 ratio relative normal uranium ratios. These relative enrichments are consistent with, and in some cases, higher than the 0.18% enrichment reported by Fried et al. (1985) for two volcanic lava samples. However, we were not able to reproduce their results on the Kilauea lava for which they report 0.18% ²³⁵U enrichment. The relative error in our MS ratios is 0.05% -- 0.07%. 1 tab
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Domestic and Personal Determinants of the Contamination of Individuals by Household Radon Daughters
Radon daughters were counted by gamma spectroscopy from 180 adult residents of eastern Pennsylvania during the winter of 1983-84. Body radon daughter contamination is an index of relative individual respiratory exposures to radon daughters. These can be related to household radon levels, and to personal risk factors such as sex and tobacco smoking. Over 75% of this Pennsylvania population appeared to have environmentally enhanced radon daughter contamination; 59% had counting rates greater than 2 s.d. above background. House radon levels were the major determinants of radon daughters contamination in the 112 subjects for which both sets of measurements were available (p<.001). Both sex (<.02) and cigarette smoking (p<.005) were found to significantly modify that relationship, after nonlinear adjustment for travel times. Using a logarithmic model, for a given radon level body contamination by radon daughters in females was 2-3.5x higher than in males. Nonsmokers had 2-4x higher levels of contamination than smokers. For female nonsmokers relative to male smokers (which in general corresponds to the population of major concern relative to the population from which risk estimates have been derived), the excesses multiply. These results are for total contamination, both internal and external
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Uranium Isotopic Composition and Uranium Concentration in Special Reference Material SRM A (Uranium in KCL/LiCL Salt Matrix)
To help assure that analysis data of known quality will be produced in support of demonstration programs at the Fuel Conditioning Facility at Argonne National Laboratory-West (Idaho Falls, ID), a special reference material has been prepared and characterized. Designated SRM A, the material consists of individual units of LiCl/KCl eutectic salt containing a nominal concentration of 2.5 wt. % enriched uranium. Analyses were performed at Argonne National Laboratory-East (Argonne, IL) to determine the uniformity of the material and to establish reference values for the uranium concentration and uranium isotopic composition. Ten units from a batch of approximately 190 units were analyzed by the mass spectrometric isotope dilution technique to determine their uranium concentration. These measurements provided a mean value of 2.5058 {+-} 0.0052 wt. % U, where the uncertainty includes estimated limits to both random and systematic errors that might have affected the measurements. Evidence was found of a small, apparently random, non-uniformity in uranium content of the individual SRM A units, which exhibits a standard deviation of 0.078% of the mean uranium concentration. Isotopic analysis of the uranium from three units, by means of thermal ionization mass spectrometry with a special, internal-standard procedure, indicated that the uranium isotopy is uniform among the pellets with a composition corresponding to 0.1115 {+-} 0.0006 wt. % {sup 234}U, 19.8336 {+-} 0.0059 wt. % {sup 235}U, 0.1337 {+-} 0.0006 wt. % {sup 236}U, and 79.9171 {+-} 0.0057 wt. % {sup 238}U