Energy Technology Data Exchange (ETDEWEB)

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Energy Technology Data Exchange (ETDEWEB)

A new method for the determination of {sup 237}Np and Pu isotopes in large soil samples has been developed that provides enhanced uranium removal to facilitate assay by inductively coupled plasma mass spectrometry (ICP-MS). This method allows rapid preconcentration and separation of plutonium and neptunium in large soil samples for the measurement of {sup 237}Np and Pu isotopes by ICP-MS. {sup 238}U can interfere with {sup 239}Pu measurement by ICP-MS as {sup 238}UH{sup +} mass overlap and {sup 237}Np via {sup 238}U peak tailing. The method provides enhanced removal of uranium by separating Pu and Np initially on TEVA Resin, then transferring Pu to DGA resin for additional purification. The decontamination factor for removal of uranium from plutonium for this method is greater than 1 x 10{sup 6}. Alpha spectrometry can also be applied so that the shorter-lived {sup 238}Pu isotope can be measured successfully. {sup 239}Pu, ...

Energy Technology Data Exchange (ETDEWEB)

The multielement determination of major-to-ultratrace elements in salmon egg was carried out by ICP-AES and ICP-MS. First, salmon eggs (30 eggs used) were digested with conc. nitric acid and 60% perchloric acid by heating almost to dryness repeatedly. Finally, the residues of salmon eggs were dissolved in 1 M nitric acid and the sample solutions were analyzed by ICP-AES and ICP-MS. About 40 elements could be determined over the concentration range in 9 orders of magnitude. The concentrations of bio-essential elements, such as Zn, Fe, and Cu, in salmon egg were 10-100 times higher than those in human blood serum. In addition, the major-to-ultratrace elements in cell cytoplasm and cell membrane were separately determined in a similar manner to those in whole egg cell. The concentrations of most bio-essential elements were higher in cell cytoplasm than in cell membrane, while those of Fe and Cu were higher in cell membrane than in cell cytoplasm ...

International Nuclear Information System (INIS)

A method was developed for the determination of plutonium in the soil samples by ICP-MS with TOA extraction chromatographic column. The optimized sample loading rate is below 0.2 mL/min (column inner diameter is 3.5 mm). Using hot 0.02 mol/L oxalic acid (H_2C_2O_4) in 0.16 mol/L HNO_3 to elute Pu from the solid phase in the column. The Pu recovery of 87.3%-96.8% in soil samples was obtained. The plutonium is separated with the ion exchange method in this work. Both extraction chroma- tography and ion-exchange methods efficiently remove the uranium and matrix interference from the ICP- MS measurement. The instrumental detection limit for "2"3"9Pu was 0.48 pg/mL, which corresponds to 1, 1 mBq/mL. (authors)

International Nuclear Information System (INIS)

A new method that allows rapid preconcentration and separation of plutonium and neptunium in water samples was developed for the measurement of "2"3"7Np and Pu isotopes by inductively-coupled plasma mass spectrometry (ICP-MS) and alpha spectrometry. "2"3"8U can interfere with "2"3"9Pu measurement by ICP-MS as "2"3"8UH"+ mass overlap and "2"3"7Np via peak tailing. The method provide enhanced removal of uranium by separating Pu and Np initially on TEVA Resin, then moving Pu to DGA resin for additional removal of uranium. The decontamination factor for uranium from Pu is almost 100,000 and the decontamination factor for U from Np is greater than 10,000. This method uses stacked extraction chromatography cartridges and vacuum box technology to facilitate rapid separations. Preconcentration is performed using a streamlined calcium phosphate precipitation method. Purified solutions are split between ICP-MS and alpha spectrometry ...

Energy Technology Data Exchange (ETDEWEB)

Since living things began their activities on the earth, the extermination of living things in large number on global scale occurred twice 230 million years ago (P-Tr boundary) and 65 million years ago (K-T boundary). As to the cause of exterminating living things in short period, there are volcano eruption theory, meteorite collision theory and so on, but still it is not decided. Therefore, as to the strata of P-Tr boundary in south-western part of China where it has been known the preservation of P-Tr strata is especially good, the existence of elements was measured by instrument neutron activation analysis and ICP-MS, and the state of change was examined. According to the results, the change occurred at the P-Tr boundary on the earth, and further, the possibility of meteorite collision by paying attention to Ir were examined. The samples, the neutron activation analysis, the ICP-MS and the results are reported. The distinction by strata and ...

International Nuclear Information System (INIS)

A set of 35 uranium ore and 10 yellow cake samples, collected worldwide from different mines and production sites, were analyzed for their impurity spectrum by ICP-MS. Pattern recognition techniques such as cluster analysis were applied to the data set in order to characterize samples with relation to their geographical origin. The results obtained show a clear relationship between samples taken from the same geological origin and constitute a satisfactory fingerprint for establishing the origin of the material. In addition to the impurity data, data on the isotopic composition of radiogenic lead is used to resolve ambiguity when impurity cluster analysis fails to deliver unambiguous origin data. (author)

Energy Technology Data Exchange (ETDEWEB)

The potentiodynamic polarization measurement of 254SMO stainless steel (UNS 31254) was conducted in 3.5% NaCl solutions with pH ranging from 0.1 to 5. The results indicated that this stainless steel offered excellent pitting corrosion resistance in corrosive environments. Further, it also exhibited various features on the polarization curves in different pH solutions. The electrochemical constant-potential passivation treatment performed at different pH followed by XPS analysis revealed that the primary constituents of the outermost layer of the passive films formed in the weak (pH 5) and strong (pH 0.8) acid solutions are iron oxides and Cr{sub 2}O{sub 3} and Cr(OH){sub 3}, respectively. Molybdenum oxides, primarily in the six-valence state, existed in the outermost layer of the passive film. Only very weak signals corresponding to that of nickel oxides were detected in the film formed in the weak acid (pH 5) solution. The ICP-MS analyses indicated selective ...

International Nuclear Information System (INIS)

In most conceptual fusion power reactor designs, it is proposed to use beryllium as a neutron multiplier in the blanket. Detailed chemical composition of beryllium is necessary for evaluation of the tritium breeding ratio, and estimating the activation and transmutation of beryllium in the fusion reactor. In the present report, special attention was paid to a detailed analysis of impurities in beryllium, relevant to the tritium breeding ratio evaluation. Two different methods were used for the study of impurities: an analysis of the local sample by the ICP-MS method, and an integral analysis of the beryllium assembly, using the pulsed neutron method. The latter method was proposed as the most effective way of analyzing the integral effect to impurities in beryllium on production of the tritium on the lithium-6. The evaluation of the integral effect was based on time behaviour observations of the thermal neutron flux, following the injection of a burst of D-T ...

International Nuclear Information System (INIS)

Along with the shrinkage of LSI geometries, a higher quality of ultrapure water has been continuously required. Analytical technology for ultrapure water has also progressed before ultrapure water production technology improvements. In this study, we performed optimization of the analytical conditions for the direct analysis of acid droplets, and established an analytical technology for measurements of trace amounts of metallic impurities deposited on a wafer surface by means of Vapor Phase Decomposition (VPD)/Inductively Coupled Plasma Mass Spectrometry (ICP-MS). As a result, analytical technology for metallic elements of the 1x10"8 atoms/cm"2 level on wafer surface has been established. By applying analytical technology to the wafer that has been contacted with ultrapure water, a new evaluation technology for ultrapure water quality by means of wafer surface contamination has been established. We confirmed good correlations between metal contamination of the ...

International Nuclear Information System (INIS)

Three CRMs of plant origin (SRM 1515 Apple Leaves, SRM 1570a Trace Elements in Spinach Leaves, and SRM 1575 Pine Needles) were used for analytical quality assurance of Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Mo, Cd, and Pb determination by ICP-MS. The samples were decomposed using microwave assisted pressurized digestion by HNO_3 and HNO_3 + H_2O_2 mixture and temperature programmed dry ashing. Concentrations of elements in samples were evaluated by external calibration. All samples, blanks, and standards were spiked to 100 #mu#g/L concentration of In and Bi as internal standards. During the measurement, signals of "5"2Cr, "5"3Cr, "5"4Fe, "5"5Mn, "5"9Co, "6"0Ni, "6"2Ni, "6"3Cu, "6"5Cu, "6"6Zn, "9"5Mo, "1"1"1Cd, "1"1"2Cd, "1"1"5In, "2"0"6Pb, "2"0"7Pb, "2"0"8Pb and "2"0"9Bi were monitored. Results of Pb, Cd, Cu, Zn, Mo and Co determination were in good agreement with certified values. In order to obtain accurate results for As at low levels, it was necessary to ...

International Nuclear Information System (INIS)

The use of environmental monitoring as a technique to identify activities related to the nuclear fuel cycle has been proposed by international safeguards organizations. The elements specific for each kind of nuclear activity, or 'nuclear signatures', inserted in the ecosystem can be intercepted by different live organisms. This work demonstrates the technical viability of using pine needles as bioindicators of nuclear signatures associated with uranium enrichment activities. Additionally, it proposes the use of HR-ICP-MS to identify the signature corresponding to that kind of activities in the ecosystem. Nitric acid solutions, used to wash pine needles sampled near nuclear facilities and containing only 0.1 #mu#g x kg"-"1 of uranium, exhibit a n("2"3"5U)/n("2"3"8U) isotopic abundance ratio of 0.0092#+-#0.0002, while solutions originated from samples collected at places located more than 200 km far from activities related to the nuclear fuel cycle exhibit a value of ...

Energy Technology Data Exchange (ETDEWEB)

The application of the large-bore direct injection high efficiency nebulizer (LB-DIHEN) for the determination of arsenic (As), cadmium (Cd), lead (Pb), and mercury (Hg) in urine by inductively coupled plasma mass spectrometry (ICP-MS) is described. The LB-DIHEN is compared with the standard method using a concentric pneumatic nebulizer and cyclonic spray chamber. In addition to the toxicological significance of As, Cd, Pb, and Hg, these elements represent a cross-section of analytical issues including spectral interferences (e.g., {sup 40}Ar{sup 35}Cl{sup +} on {sup 75}As{sup +} and {sup 98}Mo{sup 16}O{sup +} on {sup 114}Cd{sup +}) and memory effects (Hg). In this study, the low sample consumption of the LB-DIHEN is used to reduce the volume of urine needed for analysis, and to reduce the volume of final diluted sample required for analysis. Eliminating the spray chamber and reducing the dead volume of the nebulizer reduces memory effects, especially for analytes ...