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Sample records for sequential isotopic determination

  1. Sequential determination of U and Th isotopes, 226Ra, 228Ra, 210Pb, and 210Po in mushroom

    International Nuclear Information System (INIS)

    Rosa, Mychelle M.L.; Taddei, Maria Helena T.; Dias, Fabiana F.; Maihara, Vera A.

    2009-01-01

    For this study, mushroom samples were collected in Brazil at the Sao Paulo Metropolitan Region and at the Pocos de Caldas Plateau (PC; a region of elevated natural radioactivity, which houses the first Brazilian uranium mine). This paper discusses a sequential methodology to determine natural series radionuclides in mushrooms, such as uranium ( 238 U and 234 U) and thorium ( 232 Th, 230 Th, and 228 Th) isotopes, radium-226, radium-228, as well as lead-210 and polonium-210; using Alpha Spectrometry, Gamma Spectrometry, and Total Alpha and Beta Counting. The method involves total sample dissolution in a closed system in order to avoid loss of Polonium and employment of specific chromatographic resins for radionuclide purification. A subsequent interpretation of the results can provide information on pollutants present in mushrooms and infer possible contamination in the areas sampled as well as allow an association of measured concentrations to radioactive anomalies in the Plateau. (author)

  2. Direct methods and residue type specific isotope labeling in NMR structure determination and model-driven sequential assignment

    International Nuclear Information System (INIS)

    Schedlbauer, Andreas; Auer, Renate; Ledolter, Karin; Tollinger, Martin; Kloiber, Karin; Lichtenecker, Roman; Ruedisser, Simon; Hommel, Ulrich; Schmid, Walther; Konrat, Robert; Kontaxis, Georg

    2008-01-01

    Direct methods in NMR based structure determination start from an unassigned ensemble of unconnected gaseous hydrogen atoms. Under favorable conditions they can produce low resolution structures of proteins. Usually a prohibitively large number of NOEs is required, to solve a protein structure ab-initio, but even with a much smaller set of distance restraints low resolution models can be obtained which resemble a protein fold. One problem is that at such low resolution and in the absence of a force field it is impossible to distinguish the correct protein fold from its mirror image. In a hybrid approach these ambiguous models have the potential to aid in the process of sequential backbone chemical shift assignment when 13 C β and 13 C' shifts are not available for sensitivity reasons. Regardless of the overall fold they enhance the information content of the NOE spectra. These, combined with residue specific labeling and minimal triple-resonance data using 13 C α connectivity can provide almost complete sequential assignment. Strategies for residue type specific labeling with customized isotope labeling patterns are of great advantage in this context. Furthermore, this approach is to some extent error-tolerant with respect to data incompleteness, limited precision of the peak picking, and structural errors caused by misassignment of NOEs

  3. A sequential extraction procedure to determine Ra and U isotopes by alpha-particle spectrometry in selective leachates

    International Nuclear Information System (INIS)

    Aguado, J.L.; Bolivar, J.P.; San-Miguel, E.G.; Garcia-Tenorio, R.

    2003-01-01

    A radiochemical sequential extraction procedure has been developed in our laboratory to determine 226 Ra and 234,238 U by alpha spectrometry in environmental samples. This method has been validated for both radionuclides by comparing in selected samples the values obtained through its application with the results obtained by applying alternative procedures. Recoveries obtained, counting periods applied and background levels found in the alpha spectra give suitable detection limits to allow the Ra and U determination in operational forms defined in riverbed contaminated sediments. Results obtained in these speciation studies show that 226 Ra and 234,238 U contamination tend to be associated to precipitated forms of the sediments. (author)

  4. Rapid Determination of Plutonium Isotopes in Environmental Samples Using Sequential Injection Extraction Chromatography and Detection by Inductively Coupled Plasma Mass Spectrometry

    DEFF Research Database (Denmark)

    Qiao, Jixin; Hou, Xiaolin; Roos, Per

    2009-01-01

    This article presents an automated method for the rapid determination of 239Pu and 240Pu in various environmental samples. The analytical method involves the in-line separation of Pu isotopes using extraction chromatography (TEVA) implemented in a sequential injection (SI) network followed...... by detection of isolated analytes with inductively coupled plasma mass spectrometry (ICP-MS). The method has been devised for the determination of Pu isotopes at environmentally relevant concentrations, whereby it has been successfully applied to the analyses of large volumes/amounts of samples, for example......, 100−200 g of soil and sediment, 20 g of seaweed, and 200 L of seawater following analyte preconcentration. The investigation of the separation capability of the assembled SI system revealed that up to 200 g of soil or sediment can be treated using a column containing about 0.70 g of TEVA resin...

  5. Sequential Injection Method for Rapid and Simultaneous Determination of 236U, 237Np, and Pu Isotopes in Seawater

    DEFF Research Database (Denmark)

    Qiao, Jixin; Hou, Xiaolin; Steier, Peter

    2013-01-01

    An automated analytical method implemented in a novel dual-column tandem sequential injection (SI) system was developed for simultaneous determination of 236U, 237Np, 239Pu, and 240Pu in seawater samples. A combination of TEVA and UTEVA extraction chromatography was exploited to separate and purify...... target analytes, whereupon plutonium and neptunium were simultaneously isolated and purified on TEVA, while uranium was collected on UTEVA. The separation behavior of U, Np, and Pu on TEVA–UTEVA columns was investigated in detail in order to achieve high chemical yields and complete purification...

  6. Rapid and simultaneous determination of neptunium and plutonium isotopes in environmental samples by extraction chromatography using sequential injection analysis and ICP-MS

    DEFF Research Database (Denmark)

    Qiao, Jixin; Hou, Xiaolin; Roos, Per

    2010-01-01

    plutonium and neptunium in three reference materials were in agreement with the recommended or literature values at the 0.05 significance level. The developed method is suitable for the analysis of up to 10 g of soil and 20 g of seaweed samples. The extraction chromatographic separation within the SI system......This paper reports an automated analytical method for rapid and simultaneous determination of plutonium isotopes (239Pu and 240Pu) and neptunium (237Np) in environmental samples. An extraction chromatographic column packed with TrisKem TEVA® resin was incorporated in a sequential injection (SI...... for a single sample takes less than 1.5 h. As compared to batchwise procedures, the developed method significantly improves the analysis efficiency, reduces the labor intensity and expedites the simultaneous determination of plutonium and neptunium as demanded in emergency actions....

  7. Determination of Cd, Pb, Zn and Cu in Sediment Compartments by Sequential Extraction and Isotope Dilution Inductively Coupled Plasma Mass Spectrometry (ID-ICP-MS

    Directory of Open Access Journals (Sweden)

    Gardolinski Paulo C. F. C.

    2002-01-01

    Full Text Available Trace concentrations of Cd, Cu, Pb and Zn in four different sediment fractions extracted in sequence were determined by isotope dilution inductively coupled mass spectrometry (IDICPMS. The metals from each fraction were extracted following the sequential extraction procedure recommended by the Bureau Commun de Référence (BCR of the Commission of the European Communities. As an alternative to external calibration, the elements were quantified by spiking the extracted solutions with 112Cd, 63Cu, 208Pb and 66Zn and application of isotope dilution. The proposed approach was applied to a sample collected from a lake and two standard reference materials, NIST2704 river sediment from the National Institute of Standards & Technology and the BCR-277 estuarine sediment. Detection limits, for each extracted solution, varied from 0.31 to 0.53 mug L¹ for Cd, 0.92 to 2.9 mug L¹ for Cu, 0.22 to 1.1 mug L¹ for Pb and 1.3 to 7.6 mug L¹ for Zn. The sum of the metals concentration in the different fractions was compatible with 95% confidence level found amounts obtained with complete digestion of the samples and with the certified values of the standard reference materials.

  8. Sequential determination of environmental levels of isotopic thorium, uranium and the light rare earth elements within the terrestrial food chain by induced coupled plasma (ICP) and alpha spectrometry

    International Nuclear Information System (INIS)

    Linsalata, P.; Morse, R.; Ford, H.

    1986-01-01

    A radioecological study designed to measure soil to plant and soil to animal (livestock) transfer of Th, U, Ra and the light rare earth elements (REE) in typical and naturally-enhanced radiation environments required the development of radiochemical methods suitable for low-level determinations in a broad suite of environmental matrices including soil, edible vegetables and vegetation, and the major organs and tissues of various livestock. Earlier work has demonstrate the reliability of the methods summarized here for measuring the isotopic thorium and REE content of human feces, and that in the edible portions of various vegetables grown under field conditions. The very high degree of biological discrimination against Th and REE uptake in plants as well as in animal soft tissues necessitated the analysis of typical sample masses of 1-4 kg (fresh weight) to insure reasonably precise (eg., 10-20%) concentration estimates for most of the elements and isotopes of interest. As a result of the ''bone-seeking'' nature and relatively long retention times for these elements in skeletal tissue, typical analytical masses required for analysis of bone range from 40 to 70 g (fresh weight) except for the REE's in which a larger aliquot is recommended when determination is by induced coupled plasma spectrometry

  9. Plutonium determination by isotope dilution

    International Nuclear Information System (INIS)

    Lucas, M.

    1980-01-01

    The principle is to add to a known amount of the analysed solution a known amount of a spike solution consisting of plutonium 242. The isotopic composition of the resulting mixture is then determined by surface ionization mass spectrometry, and the plutonium concentration in the solution is deduced, from this measurement. For irradiated fuels neutronic studies or for fissile materials balance measurements, requiring the knowledge of the ratio U/Pu or of concentration both uranium and plutonium, it is better to use the double spike isotope dilution method, with a spike solution of known 233 U- 242 Pu ratio. Using this method, the ratio of uranium to plutonium concentration in the irradiated fuel solution can be determined without any accurate measurement of the mixed amounts of sample and spike solutions. For fissile material balance measurements, the uranium concentration is determined by using single isotope dilution, and the plutonium concentration is deduced from the ratio Pu/U and U concentration. The main advantages of isotope dilution are its selectivity, accuracy and very high sensitivity. The recent improvements made to surface ionization mass spectrometers have considerably increased the precision of the measurements; a relative precision of about 0.2% to 0.3% is obtained currently, but it could be reduced to 0.1%, in the future, with a careful control of the experimental procedures. The detection limite is around 0.1 ppb [fr

  10. Testing sequential extraction methods for the analysis of multiple stable isotope systems from a bone sample

    Science.gov (United States)

    Sahlstedt, Elina; Arppe, Laura

    2017-04-01

    Stable isotope composition of bones, analysed either from the mineral phase (hydroxyapatite) or from the organic phase (mainly collagen) carry important climatological and ecological information and are therefore widely used in paleontological and archaeological research. For the analysis of the stable isotope compositions, both of the phases, hydroxyapatite and collagen, have their more or less well established separation and analytical techniques. Recent development in IRMS and wet chemical extraction methods have facilitated the analysis of very small bone fractions (500 μg or less starting material) for PO43-O isotope composition. However, the uniqueness and (pre-) historical value of each archaeological and paleontological finding lead to preciously little material available for stable isotope analyses, encouraging further development of microanalytical methods for the use of stable isotope analyses. Here we present the first results in developing extraction methods for combining collagen C- and N-isotope analyses to PO43-O-isotope analyses from a single bone sample fraction. We tested sequential extraction starting with dilute acid demineralization and collection of both collagen and PO43-fractions, followed by further purification step by H2O2 (PO43-fraction). First results show that bone sample separates as small as 2 mg may be analysed for their δ15N, δ13C and δ18OPO4 values. The method may be incorporated in detailed investigation of sequentially developing skeletal material such as teeth, potentially allowing for the investigation of interannual variability in climatological/environmental signals or investigation of the early life history of an individual.

  11. Sequential determination of important ecotoxic radionuclides in nuclear waste samples

    International Nuclear Information System (INIS)

    Bilohuscin, J.

    2016-01-01

    In the dissertation thesis we focused on the development and optimization of a sequential determination method for radionuclides 93 Zr, 94 Nb, 99 Tc and 126 Sn, employing extraction chromatography sorbents TEVA (R) Resin and Anion Exchange Resin, supplied by Eichrom Industries. Prior to the attestation of sequential separation of these proposed radionuclides from radioactive waste samples, a unique sequential procedure of 90 Sr, 239 Pu, 241 Am separation from urine matrices was tried, using molecular recognition sorbents of AnaLig (R) series and extraction chromatography sorbent DGA (R) Resin. On these experiments, four various sorbents were continually used for separation, including PreFilter Resin sorbent, which removes interfering organic materials present in raw urine. After the acquisition of positive results of this sequential procedure followed experiments with a 126 Sn separation using TEVA (R) Resin and Anion Exchange Resin sorbents. Radiochemical recoveries obtained from samples of radioactive evaporate concentrates and sludge showed high efficiency of the separation, while values of 126 Sn were under the minimum detectable activities MDA. Activity of 126 Sn was determined after ingrowth of daughter nuclide 126m Sb on HPGe gamma detector, with minimal contamination of gamma interfering radionuclides with decontamination factors (D f ) higher then 1400 for 60 Co and 47000 for 137 Cs. Based on the acquired experiments and results of these separation procedures, a complex method of sequential separation of 93 Zr, 94 Nb, 99 Tc and 126 Sn was proposed, which included optimization steps similar to those used in previous parts of the dissertation work. Application of the sequential separation method for sorbents TEVA (R) Resin and Anion Exchange Resin on real samples of radioactive wastes provided satisfactory results and an economical, time sparing, efficient method. (author)

  12. Spectral determination of thallium isotope composition

    International Nuclear Information System (INIS)

    Polyanskij, V.A.; Turkin, Yu.I.; Yakimova, N.M.

    1986-01-01

    The photoelectric non-standard method for determination of the thallium isotope composition is developed. The analysis is carried out by measuring the brightness of the Hfs components in the line Tl Iλ535.04 nm. The relative standard deviation of the results of the isotope analysis of thallium as metal is 0.02 and of thallium salts - 0.02-0.05

  13. Determination of natural uranium, thorium and radium isotopes in water and soil samples by alpha spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Hao, Le Cong; Tao, Chau Van; Thong, Luong Van; Linh, Duong Mong [University of Science Ho Chi Minh City (Viet Nam). Faculty of Physics and Engineering Physics; Dong, Nguyen Van [University of Science Ho Chi Minh City (Viet Nam). Faculty of Chemistry

    2011-08-15

    In this study, a simple procedure for the determination of natural uranium, thorium and radium isotopes in water and soil samples by alpha spectroscopy is described. This procedure allows a sequential extraction polonium, uranium, thorium and radium radionuclides from the same sample in two to three days. It was tested and validated with the analysis of certified reference materials from the IAEA. (orig.)

  14. Uranium isotopic determination by alpha spectroscopy

    International Nuclear Information System (INIS)

    Acena, M.; Garcoa-Torano, E.

    1979-01-01

    A method for alpha-spectrometry determinations of uranium isotopes, using surface barrier detectors, is described. This method is based in the shape similarity of the most intense line groups for the nuclides 234 U, 235 U, 236 U and 238 U. The method yields analytical results sufficiently accurate in samples with 235 U contents lower than 25% in atoms. (author)

  15. Velocities of antarctic outlet glaciers determined from sequential Landsat images

    Science.gov (United States)

    MacDonald, Thomas R.; Ferrigno, Jane G.; Williams, Richard S.; Lucchitta, Baerbel K.

    1989-01-01

    Approximately 91.0 percent of the volume of present-day glacier ice on Earth is in Antarctica; Greenland contains about another 8.3 percent of the volume. Thus, together, these two great ice sheets account for an estimated 99.3 percent of the total. Long-term changes in the volume of glacier ice on our planet are the result of global climate change. Because of the relationship of global ice volume to sea level (± 330 cubic kilometers of glacier ice equals ± 1 millimeter sea level), changes in the mass balance of the antarctic ice sheet are of particular importance.Whether the mass balance of the east and west antarctic ice sheets is positive or negative is not known. Estimates of mass input by total annual precipitation for the continent have been made from scattered meteorological observations (Swithinbank 1985). The magnitude of annual ablation of the ice sheet from calving of outlet glaciers and ice shelves is also not well known. Although the velocities of outlet glaciers can be determined from field measurements during the austral summer,the technique is costly, does not cover a complete annual cycle,and has been applied to just a few glaciers. To increase the number of outlet glaciers in Antarctica for which velocities have been determined and to provide additional data for under-standing the dynamics of the antarctic ice sheets and their response to global climate change, sequential Landsat image of several outlet glaciers were measured.

  16. Determination of uranium and plutonium by sequential potentiometric titration

    International Nuclear Information System (INIS)

    Kato, Yoshiharu; Takahashi, Masao

    1976-01-01

    The determination of uranium and plutonium in mixed oxide fuels has been developed by sequential potentiometric titration. A weighed sample of uranium and plutonium oxides is dissolved in a mixture of nitric and hydrofluoric acids and the solution is fumed with sulfuric acid. After the reduction of uranium and plutonium to uranium(IV) and plutonium(III) by chromium(II) sulfate, 5 ml of buffer solution (KCl-HCl, pH 1.0) is added to the solution. Then the solution is diluted to 30 ml with water and the pH of the solution is adjusted to 1.0 -- 1.5 with 1 M sodium hydroxide. The solution is stirred until the oxidation of the excess of chromium(II) by air is completed. After the removal of dissolved oxygen by bubbling nitrogen through the solution for 10 minutes, uranium (IV) is titrated with 0.1 N cerium(IV) sulfate. Then, plutonium is titrated by 0.02 N cerium(IV) sulfate. When a mixture of uranium and plutonium is titrated with 0.1 N potassium dichromate potentiometrically, the potential change at the end point of plutonium is very small and the end point of uranium is also unclear when 0.1 N potassium permanganate is used as a titrant. In the present method, nitrate, fluoride and copper(II) interfere with the determination of plutonium and uranium. Iron interferes quantitatively with the determination of plutonium but not of uranium. Results obtained in applying the proposed method to 50 mg of mixtures of plutonium and uranium ((7.5 -- 50))% Pu were accurate to within 0.15 mg of each element. (auth.)

  17. Sequential determination of actinides in a variety of matrices

    International Nuclear Information System (INIS)

    Olsen, S.C.

    2002-01-01

    A large number of analytical procedures for the actinides have been published, each catering for a specific need. Due to the bioassay programme in our laboratory, a need arose for a method to determine natural (Th and U) and anthropogenic actinides (Np, Pu and Am/Cm) together in a variety of samples. The method would have to be suitable for routine application: simple, inexpensive, rapid and robust. In some cases, the amount of material available is not sufficient for the determination of separate groups of actinides, and a sequential separation and measurement of the analytes would therefore be required. The types of matrices vary from aqueous samples to radiological surveillance (urine and faeces) to environmental studies (soil, sediment and fish), but the separation procedure should be able to service all of these. The working range of the method would have to cater for lower levels of the transuranium actinides in particular sample types containing higher levels of the natural actinides (U and Th). The first analytical problem to be discussed, is how to get the different sample types into the same loading solution required by a single separation approach. This entails sample dissolution or decomposition in some cases, and pre-concentration or pre-separation in others. A separation scheme is presented for the clean separation of all the actinides in a form suitable for alpha spectrometry. The development of a single column separation of the analytes of interest are looked at, as well as observations made during the development of the separation scheme, such as concentration effects. Results for test samples and certified reference materials are be presented. (author)

  18. Isotopic ratio method for determining uranium contamination

    International Nuclear Information System (INIS)

    Miles, R.E.; Sieben, A.K.

    1994-01-01

    The presence of high concentrations of uranium in the subsurface can be attributed either to contamination from uranium processing activities or to naturally occurring uranium. A mathematical method has been employed to evaluate the isotope ratios from subsurface soils at the Rocky Flats Nuclear Weapons Plant (RFP) and demonstrates conclusively that the soil contains uranium from a natural source and has not been contaminated with enriched uranium resulting from RFP releases. This paper describes the method used in this determination which has widespread application in site characterizations and can be adapted to other radioisotopes used in manufacturing industries. The determination of radioisotope source can lead to a reduction of the remediation effort

  19. What determines the impact of context on sequential action?

    NARCIS (Netherlands)

    Ruitenberg, M.F.L.; Verwey, Willem B.; Abrahamse, E.L.

    2015-01-01

    In the current study we build on earlier observations that memory-based sequential action is better in the original learning context than in other contexts. We examined whether changes in the perceptual context have differential impact across distinct processing phases (preparation versus execution

  20. An automatic system for acidity determination based on sequential injection titration and the monosegmented flow approach.

    Science.gov (United States)

    Kozak, Joanna; Wójtowicz, Marzena; Gawenda, Nadzieja; Kościelniak, Paweł

    2011-06-15

    An automatic sequential injection system, combining monosegmented flow analysis, sequential injection analysis and sequential injection titration is proposed for acidity determination. The system enables controllable sample dilution and generation of standards of required concentration in a monosegmented sequential injection manner, sequential injection titration of the prepared solutions, data collecting, and handling. It has been tested on spectrophotometric determination of acetic, citric and phosphoric acids with sodium hydroxide used as a titrant and phenolphthalein or thymolphthalein (in the case of phosphoric acid determination) as indicators. Accuracy better than |4.4|% (RE) and repeatability better than 2.9% (RSD) have been obtained. It has been applied to the determination of total acidity in vinegars and various soft drinks. The system provides low sample (less than 0.3 mL) consumption. On average, analysis of a sample takes several minutes. Copyright © 2011 Elsevier B.V. All rights reserved.

  1. Lead isotopes combined with a sequential extraction procedure for source apportionment in the dry deposition of Asian dust and non-Asian dust

    International Nuclear Information System (INIS)

    Lee, Pyeong-Koo; Yu, Soonyoung

    2016-01-01

    Lead isotopic compositions were determined in leachates that were generated using sequential extractions of dry deposition samples of Asian dust (AD) and non-Asian dust (NAD) and Chinese desert soils, and used to apportion Pb sources. Results showed significant differences in "2"0"6Pb/"2"0"7Pb and "2"0"6Pb/"2"0"4Pb isotopic compositions in non-residual fractions between the dry deposition samples and the Chinese desert soils while "2"0"6Pb/"2"0"7Pb and "2"0"6Pb/"2"0"4Pb isotopic compositions in residual fraction of the dry deposition of AD and NAD were similar to the mean "2"0"6Pb/"2"0"7Pb and "2"0"6Pb/"2"0"4Pb in residual fraction of the Alashan Plateau soil. These results indicate that the geogenic materials of the dry deposition of AD and NAD were largely influenced by the Alashan Plateau soil, while the secondary sources of the dry deposition were different from those of the Chinese desert soils. In particular, the lead isotopic compositions in non-residual fractions of the dry deposition were homogenous, which implies that the non-residual four fractions (F1 to F4) shared the primary anthropogenic origin. "2"0"6Pb/"2"0"7Pb values and the predominant wind directions in the study area suggested that airborne particulates of heavily industrialized Chinese cities were one of the main Pb sources. Source apportionment calculations showed that the average proportion of anthropogenic Pb in the dry deposition of AD and NAD was 87% and 95% respectively in total Pb extraction, 92% and 97% in non-residual fractions, 15% and 49% in residual fraction. Approximately 81% and 80% of the anthropogenic Pb was contributed by coal combustion in China in the dry deposition of AD and NAD respectively while the remainder was derived from industrial Pb contamination. The research result proposes that sequential extractions with Pb isotope analysis are a useful tool for the discrimination of anthropogenic and geogenic origins in highly contaminated AD and NAD. - Highlights:

  2. Development of sequential analytical method for the determination of U-238, U-234, Th-232, Th-230, Th-228, Ra-226 and Ra-228 and its application in mineral waters

    International Nuclear Information System (INIS)

    Costa Lauria, D. da.

    1986-01-01

    A sequential analytical method for the determination of U-238, U-234, Th-232, Th-230, Th-228, Ra-226 and Ra-228 in environmental samples and applied to the analysis of mineral waters is studied. Thorium isotopes are coprecipitated with lanthanium fluoride before counting in alpha spectrometer, the uranium isotopes are determined by alpha spectrometry following extraction with TOPO onto a polymenic membrane. Radium-226 is determined with the radom emanation technique. (M.J.C.) [pt

  3. Determination of uranium, thorium and radium isotope ratio

    International Nuclear Information System (INIS)

    Sokolova, Z.A.

    1983-01-01

    The problems connected with the study of isotope composition of natural radioactive elements in natural objects are considered. It is pointed out that for minerals, ores and rocks the following ratios are usually determined: 234 U/ 238 U, 230 Th/ 238 U, 226 Ra/ 238 U, 228 Th/ 230 Th, 228 Th/ 232 Th and lead isotopes; for natural waters, besides the enumerated - 226 Ra/ 228 Ra. General content of uranium and thorium in the course of isotope investigations is determined from separate samples, most frequently by the X-ray spectral method, radium content - by usual radiochemical method, uranium and radium content in waters -respectively by calorimetric and emanation methods. Radiochemical preparation of geologic powder and aqueous samples for isotope analysis is described in detail. The technique of measuring and calculating isotope ratios (α-spectrometry for determining isotope composition of uranium and thorium and emanation method for determining 226 Ra/ 228 Ra) is presented

  4. Application of TIMS in isotope correlations for determining the isotope ratios of plutonium

    International Nuclear Information System (INIS)

    Alamelu, D.; Aggarwal, S.K.

    2003-01-01

    Thermal ionisation mass spectrometry (TIMS) is a well-recognized technique for determining the isotopic composition of Pu in irradiated nuclear fuel samples. Other mass spectrometric methods such as ICPMS, SIMS can also be employed for the isotopic analysis of Pu. In the event of non-availability of a mass spectrometer, other techniques such as gamma spectrometry and alpha spectrometry can also be used. They have a limited applicability since data on all the Pu isotopes cannot be obtained

  5. Sequential injection spectrophotometric determination of V(V) in ...

    African Journals Online (AJOL)

    2009-01-15

    Jan 15, 2009 ... The determination was based on the oxidation of dopamine (DP) by V(V) in acidic medium followed by ... To overcome some of these drawbacks some flow injec- ..... The analytical signal increased with the reactor length.

  6. Changes in hydrogen isotope ratios in sequential plumage stages: an implication for the creation of isotope-base maps for tracking migratory birds.

    Science.gov (United States)

    Duxbury, J M; Holroyd, G L; Muehlenbachs, K

    2003-09-01

    Accurate reference maps are important in the use of stable-isotopes to track the movements of migratory birds. Reference maps created by the analysis of samples collected from young at the nest site are more accurate than simply referring to naturally occurring patterns of hydrogen isotope ratios created by precipitation cycles. Ratios of hydrogen isotopes in the nutrients incorporated early in the development of young birds can be derived from endogenous, maternal sources. Base-maps should be created with the analysis of tissue samples from hatchlings after local the isotopic signature of exogenous nutrients is dominant. Migratory species such as Peregrine Falcons are known to use endogenous sources in the creation of their eggs, therefore knowledge of what plumage stage best represents the local hydrogen ratios would assist in the planning of nest visits. We conducted diet manipulation experiments involving Japanese Quail and Peregrine Falcons to determine the plumage stage when hydrogen isotope ratios were indicative of a switch in their food source. The natal down of both the quail and falcons reflected the diet of breeding adult females. The hydrogen isotope ratios of a new food source were dominant in the juvenile down of the young falcons, although a further shift was detected in the final juvenile plumage. The juvenile plumage is grown during weeks 3-4 after hatch on Peregrine Falcons. Nest visits for the purpose of collecting feathers for isotope-base-map creation should be made around 4 weeks after the presumed hatch of the young falcons.

  7. Hot vacuum extraction-isotopic dilution mass spectrometry for determination of hydrogen isotopes in zircaloys

    International Nuclear Information System (INIS)

    Shi, Y.; Leeson, P.K.; Wilkin, D.; Britton, A.; Macleod, R.

    2016-01-01

    A hot vacuum extraction-isotope dilution mass spectrometry (HVE-IDMS) was studied for determination of hydrogen isotopes in zirconium metal and alloys as nuclear reactor materials. A theoretical assessment of the completeness of the extraction of hydrogen isotopes under the chosen condition was carried out based on the hydrogen and deuterium solubility data for zirconium. The optimal isotopic spiking condition for conventional IDMS was further explored for the special case IDMS where the isotope abundance of the samples is varied and non-natural. Applying the optimal conditions, the accurate IDMS determination was realized. The agreement between the measured values and the certified or prepared values of standard reference materials and homemade standard materials validate the method developed. (author)

  8. Evaluation of sequential images for photogrammetrically point determination

    Science.gov (United States)

    Kowalczyk, M.

    2011-12-01

    Close range photogrammetry encounters many problems with reconstruction of objects three-dimensional shape. Relative orientation parameters of taken photos makes usually key role leading to right solution of this problem. Automation of technology process is hardly performed due to recorded scene complexity and configuration of camera positions. This configuration makes the process of joining photos into one set usually impossible automatically. Application of camcorder is the solution widely proposed in literature for support in 3D models creation. Main advantages of this tool are connected with large number of recorded images and camera positions. Exterior orientation changes barely between two neighboring frames. Those features of film sequence gives possibilities for creating models with basic algorithms, working faster and more robust, than with remotely taken photos. The first part of this paper presents results of experiments determining interior orientation parameters of some sets of frames, presenting three-dimensional test field. This section describes calibration repeatability of film frames taken from camcorder. It is important due to stability of interior camera geometric parameters. Parametric model of systematical errors was applied for correcting images. Afterwards a short film of the same test field had been taken for determination of check points group. This part has been done for controlling purposes of camera application in measurement tasks. Finally there are presented some results of experiments which compare determination of recorded object points in 3D space. In common digital photogrammetry, where separate photos are used, first levels of image pyramids are taken to connect with feature based matching. This complicated process creates a lot of emergencies, which can produce false detections of image similarities. In case of digital film camera, authors of publications avoid this dangerous step, going straightly to area based matching, aiming

  9. New sequential separation procedure for Sr, Nd and Pb isotope ratio measurement in geological material using MC-ICP-MS and TIMS

    Digital Repository Service at National Institute of Oceanography (India)

    Makishima, A.; Nath, B.N.; Nakamura, E.

    A new 3-step sequential separation chemistry for Sr, Nd and Pb from silicate samples, which is suitable for isotope analysis by MC-ICP-MS as well as TIMS, has been developed. The chemistry is designed to minimize the number of evaporation steps...

  10. Bootstrap Sequential Determination of the Co-integration Rank in VAR Models

    DEFF Research Database (Denmark)

    Guiseppe, Cavaliere; Rahbæk, Anders; Taylor, A.M. Robert

    with empirical rejection frequencies often very much in excess of the nominal level. As a consequence, bootstrap versions of these tests have been developed. To be useful, however, sequential procedures for determining the co-integrating rank based on these bootstrap tests need to be consistent, in the sense...... in the literature by proposing a bootstrap sequential algorithm which we demonstrate delivers consistent cointegration rank estimation for general I(1) processes. Finite sample Monte Carlo simulations show the proposed procedure performs well in practice....

  11. Isotope determination of sulfur by mass spectrometry in soil samples

    Directory of Open Access Journals (Sweden)

    Alexssandra Luiza Rodrigues Molina Rossete

    2012-12-01

    Full Text Available Sulphur plays an essential role in plants and is one of the main nutrients in several metabolic processes. It has four stable isotopes (32S, 33S, 34S, and 36S with a natural abundance of 95.00, 0.76, 4.22, and 0.014 in atom %, respectively. A method for isotopic determination of S by isotope-ratio mass spectrometry (IRMS in soil samples is proposed. The procedure involves the oxidation of organic S to sulphate (S-SO4(2-, which was determined by dry combustion with alkaline oxidizing agents. The total S-SO4(2- concentration was determined by turbidimetry and the results showed that the conversion process was adequate. To produce gaseous SO2 gas, BaSO4 was thermally decomposed in a vacuum system at 900 ºC in the presence of NaPO3. The isotope determination of S (atom % 34S atoms was carried out by isotope ratio mass spectrometry (IRMS. In this work, the labeled material (K2(34SO4 was used to validate the method of isotopic determination of S; the results were precise and accurate, showing the viability of the proposed method.

  12. Determination of marble provenance: limits of isotopic analysis

    International Nuclear Information System (INIS)

    Germann, K.; Holzmann, G.; Winkler, F.J.

    1980-01-01

    Provenance determination of Thessalian stelae marbles using the C/O isotopic analysis proved to be misleading, as the isotopic composition even in very small quarrying areas is heterogeneous and isotopic coincidence of marbles from very distant sources occurs. Therefore additional geological features must be taken into consideration and preference should be given to combinations of both petrographical and geochemical properties. Geological field work to establish the range of possible marble sources and the variability within these sources is one of the prerequisites of provenance studies. (author)

  13. Comparison of ERBS orbit determination accuracy using batch least-squares and sequential methods

    Science.gov (United States)

    Oza, D. H.; Jones, T. L.; Fabien, S. M.; Mistretta, G. D.; Hart, R. C.; Doll, C. E.

    1991-01-01

    The Flight Dynamics Div. (FDD) at NASA-Goddard commissioned a study to develop the Real Time Orbit Determination/Enhanced (RTOD/E) system as a prototype system for sequential orbit determination of spacecraft on a DOS based personal computer (PC). An overview is presented of RTOD/E capabilities and the results are presented of a study to compare the orbit determination accuracy for a Tracking and Data Relay Satellite System (TDRSS) user spacecraft obtained using RTOS/E on a PC with the accuracy of an established batch least squares system, the Goddard Trajectory Determination System (GTDS), operating on a mainframe computer. RTOD/E was used to perform sequential orbit determination for the Earth Radiation Budget Satellite (ERBS), and the Goddard Trajectory Determination System (GTDS) was used to perform the batch least squares orbit determination. The estimated ERBS ephemerides were obtained for the Aug. 16 to 22, 1989, timeframe, during which intensive TDRSS tracking data for ERBS were available. Independent assessments were made to examine the consistencies of results obtained by the batch and sequential methods. Comparisons were made between the forward filtered RTOD/E orbit solutions and definitive GTDS orbit solutions for ERBS; the solution differences were less than 40 meters after the filter had reached steady state.

  14. Comparison of ERBS orbit determination accuracy using batch least-squares and sequential methods

    Science.gov (United States)

    Oza, D. H.; Jones, T. L.; Fabien, S. M.; Mistretta, G. D.; Hart, R. C.; Doll, C. E.

    1991-10-01

    The Flight Dynamics Div. (FDD) at NASA-Goddard commissioned a study to develop the Real Time Orbit Determination/Enhanced (RTOD/E) system as a prototype system for sequential orbit determination of spacecraft on a DOS based personal computer (PC). An overview is presented of RTOD/E capabilities and the results are presented of a study to compare the orbit determination accuracy for a Tracking and Data Relay Satellite System (TDRSS) user spacecraft obtained using RTOS/E on a PC with the accuracy of an established batch least squares system, the Goddard Trajectory Determination System (GTDS), operating on a mainframe computer. RTOD/E was used to perform sequential orbit determination for the Earth Radiation Budget Satellite (ERBS), and the Goddard Trajectory Determination System (GTDS) was used to perform the batch least squares orbit determination. The estimated ERBS ephemerides were obtained for the Aug. 16 to 22, 1989, timeframe, during which intensive TDRSS tracking data for ERBS were available. Independent assessments were made to examine the consistencies of results obtained by the batch and sequential methods. Comparisons were made between the forward filtered RTOD/E orbit solutions and definitive GTDS orbit solutions for ERBS; the solution differences were less than 40 meters after the filter had reached steady state.

  15. Determination of hydrogen isotope composition in organic compounds

    International Nuclear Information System (INIS)

    Ordzhonikidze, K.G.; Parulava, L.P.; Vakhaniya, G.V.; Tarielashvili, V.O.

    1989-01-01

    method for determination of hydrogen isotope composition just in organic compounds using mass-spectrometer of the second class is suggested. The method enables to determine atomic fraction of hydrogen without multiplet separation. The accuracy of determination of deuterium atomic fraction in acetone in 1-99% range was equal to 3-0.2% respectively

  16. Determination of zinc stable isotopes in biological materials using isotope dilution inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Patterson, K.Y.; Veillon, Claude

    1992-01-01

    A method is described for using isotope dilution to determine both the amount of natural zinc and enriched isotopes of zinc in biological samples. Isotope dilution inductively coupled plasma mass spectrometry offers a way to quantify not only the natural zinc found in a sample but also the enriched isotope tracers of zinc. Accurate values for the enriched isotopes and natural zinc are obtained by adjusting the mass count rate data for measurable instrumental biases. Analytical interferences from the matrix are avoided by extracting the zinc from the sample matrix using diethylammonium diethyldithiocarbamate. The extraction technique separates the zinc from elements which form interfering molecular ions at the same nominal masses as the zinc isotopes. Accuracy of the method is verified using standard reference materials. The detection limit is 0.06 μg Zn per sample. Precision of the abundance ratios range from 0.3-0.8%. R.S.D. for natural zinc concentrations is about 200-600 μg g -1 . The accuracy and precision of the measurements make it possible to follow enriched isotopic tracers of zinc in biological samples in metabolic tracer studies. (author). 19 refs.; 1 fig., 4 tabs

  17. Determination of uranium isotopes in urine

    International Nuclear Information System (INIS)

    Lellis, I.R.; Silva, D.V.F.M. Rey; Taddei, M.H.T.

    2017-01-01

    Variable concentrations of uranium occur naturally in waters, plant products and soils. Small amounts of this element are routinely incorporated by man. Occupationally exposed individuals (IOEs) are subject to the incorporation of higher amounts of uranium into their work routines. The effects on human health resulting from the incorporation of uranium in environmental doses are not very well established and are currently recognized as of little relevance. The incorporation resulting from occupational activities, where higher doses can be found, represents a health risk resulting from chemical damages to the kidneys. Considering that uranium is eliminated from the human body through urine and feces, and that the concentration in the urine can be obtained by means of radiochemical analyzes, this can be considered an efficient indirect method to verify the incorporation of this element. In the work the isotopes of 234 U, 235 U and 238 U were analyzed in urine samples of IOEs and the rate of uranium present in them was verified

  18. Semiempirical method to determine the uranium isotopic compositions

    International Nuclear Information System (INIS)

    Tegas Sutondo

    2008-01-01

    In a nuclear reactor design calculation, some variations of U 235 enrichment are commonly needed. This will affect the isotopic compositions of the 3 main uranium isotopes i.e. U 234 , U 235 and U 238 for the respective enrichment. Due to the limited compositions data available, it is urgent to make an approximate way that can be used to determine the compositions of the 3 isotopes, for the desired enrichments. This paper presents the theoretical background used for constructing a semi empirical formula to estimate the composition of the 3 uranium isotopes as a function of U 235 enrichment, obtained based on the measurement data available. Based on the available data, and the lack of compositions data within the enrichment range between 3.5 % and around 12 %, it is concluded that 2 separate linear equations i.e. for ≤ 3.5 % and ≥ 3.5 % might be needed for U 235 isotope. For the U 234 isotope, a polynomial equation of 4 th order is well suited to be used for the whole range of enrichment between 0.711 % and 20 %, whilst for higher enrichment (> 20 %), a power function seems to give a better approach. The composition of U 238 can then be determined from the U 235 and U 234 composition at the desired enrichment of U 235 . (author)

  19. Electrochemical separation and isotopic determination of thallium at the nanogram level by surface ionisation mass spectrometry

    International Nuclear Information System (INIS)

    Arden, J.W.

    1983-01-01

    A rapid low-blank procedure is described for the co-separation of thallium and lead by sequential cathodic and anodic electrodeposition from natural samples, especially complex natural silicates, for subsequent mass spectrometry. A micro anion-exchange procedure is also described for the separation of thallium and lead. Ion currents of 10 - 10 A can be obtained from 1 ng of thallium. The isotopic composition of 1 ng of thallium can be measured on a Faraday detector with a precision of 0.05-0.1%. The total procedural blank is 3 pg. By using stable isotope dilution, 0.2 ng of thallium can be measured with a precision of 0.6% with only a 2% blank correction. This allows the accurate determination of thallium in natural samples down to concentration levels of about 50 pg g - 1 . The detection limit is 50 fg. This procedure has been applied to meteorites and terrestrial rocks. The stable isotope dilution technique is suitable for geochemical, environmental and toxicological studies requiring a highly sensitive, accurate and precise method for the determination of thallium. (Auth.)

  20. An on-line potentiometric sequential injection titration process analyser for the determination of acetic acid.

    Science.gov (United States)

    van Staden, J F; Mashamba, Mulalo G; Stefan, Raluca I

    2002-09-01

    An on-line potentiometric sequential injection titration process analyser for the determination of acetic acid is proposed. A solution of 0.1 mol L(-1) sodium chloride is used as carrier. Titration is achieved by aspirating acetic acid samples between two strong base-zone volumes into a holding coil and by channelling the stack of well-defined zones with flow reversal through a reaction coil to a potentiometric sensor where the peak widths were measured. A linear relationship between peak width and logarithm of the acid concentration was obtained in the range 1-9 g/100 mL. Vinegar samples were analysed without any sample pre-treatment. The method has a relative standard deviation of 0.4% with a sample frequency of 28 samples per hour. The results revealed good agreement between the proposed sequential injection and an automated batch titration method.

  1. Sequential extraction procedure for determination of uranium, thorium, radium, lead and polonium radionuclides by alpha spectrometry in environmental samples

    Science.gov (United States)

    Oliveira, J. M.; Carvalho, F. P.

    2006-01-01

    A sequential extraction technique was developed and tested for common naturally-occurring radionuclides. This technique allows the extraction and purification of uranium, thorium, radium, lead, and polonium radionuclides from the same sample. Environmental materials such as water, soil, and biological samples can be analyzed for those radionuclides without matrix interferences in the quality of radioelement purification and in the radiochemical yield. The use of isotopic tracers (232U, 229Th, 224Ra, 209Po, and stable lead carrier) added to the sample in the beginning of the chemical procedure, enables an accurate control of the radiochemical yield for each radioelement. The ion extraction procedure, applied after either complete dissolution of the solid sample with mineral acids or co-precipitation of dissolved radionuclide with MnO2 for aqueous samples, includes the use of commercially available pre-packed columns from Eichrom® and ion exchange columns packed with Bio-Rad resins, in altogether three chromatography columns. All radioactive elements but one are purified and electroplated on stainless steel discs. Polonium is spontaneously plated on a silver disc. The discs are measured using high resolution silicon surface barrier detectors. 210Pb, a beta emitter, can be measured either through the beta emission of 210Bi, or stored for a few months and determined by alpha spectrometry through the in-growth of 210Po. This sequential extraction chromatography technique was tested and validated with the analysis of certified reference materials from the IAEA. Reproducibility was tested through repeated analysis of the same homogeneous material (water sample).

  2. Sequential Injection Determination of D-Glucose by Chemiluminescence Using an Open Tubular Immobilised Enzyme Reactor

    DEFF Research Database (Denmark)

    Liu, Xuezhu; Hansen, Elo Harald

    1996-01-01

    A sequential injection analysis system is described that incorporates a nylon tubular reactor containing immobilised glucose oxidase, allowing determination of D-glucose by means of subsequent luminol chemiluminescence detection of the hydrogen peroxide generated in the enzymatic reaction....... The operating parameters were optimised by fractional factorial screening and response surface modelling. The linear range of D-glucose determination was 30-600 mu M, With a detection limit of 15 mu M using a photodiode detector. The sampling frequency was 54 h(-1). Lower LOD (0.5 mu M D-glucose) could...

  3. Determination of photooxygenation products of rotenone with isotope dilution method

    International Nuclear Information System (INIS)

    Chubachi, Mitsuo; Hamada, Masayuki

    1975-01-01

    When rotenone dissolved in certain solvent was photochemically oxidized, rotenolones, dehydrorotenone and rotenonone were obtained as main products. In order to determine the quantitative yields of these compounds in photooxygenation products, four compounds mentioned above were labeled with carbon-14 and the isotope dilution method by these labeled compounds was applied to the product analysis. (auth.)

  4. Simultaneous determination of two active components of pharmaceutical preparations by sequential injection method using heteropoly complexes

    Directory of Open Access Journals (Sweden)

    Mohammed Khair E. A. Al-Shwaiyat

    2014-12-01

    Full Text Available New approach has been proposed for the simultaneous determination of two reducing agents based on the dependence of their reaction rate with 18-molybdo-2-phosphate heteropoly complex on pH. The method was automated using the manifold typical for the sequential analysis method. Ascorbic acid and rutin were determined by successive injection of two samples acidified to different pH. The linear range for rutin determination was 0.6-20 mg/L and the detection limit was 0.2 mg/L (l = 1 cm. The determination of rutin was possible in the presence of up to a 20-fold excess of ascorbic acid. The method was successfully applied to the determination of ascorbic acid and rutin in ascorutin tablets. The applicability of the proposed method for the determination of total polyphenol content in natural plant samples was shown.

  5. Applications of stable Isotope ratios determinations in fruit juice authentication

    International Nuclear Information System (INIS)

    Magdas, Dana Alina; Dehelean, Adriana; Voica, Cezara; Puscas, Romulus

    2010-01-01

    Full text: Adulteration of a product consists in making it impure by fraudulent addition of a foreign or inferior substance. The result is either an alteration of the product and of its quality or a falsification. The falsification is a voluntary act with the intention of abuse. The falsification may be more or less sophisticated and its sophistication as well as its costs increases with the improvement of analytical methods. Vacuum concentration with aroma does not affect the chemical composition of fruit juices and therefore the determination of deuterium (D) and oxygen-18 content in waters is the most confident procedure for differentiating between a natural single strength juice and a juice rediluted from a concentrate. This technique is based on the fact that when absorbed by a plant, the rainwater or the irrigation water is fractionated by evapotranspiration, and enriched in the heavy isotopes (deuterium and oxygen-18) with respect to the light isotope (hydrogen and oxygen-16, respectively). It is known that climatic conditions affect the isotope content of rain waters and therefore that of fruit juices waters: the warmer climate, the higher the deuterium and oxygen-18 contents in water. Rainwater and tap water have nearly the same isotopic content and the water of fruit juices derived from concentrate by dilution with tap water has an isotopic content close to that of tap water. This makes it easy to distinguish diluted concentrates from the isotopically more enriched water of authentic single strength juice. In this study, single strength juice, in Romanian fruits, were investigated by mean of stable isotope measurements (oxygen, hydrogen and carbon) in order to offer a discussion basis for the authenticity of some fruit juices currently available on Romanian market. (authors)

  6. Sulfur isotope in nature. Determination of sulfur isotope ratios in coal and petroleum by mass spectrometry

    International Nuclear Information System (INIS)

    Derda, M.

    1999-01-01

    Elementary sulfur or in chemical compounds is one of the elements widespread in the earth's crust and biosphere. Its participation in earth's crust amounts to 0.26 % by weight. Measurement of isotope composition of natural samples can deliver many information about origin, creation and transformation ranges of rocks and minerals. Sulfur isotope ratio contained in minerals is variable and for this reason investigation of isotope sulfur composition can deliver useful information about the geochemistry of each component. Therefore in the investigated sample it is necessary to determine not only the content of sulfur but also the isotope composition of each component. Differentiation of contents of sulfur-34 in natural sulfur compounds can reach up to 110 per mile. So large divergences can be explained by a kinetic effect or by bacterial reduction of sulphates. In this report a wide review of the results of investigations of isotope sulfur compositions in coal and petroleum are presented as well as the methods for the preparation of samples for mass spectrometry analysis are proposed. (author)

  7. Can standard sequential extraction determinations effectively define heavy metal species in superfund site soils?

    Energy Technology Data Exchange (ETDEWEB)

    Dahlin, Cheryl L.; Williamson, Connie A.; Collins, Wesley K.; Dahlin, David C.

    2001-01-01

    Speciation and distribution of heavy metals in soils controls the degree to which metals and their compounds are mobile, extractable, and plant-available. Consequently, speciation impacts the success of remediation efforts both by defining the relationship of the contaminants with their environment and by guiding development and evaluation of workable remediation strategies. The U.S. Department of Energy, Albany Research Center (Albany, OR), under a two-year interagency project with the U.S. Environmental Protection Agency (EPA), examined the suitability of sequential extraction as a definitive means to determine species of heavy metals in soil samples. Representative soil samples, contaminated with lead, arsenic, and/or chromium, were collected by EPA personnel from two Superfund sites, the National Lead Company site in Pedricktown, NJ, and the Roebling Steel, Inc., site in Florence, NJ. Data derived from Tessier=s standard three-stage sequential-extraction procedure were compared to data from a comprehensive characterization study that combined optical- and scanning-electron microscopy (with energy-dispersive x-ray and wavelength-dispersive x-ray analyses), x-ray diffraction, and chemical analyses. The results show that standard sequential-extraction procedures that were developed for characterizing species of contaminants in river sediments may be unsuitable for sole evaluation of contaminant species in industrial-site materials (particularly those that contain larger particles of the contaminants, encapsulated contaminants, and/or man-made materials such as slags, metals, and plastics). However, each sequential extraction or comprehensive characterization procedure has it=s own strengths and weaknesses. Findings of this study indicate that the use of both approaches, during the early stages of site studies, would be a best practice. The investigation also highlights the fact that an effective speciation study does not simply identify metal contaminants as

  8. Plutonium isotopic determination from gamma-ray spectra

    International Nuclear Information System (INIS)

    Skourikhine, A.N.; Strittmatter, R.B.; Zardecki, A.

    1998-01-01

    The use of low- and medium-resolution room-temperature detectors for the nondestructive assay of nuclear materials has widespread applications to the safeguarding of nuclear materials. The challenge to using these detectors is the inherent difficulty of the spectral analysis to determine the amount of specific nuclear materials in the measured samples. This is especially true for extracting plutonium isotopic content from low- and medium-resolution spectral lines that are not well resolved. In this paper, neural networks trained by stochastic and singular value decomposition algorithms are applied to retrieve the plutonium isotopic content from a simulated NaI spectra. The simulated sample consists of isotopes 238 Pu, 239 Pu, 240 Pu, 241 Pu, 242 Pu, and 241 Am. It is demonstrated that the neutral network optimized by singular value decomposition (SVD) and stochastic training algorithms is capable of estimating plutonium content consistently resulting in an average error much smaller than the error previously reported

  9. Determination of traces of phosphorus using isotope exchange

    International Nuclear Information System (INIS)

    Zeman, A.; Kratzer, K.

    1976-01-01

    A simple and selective radioanalytical method for the determination of phosphorus (0.015 - 5 μg in a 5 ml sample), based on the heterogeneous isotope exchange, has been developed. The sample containing phosphorus is shaken in the presence of molybdate with a standard solution of tetraphenylarsonium molybdophosphate labelled with phosphorus-32 in 1-2 dicloroethan. From the distribution of the activity between the aqueous and organic phases the amount of phosphorus in the sample can be determined. (Authors)

  10. Determination of microquantities of silver in platinum by isotope dilution

    International Nuclear Information System (INIS)

    Yedinakova, V.; Sladkovska, Y.

    1980-01-01

    A method is described for determining microquantities of silver in platinum. It is based on isotope dilution by means of substoichiometric extraction of dithizonates with carbon tetrachloride. The determination of silver according to this technique is not interfered by zinc or gold in quantities exceeding the silver content by one order of magnitude nor by a great excess of platinum. In the presence of copper the addition of complexon is necessary. (author)

  11. Facile Determination of Sodium Ion and Osmolarity in Artificial Tears by Sequential DNAzymes.

    Science.gov (United States)

    Kim, Eun Hye; Lee, Eun-Song; Lee, Dong Yun; Kim, Young-Pil

    2017-12-07

    Despite high relevance of tear osmolarity and eye abnormality, numerous methods for detecting tear osmolarity rely upon expensive osmometers. We report a reliable method for simply determining sodium ion-based osmolarity in artificial tears using sequential DNAzymes. When sodium ion-specific DNAzyme and peroxidase-like DNAzyme were used as a sensing and detecting probe, respectively, the concentration of Na⁺ in artificial tears could be measured by absorbance or fluorescence intensity, which was highly correlated with osmolarity over the diagnostic range ( R ² > 0.98). Our approach is useful for studying eye diseases in relation to osmolarity.

  12. Sequential potentiometric determination of uranium and plutonium in a single aliquot

    International Nuclear Information System (INIS)

    Rao, V.K.; Charyulu, M.M.; Natarajan, P.R.

    1983-01-01

    A method is reported for sequential potentiometric determination of uranium and plutonium present is an aliquot. Plutonium is first determined by oxidizing it to the hexavalent state with perchloric acid followed by iron(II) reduction and titration of excess ferrous iron with chromium(VI). Uranium is subsequently determined by reduction to the quadrivalent state using titanium(III) and titration with vanadium(V). The interference of plutonium and iron(II) is eliminated by the addition of a mixture containing sulfamic acid, nitric acid, and molybdenum(VI). The results of the analysis of mixture containing 3-5 mg quantities of uranium and plutonium are reliable with errors less than 0.3% and 0.2%, respectively. The application of the method for the analysis of mixtures containing various amounts of uranium and plutonium has been examined. (author)

  13. Exploiting an automated microfluidic hydrodynamic sequential injection system for determination of phosphate.

    Science.gov (United States)

    Khongpet, Wanpen; Pencharee, Somkid; Puangpila, Chanida; Kradtap Hartwell, Supaporn; Lapanantnoppakhun, Somchai; Jakmunee, Jaroon

    2018-01-15

    A microfluidic hydrodynamic sequential injection (μHSI) spectrophotometric system was designed and fabricated. The system was built by laser engraving a manifold pattern on an acrylic block and sealing with another flat acrylic plate to form a microfluidic channel platform. The platform was incorporated with small solenoid valves to obtain a portable setup for programmable control of the liquid flow into the channel according to the HSI principle. The system was demonstrated for the determination of phosphate using a molybdenum blue method. An ascorbic acid, standard or sample, and acidic molybdate solutions were sequentially aspirated to fill the channel forming a stack zone before flowing to the detector. Under the optimum condition, a linear calibration graph in the range of 0.1-6mg P L -1 was obtained. The detection limit was 0.1mgL -1 . The system is compact (5.0mm thick, 80mm wide × 140mm long), durable, portable, cost-effective, and consumes little amount of chemicals (83μL each of molybdate and ascorbic acid, 133μL of the sample solution and 1.7mL of water carrier/run). It was applied for the determination of phosphate content in extracted soil samples. The percent recoveries of the analysis were obtained in the range of 91.2-107.3. The results obtained agreed well with those of the batch spectrophotometric method. Copyright © 2017 Elsevier B.V. All rights reserved.

  14. Acetone and acetaldehyde determination in tomato juice by isotopic dilution

    International Nuclear Information System (INIS)

    Piva, M.-T.; Crouzet, J.

    1977-01-01

    Acetone and acetaldehyde content of tomato juice were determined by isotope dilution techniques. The juice is added to 14 C labelled compounds, carried along by nitrogen at low pressure. The mixture of 2.4 dinitrophenylhydrazones obtained from volatile compounds is separated by thin layer chromatography on silica gel and then on alumina. A determination of radioactivity and concentration of acetone and acetaldehyde 2,4 dinitrophenylhydrazones obtained after separation and elution allow to calculate the content of these two compounds in the initial product with the same sample. This technique could be used for determination of methanol and ethanol after transformation in 3,5 dinitrobenzoates [fr

  15. PIDIE, plutonium isotopic determination inter-comparison exercise

    International Nuclear Information System (INIS)

    Harry, R.J.S.

    1990-07-01

    PIDIE (Plutonium Isotopic Determination Inter-comparison Exercise) is one of the projects of the ESARDA Working Group on Techniques and Standards for Non-Destructive Analysis. PIDIE is placed against the historical background of the general development of international standards. Its results are also reviewed in the light of the original purpose of the project. Sets of seven sealed Pu samples of different isotopic composition, each containing 0,45 grammes, were sent to the 9 participating laboratories for three separate determinations of the unknown isotopic composition, to investigate error sources and , if possible to improve the knowledge of γ-emission probabilities. An additional question was to examine the possible improvement of such measurements using reference samples. No important bias has been observed in the results of this inter-comparison. The apparent improvement in the precision and accuracy of the result seems to arise from both better equipment and more elaborate spectrum evaluation methods. (author). 39 refs.; 1 fig.; 5 tabs

  16. Simultaneous determination of U and Pu isotopes by alpha spectrometry

    International Nuclear Information System (INIS)

    Equillor, H.E.; Campos, J.M.

    2011-01-01

    Determination of actinides by alpha spectrometry is usually carried out after full separation of each of the components of the sample. The procedure presented in this paper permits U and Pu isotopes to be measured together allowing faster sample processing and measurement. The method consists in the extraction with tributyl phosphate of U and Pu isotopes from the rest of the matrix, followed by a cathodic electrodeposition to obtain alpha spectrometry suitable pieces. It can be applied to various environmental samples, such as water, filters and soil (about 0.5 g of solid sample for the described conditions). High-quality electroplated discs are essential for simultaneous processing, so a technique to achieve this requirement is also explained. (authors) [es

  17. Simultaneous determination of rutin and ascorbic acid in a sequential injection lab-at-valve system.

    Science.gov (United States)

    Al-Shwaiyat, Mohammed Khair E A; Miekh, Yuliia V; Denisenko, Tatyana A; Vishnikin, Andriy B; Andruch, Vasil; Bazel, Yaroslav R

    2018-02-05

    A green, simple, accurate and highly sensitive sequential injection lab-at-valve procedure has been developed for the simultaneous determination of ascorbic acid (Asc) and rutin using 18-molybdo-2-phosphate Wells-Dawson heteropoly anion (18-MPA). The method is based on the dependence of the reaction rate between 18-MPA and reducing agents on the solution pH. Only Asc is capable of interacting with 18-MPA at pH 4.7, while at pH 7.4 the reaction with both Asc and rutin proceeds simultaneously. In order to improve the precision and sensitivity of the analysis, to minimize reagent consumption and to remove the Schlieren effect, the manifold for the sequential injection analysis was supplemented with external reaction chamber, and the reaction mixture was segmented. By the reduction of 18-MPA with reducing agents one- and two-electron heteropoly blues are formed. The fraction of one-electron heteropoly blue increases at low concentrations of the reducer. Measurement of the absorbance at a wavelength corresponding to the isobestic point allows strictly linear calibration graphs to be obtained. The calibration curves were linear in the concentration ranges of 0.3-24mgL -1 and 0.2-14mgL -1 with detection limits of 0.13mgL -1 and 0.09mgL -1 for rutin and Asc, respectively. The determination of rutin was possible in the presence of up to a 20-fold molar excess of Asc. The method was applied to the determination of Asc and rutin in ascorutin tablets with acceptable accuracy and precision (1-2%). Copyright © 2017 Elsevier B.V. All rights reserved.

  18. Stable carbon isotopic composition of gasolines determined by isotope ratio monitoring gas chromatography mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Smallwood, B.J.; Philp, R.P.; Allen, J.D. [University of Oklahoma, Norman, OK (United States). School of Geology and Geophysics

    2002-07-01

    A large number of underground gasoline storage facilities in the United States continuously leak gasoline into the subsurface, which makes gasoline a major groundwater contaminant. Gas chromatography (GC) and gas chromatography-mass spectrometry (GC-MS) are used currently to characterize contaminated groundwater and soils. Correlations of contaminants with suspected source(s) are extremely difficult by these techniques because many gasolines have similar hydrocarbon distributions. The present study applied the technique of isotope ratio monitoring gas chromatography-mass spectrometry (irmGC-MS) to 19 gasoline samples from different areas of the USA. This allows a much better correlation of gasoline contaminants to source. Data obtained indicate a wide range of {sup {delta}}{sup 13}C values for 16 ubiquitous compounds in the gasolines. The majority of samples could be distinguished from each other on the basis of {sup {delta}}{sup 13}C hydrocarbon composition. The oxygenated additive methyl tertiary butyl ether (MTBE) was present in ten of the gasolines analyzed, and had a relatively narrow range of {sup {delta}}{sup 13}C values (-30.4 to -28.3 per mille). Preliminary investigations were also made to determine the extent of carbon isotopic fractionation after simple water washing and evaporation experiments. Results indicate that the majority of compounds did not undergo significant carbon isotopic fractionation as a result of these processes. (author)

  19. Determination and partitioning of metals in sediments along the Suez Canal by sequential extraction

    Science.gov (United States)

    Abd El-Azim, H.; El-Moselhy, Kh. M.

    2005-06-01

    The application of sequential extraction technique was used to determine the chemical association of heavy metals in five different chemical phases (exchangeable F1, bound to carbonate F2, bound to Fe-Mn oxides F3, bound to organic matter F4 and residual F5) for sediment samples collected from the Suez Canal. From the obtained data, it can be seen that the surplus of metal contaminants introduced into the sediment from sources usually exists in relatively unstable chemical forms. A high proportion of the studied metals remained in the residual fraction. Most of remaining portion of metals was bound to ferromanganese oxides fraction. The low concentrations of metals in the exchangeable fraction indicated that the sediments of Suez Canal were relatively unpolluted.

  20. Comparative determination of sucrose content in sugar beet by polarimetric and isotope dilution methods

    Energy Technology Data Exchange (ETDEWEB)

    Malec, K; Szuchnik, A [Institute of Nuclear Research, Warsaw (Poland); Rydel, S; Walerianaczyk, E [Instytut Przemyslu Cukrowniczego, Warsaw (Poland)

    1976-01-01

    The comparative determination of sucrose content in sugar beets has been investigated by following methods: polarimetric, direct isotope dilution and double carrier-isotope dilution analysis. Basing upon the obtained results it has been ascertained, that in the case of worse quality beets the polarimetric determinations differ greatly from isotopic data.

  1. The fractioning factor and the number of theorical plates in isotopic enrichment columns determined simultaneously

    International Nuclear Information System (INIS)

    Ducatti, Carlos

    1997-01-01

    Using an analytical approach and an analytical graphical method, it was determined simultaneously the fractioning factor and the number of theoretical plates in isotopic enrichment columns during the conditions of dinamical isotopic equilibrium. (author). 5 refs., 2 figs., 2 tabs

  2. Sequential injection redox or acid-base titration for determination of ascorbic acid or acetic acid.

    Science.gov (United States)

    Lenghor, Narong; Jakmunee, Jaroon; Vilen, Michael; Sara, Rolf; Christian, Gary D; Grudpan, Kate

    2002-12-06

    Two sequential injection titration systems with spectrophotometric detection have been developed. The first system for determination of ascorbic acid was based on redox reaction between ascorbic acid and permanganate in an acidic medium and lead to a decrease in color intensity of permanganate, monitored at 525 nm. A linear dependence of peak area obtained with ascorbic acid concentration up to 1200 mg l(-1) was achieved. The relative standard deviation for 11 replicate determinations of 400 mg l(-1) ascorbic acid was 2.9%. The second system, for acetic acid determination, was based on acid-base titration of acetic acid with sodium hydroxide using phenolphthalein as an indicator. The decrease in color intensity of the indicator was proportional to the acid content. A linear calibration graph in the range of 2-8% w v(-1) of acetic acid with a relative standard deviation of 4.8% (5.0% w v(-1) acetic acid, n=11) was obtained. Sample throughputs of 60 h(-1) were achieved for both systems. The systems were successfully applied for the assays of ascorbic acid in vitamin C tablets and acetic acid content in vinegars, respectively.

  3. Visual detection and sequential injection determination of aluminium using a cinnamoyl derivative.

    Science.gov (United States)

    Elečková, Lenka; Alexovič, Michal; Kuchár, Juraj; Balogh, Ioseph S; Andruch, Vasil

    2015-02-01

    A cinnamoyl derivative, 3-[4-(dimethylamino)cinnamoyl]-4-hydroxy-6-methyl-3,4-2H-pyran-2-one, was used as a ligand for the determination of aluminium. Upon the addition of an acetonitrile solution of the ligand to an aqueous solution containing Al(III) and a buffer solution at pH 8, a marked change in colour from yellow to orange is observed. The colour intensity is proportional to the concentration of Al(III); thus, the 'naked-eye' detection of aluminium is possible. The reaction is also applied for sequential injection determination of aluminium. Beer׳s law is obeyed in the range from 0.055 to 0.66 mg L(-1) of Al(III). The limit of detection, calculated as three times the standard deviation of the blank test (n=10), was found to be 4 μg L(-1) for Al(III). The method was applied for the determination of aluminium in spiked water samples and pharmaceutical preparations. Copyright © 2014 Elsevier B.V. All rights reserved.

  4. Amperometric Determination of Sulfite by Gas Diffusion- Sequential Injection with Boron-Doped Diamond Electrode

    Directory of Open Access Journals (Sweden)

    Orawon Chailapakul

    2008-03-01

    Full Text Available A gas diffusion sequential injection system with amperometric detection using aboron-doped diamond electrode was developed for the determination of sulfite. A gasdiffusion unit (GDU was used to prevent interference from sample matrices for theelectrochemical measurement. The sample was mixed with an acid solution to generategaseous sulfur dioxide prior to its passage through the donor channel of the GDU. Thesulfur dioxide diffused through the PTFE hydrophobic membrane into a carrier solution of 0.1 M phosphate buffer (pH 8/0.1% sodium dodecyl sulfate in the acceptor channel of theGDU and turned to sulfite. Then the sulfite was carried to the electrochemical flow cell anddetected directly by amperometry using the boron-doped diamond electrode at 0.95 V(versus Ag/AgCl. Sodium dodecyl sulfate was added to the carrier solution to preventelectrode fouling. This method was applicable in the concentration range of 0.2-20 mgSO32−/L and a detection limit (S/N = 3 of 0.05 mg SO32−/L was achieved. This method wassuccessfully applied to the determination of sulfite in wines and the analytical resultsagreed well with those obtained by iodimetric titration. The relative standard deviations forthe analysis of sulfite in wines were in the range of 1.0-4.1 %. The sampling frequency was65 h−1.

  5. Enhanced Silver Nanoparticle Chemiluminescence Method for the Determination of Gemifloxacin Mesylate using Sequential Injection Analysis

    International Nuclear Information System (INIS)

    Alarfaj, N.A.; Aly, F.A.; Tamimi, A.A.

    2013-01-01

    A sequential injection analysis (SIA) with chemiluminescence detection has been proposed for the determination of the antibiotic gemifloxacin mesylate (GFX). The developed method is based on the enhancement effect of silver nanoparticles (Ag NPs) on the chemiluminescence (CL) signal of luminol-potassium ferricyanide reaction in alkaline medium. The introduction of gemifloxacin in this system produced a significant decrease in the CL intensity in presence of (Ag NPs). The optimum conditions for CL emission were investigated. Linear relationship between the decrease in CL intensity and concentration was obtained in the range 0.01-1000 ng mL-1, (r = 0.9997) with detection limit of 2.0 pg mL-1 and quantification limit of 0.01 pg mL-1. The relative standard deviation was 1.3 %. The proposed method was employed for the determination of gemifloxacin in bulk drug, in its pharmaceutical dosage forms and biological fluids such as human serum and urine. The interference of some common additive compounds such as glucose, lactose, starch, talc and magnesium stearate was investigated, and no interference was found from these excipients. The obtained SIA results were statistically compared with those obtained from a reported method and did not show any significant difference at confidence level 95%. (author)

  6. Determination of uranium and its isotopic ratios in environmental samples

    International Nuclear Information System (INIS)

    Flues Szeles, M.S.M.

    1990-01-01

    A method for the determination of uranium and its isotopic ratios ( sup(235)U/ sup(238)U and sup(234U/ sup(238)U) is established in the present work. The method can be applied in environmental monitoring programs of uranium enrichment facilities. The proposed method is based on the alpha spectrometry technique which is applied after a purification of the sample by using an ionic exchange resin. The total yield achieved was (91 + 5)% with a precision of 5%, an accuracy of 8% and a lower limit of detection of 7,9 x 10 sup(-4)Bq. The uranium determination in samples containing high concentration of iron, which is an interfering element present in environmental samples, particularly in soil and sediment, was also studied. The results obtained by using artificial samples containing iron and uranium in the ratio 1000:1, were considered satisfactory. (author)

  7. Determination of fission gas yields from isotope ratios

    DEFF Research Database (Denmark)

    Mogensen, Mogens Bjerg

    1983-01-01

    This paper describes a method of calculating the actual fission yield of Kr and Xe in nuclear fuel including the effect of neutron capture reactions and decay. The bases for this calculation are the cumulative yields (ref. 1) of Kr and Xe isotopes (or pairs of isotopes) which are unaffected...... by neutron capture reactions, and measured Kr and Xe isotope ratios. Also the burnup contribution from the different fissile heavy isotopes must be known in order to get accurate fission gas yields....

  8. Isotopic-spectral determination of hydrogen, nitrogen, oxygen and carbon in semiconductor materials

    International Nuclear Information System (INIS)

    Dudich, G.K.; Eremeev, V.A.; Li, V.N.; Nemets, V.M.

    1981-01-01

    Techniques of low-temperature isotopic-spectral determination of impurities of hydrogen, nitrogen, oxygen and carbon in semiconductor materials Bi, Ge, Pb tellurides are developed. The techniques include selection into special vessel with the known volume (exchanger) of sample analyzed, dosed introduction into exchanger of rare isotope of the element determined ( 2 H, 15 N, 18 O, 13 C) in the form of isotope-containing gas, balancing of the determined element isotopes in the system sample-isotope, containing gas, spectroscopic, determination of its isotope composition in gaseous phase of the system and calculation of the amount of the element determined in the sample. The lower boundaries of the amounts determined constitute 10 -7 , 10 -7 , 10 -6 and 10 -5 mass % respectively when sample of 20 g are used [ru

  9. Determination of isotopic uranium in food and water

    International Nuclear Information System (INIS)

    Baratta, E.J.; Mackill, P.

    2001-01-01

    The U.S. Food and Drug Administration (FDA) conducts surveys of foods both domestic and imported for the presence of radioactivity. It does not routinely analyze for the actinides, specifically uranium, as it has been shown by previously by studies as reported by WELFORD and others that the concentration in food is very low. This was the result of a 'Tri-City' study. However, at specific sites, the FDA has been requested to analyze for uranium. The concern is that either 'enriched' or 'depleted' uranium has been introduced into the environment and possibly contaminated the food supply. In addition some concern has been raised that water from wells or other sources used for processing food may contain uranium, both natural, depleted or enriched. Methodology for the determination of isotopic uranium, specifically for uranium-238 (depleted) and/or uranium-235 (enriched) in the analyses of food and water samples and the results of these surveys are discussed. (author)

  10. Sequential injection approach for simultaneous determination of ultratrace plutonium and neptunium in urine with accelerator mass spectrometry

    DEFF Research Database (Denmark)

    Qiao, Jixin; Hou, Xiaolin; Roos, Per

    2013-01-01

    An analytical method was developed for simultaneous determination of ultratrace level plutonium (Pu) and neptunium (Np) using iron hydroxide coprecipitation in combination with automated sequential injection extraction chromatography separation and accelerator mass spectrometry (AMS) measurement...... show that preboiling and aging are important for obtaining high chemical yields for both Pu and Np, which is possibly related to the aggregation and adsorption behavior of organic substances contained in urine. Although the optimal condition for Np and Pu simultaneous determination requires 5-day aging...

  11. Multivariate Stable Isotope Analysis to Determine Linkages between Benzocaine Seizures

    Science.gov (United States)

    Kemp, H. F.; Meier-Augenstein, W.; Collins, M.; Salouros, H.; Cunningham, A.; Harrison, M.

    2012-04-01

    In July 2010, a woman was jailed for nine years in the UK after the prosecution successfully argued that attempting to import a cutting agent was proof of involvement in a conspiracy to supply Cocaine. That landmark ruling provided law enforcement agencies with much greater scope to tackle those involved in this aspect of the drug trade, specifically targeting those importing the likes of benzocaine or lidocaine. Huge quantities of these compounds are imported into the UK and between May and August 2010, four shipments of Benzocaine amounting to more then 4 tons had been seized as part of Operation Kitley, a joint initiative between the UK Border Agency and the Serious Organised Crime Agency (SOCA). By diluting cocaine, traffickers can make it go a lot further for very little cost, leading to huge profits. In recent years, dealers have moved away from inert substances, like sugar and baby milk powder, in favour of active pharmaceutical ingredients (APIs), including anaesthetics like Benzocaine and Lidocaine. Both these mimic the numbing effect of cocaine, and resemble it closely in colour, texture and some chemical behaviours, making it easier to conceal the fact that the drug has been diluted. API cutting agents have helped traffickers to maintain steady supplies in the face of successful interdiction and even expand the market in the UK, particularly to young people aged from their mid teens to early twenties. From importation to street-level, the purity of the drug can be reduced up to a factor of 80 and street level cocaine can have a cocaine content as low as 1%. In view of the increasing use of Benzocaine as cutting agent for Cocaine, a study was carried out to investigate if 2H, 13C, 15N and 18O stable isotope signatures could be used in conjunction with multivariate chemometric data analysis to determine potential linkage between benzocaine exhibits seized from different locations or individuals to assist with investigation and prosecution of drug

  12. Development of a Sequential Injection Analysis System for the Determination of Saccharin

    Directory of Open Access Journals (Sweden)

    Budi Wibowotomo

    2017-12-01

    Full Text Available Saccharin is a powerfully sweet nonnutritive sweetener that has been approved for food-processing applications within the range of 100–1200 mg/kg. A simple, rapid, and cost-effective sequential injection analysis (SIA technique was developed to determine the saccharin level. This method is based on the reaction of saccharin with p-chloranil in an ethanol medium with a hydrogen peroxide (H2O2 acceleration, and the resultant violet-red compound was detected using a UV-Vis spectrophotometer at λmax = 420 nm. To ascertain the optimal conditions for the SIA system, several parameters were investigated, including buffer flow rate and volume, p-chloranil concentration, and reactant volumes (saccharin, p-chloranil, and H2O2. The optimum setup of the SIA system was achieved with a buffer flow rate, buffer volume, and draw-up time of 1.2 mL/min, 2900 µL, and ~145 s, respectively. The optimal p-chloranil concentration is 30 mM, and the best reactant volumes, presented in an ordered sequence, are as follows: 30 µL of H2O2, 450 µL of saccharin, and 150 µL of p-chloranil. The optimized SIA configuration produced a good linear calibration curve with a correlation coefficient (R2 = 0.9812 in the concentration range of 20–140 mg/L and with a detection limit of 19.69 mg/L. Analytical applications in different food categories also showed acceptable recovery values in the range of 93.1–111.5%. This simple and rapid SIA system offers great feasibility for the saccharin quality control in food-product processing.

  13. Development of a Sequential Injection Analysis System for the Determination of Saccharin.

    Science.gov (United States)

    Wibowotomo, Budi; Eun, Jong-Bang; Rhee, Jong Il

    2017-12-12

    Saccharin is a powerfully sweet nonnutritive sweetener that has been approved for food-processing applications within the range of 100-1200 mg/kg. A simple, rapid, and cost-effective sequential injection analysis (SIA) technique was developed to determine the saccharin level. This method is based on the reaction of saccharin with p-chloranil in an ethanol medium with a hydrogen peroxide (H₂O₂) acceleration, and the resultant violet-red compound was detected using a UV-Vis spectrophotometer at λ max = 420 nm. To ascertain the optimal conditions for the SIA system, several parameters were investigated, including buffer flow rate and volume, p-chloranil concentration, and reactant volumes (saccharin, p-chloranil, and H₂O₂). The optimum setup of the SIA system was achieved with a buffer flow rate, buffer volume, and draw-up time of 1.2 mL/min, 2900 µL, and ~145 s, respectively. The optimal p-chloranil concentration is 30 mM, and the best reactant volumes, presented in an ordered sequence, are as follows: 30 µL of H₂O₂, 450 µL of saccharin, and 150 µL of p-chloranil. The optimized SIA configuration produced a good linear calibration curve with a correlation coefficient (R² = 0.9812) in the concentration range of 20-140 mg/L and with a detection limit of 19.69 mg/L. Analytical applications in different food categories also showed acceptable recovery values in the range of 93.1-111.5%. This simple and rapid SIA system offers great feasibility for the saccharin quality control in food-product processing.

  14. Spectral isotopic methods of determining nitrogen and carbon in plant specimens with laser volatization

    International Nuclear Information System (INIS)

    Lazeeva, G.S.

    1986-01-01

    Methods have been devised for the local determination of nitrogen and carbon isotope compositions in plant specimens, which provide separate and joint determination. Local laser evaporation has been combined with spectroscopic determination of the isotope compositions in the gas phase. A continuous-wave CO 2 laser is preferable for the local evaporation; the carbon isotope composition may be determined directly on the sum of the evaporation products, whereas nitrogen must first be separated as N 2 . Methods have also been developed for the local determination of total nitrogen and carbon in a sample with isotope dilution on the basis of laser evaporation. In order to eliminate systematic errors in determining total carbon in plant material, an evaporation method free from a rim has been devised. These methods have been used in determining isotope concentration profiles in plant specimens grown in experiments employing labeled nitrogen and carbon

  15. Rapid method for the sequential measurement of isotopes of Am and Pu in liquid matrices by alpha spectrometry

    International Nuclear Information System (INIS)

    Mantero Cabrera, J.

    2014-01-01

    : In radiological emergencies it's necessary a fast response from the laboratories in the quantification of certain radionuclides, in order to take decisions. In these cases, is the reaction time the key parameter to consider (without neglecting the quality of the measurement). In this work, it is shown a method for aqueous matrices that generates Pu and Am isotopes sources in one single day of work, to be measured subsequently by alpha spectrometry. The developed methodology has been validated through its application to reference samples and also taking part intercom- parison exercises, having in both cases, satisfactory results. This way, we check the validity of this fast method that let us generate in 24 hours (since the sample arrives our laboratory), one measurement with a Minimun Detectable Activity (MDA) of about 0.004Bq/L for Pu and Am isotopes in liquid matrices. [es

  16. Carbon and Oxygen isotopic composition in paleoenvironmental determination

    International Nuclear Information System (INIS)

    Silva, J.R.M. da.

    1978-01-01

    This work reports that the carbon and oxygen isotopic composition separate the mollusks from marine environment of the mollusks from continental environment in two groups isotopically different, making the biological control outdone by environment control, in the isotopic fragmentation mechanisms. The patterns from the continental environment are more rich in O 16 than the patterns from marine environments. The C 12 is also more frequent in the mollusks from continental environments. The carbon isotopic composition in paterns from continental environments is situated betwen - 10.31 and - 4,05% and the oxygen isotopic composition is situated between - 6,95 and - 2,41%. To the marine environment patterns the carbon isotopic composition is between - 2,08 and + 2,65% and the oxigen isotopic composition is between - 2,08 and + 0,45%. Was also analysed fossil marine mollusks shells and their isotopic composition permit the formulation of hypothesis about the environment which they lived. (C.D.G.) [pt

  17. Comparative study using different resins to determine thorium isotopes

    Energy Technology Data Exchange (ETDEWEB)

    Rosa, Mychelle M.L.; Silva, Paulo S.C.; Maihara, Vera A., E-mail: my_linhares@yahoo.com.br, E-mail: pscsilva@ipen.br, E-mail: vmaihara@ipen.br [Instituto de Pesquisas Energéticas e Nucleares (IPEN/CNEN-SP), São Paulo, SP (Brazil); Taddei, Maria Helena T., E-mail: mhtaddei@cnen.gov.br [Comissão Nacional de Energia Nuclear (LAPOC/CNEN), Poços de Caldas, MG (Brazil). Laboratório de Pocos de Caldas; Cheberle, Luan T.V., E-mail: luancheberle@gmail.com [Ambientis Radioproteção, Barueri, SP (Brazil)

    2017-07-01

    Thorium is a naturally occurring radioactive element that is widely distributed in the crust of the Earth. This element is very common in mineral formations in regions with high levels of natural radioactivity, therefore, its determination in environmental samples is important. Thorium isotopes ({sup 228}Th, {sup 230}Th, and {sup 232}Th) were determined in a reference material, the IAEA Soil 327 sample, to validate the two methods employed using different resins. The initial preparation with acid dissolution is the same to both, in the first is used anion exchange resin (DOWEX 1 x 2) and electrodeposition in silver planchets. And in the second method is used a specific chromatographic resin (TEVA) and cerium fluoride microprecipitation. At the end both analysis are quantified by alpha spectrometry. The two methods the results obtained were satisfactory for the reference material used, with relative error of less than 4% for {sup 228}Th, {sup 230}Th, and {sup 232}Th. The main differences found between them were spectrums resolutions, time and cost of analysis. (author)

  18. Use of radioanalytical methods for determination of uranium, neptunium, plutonium, americium and curium isotopes in radioactive wastes

    International Nuclear Information System (INIS)

    Geraldo, Bianca

    2012-01-01

    Activated charcoal is a common type of radioactive waste that contains high concentrations of fission and activation products. The management of this waste includes its characterization aiming the determination and quantification of the specific radionuclides including those known as Difficult-to-Measure Radionuclides (RDM). The analysis of the RDM's generally involves complex radiochemical analysis for purification and separation of the radionuclides, which are expensive and time-consuming. The objective of this work was to define a methodology for sequential analysis of the isotopes of uranium, neptunium, plutonium, americium and curium present in a type of radioactive waste, evaluating chemical yield, analysis of time spent, amount of secondary waste generated and cost. Three methodologies were compared and validated that employ ion exchange (TI + EC), extraction chromatography (EC) and extraction with polymers (ECP). The waste chosen was the activated charcoal from the purification system of primary circuit water cooling the reactor IEA-R1. The charcoal samples were dissolved by acid digestion followed by purification and separation of isotopes with ion exchange resins, extraction and chromatographic extraction polymers. Isotopes were analyzed on an alpha spectrometer, equipped with surface barrier detectors. The chemical yields were satisfactory for the methods TI + EC and EC. ECP method was comparable with those methods only for uranium. Statistical analysis as well the analysis of time spent, amount of secondary waste generated and cost revealed that EC method is the most effective for identifying and quantifying U, Np, Pu, Am and Cm present in charcoal. (author)

  19. Peculiarities of spectroscopic determination of the isotopic hydrogen composition in a mixture with neon and argon

    International Nuclear Information System (INIS)

    Nemets, V.M.; Petrov, A.A.; Solov'ev, A.A.

    1987-01-01

    The dependence of the relative intensity of atomic lines of hydrogen isotopes in the mixture with neon and argon during excitation in a high-frequency discharge under medium and high pressures is investigated. A physical model is suggested for processes determining the isotopic effects in the atomic hydrogen spectrum due to isotopic differences in velocity constants of dissociation-association, transfer and ionic-molecular reactions in a gas discharge plasma

  20. Comparison of three gamma ray isotopic determination codes: FRAM, MGA, and TRIFID

    International Nuclear Information System (INIS)

    Cremers, T.L.; Malcom, J.E.; Bonner, C.A.

    1994-01-01

    The determination of the isotopic distribution of plutonium and the americium concentration is required for the assay of nuclear material by calorimetry or neutron coincidence counting. The isotopic information is used in calorimetric assay to compute the effective specific power from the measured isotopic fractions and the known specific power of each isotope. The effective specific power is combined with the heat measurement to obtain the mass of plutonium in the assayed nuclear material. The response of neutron coincidence counters is determined by the 240 Pu isotopic fraction with contributions from the other even plutonium isotopes. The effect of the 240 Pu isotopic fraction and the other neutron contributing isotopes are combined as 240 Pu effective. This is used to calculate the mass of nuclear material from the neutron counting data in a manner analogous to the effective specific power in calorimeter. Comparisons of the precision and accuracy of calorimetric assay and neutron coincidence counting often focus only on the precision and accuracy of the heat measurement (calorimetry) compared to the precision and accuracy of the neutron coincidence counting statistics. The major source of uncertainty for both calorimetric assay and neutron coincidence counting often lies in the determination of the plutonium isotopic distribution ad determined by gamma ray spectroscopy. Thus, the selection of the appropriate isotopic distribution code is of paramount importance to good calorimetric assay and neutron coincidence counting. Three gamma ray isotopic distribution codes, FRAM, MGA, and TRIFID have been compared at the Los Alamos Plutonium Facility under carefully controlled conditions of similar count rates, count times, and 240 Pu isotopic fraction

  1. Simultaneous determination of radioactive halogen isotopes and 99Tc

    International Nuclear Information System (INIS)

    Kabai, E.; Vajda, N.; Gaca, P.

    2003-01-01

    The purpose of this study was to develop a simplified method for simultaneous determination of radiologically important halogen isotopes and 99 Tc from different types of samples like environmental, biological and waste samples. Due to their long half-lives (longer than 10 5 years) they play important role in the nuclear cycle, especially in environmental monitoring and protection. For a rapid response in the evaluation of 129 I, 36 Cl and 99 Tc contamination levels of these samples it is advantageous to combine the existing individual methods. According to the present procedure, iodine, chlorine and technetium are separated selectively from the same sample aliquot followed by the β spectrometry of the purified fractions. Increased sensitivities can be achieved by neutron activation (NA) especially in the case of 129 I. Our work intends to solve the problem by combining the well-known hot acidic distillation method for iodine separation with the organic extraction process characteristic for technetium separation. The major objective of the work was to separate the disturbing halides from iodine. For this purpose a selective oxidant was applied. For the sample destruction and fractionated distillation an air flow-through installation was used with hot concentrated sulphuric and nitric acids. The trap for iodine contained 3 M NaOH solution. After iodine separation the trap was exchanged for a new one containing the same solution for trapping chlorine or bromine with an addition of 0.01 M KMnO 4 solution as an oxidative agent. As expected, the main part of technetium was contained in the acidic residue after distillation. Tc purification was performed by organic extraction with TBP and TEVA column. (author)

  2. Simultaneous determination of stable carbon, oxygen, and hydrogen isotopes in cellulose.

    Science.gov (United States)

    Loader, N J; Street-Perrott, F A; Daley, T J; Hughes, P D M; Kimak, A; Levanič, T; Mallon, G; Mauquoy, D; Robertson, I; Roland, T P; van Bellen, S; Ziehmer, M M; Leuenberger, M

    2015-01-06

    A technological development is described through which the stable carbon-, oxygen-, and nonexchangeable hydrogen-isotopic ratios (δ(13)C, δ(18)O, δ(2)H) are determined on a single carbohydrate (cellulose) sample with precision equivalent to conventional techniques (δ(13)C 0.15‰, δ(18)O 0.30‰, δ(2)H 3.0‰). This triple-isotope approach offers significant new research opportunities, most notably in physiology and medicine, isotope biogeochemistry, forensic science, and palaeoclimatology, when isotopic analysis of a common sample is desirable or when sample material is limited.

  3. Radium 226 and uranium isotopes simultaneously determination in water samples using liquid scintillation counter

    International Nuclear Information System (INIS)

    Al-Masri, M.S.; Al-Akel, B.; Saaid, S.; Nashawati, A.

    2007-04-01

    In this work a method has been developed to determine simultaneously Radium 226 and Uranium isotopes in water samples by low back ground Liquid Scintillation Counter. Radium 226 was determined by its progeny Polonium 214 after one month of sample storage in order to achieve the equilibrium between Radium 226 and Polonium 214. Uranium isotopes were determined by subtracting Radium 226 activity from total alpha activity. The method detection limits were 0.049 Bq/L and 0.176 Bq/L for Radium 226 and Uranium isotopes respectively. The repeatability limits were ± 0.32 Bq/L and ± 0.9 Bq/L for Radium 226 and Uranium isotopes respectively. While relative errors were % 9.5 and %18.2 for Radium 226 and Uranium isotopes respectively. On the other hand, the report presented the results of different standard and natural samples.(author)

  4. Soil organic matter (SOM) dynamics determined by stable isotope techniques

    International Nuclear Information System (INIS)

    Gerzabek, M. H.

    1998-09-01

    Being aware of limitations and possible bias the 13 C natural abundance technique using the different 13 C enrichments in plants with differing photosynthetic pathways in a powerful tool to quantify turnover processes, both in long-term field studies and short-term laboratory experiments. Special care is needed in choosing reference plots and the proper number of replicate samples. The combination of 13 C and 14 C measurements has a high potential for a further improvement of isotope techniques in SOM studies. Natural abundance of 15 N is less powerful with respect to quantification of SOM processes than the isotope dilution technique. However its usefulness could be distinctly improved by introducing other stable isotopes into the studies.(author)

  5. Greek marbles: determination of provenance by isotopic analysis.

    Science.gov (United States)

    Craig, H; Craig, V

    1972-04-28

    A study has been made of carbon-13 and oxygen-18 variations in Greek marbles from the ancient quarry localities of Naxos, Paros, Mount Hymettus, and Mount Pentelikon. Parian, Hymettian, and Pentelic marbles can be clearly distinguished by the isotopic relationships; Naxian marbles fall into two groups characterized by different oxygen-18/oxygen-16 ratios. Ten archeological samples were also analyzed; the isotopic data indicate that the "Theseion" is made of Pentelic marble and a block in the Treasury of Siphnos at Delphi is probably Parian marble.

  6. Distributions and concentrations of thallium in Korean soils determined by single and sequential extraction procedures.

    Science.gov (United States)

    Lee, Jin-Ho; Kim, Dong-Jin; Ahn, Byung-Koo

    2015-06-01

    The objectives of this study were to investigate the distribution of thallium in soils collected near suspected areas such as cement plants, active and closed mines, and smelters and to examine the extraction of thallium in the soils using 19 single chemical and sequential chemical extraction procedures. Thallium concentrations in soils near cement plants were distributed between 1.20 and 12.91 mg kg(-1). However, soils near mines and smelters contained relatively low thallium concentrations ranging from 0.18 to 1.09 mg kg(-1). Thallium extractability with 19 single chemical extractants from selected soils near cement plants ranged from 0.10% to 8.20% of the total thallium concentration. In particular, 1.0 M NH4Cl, 1.0 M (NH4)2SO4, and 1.0 M CH3COONH4 extracted more thallium than other extractants. Sequential fractionation results of thallium from different soils such as industrially and artificially contaminated soils varied with the soil properties, especially soil pH and the duration of thallium contamination.

  7. Observation and spectroscopy of new proton-unbound isotopes {sup 30}Ar and {sup 29}Cl - an interplay of prompt two-proton and sequential decay

    Energy Technology Data Exchange (ETDEWEB)

    Mukha, Ivan [Helmholzzentrum GSI, Darmstadt (Germany)

    2016-07-01

    Previously unknown isotopes {sup 30}Ar and {sup 29}Cl have been identified by measurement of the trajectories of their in-flight decay products {sup 28}S+p+p and {sup 28}S+p, respectively. The analysis of angular correlations of the fragments provided information on decay energies and structure of the parent states. The lowest states in {sup 30}Ar, {sup 29}Cl point to a violation of isobaric symmetry in structure of these unbound nuclei. The two-proton decay has been identified in a transition region between simultaneous two-proton and sequential proton emissions from the {sup 30}Ar ground state, which is characterized by an interplay of three-body and two-body decay mechanisms. Such a phenomenon, never observed before, may be common in 2p-unbound nuclei, and could be of interest for other disciplines dealing with few-body systems. In addition, the dramatic change of odd-even mass staggering in 2p-unbound nuclei and the fine structure in the 2p decay of the {sup 30}Ar*(2.9 MeV) state were indicated. An Optical Time-Projection Chamber was used in the same experiment to observe beta decays of stopped {sup 31}Ar ions, which passed the secondary target intact. With this detector, β-delayed 3p emission from {sup 31}Ar was observed.

  8. Determination of the variation of mercury isotope concentration based on spectral-phase effects

    International Nuclear Information System (INIS)

    Ganeev, A.A.; Man', D.D.; Turkin, Yu.I.

    1988-01-01

    A method of isotopic atomic-absorption analysis, based on spectral-phase effects in which there is no need to use several sources of radiation with pure isotopes of the analyte element, was developed. The method made it possible to simplify the analysis and to determine the variation of the concentration of mercury isotopes from one deposit to another with an accuracy several times higher that of traditional methods of spectral isotopic analysis. The method was tested on mercury 198 and mercury 202. The isotopic analyzer is diagramed and described. The mechanism of spectral-phase effects was determined by the difference in effective photon lifetimes, corresponding to different components of the hyperfine structure of the resonance line of mercury at 254 nm

  9. Determination of liver and spleen perfusion by quantitative sequential scintigraphy: results in normal subjects and in patients with portal hypertension

    International Nuclear Information System (INIS)

    Biersack, H.J.; Torres, J.; Thelen, M.; Monzon, O.; Winkler, C.

    1981-01-01

    Quantitative sequential hepatosplenic scintigraphy was performed to determine the arterial and portal components of the total liver circulation in 135 patients (no liver disease in 20, liver cirrhosis and portal ;hypertension in 115). Portal circulation in healthy patients is calculated to be 70.4 +/- 6.2% of the total liver blood flow, whereas patients with portal hypertension showed a clear reduction of portal perfusion to 20.2 +/- 10.9%. Thirteen of 20 patients having portosystemic shunt surgery showed no portal perfusion. This new, noninvasive diagnostic technique yields vital information particularly useful in ;the surgical evaluation of portal hypertension. Other indications are also discussed

  10. Determining the isotopic compositions of uranium and fission products in radioactive environmental microsamples using laser ablation ICP-MS with multiple ion counters

    International Nuclear Information System (INIS)

    Boulyga, Sergei F.; Prohaska, Thomas

    2008-01-01

    This paper presents the application of a multicollector inductively coupled plasma mass spectrometer (MC-ICP-MS) - a Nu Plasma HR - equipped with three ion-counting multipliers and coupled to a laser ablation system (LA) for the rapid and sensitive determination of the 235 U/ 238 U, 236 U/ 238 U, 145 Nd/ 143 Nd, 146 Nd/ 143 Nd, 101 Ru/( 99 Ru+ 99 Tc) and 102 Ru/( 99 Ru+ 99 Tc) isotope ratios in microsamples collected in the vicinity of Chernobyl. Microsamples with dimensions ranging from a hundred μm to about 1 mm and with surface alpha activities of 3-38 mBq were first identified using nuclear track radiography. U, Nd and Ru isotope systems were then measured sequentially for the same microsample by LA-MC-ICP-MS. The application of a zoom ion optic for aligning the ion beams into the ion counters allows fast switching between different isotope systems, which enables all of the abovementioned isotope ratios to be measured for the same microsample within a total analysis time of 15-20 min (excluding MC-ICP-MS optimization and calibration). The 101 Ru/( 99 Ru+ 99 Tc) and 102 Ru/( 99 Ru+ 99 Tc) isotope ratios were measured for four microsamples and were found to be significantly lower than the natural ratios, indicating that the microsamples were contaminated with the corresponding fission products (Ru and Tc). A slight depletion in 146 Nd of about 3-5% was observed in the contaminated samples, but the Nd isotopic ratios measured in the contaminated samples coincided with natural isotopic composition within the measurement uncertainty, as most of the Nd in the analyzed samples originates from the natural soil load of this element. The 235 U/ 238 U and 236 U/ 238 U isotope ratios were the most sensitive indicators of irradiated uranium. The present work yielded a significant variation in uranium isotope ratios in microsamples, in contrast with previously published results from the bulk analysis of contaminated samples originating from the vicinity of Chernobyl. Thus

  11. Determining the isotopic compositions of uranium and fission products in radioactive environmental microsamples using laser ablation ICP-MS with multiple ion counters.

    Science.gov (United States)

    Boulyga, Sergei F; Prohaska, Thomas

    2008-01-01

    This paper presents the application of a multicollector inductively coupled plasma mass spectrometer (MC-ICP-MS)--a Nu Plasma HR--equipped with three ion-counting multipliers and coupled to a laser ablation system (LA) for the rapid and sensitive determination of the 235U/238U, 236U/238U, 145Nd/143Nd, 146Nd/143Nd, 101Ru/(99Ru+99Tc) and 102Ru/(99Ru+99Tc) isotope ratios in microsamples collected in the vicinity of Chernobyl. Microsamples with dimensions ranging from a hundred mum to about 1 mm and with surface alpha activities of 3-38 mBq were first identified using nuclear track radiography. U, Nd and Ru isotope systems were then measured sequentially for the same microsample by LA-MC-ICP-MS. The application of a zoom ion optic for aligning the ion beams into the ion counters allows fast switching between different isotope systems, which enables all of the abovementioned isotope ratios to be measured for the same microsample within a total analysis time of 15-20 min (excluding MC-ICP-MS optimization and calibration). The 101Ru/(99Ru+99Tc) and 102Ru/(99Ru+99Tc) isotope ratios were measured for four microsamples and were found to be significantly lower than the natural ratios, indicating that the microsamples were contaminated with the corresponding fission products (Ru and Tc). A slight depletion in 146Nd of about 3-5% was observed in the contaminated samples, but the Nd isotopic ratios measured in the contaminated samples coincided with natural isotopic composition within the measurement uncertainty, as most of the Nd in the analyzed samples originates from the natural soil load of this element. The 235U/238U and 236U/238U isotope ratios were the most sensitive indicators of irradiated uranium. The present work yielded a significant variation in uranium isotope ratios in microsamples, in contrast with previously published results from the bulk analysis of contaminated samples originating from the vicinity of Chernobyl. Thus, the 235U/238U ratios measured in ten

  12. Sequential injection titration method using second-order signals: determination of acidity in plant oils and biodiesel samples.

    Science.gov (United States)

    del Río, Vanessa; Larrechi, M Soledad; Callao, M Pilar

    2010-06-15

    A new concept of flow titration is proposed and demonstrated for the determination of total acidity in plant oils and biodiesel. We use sequential injection analysis (SIA) with a diode array spectrophotometric detector linked to chemometric tools such as multivariate curve resolution-alternating least squares (MCR-ALS). This system is based on the evolution of the basic specie of an acid-base indicator, alizarine, when it comes into contact with a sample that contains free fatty acids. The gradual pH change in the reactor coil due to diffusion and reaction phenomenona allows the sequential appearance of both species of the indicator in the detector coil, recording a data matrix for each sample. The SIA-MCR-ALS method helps to reduce the amounts of sample, the reagents and the time consumed. Each determination consumes 0.413ml of sample, 0.250ml of indicator and 3ml of carrier (ethanol) and generates 3.333ml of waste. The frequency of the analysis is high (12 samples h(-1) including all steps, i.e., cleaning, preparing and analysing). The utilized reagents are of common use in the laboratory and it is not necessary to use the reagents of perfect known concentration. The method was applied to determine acidity in plant oil and biodiesel samples. Results obtained by the proposed method compare well with those obtained by the official European Community method that is time consuming and uses large amounts of organic solvents.

  13. Determination of natural alpha-emitting isotopes of uranium and thorium in environmental and geological samples

    International Nuclear Information System (INIS)

    Crespo, M.T.

    1996-01-01

    It is described the complete radiochemical procedure used for the determination of uranium and thorium isotopes in environmental and geological samples by alpha spectrometry. Source preparation methods, alpha-counting and spectral analysis are also included

  14. Stable isotopes determination in some Romanian fruit juices.

    Science.gov (United States)

    Magdas, Dana Alina; Puscas, Romulus

    2011-09-01

    The characterisation of 45 Romanian single-strength fruit juices (apples, pears, plums and grapes) collected from different Transylvanian areas by means of stable isotope approach are presented and discussed in this study. We measured (2)H/(1)H, (18)O/(16)O ratios from water juice and (13)C/(12)C from pulp and compared these results with those already reported in the literature for single-strength juices, in order to see how the geographical and climatic conditions of Transylvania and the meteorological peculiarities of the year 2010 influence the isotopic composition of the investigated fruit juices. The δ(13)C mean values that we found for apple pulp picked up from different Transylvanian areas show slight differences, probably due to the environmental conditions of the plants. No significant correlation either between the variety of apple or the geographical origin and δ(13)C value was established.

  15. Determination of kinetic parameters of heterogeneous isotopic exchange reaction

    International Nuclear Information System (INIS)

    Huang, Ting-Chia; Tsai, Fuan-Nan

    1977-01-01

    A mathematical model has been proposed for a heterogeneous isotopic exchange reaction which involves film diffusion, surface chemical reaction and intraparticle diffusion. The exchange equation to predict the exchange fraction as a function of time for the spherical particles immersed in a solution of finite volume has been derived. The relations between the exchange fraction and dimensionless time are plotted with xi(=ak sub(f)/KD sub(e)), xi 1 (=K 1 a 2 /D sub(e)) and final fractional uptake as parameters. From the values of the kinetic parameters xi and xi 1 , the relative importance of each limiting step is discussed. Experimental results of the isotopic exchange reaction of calcium ion in both system CaCO 3 (s)/Ca 2+ (aq) and system calcium type resin Dowex 50W-X8/Ca 2+ (aq) are coincident with the theoretical equation proposed in this study. (auth.)

  16. Studies in the determination of lead isotope ratios by inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Date, A.R.; Yuk Ying Cheung

    1987-01-01

    The application of ICP-MS to the determination of lead isotope ratios in geological materials is described. Data presented for a series of lead mineral concentrates are compared with reference values obtained by conventional solid source thermal ionisation mass spectrometry. The simultaneous determination of lead isotope ratios and trace elements is carried out in a rapid analysis mode. The application of an electrothermal vaporisation technique for small solution aliquots is described. Lead isotope ratio data for the United States Geological Survey standard reference silicate rock BCR-1, obtained without separation of lead from the matrix, are compared with previously published values obtained after separation. (author)

  17. Ground-water pollution determined by boron isotope systematics

    International Nuclear Information System (INIS)

    Vengosh, A.; Kolodny, Y.; Spivack, A.J.

    1998-01-01

    Boron isotopic systematics as related to ground-water pollution is reviewed. We report isotopic results of contaminated ground water from the coastal aquifers of the Mediterranean in Israel, Cornia River in north-western Italy, and Salinas Valley, California. In addition, the B isotopic composition of synthetic B compounds used for detergents and fertilizers was investigated. Isotopic analyses were carried out by negative thermal ionization mass spectrometry. The investigated ground water revealed different contamination sources; underlying saline water of a marine origin in saline plumes in the Mediterranean coastal aquifer of Israel (δ 11 B=31.7 per mille to 49.9 per mille, B/Cl ratio ∼1.5x10 -3 ), mixing of fresh and sea water (25 per mille to 38 per mille, B/Cl∼7x10 -3 ) in saline water associated with salt-water intrusion to Salinas Valley, California, and a hydrothermal contribution (high B/Cl of ∼0.03, δ 11 B=2.4 per mille to 9.3 per mille) in ground water from Cornia River, Italy. The δ 11 B values of synthetic Na-borate products (-0.4 per mille to 7.5 per mille) overlap with those of natural Na-borate minerals (-0.9 per mille to 10.2 per mille). In contrast, the δ 11 B values of synthetic Ca-borate and Na/Ca borate products are significantly lower (-15 per mille to -12.1 per mille) and overlap with those of the natural Ca-borate minerals. We suggest that the original isotopic signature of the natural borate minerals is not modified during the manufacturing process of the synthetic products, and it is controlled by the crystal chemistry of borate minerals. The B concentrations in pristine ground-waters are generally low ( 11 B=39 per mille), salt-water intrusion and marine-derived brines (40 per mille to 60 per mille) are sharply different from hydrothermal fluids (δ 11 B=10 per mille to 10 per mille) and anthropogenic sources (sewage effluent: δ 11 B=0 per mille to 10 per mille; boron-fertilizer: δ 11 B=-15 per mille to 7 per mille). some

  18. Determination of uranium isotopes in environmental samples by anion exchange in sulfuric and hydrochloric acid media

    International Nuclear Information System (INIS)

    Popov, L.

    2016-01-01

    Method for determination of uranium isotopes in various environmental samples is presented. The major advantages of the method are the low cost of the analysis, high radiochemical yields and good decontamination factors from the matrix elements, natural and man-made radionuclides. The separation and purification of uranium is attained by adsorption with strong base anion exchange resin in sulfuric and hydrochloric acid media. Uranium is electrodeposited on a stainless steel disk and measured by alpha spectrometry. The analytical method has been applied for the determination of concentrations of uranium isotopes in mineral, spring and tap waters from Bulgaria. The analytical quality was checked by analyzing reference materials. - Highlights: • The method allows cost-effective determination of U isotopes. • High amounts of environmental samples can be analyzed. • High chemical yields, energy resolution and decontamination factors were achieved. • Uranium isotope concentrations in mineral waters from Bulgaria are presented.

  19. Isotope determinations of renal clearance equivalent with physiological clearance measurements

    International Nuclear Information System (INIS)

    Junges, R.

    1983-01-01

    The concept of renal clearance in nuclear medicine describes the tubular secretion and glomerular filtration of a substance being removed from the blood plasma. The concept of clearance as used physiologically is rather wider and includes consideration of the outflow of the substances remained back in the kidneys. The present paper discusses clearance measurements as seen from a thermodynamic point of view, in which isotope clearances become equivalent with the physiological concept of clearance. In addition, it is possible to quantify each single step of the excretory function of each kidney separately. (orig.) [de

  20. Determination of zinc nutrient in the soil using isotope technique

    International Nuclear Information System (INIS)

    Suwadji, E.

    1975-01-01

    In this experiment the availability of soil Zn nutrient in various soil conditions (dry and submerged), and the efficiency of the application of Zn fertilizer in rice nutrition were measured in glasshouse using isotope dilution technique. The amount of soil Zn nutrient available to plants can be expressed in 'E' and 'L' values. Submerged conditions generally showed an increase in the 'E' and 'L' value compared to dry conditions. Mixed treatment with ZnSO 4 fertilizer is more efficient for Zn absorption than surface treatment. (author)

  1. Experimental determination of one- and two-neutron separation energies for neutron-rich copper isotopes

    Science.gov (United States)

    Yu, Mian; Wei, Hui-Ling; Song, Yi-Dan; Ma, Chun-Wang

    2017-09-01

    A method is proposed to determine the one-neutron S n or two-neutron S 2n separation energy of neutron-rich isotopes. Relationships between S n (S 2n) and isotopic cross sections have been deduced from an empirical formula, i.e., the cross section of an isotope exponentially depends on the average binding energy per nucleon B/A. The proposed relationships have been verified using the neutron-rich copper isotopes measured in the 64A MeV 86Kr + 9Be reaction. S n, S 2n, and B/A for the very neutron-rich 77,78,79Cu isotopes are determined from the proposed correlations. It is also proposed that the correlations between S n, S 2n and isotopic cross sections can be used to find the location of neutron drip line isotopes. Supported by Program for Science and Technology Innovation Talents at Universities of Henan Province (13HASTIT046), Natural and Science Foundation in Henan Province (162300410179), Program for the Excellent Youth at Henan Normal University (154100510007) and Y-D Song thanks the support from the Creative Experimental Project of National Undergraduate Students (CEPNU 201510476017)

  2. The use of stable isotopes in quantitative determinations of exogenous water and added ethanol in wines

    Science.gov (United States)

    Magdas, D. A.; Moldovan, Z.; Cristea, G.

    2012-02-01

    The application of oxygen isotope ratios analysis to wine water according to EU regulation no. 822/97 to determine wine's origin and also, the possible water addition to wines, gained great importance in wines authenticity control. In the natural cycle of water isotopic fractionation, during water evaporation process, the water vapors are depleted in heavy isotopes. On the other hand inside the plants take place an isotope enrichment of heavy stable isotopes of water compared with meteoric water due to photosynthesis and plants transpiration. This process makes possible the detection of exogenous water from wines 18O/16O ratios. Carbon isotopic ratios were used to estimate the supplementary addition of ethanol obtained from C4 plants (sugar cane or corn). This work presents the way in which the isotopic fingerprints (δ13C and δ18O) were used to determine the content of exogenous water from wines and the added supplementary ethanol coming from C4 plants. By using this method, the calculated values obtained for the degree of wine adulteration were in a good agreement with the real exogenous percent of water and ethanol from investigated samples.

  3. Design of LabVIEW®-based software for the control of sequential injection analysis instrumentation for the determination of morphine

    Science.gov (United States)

    Lenehan, Claire E.; Lewis, Simon W.

    2002-01-01

    LabVIEW®-based software for the automation of a sequential injection analysis instrument for the determination of morphine is presented. Detection was based on its chemiluminescence reaction with acidic potassium permanganate in the presence of sodium polyphosphate. The calibration function approximated linearity (range 5 × 10-10 to 5 × 10-6 M) with a line of best fit of y=1.05x+8.9164 (R2 =0.9959), where y is the log10 signal (mV) and x is the log10 morphine concentration (M). Precision, as measured by relative standard deviation, was 0.7% for five replicate analyses of morphine standard (5 × 10-8 M). The limit of detection (3σ) was determined as 5 × 10-11 M morphine. PMID:18924729

  4. Design of LabVIEW-based software for the control of sequential injection analysis instrumentation for the determination of morphine.

    Science.gov (United States)

    Lenehan, Claire E; Barnett, Neil W; Lewis, Simon W

    2002-01-01

    LabVIEW-based software for the automation of a sequential injection analysis instrument for the determination of morphine is presented. Detection was based on its chemiluminescence reaction with acidic potassium permanganate in the presence of sodium polyphosphate. The calibration function approximated linearity (range 5 x 10(-10) to 5 x 10(-6) M) with a line of best fit of y=1.05(x)+8.9164 (R(2) =0.9959), where y is the log10 signal (mV) and x is the log10 morphine concentration (M). Precision, as measured by relative standard deviation, was 0.7% for five replicate analyses of morphine standard (5 x 10(-8) M). The limit of detection (3sigma) was determined as 5 x 10(-11) M morphine.

  5. Sequential determination of fat- and water-soluble vitamins in green leafy vegetables during storage.

    Science.gov (United States)

    Santos, J; Mendiola, J A; Oliveira, M B P P; Ibáñez, E; Herrero, M

    2012-10-26

    The simultaneous analysis of fat- and water-soluble vitamins from foods is a difficult task considering the wide range of chemical structures involved. In this work, a new procedure based on a sequential extraction and analysis of both types of vitamins is presented. The procedure couples several simple extraction steps to LC-MS/MS and LC-DAD in order to quantify the free vitamins contents in fresh-cut vegetables before and after a 10-days storage period. The developed method allows the correct quantification of vitamins C, B(1), B(2), B(3), B(5), B(6), B(9), E and provitamin A in ready-to-eat green leafy vegetable products including green lettuce, ruby red lettuce, watercress, swiss chard, lamb's lettuce, spearmint, spinach, wild rocket, pea leaves, mizuna, garden cress and red mustard. Using this optimized methodology, low LOQs were attained for the analyzed vitamins in less than 100 min, including extraction and vitamin analysis using 2 optimized procedures; good repeatability and linearity was achieved for all vitamins studied, while recoveries ranged from 83% to 105%. The most abundant free vitamins found in leafy vegetable products were vitamin C, provitamin A and vitamin E. The richest sample on vitamin C and provitamin A was pea leaves (154 mg/g fresh weight and 14.4 mg/100g fresh weight, respectively), whereas lamb's lettuce was the vegetable with the highest content on vitamin E (3.1 mg/100 g fresh weight). Generally, some losses of vitamins were detected after storage, although the behavior of each vitamin varied strongly among samples. Copyright © 2012 Elsevier B.V. All rights reserved.

  6. Results from an interlaboratory exercise on the determination of plutonium isotopic ratios by gamma spectrometry

    International Nuclear Information System (INIS)

    Ottmar, H.

    1981-07-01

    Results form interlaboratory comparison measurements on the determination of plutonium isotopic ratios by gamma spectrometry, organized by the ESARDA Working Group on Techniques and Standards for Nondestructive Analysis, are presented and discussed. Nine laboratories from nine countries or international organizations participated in the intercomparison exercise, which included both laboratories' own measurements on the plutonium isotopic reference materials NBS-SRM 946, 947, 948 and comparison analyses of gamma spectra from these materials distributed to the participating laboratories. Results from the intercomparison analyses have been used to reevaluate some gamma branching intensity ratios required for plutonium isotopic ratio measurements. (orig.) [de

  7. ICP-oa TOFMS utilisation to determine the Gd isotopic abundance in gadolinium nitrate

    International Nuclear Information System (INIS)

    Dragomir, M.; Ohai, D.; Dumitrescu, I.; Furtuna, I.

    2010-01-01

    This paper is describes the development of a method that should permit the determination of isotope abundance of gadolinium in gadolinium nitrate, used as burnable poison at Cernavoda NPP. To determine the isotopic abundance of gadolinium the inductively coupled plasma orthogonal acceleration time-of-flight mass spectrometer (ICP-oa TOFMS) was used. The ICP-oa TOFMS allows the elimination of noise associated with instrumental drift and instability (flicker noise). The absence of flicker noise in the ICP-oa TOFMS means that the isotope ratios can be measured up to the statistical limit of ion counting. With TOFMS, each spectrum acquired represents signals from ions extracted from the plasma during the same time interval, formed from identical plasma and sample introduction events. Therefore, the ICP-oa TOFMS, Optimass 8000, has been successfully used for isotope ratio measurements of Gd in gadolinium nitrate [Gd (NO 3 ) 3 x 6H 2 O] sample solutions. (authors)

  8. Determination of carbon isotope ratios in plant starch via selective enzymatic hydrolysis

    International Nuclear Information System (INIS)

    Schimmelmann, A.; DeNiro, M.J.

    1983-01-01

    A method for the determination of the carbon isotope ratios in bipolymers hydrolyzed by enzymatic action consists of separating the monomer by passage through a dialysis membrane and then combusting the monomer prior to isotopic analysis. The method is described for application to the analysis of starch, but it should find application for polymers than can be degraded quantitatively to monomers and/or oligomers using specific hydrolytic enzymes

  9. Special features of the isotope ratio determination using mass-spectrometer with induction-bound plasma

    International Nuclear Information System (INIS)

    Stepanov, A.I.; Ramendik, G.I.; Fatyushina, E.V.

    2000-01-01

    The origin of the errors arising upon measuring relative abundance of Nd, Yb, and Gd isotopes on a HP-4500 mass-spectrometer (USA) is studied. It is shown that the main origin of the error is the different sensitivity of the mass-spectrometer to ions of different masses. Optimal content of the elements in the solutions is established upon determination of their isotopic abundance [ru

  10. Isotope Methods in Determining The Water Budget Elements; Su Buetcesi Elemanlarinin Bulunmasinda Izotop Yoentemi

    Energy Technology Data Exchange (ETDEWEB)

    Oezaydin, V [DSI, Technical Research and Quality Control Department, Ankara (Turkey)

    2002-07-01

    One of the main aims of the water engineers is the determination of the inflows to and outflows from a natural or artificial lake. According to the classical water balance equation inflows (precipitation on the lake surface, surface and subsurface inflows) mines the outflows (evaporation from lake surface, surface and subsurface outflows) should be equal to the volume change in a specified time interval. With the classical water budget equation it is possible to determine the total absolute subsurface inflow mines outflow but it is not possible to determine them separately. The two unknowns could be determined with one more equation. The isotopes, oxygen-18, deuterium or tritium, which are naturally present in water, could provide the extra equation by writing the isotopic mass balance equation. In this study, the theoretical background of isotope technique and application to Mogan Lake, will be presented which is used in determining the water budget of lakes.

  11. The determination of minor isotope abundances in naturally occurring uranium materials. The tracing power of isotopic signatures for uranium

    Energy Technology Data Exchange (ETDEWEB)

    Ovaskainen, R

    1999-11-01

    The mass spectrometric determination of minor abundant isotopes, {sup 234}U and {sup 236}U in naturally occurring uranium materials requires instruments of high abundance sensitivity and the use of highly sensitive detection systems. In this study the thermal ionisation mass spectrometer Finnigan MAT 262RPQ was used. It was equipped with 6 Faraday cups and a Secondary Electron Multiplier (SEM), which was operated in pulse counting mode for the detection of extremely low ion currents. The dynamic measurement range was increased considerably combining these two different detectors. The instrument calibration was performed carefully. The linearity of each detector, the deadtime of the ion counting detector, the detector normalisation factor, the baseline of each detector and the mass discrimination in the ion source were checked and optimised. A measurement technique based on the combination of a Gas Source Mass Spectrometry (GSMS) and a Thermal Ionisation Mass Spectrometry (TIMS) was developed for the accurate determination of isotopic composition in naturally occurring uranium materials. Because the expected ratio of n({sup 234}U)/n({sup 238}U) exceeded the dynamic measurement range of the Faraday detectors of the TIMS instrument, an experimental design using a combination of two detectors was developed. The n({sup 234}U)/n({sup 235}U) and n({sup 236}U)/n({sup 235}U) ratios were determined using ion counting in combination with the decelerating device. The n({sup 235}U)/n({sup 238}U) ratio was determined by the Faraday detector. This experimental design allowed the detector cross calibration to be circumvented. Precisions of less than 1 percent for the n({sup 234}U)/n({sup 235}U) ratios and 5-25 percent for the n({sup 236}U)/n({sup 235}U) ratios were achieved. The purpose of the study was to establish a register of isotopic signatures for natural uranium materials. The amount ratio, and isotopic composition of 18 ore concentrates, collected by the International

  12. The determination of minor isotope abundances in naturally occurring uranium materials. The tracing power of isotopic signatures for uranium

    International Nuclear Information System (INIS)

    Ovaskainen, R.

    1999-01-01

    The mass spectrometric determination of minor abundant isotopes, 234 U and 236 U in naturally occurring uranium materials requires instruments of high abundance sensitivity and the use of highly sensitive detection systems. In this study the thermal ionisation mass spectrometer Finnigan MAT 262RPQ was used. It was equipped with 6 Faraday cups and a Secondary Electron Multiplier (SEM), which was operated in pulse counting mode for the detection of extremely low ion currents. The dynamic measurement range was increased considerably combining these two different detectors. The instrument calibration was performed carefully. The linearity of each detector, the deadtime of the ion counting detector, the detector normalisation factor, the baseline of each detector and the mass discrimination in the ion source were checked and optimised. A measurement technique based on the combination of a Gas Source Mass Spectrometry (GSMS) and a Thermal Ionisation Mass Spectrometry (TIMS) was developed for the accurate determination of isotopic composition in naturally occurring uranium materials. Because the expected ratio of n( 234 U)/n( 238 U) exceeded the dynamic measurement range of the Faraday detectors of the TIMS instrument, an experimental design using a combination of two detectors was developed. The n( 234 U)/n( 235 U) and n( 236 U)/n( 235 U) ratios were determined using ion counting in combination with the decelerating device. The n( 235 U)/n( 238 U) ratio was determined by the Faraday detector. This experimental design allowed the detector cross calibration to be circumvented. Precisions of less than 1 percent for the n( 234 U)/n( 235 U) ratios and 5-25 percent for the n( 236 U)/n( 235 U) ratios were achieved. The purpose of the study was to establish a register of isotopic signatures for natural uranium materials. The amount ratio, and isotopic composition of 18 ore concentrates, collected by the International Atomic Energy Agency (IAEA) from uranium milling and mining

  13. Sequential determination of urea and HMTA in the process solution of sol-gel route of advanced nuclear fuel fabrication

    International Nuclear Information System (INIS)

    Sawant, R.M.; Chaudhuri, N.K.; Ramakumar, K.L.

    2002-01-01

    Determinations of hexamethylene tetramine (HMTA) and urea in the process solutions are required to optimize their concentrations for obtaining high quality ceramic oxide microspheres, for monitoring the washing procedure and for their subsequent recovery, recycling or waste disposal. Determination of urea is the feed solution by conventional procedures is difficult as it contains HMTA. It is more so in the effluent as it contains hydrolytic products like formaldehyde, methylol derivatives of urea, ammonium nitrate and ammonium hydroxide used for washing the gel microspheres. A derivative potentiometric method using a microprocessor-based autotitrator is described. Peaks on the first derivative of the titration plot corresponded to constituents of different basicities. Urea was selectively hydrolyzed at room temperature by the catalytic action of urease enzyme leaving HMTA unaffected. Ammonium hydroxide and ammonium bicarbonate produced from urea and HMTA were sequentially titrated for the analysis of the feed solution to obtain the three corresponding peaks respectively. Two separate titrations were required for the analysis of the effluent solution, which contained free ammonia also. One aliquot was first titrated directly without adding urease (for free ammonia and HMTA) and another aliquot was titrated after treatment with urease. The end points due to the ammonia used for washing and that from urea hydrolysis merged resulting in the appearance of three peaks again. Using this sequential method the relative standard deviations were found to be 0.81% and 1.38% for urea and HMTA, respectively, in eight determinations when the aliquots contained 50 to 75 mg of urea and 75 to 125 mg of HMTA. Feed and effluent solutions of the process stream were analyzed. (author)

  14. Features of the spectroscopic determination of the isotope composition of trace amounts of hydrogen in helium

    International Nuclear Information System (INIS)

    Nemets, V.M.; Petrov, A.A.; Solov'ev, A.A.

    1986-01-01

    The investigation of the magnitude of the isotope effect in the intensiti of the beta lines of the Balmer series was carried out with the excitation of a high-frequency discharge in a quartz tube having a diameter of ca.6.5 at pressures of the gaseous mixture ranging from 1 to 70 kPa. From the experimental results here it follows that as the isotopes of hydrogen are diluted with helium, the value of K decreases from 1.2-1.1 to 0.84-0.86, and the maximum of the plots of K= f(P) broaden and move toward higher pressures. In order to account for the laws obtained, the authors examined a set of elementary processes and reactions for which the isotope-related differences in the rate constants (alpha) can influence the relative concentrations of the excited atoms of the isotopes of hydrogen in a discharge. The physical model presented in this paper of the shaping of the isotope effects in the atomic spectrum of hydrogen makes it possible to account for the observed laws governing the excitation of a discharge in a mixture of the isotopes of hydrogen with helium and thus greatly facilitates the selection of the optimal conditions for the excitation of the analytical spectrum in devising procedures for the spectroscopic isotope determination of trace impurities of hydrogen in helium

  15. Film thickness determining method of the silicon isotope superlattices by SIMS

    International Nuclear Information System (INIS)

    Takano, Akio; Shimizu, Yasuo; Itoh, Kohei M.

    2008-01-01

    It is becoming important to evaluate silicon self-diffusion with progress of a silicon semiconductor industry. In order to evaluate the self-diffusion of silicon, silicon isotope superlattices (SLs) is the only marker. For this reason, it is important to correctly evaluate a film thickness and a depth distribution of isotope SLs by secondary ion mass spectrometry (SIMS). As for film thickness, it is difficult to estimate the thicknesses correctly if the cycles of SLs are short. In this work, first, we report the determination of the film thickness for short-period SLs using mixing roughness-information (MRI) analysis to SIMS profile. Next, the uncertainty of the conventional method to determine the film thicknesses of SLs is determined. It was found that the conventional methods cannot correctly determine film thickness of short-period-isotope SLs where film thickness differs for every layer

  16. Sub-1min separation in sequential injection chromatography for determination of synthetic water-soluble dyes in pharmaceutical formulation.

    Science.gov (United States)

    Davletbaeva, Polina; Chocholouš, Petr; Bulatov, Andrey; Šatínský, Dalibor; Solich, Petr

    2017-09-05

    Sequential Injection Chromatography (SIC) evolved from fast and automated non-separation Sequential Injection Analysis (SIA) into chromatographic separation method for multi-element analysis. However, the speed of the measurement (sample throughput) is due to chromatography significantly reduced. In this paper, a sub-1min separation using medium polar cyano monolithic column (5mm×4.6mm) resulted in fast and green separation with sample throughput comparable with non-separation flow methods The separation of three synthetic water-soluble dyes (sunset yellow FCF, carmoisine and green S) was in a gradient elution mode (0.02% ammonium acetate, pH 6.7 - water) with flow rate of 3.0mLmin -1 corresponding with sample throughput of 30h -1 . Spectrophotometric detection wavelengths were set to 480, 516 and 630nm and 10Hz data collection rate. The performance of the separation was described and discussed (peak capacities 3.48-7.67, peak symmetries 1.72-1.84 and resolutions 1.42-1.88). The method was represented by validation parameters: LODs of 0.15-0.35mgL -1 , LOQs of 0.50-1.25mgL -1 , calibration ranges 0.50-150.00mgL -1 (r>0.998) and repeatability at 10.0mgL -1 of RSD≤0.98% (n=6). The method was used for determination of the dyes in "forest berries" colored pharmaceutical cough-cold formulation. The sample matrix - pharmaceuticals and excipients were not interfering with vis determination because of no retention in the separation column and colorless nature. The results proved the concept of fast and green chromatography approach using very short medium polar monolithic column in SIC. Copyright © 2017 Elsevier B.V. All rights reserved.

  17. Uranium isotopes determination in urine samples using alpha spectrometry and ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Rosa, Mychelle M.L.; Maihara, Vera A. [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil); Tine, Fernanda D.; Santos, Sandra M.C.; Bonifacio, Rodrigo L.; Taddei, Maria HelenaT. [Comissao Nacional de Energia Nuclear (LAPOC/CNEN-MG), Pocos de Caldas, MG (Brazil). Laboratorio de Pocos de Caldas

    2015-07-01

    The action of determining the concentration of uranium isotopes in biological samples, 'in vitro' bioassay, is an indirect method for evaluating the incorporation and quantification of these radionuclides internally deposited. When incorporated, these radionuclides tend to be disposed through excretion, with urine being the main source of data because it can be easily collected and analyzed. The most widely used methods for determination of uranium isotopes ({sup 234}U, {sup 235}U and {sup 238}U) are Alpha Spectrometry and ICP-MS. This work presents a comparative study for the determination of uranium isotopes using these two methodologies in real samples from occupationally exposed workers. In order to validate the methodology, a sample of the intercomparison exercise organized by PROCORAD (Association pour la Promotion du Controle de Qualite des Analyses de Biologie Medicale em Radiotoxicologie) was used, and the results were statistically compared applying the Student's t-test. (author)

  18. Uranium isotopes determination in urine samples using alpha spectrometry and ICP-MS

    International Nuclear Information System (INIS)

    Rosa, Mychelle M.L.; Maihara, Vera A.; Tine, Fernanda D.; Santos, Sandra M.C.; Bonifacio, Rodrigo L.; Taddei, Maria HelenaT.

    2015-01-01

    The action of determining the concentration of uranium isotopes in biological samples, 'in vitro' bioassay, is an indirect method for evaluating the incorporation and quantification of these radionuclides internally deposited. When incorporated, these radionuclides tend to be disposed through excretion, with urine being the main source of data because it can be easily collected and analyzed. The most widely used methods for determination of uranium isotopes ( 234 U, 235 U and 238 U) are Alpha Spectrometry and ICP-MS. This work presents a comparative study for the determination of uranium isotopes using these two methodologies in real samples from occupationally exposed workers. In order to validate the methodology, a sample of the intercomparison exercise organized by PROCORAD (Association pour la Promotion du Controle de Qualite des Analyses de Biologie Medicale em Radiotoxicologie) was used, and the results were statistically compared applying the Student's t-test. (author)

  19. Sequential Spectrophotometric Method for the Simultaneous Determination of Amlodipine, Valsartan, and Hydrochlorothiazide in Coformulated Tablets

    Directory of Open Access Journals (Sweden)

    Hany W. Darwish

    2013-01-01

    Full Text Available A new, simple and specific spectrophotometric method was developed and validated in accordance with ICH guidelines for the simultaneous estimation of Amlodipine (AML, Valsartan (VAL, and Hydrochlorothiazide (HCT in their ternary mixture. In this method three techniques were used, namely, direct spectrophotometry, ratio subtraction, and isoabsorptive point. Amlodipine (AML was first determined by direct spectrophotometry and then ratio subtraction was applied to remove the AML spectrum from the mixture spectrum. Hydrochlorothiazide (HCT could then be determined directly without interference from Valsartan (VAL which could be determined using the isoabsorptive point theory. The calibration curve is linear over the concentration ranges of 4–32, 4–44 and 6–20 μg/mL for AML, VAL, and HCT, respectively. This method was tested by analyzing synthetic mixtures of the above drugs and was successfully applied to commercial pharmaceutical preparation of the drugs, where the standard deviation is <2 in the assay of raw materials and tablets. The method was validated according to the ICH guidelines and accuracy, precision, repeatability, and robustness were found to be within the acceptable limits.

  20. Experimental results to determine the separation performance of the packages used in cryogenic distillation isotopes

    International Nuclear Information System (INIS)

    Bornea, A.M.; Stefanescu, I.; Zamfirache, M.; Balteanu, O.; Preda, A.

    2007-01-01

    The cryogenic distillation of the hydrogen isotopes represents the back-end separation process most efficient and usually used in detritiation technologies. In our institute there were made many researches in the field of hydrogen isotopes separation. The first results were obtained based on an experimental installation - Pilot Plant for heavy water production - and in present days using a Detritiation Pilot Plant. In our Institute, was manufactured and patented a lot of hydrophilic package for isotopic distillation of water and hydrogen and also catalysts used for isotopic exchange waterhydrogen. This items was continuously developed in order to increase the isotopic separation efficiency. The goal of this paper is to determine by experimental work the performance of the package manufactured in our institute used in the cryogenic distillation process. To describe the separation performances was developed a mathematical model for the cryogenic distillation of the hydrogen isotopes. In order to determine the characteristics of the package, the installation was operated in the total reflux mode, for different flow rate for the liquid. There were made several experiments considering different operating conditions corresponding to various values for the refrigeration power in the column condenser. From the bottom and the top of the distillation column there were extracted samples in order to determine the isotopic composition. Processing the experimental data obtained from these tests using the Fenske relation, we obtained the separation efficiency function of the power inside the column boiler, operating pressure and also pressure drop along the package. This efficiency is describe by the number of theoretical plates per meter (NTT/m) or by equivalent height of one theoretical plate (IETT). (orig.)

  1. Experimental results to determine the separation performance of the packages used in cryogenic distillation isotopes

    Energy Technology Data Exchange (ETDEWEB)

    Bornea, A.M.; Stefanescu, I.; Zamfirache, M.; Balteanu, O.; Preda, A.

    2007-07-01

    The cryogenic distillation of the hydrogen isotopes represents the back-end separation process most efficient and usually used in detritiation technologies. In our institute there were made many researches in the field of hydrogen isotopes separation. The first results were obtained based on an experimental installation - Pilot Plant for heavy water production - and in present days using a Detritiation Pilot Plant. In our Institute, was manufactured and patented a lot of hydrophilic package for isotopic distillation of water and hydrogen and also catalysts used for isotopic exchange waterhydrogen. This items was continuously developed in order to increase the isotopic separation efficiency. The goal of this paper is to determine by experimental work the performance of the package manufactured in our institute used in the cryogenic distillation process. To describe the separation performances was developed a mathematical model for the cryogenic distillation of the hydrogen isotopes. In order to determine the characteristics of the package, the installation was operated in the total reflux mode, for different flow rate for the liquid. There were made several experiments considering different operating conditions corresponding to various values for the refrigeration power in the column condenser. From the bottom and the top of the distillation column there were extracted samples in order to determine the isotopic composition. Processing the experimental data obtained from these tests using the Fenske relation, we obtained the separation efficiency function of the power inside the column boiler, operating pressure and also pressure drop along the package. This efficiency is describe by the number of theoretical plates per meter (NTT/m) or by equivalent height of one theoretical plate (IETT). (orig.)

  2. Determination of the interchangeable heavy-metal fraction in soils by isotope dilution mass spectrometry

    International Nuclear Information System (INIS)

    Gaebler, H.E.; Bahr, A.; Mieke, B.

    1999-01-01

    An isotope dilution technique using enriched stable isotopes is applied to determine the interchangeable heavy-metal fraction in soils. Metals in two soil samples are extracted at constant pH, with water, NH 4 NO 3 , and EDTA. A spike of enriched stable isotopes is added to the suspension of sample and eluant at the beginning of the extraction. The heavy-metal fraction which exchanges with the added spike during the extraction is called the interchangeable fraction. The extractable heavy-metal fractions are obtained from the heavy-metal concentrations in the eluates. Isotope ratios and concentrations are determined by HR-ICP-MS. The isotope dilution technique described enables both the extractable and the interchangeable heavy-metal fractions to be determined in the same experiment. The combination of both results gives additional information on elemental availability under different conditions that cannot be obtained by analyzing the extractable heavy-metal fractions alone. It is demonstrated that in some cases different eluants just shift the distribution of the interchangeable fraction of an element between the solid and liquid phases (e.g., Pb and Cd in a topsoil sample) while the amount of the interchangeable fraction itself remains constant. For other elements, as Ni, Zn, and Cr, the use of different eluants (different pH, complexing agents) sometimes enlarges the interchangeable fraction. (orig.)

  3. Determination of trace quantities of uranium in rocks mass spectrometric isotope dilution technique

    International Nuclear Information System (INIS)

    Kakazu, Mauricio Hiromitu

    1980-01-01

    A detailed experimental investigation on the thermionic emission of uranium deposited on a single flat type rhenium filament has been carried out. The study was aimed at determining the influence of various forms of deposition on the emission sensitivity and thermal stability of U + , UO + and UO 2 + ions. Based on these investigations, a technique, involving an addition of a small quantity of colloidal suspension of graphite on top of the uranyl nitrate sample deposited, was chosen because of its higher, emission sensitivity for uranium metal ions. The experimental parameters of the technique were optimised and the technique was employed in the determination of trace quantities of uranium in rock samples using mass spectrometric isotope dilution method. For the mass spectrometric isotope dilution analysis National Bureau of Standards uranium isotopic standard NBS-U 970 was employed as a tracer, where as the mass discrimination effect in the uranium isotope analysis was corrected using the uranium isotopic standard NBS-U500. Uranium was determined in each of the seven granite samples from Wyoming, USA and two USGS standard rocks. The precision of the analysis was found to be ±1% . The uranium values obtained on the rock samples were compared with the analyses of other investigators. Influence of the sample splitting on the uranium analysis was discussed in the light of the analytical results obtained.(author)

  4. Exploiting flow Injection and sequential injection schemes for trace metal determinations by electrothermal atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Hansen, Elo Harald

    Determination of low or trace-level amounts of metals by electrothermal atomic absorption spectrometry (ETAAS) often requires the use of suitable preconcentration and/or separation procedures in order to attain the necessary sensitivity and selectivity. Such schemes are advantageously executed...... by superior performance and versatility. In fact, two approaches are conceivable: The analyte-loaded ion-exchange beads might either be transported directly into the graphite tube where they are pyrolized and the measurand is atomized and quantified; or the loaded beads can be eluted and the eluate forwarded...

  5. Sequential spectrofluorimetric determination of free and total glycerol in biodiesel in a multicommuted flow system

    Energy Technology Data Exchange (ETDEWEB)

    Silva, Sidnei G. [Universidade de Sao Paulo, Instituto de Quimica, Sao Paulo (Brazil); Morales-Rubio, Angel; Guardia, Miguel de la [Universidad de Valencia, Department of Analytical Chemistry, Burjassot, Valencia (Spain); Rocha, Fabio R.P. [Universidade de Sao Paulo, Centro de Energia Nuclear na Agricultura, Piracicaba (Brazil)

    2011-07-15

    A new procedure for spectrofluorimetric determination of free and total glycerol in biodiesel samples is presented. It is based on the oxidation of glycerol by periodate, forming formaldehyde, which reacts with acetylacetone, producing the luminescent 3,5-diacetyl-1,4-dihydrolutidine. A flow system with solenoid micro-pumps is proposed for solution handling. Free glycerol was extracted off-line from biodiesel samples with water, and total glycerol was converted to free glycerol by saponification with sodium ethylate under sonication. For free glycerol, a linear response was observed from 5 to 70 mg L{sup -1} with a detection limit of 0.5 mg L{sup -1}, which corresponds to 2 mg kg{sup -1} in biodiesel. The coefficient of variation was 0.9% (20 mg L{sup -1}, n = 10). For total glycerol, samples were diluted on-line, and the linear response range was 25 to 300 mg L{sup -1}. The detection limit was 1.4 mg L{sup -1} (2.8 mg kg{sup -1} in biodiesel) with a coefficient of variation of 1.4% (200 mg L{sup -1}, n = 10). The sampling rate was ca. 35 samples h{sup -1} and the procedure was applied to determination of free and total glycerol in biodiesel samples from soybean, cottonseed, and castor beans. (orig.)

  6. Microcomputer Assisted Interpretative Reporting of Sequential Creatine Kinase (CK) and Lactate Dehydrogenase (LDH) Isoenzyme Determination

    Science.gov (United States)

    Talamo, Thomas S.; Losos, Frank J.; Mercer, Donald W.

    1984-01-01

    We have developed a microcomputer based system for interpretative reporting of creatine kinase (CK) and lactate dehydrogenase (LDH) isoenzyme studies. Patient demographic data and test results (total CK, CK-MB, LD-1, and LD-2) are entered manually through the keyboard. The test results are compared with normal range values and an interpretative report is generated. This report consists of all pertinent demographic information with a graphic display of up to 12 previous CK and LDH isoenzyme determinations. Diagnostic interpretative statements are printed beneath the graphic display following analysis of previously entered test results. The combination of graphic data display and interpretations based on analysis of up to 12 previous specimens provides useful and accurate information to the cardiologist.

  7. Determination of thorium and uranium isotopes in the mining lixiviation liquor samples

    Energy Technology Data Exchange (ETDEWEB)

    Reis Júnior, Aluísio de Souza; Monteiro, Roberto Pellacani Guedes, E-mail: reisas@cdtn.br [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN-MG), Belo Horizonte, MG (Brazil)

    2017-07-01

    The alpha spectrometric analysis refers to determination of thorium and uranium isotopes in the mining lixiviation liquor samples. The analytical procedure involves sample preparation steps for rare earth elements, thorium and uranium separation using selective etching with hydrofluoric acid and further radiochemical separation of these using TRU chromatographic resins (Eichrom Industries Inc. USA) besides electroplating of the isolated radionuclides. An isotopic tracer is used to determine the overall chemical yield and to ensure traceability to a national standard. The results are compared to results obtained for the same samples by Becquerel laboratory. We improved the method looking for reproducibility and isotopes isolation as required by alpha spectrometry and the method showing effective in analysis of mining liquor. (author)

  8. Determination of thorium and uranium isotopes in the mining lixiviation liquor samples

    International Nuclear Information System (INIS)

    Reis Júnior, Aluísio de Souza; Monteiro, Roberto Pellacani Guedes

    2017-01-01

    The alpha spectrometric analysis refers to determination of thorium and uranium isotopes in the mining lixiviation liquor samples. The analytical procedure involves sample preparation steps for rare earth elements, thorium and uranium separation using selective etching with hydrofluoric acid and further radiochemical separation of these using TRU chromatographic resins (Eichrom Industries Inc. USA) besides electroplating of the isolated radionuclides. An isotopic tracer is used to determine the overall chemical yield and to ensure traceability to a national standard. The results are compared to results obtained for the same samples by Becquerel laboratory. We improved the method looking for reproducibility and isotopes isolation as required by alpha spectrometry and the method showing effective in analysis of mining liquor. (author)

  9. Interlaboratory determinations of isotopically enriched metals by field desorption mass spectroscopy

    International Nuclear Information System (INIS)

    Bahr, U.; Schulten, H.R.; Achenbach, C.; Ziskoven, R.

    1982-01-01

    The isotopic distribution of stable isotopes in six enriched metals (calcium, copper, barium, rubidium, strontium and thallium) has been determined by field desorption mass spectrometry. A first evaluation of the interlaboratory reproducibility of the application of this method for trace determination of metals was made using three different types of mass spectrometers in three different laboratories. The standard deviations for the most abundant isotopes of the metals investigated are between +-0.1 and +-0.5%. Within these standard deviations, the values obtained by the three mass spectrometry groups are the same. To support the accuracy of our quantification, thermal ionization mass spectrometry has been employed and confirms the results of the field desorption method. (orig.) [de

  10. Growth versus metabolic tissue replacement in mouse tissues determined by stable carbon and nitrogen isotope analysis

    Science.gov (United States)

    Macavoy, S. E.; Jamil, T.; Macko, S. A.; Arneson, L. S.

    2003-12-01

    Stable isotope analysis is becoming an extensively used tool in animal ecology. The isotopes most commonly used for analysis in terrestrial systems are those of carbon and nitrogen, due to differential carbon fractionation in C3 and C4 plants, and the approximately 3‰ enrichment in 15N per trophic level. Although isotope signatures in animal tissues presumably reflect the local food web, analysis is often complicated by differential nutrient routing and fractionation by tissues, and by the possibility that large organisms are not in isotopic equilibrium with the foods available in their immediate environment. Additionally, the rate at which organisms incorporate the isotope signature of a food through both growth and metabolic tissue replacement is largely unknown. In this study we have assessed the rate of carbon and nitrogen isotopic turnover in liver, muscle and blood in mice following a diet change. By determining growth rates, we were able to determine the proportion of tissue turnover caused by growth versus that caused by metabolic tissue replacement. Growth was found to account for approximately 10% of observed tissue turnover in sexually mature mice (Mus musculus). Blood carbon was found to have the shortest half-life (16.9 days), followed by muscle (24.7 days). Liver carbon turnover was not as well described by the exponential decay equations as other tissues. However, substantial liver carbon turnover was observed by the 28th day after diet switch. Surprisingly, these tissues primarily reflect the carbon signature of the protein, rather than carbohydrate, source in their diet. The nitrogen signature in all tissues was enriched by 3 - 5‰ over their dietary protein source, depending on tissue type, and the isotopic turnover rates were comparable to those observed in carbon.

  11. Determination of the total acidity in soft drinks using potentiometric sequential injection titration.

    Science.gov (United States)

    van Staden, J Koos F; Mashamba, M Mulalo G; Stefan, R Raluca I

    2002-12-06

    A potentiometric SI titration system for the determination of total acidity in soft drinks is proposed. The concept is based on the aspiration of the acid soft drink sample between two base zones into a holding coil with the volume of the first base zone twice to that of the second one and channelled by flow reversal through a reaction coil to a potentiometric sensor. A solution of 0.1 mol l(-1) sodium chloride is used as ionic strength adjustment buffer in the carrier stream. The system has been applied to the analysis of some South African soft drinks having a total acidity level of about 0.2-0.3% (w/v). The method has a sample frequency of 45 samples per h with a linear range of 0.1 and 0.6% (w/v). It is easy to use, fully computerised, and gives the results that are comparable to both automated batch titration and manual titration.

  12. ICP-MS as the method of the determination of gallium, indium and thallium isotope ratios in the studies of isotope effects in the chromatography systems

    International Nuclear Information System (INIS)

    Herdzik, I.

    2006-01-01

    The procedure of the determination of gallium, indium and thallium isotope ratios and its application to the studies of the isotope effects in chromatography systems by the ICP-MS method (inductively coupled plasma-mass spectrometry) are presented. It was shown that it is possible to determine the isotope ratios of gallium ( 69/71 Ga), indium ( 113/115 In) and thallium ( 203/205 Tl) with the relative standard deviation 0.03-0.07%. Such precision appeared to be sufficient to calculate the unit separation factors in the column chromatographic processes. (author) [pl

  13. Determination of the hydrogen isotopic compositions of organic materials and hydrous minerals using thermal combustion laser spectroscopy.

    Science.gov (United States)

    Koehler, Geoff; Wassenaar, Leonard I

    2012-04-17

    Hydrogen isotopic compositions of hydrous minerals and organic materials were measured by combustion to water, followed by optical isotopic analysis of the water vapor by off-axis integrated cavity output spectroscopy. Hydrogen and oxygen isotopic compositions were calculated by numerical integration of the individual isotopologue concentrations measured by the optical spectrometer. Rapid oxygen isotope exchange occurs within the combustion reactor between water vapor and molecular oxygen so that only hydrogen isotope compositions may be determined. Over a wide range in sample sizes, precisions were ±3-4 per mil. This is comparable but worse than continuous flow-isotope ratio mass spectroscopy (CF-IRMS) methods owing to memory effects inherent in water vapor transfer. Nevertheless, the simplicity and reduced cost of this analysis compared to classical IRMS or CF-IRMS methods make this an attractive option to determine the hydrogen isotopic composition of organic materials where the utmost precision or small sample sizes are not needed.

  14. Sequential determination of multi-nutrient elements in natural water samples with a reverse flow injection system.

    Science.gov (United States)

    Lin, Kunning; Ma, Jian; Yuan, Dongxing; Feng, Sichao; Su, Haitao; Huang, Yongming; Shangguan, Qipei

    2017-05-15

    An integrated system was developed for automatic and sequential determination of NO 2 - , NO 3 - , PO 4 3- , Fe 2+ , Fe 3+ and Mn 2+ in natural waters based on reverse flow injection analysis combined with spectrophotometric detection. The system operation was controlled by a single chip microcomputer and laboratory-programmed software written in LabVIEW. The experimental parameters for each nutrient element analysis were optimized based on a univariate experimental design, and interferences from common ions were evaluated. The upper limits of the linear range (along with detection limit, µmolL -1 ) of the proposed method was 20 (0.03), 200 (0.7), 12 (0.3), 5 (0.03), 5 (0.03), 9 (0.2) µmolL -1 , for NO 2 - , NO 3 - , PO 4 3- , Fe 2+ , Fe 3+ and Mn 2+ , respectively. The relative standard deviations were below 5% (n=9-13) and the recoveries varied from 88.0±1.0% to 104.5±1.0% for spiked water samples. The sample throughput was about 20h -1 . This system has been successfully applied for the determination of multi-nutrient elements in different kinds of water samples and showed good agreement with reference methods (slope 1.0260±0.0043, R 2 =0.9991, n=50). Copyright © 2017 Elsevier B.V. All rights reserved.

  15. Speciation of 210Po and 210Pb in air particulates determined by sequential extraction

    International Nuclear Information System (INIS)

    Al-Masri, M.S.; Al-Karfan, K.; Khalili, H.; Hassan, M.

    2006-01-01

    Speciation of 210 Po and 210 Pb in air particulates of two Syrian phosphate sites with different climate conditions has been studied. The sites are the mines and Tartous port at the Mediterranean Sea. Air filters were collected during September 2000 until February 2002 and extracted chemically using different selective fluids in an attempt to identify the different forms of these two radionuclides. The results have shown that the inorganic and insoluble 21 Po and 21 Pb (attached to silica and soluble in mineral acids) portion was found to be high in both sites and reached a maximum value of 94% and 77% in the mine site and Tartous port site, respectively. In addition, only 24% of 21 Pb in air particulates was found to be associated with organic materials probably produced from the incomplete burning of fuel vehicle and similar activities. Moreover, the 210 Po/ 21- Pb activity ratio in air particulates was higher than that in all samples at both sites and varied between 3.85 in November 2000 at Tartous port site and 20 in April 2001 at the mine area. These activity ratios were also higher than the natural levels. The 210 Po/ 210 Pb activity ratio was also determined in each portion resulting from the selective extraction and found to be higher than that in most samples. The sources of 210 Po excess in these portions are discussed. Soil suspension, which is common in the dry climate dominant in the area, sea water spray and heating of phosphate ores were considered; polonium is more volatile than the lead compounds at even moderate temperature. Furthermore, variations in the chemical forms of 210 Po and 210 Pb during the year were also investigated. However, the results of this study can also be utilized for dose assessment to phosphate industry workers

  16. Speciation of 210Po and 210Pb in air particulates determined by sequential extraction.

    Science.gov (United States)

    Al-Masri, M S; Al-Karfan, K; Khalili, H; Hassan, M

    2006-01-01

    Speciation of (210)Po and (210)Pb in air particulates of two Syrian phosphate sites with different climate conditions has been studied. The sites are the mines and Tartous port at the Mediterranean Sea. Air filters were collected during September 2000 until February 2002 and extracted chemically using different selective fluids in an attempt to identify the different forms of these two radionuclides. The results have shown that the inorganic and insoluble (210)Po and (210)Pb (attached to silica and soluble in mineral acids) portion was found to be high in both sites and reached a maximum value of 94% and 77% in the mine site and Tartous port site, respectively. In addition, only 24% of (210)Pb in air particulates was found to be associated with organic materials probably produced from the incomplete burning of fuel vehicle and similar activities. Moreover, the (210)Po/(210)Pb activity ratio in air particulates was higher than that in all samples at both sites and varied between 3.85 in November 2000 at Tartous port site and 20 in April 2001 at the mine area. These activity ratios were also higher than the natural levels. The (210)Po/(210)Pb activity ratio was also determined in each portion resulting from the selective extraction and found to be higher than that in most samples. The sources of (210)Po excess in these portions are discussed. Soil suspension, which is common in the dry climate dominant in the area, sea water spray and heating of phosphate ores were considered; polonium is more volatile than the lead compounds at even moderate temperature. Furthermore, variations in the chemical forms of (210)Po and (210)Pb during the year were also investigated. However, the results of this study can also be utilized for dose assessment to phosphate industry workers.

  17. Spectrophotometric-isotope dilution determination of arsenic in soils and rock

    Science.gov (United States)

    Brown, F.W.; Simon, F.O.; Greenland, L.P.

    1975-01-01

    Arsenic in soil and rock samples may be determined in part-per-million concentrations using a radiochemical-isotope dilution method. Arsenic in the sample plus added As76 tracer is separated as arsine and determined spectrophotometrically as a molybdenum blue complex. The As76 activity in the absorbing solution allows corrections for chemical losses. A lower limit of 1 ppm is determinate in a 0.5-g sample.

  18. Determination of cortisol in blood plasma by isotopic dilution

    International Nuclear Information System (INIS)

    Shimizu, T.

    1978-01-01

    A method to measure cortisol in blood plasma is developed using tritium a tracer. Thin-layer chromatographer is used for very accurate separation and determination of cortisol free of impurities. Results show a concentration of 14,02+-5,79 μg/100ml for cortisol in blod. This method appears to be especially useful when interfering substances are present [pt

  19. Direct isotope determination of isotopically labelled lipids by field desorption mass spectrometry

    International Nuclear Information System (INIS)

    Lehmann, W.D.; Kessler, M.

    1982-01-01

    Lipids labelled with deuterium or carbon-14 have been investigated by field desorption mass spectrometry for determination of their degree of labelling. This application is demonstrated for free fatty acids, cholesterol, cholesteryl esters, triglycerides, and L-α-phosphatidylcholines. Comparison of the molecular ion groups of the non-labelled and of the labelled compounds enables a fast and reliable determination of the degree of labelling. For multiply labelled compounds the label distribution is also obtained from the molecular ion group. In addition, for cholesteryl esters and for phosphatidylcholines structurally significant fragment ions provide information about the position of the label. Several hundred nanograms of the compound are typically required for a single analysis with a relative standard error of 0.5-2% in the value calculated for atom% hydrogen-2 or for the specific carbon-14 activity. (orig.) [de

  20. Analysis of carbon stable isotope to determine the origin and migration of gaseous hydrocarbon in the Brazilian sedimentary basins

    International Nuclear Information System (INIS)

    Takaki, T.; Rodrigues, R.

    1986-01-01

    The carbon isotopic composition of natural gases to determine the origin and gaseous hydrocarbon migration of Brazilian sedimentar basins is analysed. The carbon isotopic ratio of methane from natural gases depends on the process of gas formation and stage of organic matter maturation. In the geochemical surface exploration the biogenic gases are differentiated from thermogenic gases, because the last one is isotopically heavier. As the isotopic composition of methane has not changed during migration, the migrated gases from deeper and more mature source rocks are identified by its relative 13 C enrichment. The methane was separated from chromatography and and the isotopic analysis was done with mass spectrometer. (M.C.K.) [pt

  1. Nuclear yield determinations using isotope-separator-on-line arrangements

    International Nuclear Information System (INIS)

    Rudstam, G.

    1975-01-01

    The delay between the formation of a nuclear reaction product and its collection in front of measuring equipment in ISOL arrangements using integrated target-ion source systems has been analyzed. It is shown that a typical delay function takes the form const x (1-esup(-γt))esup(-μt) with γ >> μ. The results can be used for decay corrections in nuclear yield determinations. (Auth.)

  2. Determination of the isotopic composition of natural and slightly enriched uranium by alpha-spectrometry

    DEFF Research Database (Denmark)

    Kunzendorf, Helmar

    1968-01-01

    Determinations of the isotope contents of 238U, 235U and 234U in five uranium samples containing 0–5 at% 235U were carried out on the basis of a least-squares fit of the α-spectra from the samples, measured with a semiconductor detector, to the theoretically expected α-spectra. With a simple source...

  3. Determination of traces of iridium with thiodibenzoylmethane by substoichiometric isotope dilution analysis

    International Nuclear Information System (INIS)

    Roebisch, G.; Bansse, W.; Ludwig, E.

    1980-01-01

    Iridium(III or IV) reacts with thiodibenzoylmethane on heating at pH 6 to form a 1:3 complex, which can be concentrated by extraction into chloroform. Based on this reaction, a reproducible, selective determination of iridium is achieved by means of substoichiometric isotope dilution analysis, based on 192 Ir. The linear range is 1-11 nmol of iridium. (Auth.)

  4. Alpha low activity determination from limitter isotopes of uranium, thorium ands radium in natural waters

    International Nuclear Information System (INIS)

    Gascon, J.L.; Crespo, M.T.; Acena, M.L.

    1989-01-01

    A method to concentrate uranium, thorium and radium in natural waters has been developed. The method, based on the adsorbing propert-ies of manganes dioxide, has been applied to determine the alpha emitter isotopes of these elements in drinking water of Madrid. In this work we present the description of the method, the analytical procedu-res and the obtained results. (Author)

  5. Determination of tin equilibrium isotope fractionation factors from synchrotron radiation experiments

    NARCIS (Netherlands)

    Polyakov, VB; Mineev, SD; Clayton, RN; Hu, G; Mineev, KS

    2005-01-01

    A method of determination of the reduced isotopic partition function ratio (beta-factor) from the partial density of state (PDOS) obtained by inelastic nuclear resonant X-ray scattering (INRXS) in synchrotron radiation experiments has been established. The method has been demonstrated by the example

  6. Thallium determination in reference materials by isotope dilution mass spectrometry (IDMS) using thermal ionization

    International Nuclear Information System (INIS)

    Waidmann, E.; Hilpert, K.; Stoeppler, M.

    1990-01-01

    Using Isotope Dilution Mass Spectrometry (IDMS) with thermal ionization, thallium concentrations were determined in reference materials from NIST and BCR, from other sources, and reference materials from the German Environmental Specimen Bank 203 Tl spike solution is applied for the isotope dilution technique. Thallium concentrations in the investigated materials range from 2.67 μg Tl.kg -1 to 963 μg Tl.kg -1 with a relative standard deviation from 0.14 to 10%. The detection limit was 0.1 ng thallium for this work. (orig.)

  7. Determination of molybdenum in plant reference material by thermal-ionization isotope-dilution mass spectrometry

    International Nuclear Information System (INIS)

    Saumer, M.; Gantner, E.; Reinhardt, J.; Ache, H.J.

    1992-01-01

    An analytical method is described for the determination of the concentration and the isotopic composition of molybdenum in plant samples using thermal ionization mass spectrometry. After microwave acid digestion and liquid-liquid extractive separation with Amberlite LA-2, the molybdenum isotopes are measured as MoO 3 - -ions in a quadrupole mass spectrometer. In all cases, the relative standard deviation of the measurements of both natural and spike molybdenum was better than 3% for all ratios measured. The concentration of molybdenum found in three different plant reference materials agreed well with the certified values. (orig.)

  8. Determination of plutonium isotopic ratios and total concentration by gamma ray spectrometry

    International Nuclear Information System (INIS)

    Despres, Michele.

    1980-11-01

    A non-destructive method of analysis is being investigated for the control in situ of plutonium isotopic composition and total concentration in different matrix without preliminary calibration. The plutonium isotopic composition is determined by gamma-ray spectrometry using germanium detector systems. The same apparatus is used for direct measuring of the total plutonium concentration in solutions or solids by a differential attenuation technique based on two transmitted gamma rays with energies on both sides of the k shell absorption edge of plutonium [fr

  9. Determination of plutonium isotopes in waters and environmental solids: A review

    DEFF Research Database (Denmark)

    Qiao, Jixin; Hou, Xiaolin; Miró, Manuel

    2009-01-01

    A number of analytical methods have been developed in the past few years for environmental monitoring of plutonium (Pu) isotopes around nuclear facilities within protocols for emergency preparedness as well as for risk assessment of contaminated areas resulting from nuclear weapon tests, nuclear...... accidents, and the discharge of nuclear waste. This article summarizes and critically compares recently reported methods for determination of Pu isotopes in waters and environmental solid substrates, in which sample pre-treatment is imperative for separation of the target species from matrix ingredients and...

  10. Determining Isotopic Composition of Dissolved Nitrate Using Bacterial Denitrification Followed by Laser Spectroscopy

    International Nuclear Information System (INIS)

    Yan Tiezhu; Lee Zhi Yi, Amelia; Heiling, Maria; Weltin, Georg; Toloza, Arsenio; Resch, Christian

    2016-01-01

    Nitrate (NO 3 - ) pollution is a prevalent problem that can cause water quality degradation and eutrophication of water bodies. Quantifying the nitrogen and oxygen isotopic composition of nitrates will allow for better identification of their potential sources, which in turn will assist in remediation of contaminated water and the designing of future water management practices. In this research bacterial denitrification followed by laser spectroscopy are used to determine isotopic composition of δ 15 N and δ 18 O of dissolved nitrates. The objective of the project is to establish a standard operating procedure (SOP) that outlines the best practices for both methods in sequence and designed to be used as a technical guideline

  11. Comparison of different methods of determining plutonium content and isotopic composition

    International Nuclear Information System (INIS)

    Dowell, M.R.W.

    1985-05-01

    At Rockwell Hanford Operations, several different methods are used to determine plutonium content and isotopic composition. These include alpha particle energy analysis, calorimetry/gamma-ray analysis, mass spectrometry, and low energy ray assay. Each is used in a process control environment and has its advantages and disadvantages in terms of sample matrix, sample preparation, concentration, error ranges, detection limits, and turn around time. Of the methods discussed, special attention is paid to the Plutonium Isotopics Solution Counter, a low energy gamma ray assay system designed to provide plutonium and americium content and isotopic composition of Pu-238 through Pu-241 and Am-241. It is qualitatively and quantitatively compared to the other methods. A brief description of sample types which the Solution Counter analyzes is presented. 4 refs., 4 tabs

  12. Comparison of different methods of determining plutonium content and isotopic composition

    International Nuclear Information System (INIS)

    Anon.

    1986-01-01

    At Rockwell Hanford Operations, several different methods are used to determine plutonium content and isotopic composition. These include alpha particle energy analysis, calorimetry/gamma-ray analysis, mass spectrometry, and low energy gamma-ray assay. Each is used in a process control environment and has its advantages and disadvantages in terms of sample matrix, sample preparation, concentration, error ranges, detection limits, and turn around time. Of the methods discussed, special attention is paid to the Plutonium Isotopics Solution Counter, a low energy gamma-ray assay system designed to provide plutonium and americium content and isotopic composition of Pu-238 through Pu-241 and Am-241. It is qualitatively and quantitatively compared to the other methods. A brief description of sample types which the Solution Counter analyzes is presented

  13. Sequential Path Analysis for Determination of Relationship Between Yield and Yield Components in Bread Wheat (Triticum aestivum.L.

    Directory of Open Access Journals (Sweden)

    Mohtasham MOHAMMADI

    2014-03-01

    Full Text Available An experiment was conducted to evaluate 295 wheat genotypes in Alpha-Lattice design with two replications. The arithmetic mean and standard deviation of grain yield was 2706 and 950 (kg/ha,respectively. The results of correlation coefficients indicated that grain yield had significant and positive association with plant height, spike length, early growth vigor and agronomic score. Whereas there were negative correlation coefficients between grain yield and days to physiological maturity and canopy temperature before and during anthesis. Path analysis indicated agronomic score and plant height had high positive direct effects on grain yield, while canopy temperature before and during anthesis, and days to maturity, wes another trait having negative direct effect on grain yield. The results of sequential path analysis showed the traits that accounted as a criteria variable for high grain yield were agronomic score, plant height, canopy temperature, spike length, chlorophyll content and early growth vigor, which were determined as first, second and third order variables and had strong effects on grain yield via one or more paths. More important, as canopy temperature, agronomic score and early growth vigor can be evaluated quickly and easily, these traits may be used for evaluation of large populations.

  14. Experimental determination of the Mo isotope fractionation factor between metal and silicate liquids

    Science.gov (United States)

    Hin, R. C.; Burkhardt, C.; Schmidt, M. W.; Bourdon, B.

    2011-12-01

    The conditions and chemical consequences of core formation have mainly been reconstructed from experimentally determined element partition coefficients between metal and silicate liquids. However, first order questions such as the mode of core formation or the nature of the light element(s) in the Earth's core are still debated [1]. In addition, the geocentric design of most experimental studies leaves the conditions of core formation on other terrestrial planets and asteroids even more uncertain than for Earth. Through mass spectrometry, records of mass-dependent stable isotope fractionation during high-temperature processes such as metal-silicate segregation are detectable. Stable isotope fractionation may thus yield additional constrains on core formation conditions and its consequences for the chemical evolution of planetary objects. Experimental investigations of equilibrium mass-dependent stable isotope fractionation have shown that Si isotopes fractionate between metal and silicate liquids at temperatures of 1800°C and pressures of 1 GPa, while Fe isotopes leave no resolvable traces of core formation processes [2,3]. Molybdenum is a refractory and siderophile trace element in the Earth, and thus much less prone to complications arising from mass balancing core and mantle and from potential volatile behaviour than other elements. To determine equilibrium mass-dependent Mo isotope fractionation during metal-silicate segregation, we have designed piston cylinder experiments with a basaltic silicate composition and an iron based metal with ~8 wt% Mo, using both graphite and MgO capsules. Metal and silicate phases are completely segregated by the use of a centrifuging piston cylinder at ETH Zurich, thus preventing analysis of mixed metal and silicate signatures. Molybdenum isotope compositions were measured using a Nu Instruments 1700 MC-ICP-MS at ETH Zurich. To ensure an accurate correction of analytical mass fractionation a 100Mo-97Mo double spike was admixed

  15. A high volume sampling system for isotope determination of volatile halocarbons and hydrocarbons

    Directory of Open Access Journals (Sweden)

    E. Bahlmann

    2011-10-01

    Full Text Available The isotopic composition of volatile organic compounds (VOCs can provide valuable information on their sources and fate not deducible from mixing ratios alone. In particular the reported carbon stable isotope ratios of chloromethane and bromomethane from different sources cover a δ13C-range of almost 100‰ making isotope ratios a very promising tool for studying the biogeochemistry of these compounds. So far, the determination of the isotopic composition of C1 and C2 halocarbons others than chloromethane is hampered by their low mixing ratios.

    In order to determine the carbon isotopic composition of C1 and C2 halocarbons with mixing ratios as low as 1 pptv (i a field suitable cryogenic high volume sampling system and (ii a chromatographic set up for processing these samples have been developed and validated. The sampling system was tested at two different sampling sites, an urban and a coastal location in Northern Germany. The average δ13C-values for bromomethane at the urban site were −42.9 ± 1.1‰ and agreed well with previously published results. But at the coastal site bromomethane was substantially enriched in 13C by almost 10‰. Less pronounced differences were observed for chlorodifluoromethane, 1,1,1-trichloroethane and chloromethane. We suggest that these differences are related to the turnover of these compounds in ocean surface waters. Furthermore we report first carbon isotope ratios for iodomethane (−40.4‰ to −79.8‰, bromoform (−13.8‰ to 22.9‰, and other halocarbons.

  16. Determination of natural Ra isotopes in samples from northern Sao Paulo state coastal area

    International Nuclear Information System (INIS)

    Teixeira, Washington Eugenio

    2004-01-01

    The present work aims the determination of natural Ra isotopes in coastal samples collected at Ubatuba region, with the application of the obtained inventories to estimate coastal water mixing rates and assess submarine groundwater discharge. Since these radionuclides are present in sea water in trace form (10''- 16 g/ L), the methodology included pre-concentration of huge volumes of sea water using MnO 2 coated acrylic fiber, leaching of these fibers in HCl media and co-precipitation of the long-lived Ra isotopes with BaSO 4 . Before long-lived radium isotopes determination, the isotopes 223 Ra e 224 Ra were quantified using a delayed coincidence system. The delayed coincidence system utilizes the difference in decay constants of the short-lived Po daughters of radon 219 Rn and 220 Rn to identify alpha particles derived from its decay products. The activities of 226 Ra and 228 Ra were determined by gross alpha and beta counting respectively, of the Ba(Ra)SO 4 precipitate in low-level gas flow proportional detector. Considering the results obtained in 2002 and 2003, the coastal waters exchange time were estimated for Flamengo, Fortaleza and Mar Virado embayments using the activity concentrations of 223 Ra, 224 Ra, 226 Ra and 228 Ra. (author)

  17. Sequential extraction combined with isotope analysis as a tool for the investigation of lead mobilisation in soils: Application to organic-rich soils in an upland catchment in Scotland

    International Nuclear Information System (INIS)

    Bacon, Jeffrey R.; Farmer, John G.; Dunn, Sarah M.; Graham, Margaret C.; Vinogradoff, Susan I.

    2006-01-01

    Sequential extraction (modified BCR procedure) combined with isotope analysis has been investigated as a tool for assessing mobilisation of lead into streams at an upland catchment in NE Scotland. The maximum lead concentrations (up to 110 mg kg -1 in air-dried soil) occurred not at the surface but at about 10 cm depth. The lowest 206 Pb/ 207 Pb ratios in any profile occurred, with one exception, at 2.5-5 cm depth. In the one exception, closest to the only road in the area, significantly lower 206 Pb/ 207 Pb ratios in the surface soil together with much increased chloride concentrations (in comparison to other surface waters) indicated the possible mobilisation of roadside lead and transfer to the stream. The 206 Pb/ 207 Pb ratios in extractable fractions tended at depth towards the ratio measured in the residual phase but the ratios in the oxidizable fraction increased to a value higher than that of the residual phase. - Sequential extraction combined with isotope analysis was used as a tool to assess mobilisation of lead into streams

  18. Determination of phosphorus traces in platinum alloys by two-phase isotope exchange

    International Nuclear Information System (INIS)

    Vlacil, F.

    1980-01-01

    The method of ZEMAN and KRATZER for the determination of phosphorus traces by means of two-phase isotope exchange was modified for the determination of phosphorus in pure platinum or pure platinum alloys. It was found that Pt, Rh, Ag and As do not interfere with the determination. Among the elements usually present in platinum metal or platinum alloys, only gold interferes. It was removed by extraction from 7M HCl by MIBK and AmOAc. Hydrochloric acid also interferes but it can be removed by evaporation. The analytical procedure is given for the solution obtained by pressure decomposition of the sample (0.5 g) in a steel bomb with PTFE inlay. It is possible to determine > 2 ppm P (approximate error -10%). If using calibration dependence instead of the well known equation for isotope exchange it is not necessary to know the content of P in the standard solution labelled with 32 P. (author)

  19. Determination of radium isotopes by BaSO4 coprecipitation for the preparation of alpha-spectrometric sources

    International Nuclear Information System (INIS)

    Lozano, J.C.; Fernandez, F.; Gomez, J.M.G.

    1997-01-01

    A coprecipitation procedure for the preparation of α-spectrometric sources for radium, using BaSO 4 as carrier, has been applied to the determination of alpha radium isotopes in water samples. The use of 133 Ba as a suitable tracer for radium determination and possible losses of radon isotopes from the sources are studied and discussed. (author)

  20. High-Precision Direct Mass Determination of Unstable Isotopes

    CERN Multimedia

    2002-01-01

    The extension of systematic high-precision measurements of the nuclear mass to nuclei far from the valley of $\\beta$ stability is of great interest in nuclear physics and astrophysics. The mass, or binding energy, is a fundamental gross property and a key input parameter for nuclear matter calculations. It is also a sensitive probe for collective and single-particle effects in nuclear structure. \\\\ \\\\ For such purposes, nuclear masses need to be known to an accuracy of about 10$^{-7}$ (i.e. $\\Delta$M~$\\leq$~10~keV for A~=~100). To resolve a particular mass from its nuclear isomers and isobars, resolving power of 10$^6$ are often required. To achieve this, the ions delivered by the on-line mass separator ISOLDE are confined in a Penning quadrupole trap. This trap is placed in the very homogeneous and stable magnetic field of a superconducting magnet. Here, the cyclotron frequency and hence the mass are determined. \\\\ \\\\ The first measurements using this new technique have been completed for a long chain of Cs ...

  1. Magnesium isotope compositions of Solar System materials determined by double spiking

    Science.gov (United States)

    Hin, R.; Lai, Y. J.; Coath, C.; Elliott, T.

    2015-12-01

    As a major element, magnesium is of interest for investigating large scale processes governing the formation and evolution of rocky planetary bodies. Determining the Mg isotope composition of the Earth and other planetary bodies has hence been a topic of interest ever since mass-dependent fractionation of 'non-traditional' stable isotopes has been used to study high-temperature processes. Published results, however, suffer from disagreement on the Mg isotope compositions of the Earth and chondrites [1-5], which is attributed to residual matrix effects. Nonetheless, most recent studied have converged towards a homogeneous (chondritic) Mg isotope composition in the Solar System [2-5]. However, in several of the recent studies there is a hint of a systematic difference of about 0.02-0.06‰ in the 26Mg/24Mg isotope compositions of chondrites and Earth. Such difference, however, is only resolvable by taking standard errors, which assumes robust data for homogenous sample sets. The discrepancies between various studies unfortunately undermine the confidence in such robustness and homogeneity. The issues with matrix effects during isotopic analyses can be overcome by using a double spike approach. Such methodology generally requires three isotope ratios to solve for three unknowns, a requirement that cannot be met for Mg. However, using a newly developed approach, we present Mg isotope compositions obtained by critical mixture double spiking. This new approach should allow greater confidence in the robustness of the data and hence enable improvement of. Preliminary data indicate that chondrites have a resolvable ~0.04‰ lighter 26Mg/24Mg than (ultra)mafic rocks from Earth, Mars and the eucrite parent body, which appear indistinguishable from each other. It seems implausible that this difference is caused by magmatic process such as partial melting or crystallisation. More likely, Mg isotopes are fractionated by a non-magmatic process during the formation of planets, e

  2. Neutron activation determination of phosphorus and sulfur in semiconductor materials by 32P-isotope

    International Nuclear Information System (INIS)

    Nikolaev, A.V.; Gol'dshtejn, M.M.; Gil'bert, Eh.N.; Verevkin, G.V.; Yudelevich, I.G.

    1977-01-01

    A neutron-activation method has been developed for determining phosphorus and sulphur in germanium, gallium, gallium arsenide, and silicon structures using 32 P isotope. The dioctyl-sulphoxide (DOSO) extraction of phosphoric molybdenum acid (PMA) has been used to separate 32 P in a radiochemically pure form. Correction factors have been calculated due to the 2nd order interference on 30 Si nuclei in determining phosphorus in silicon for various irradiation times and at various cadmium proportions

  3. Natural Radionuclides and Isotopic Signatures for Determining Carbonaceous Aerosol Sources, Aerosol Lifetimes, and Washout Processes

    International Nuclear Information System (INIS)

    Gaffney, Jeffrey

    2012-01-01

    This is the final technical report. The project description is as follows: to determine the role of aerosol radiative forcing on climate, the processes that control their atmospheric concentrations must be understood, and aerosol sources need to be determined for mitigation. Measurements of naturally occurring radionuclides and stable isotopic signatures allow the sources, removal and transport processes, as well as atmospheric lifetimes of fine carbonaceous aerosols, to be evaluated.

  4. Natural Radionuclides and Isotopic Signatures for Determining Carbonaceous Aerosol Sources, Aerosol Lifetimes, and Washout Processes

    Energy Technology Data Exchange (ETDEWEB)

    Gaffney, Jeffrey [Univ. of Arkansas, Little Rock, AR (United States)

    2012-12-12

    This is the final technical report. The project description is as follows: to determine the role of aerosol radiative forcing on climate, the processes that control their atmospheric concentrations must be understood, and aerosol sources need to be determined for mitigation. Measurements of naturally occurring radionuclides and stable isotopic signatures allow the sources, removal and transport processes, as well as atmospheric lifetimes of fine carbonaceous aerosols, to be evaluated.

  5. The separation and determination of fatty acids by isotopic dilution and radiogas-liquid chromatography

    International Nuclear Information System (INIS)

    Beardsley, D.A.

    1981-01-01

    A number of static phases have been evaluated for the GLC separation of fatty acids. Of those investigated, only AT 1200 was capable of resolving the isomeric forms of the acids. A radiogas-liquid chromatographic method incorporating isotopic dilution analysis has been developed for the determination of n-butyric acid. The proposed method has been applied to the determination of the acid in hydrolysed butter fat and milk chocolate extracts. (author)

  6. Highly sensitive determination of mercury using copper enhancer by diamond electrode coupled with sequential injection–anodic stripping voltammetry

    Energy Technology Data Exchange (ETDEWEB)

    Chaiyo, Sudkate [Department of Chemistry, Faculty of Science, Srinakharinwirot University (Thailand); Chailapakul, Orawon [Department of Chemistry, Faculty of Science, Chulalongkorn University (Thailand); Center for Petroleum, Petrochemicals, and Advanced Materials, Chulalongkorn University (Thailand); Siangproh, Weena, E-mail: weena@swu.ac.th [Department of Chemistry, Faculty of Science, Srinakharinwirot University (Thailand)

    2014-12-10

    Highlights: • Highly sensitive determination of Hg(II) using SI–ASV-BDD was achieved. • Electrochemical detection of Hg(II) using Cu(II) enhancer was accomplished. • LOD and LOQ were found to be very low at 40.0 ppt and 135.0 ppt. • This method was successfully applied for determination of Hg(II) in real samples. - Abstract: A highly sensitive determination of mercury in the presence of Cu(II) using a boron-doped diamond (BDD) thin film electrode coupled with sequential injection–anodic stripping voltammetry (SI–ASV) was proposed. The Cu(II) was simultaneously deposited with Hg(II) in a 0.5 M HCl supporting electrolyte by electrodeposition. In presence of an excess of Cu(II), the sensitivity for the determination of Hg(II) was remarkably enhanced. Cu(II) and Hg(II) were on-line deposited onto the BDD electrode surface at −1.0 V (vs. Ag/AgCl, 3 M KCl) for 150 s with a flow rate of 14 μL s{sup −1}. An anodic stripping voltammogram was recorded from −0.4 V to 0.25 V using a frequency of 60 Hz, an amplitude of 50 mV, and a step potential of 10 mV at a stopped flow. Under the optimal conditions, well-defined peaks of Cu(II) and Hg(II) were found at −0.25 V and +0.05 V (vs. Ag/AgCl, 3 M KCl), respectively. The detection of Hg(II) showed two linear dynamic ranges (0.1–30.0 ng mL{sup −1} and 5.0–60.0 ng mL{sup −1}). The limit of detection (S/N = 3) obtained from the experiment was found to be 0.04 ng mL{sup −1}. The precision values for 10 replicate determinations were 1.1, 2.1 and 2.9% RSD for 0.5, 10 and 20 ng mL{sup −1}, respectively. The proposed method has been successfully applied for the determination of Hg(II) in seawater, salmon, squid, cockle and seaweed samples. A comparison between the proposed method and an inductively coupled plasma optical emission spectrometry (ICP-OES) standard method was performed on the samples, and the concentrations obtained via both methods were in agreement with the certified values of Hg

  7. Liquid and gas chromatography coupled to isotope ratio mass spectrometry for the determination of 13C-valine isotopic ratios in complex biological samples.

    Science.gov (United States)

    Godin, Jean-Philippe; Breuillé, Denis; Obled, Christiane; Papet, Isabelle; Schierbeek, Henk; Hopfgartner, Gérard; Fay, Laurent-Bernard

    2008-10-01

    On-line gas chromatography-combustion-isotope ratio mass spectrometry (GC-C-IRMS) is commonly used to measure isotopic ratios at natural abundance as well as for tracer studies in nutritional and medical research. However, high-precision (13)C isotopic enrichment can also be measured by liquid chromatography-isotope ratio mass spectrometry (LC-IRMS). Indeed, LC-IRMS can be used, as shown by the new method reported here, to obtain a baseline separation and to measure (13)C isotopic enrichment of underivatised amino acids (Asp, Thr-Ser, Glu, Pro, Gly, Ala, Cys and Val). In case of Val, at natural abundance, the SD(delta(13)C) reported with this method was found to be below 1 per thousand . Another key feature of the new LC-IRMS method reported in this paper is the comparison of the LC-IRMS approach with the conventional GC-C-IRMS determination. To perform this comparative study, isotopic enrichments were measured from underivatised Val and its N(O, S)-ethoxycarbonyl ethyl ester derivative. Between 0.0 and 1.0 molar percent excess (MPE) (delta(13)C= -12.3 to 150.8 per thousand), the calculated root-mean-square (rms) of SD was 0.38 and 0.46 per thousand and the calculated rms of accuracy was 0.023 and 0.005 MPE, respectively, for GC-C-IRMS and LC-IRMS. Both systems measured accurately low isotopic enrichments (0.002 atom percent excess (APE)) with an SD (APE) of 0.0004. To correlate the relative (delta(13)C) and absolute (atom%, APE and MPE) isotopic enrichment of Val measured by the GC-C-IRMS and LC-IRMS devices, mathematical equations showing the slope and intercept of the curves were established and validated with experimental data between 0.0 to 2.3 MPE. Finally, both GC-C-IRMS and LC-IRMS instruments were also used to assess isotopic enrichment of protein-bound (13)C-Val in tibial epiphysis in a tracer study performed in rats. Isotopic enrichments measured by LC-IRMS and GC-C-IRMS were not statistically different (p>0.05). The results of this work indicate that

  8. Single peak parameters technique for simultaneous measurements: Spectrophotometric sequential injection determination of Fe(II) and Fe(III).

    Science.gov (United States)

    Kozak, J; Paluch, J; Węgrzecka, A; Kozak, M; Wieczorek, M; Kochana, J; Kościelniak, P

    2016-02-01

    Spectrophotometric sequential injection system (SI) is proposed to automate the method of simultaneous determination of Fe(II) and Fe(III) on the basis of parameters of a single peak. In the developed SI system, sample and mixture of reagents (1,10-phenanthroline and sulfosalicylic acid) are introduced into a vessel, where in an acid environment (pH≅3) appropriate compounds of Fe(II) and Fe(III) with 1,10-phenanthroline and sulfosalicylic acid are formed, respectively. Then, in turn, air, sample, EDTA and sample again, are introduced into a holding coil. After the flow reversal, a segment of air is removed from the system by an additional valve and as EDTA replaces sulfosalicylic acid forming a more stable colorless compound with Fe(III), a complex signal is registered. Measurements are performed at wavelength 530 nm. The absorbance measured at minimum of the negative peak and the area or the absorbance measured at maximum of the signal can be used as measures corresponding to Fe(II) and Fe(III) concentrations, respectively. The time of the peak registration is about 2 min. Two-component calibration has been applied to analysis. Fe(II) and Fe(III) can be determined within the concentration ranges of 0.04-4.00 and 0.1-5.00 mg L(-1), with precision less than 2.8% and 1.7% (RSD), respectively and accuracy better than 7% (RE). The detection limit is 0.04 and 0.09 mg L(-1) for Fe(II) and Fe(III), respectively. The method was applied to analysis of artesian water samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  9. Determination of picloram in natural waters employing sequential injection square wave voltammetry using the hanging mercury drop electrode.

    Science.gov (United States)

    Dos Santos, Luciana B O; Masini, Jorge C

    2007-05-15

    This paper describes the development of a sequential injection analysis method to automate the determination of picloram by square wave voltammetry exploiting the concept of monosegmented flow analysis to perform in-line sample conditioning and standard addition. To perform these tasks, an 800muL monosegment is formed, composed by 400muL of sample and 400muL of conditioning/standard solution, in medium of 0.10molL(-1) H(2)SO(4). Homogenization of the monosegment is achieved by three flow reversals. After homogenization the mixture zone is injected toward the flow cell, which is adapted to the capillary of a hanging drop mercury electrode, at a flow rate of 50muLs(-1). After a suitable delay time, the potential is scanned from -0.5 to -1.0V versus Ag/AgCl at frequency of 300Hz and pulse height of 25mV. The linear dynamic range is observed for picloram concentrations between 0.10 and 2.50mgL(-1) fitting to the linear equation I(p)=(-2.19+/-0.03)C(picloram)+(0.096+/-0.039), with R(2)=0.9996, for which the slope is given in muALmg(-1). The detection and quantification limits are 0.036 and 0.12mgL(-1), respectively. The sampling frequency is 37h(-1) when the standard addition protocol is followed, but can be increased to 41h(-1) if the protocol to obtain in-line external calibration curve is used for quantification. The method was applied for determination of picloram in spiked water samples and the accuracy was evaluated by comparison with high performance liquid chromatography using molecular absorption at 220nm for detection. No evidences of statistically significant differences between the two methods were observed.

  10. Population variation in isotopic composition of shorebird feathers: Implications for determining molting grounds

    Science.gov (United States)

    Torres-Dowdall, J.; Farmer, A.H.; Bucher, E.H.; Rye, R.O.; Landis, G.

    2009-01-01

    Stable isotope analyses have revolutionized the study of migratory connectivity. However, as with all tools, their limitations must be understood in order to derive the maximum benefit of a particular application. The goal of this study was to evaluate the efficacy of stable isotopes of C, N, H, O and S for assigning known-origin feathers to the molting sites of migrant shorebird species wintering and breeding in Argentina. Specific objectives were to: 1) compare the efficacy of the technique for studying shorebird species with different migration patterns, life histories and habitat-use patterns; 2) evaluate the grouping of species with similar migration and habitat use patterns in a single analysis to potentially improve prediction accuracy; and 3) evaluate the potential gains in prediction accuracy that might be achieved from using multiple stable isotopes. The efficacy of stable isotope ratios to determine origin was found to vary with species. While one species (White-rumped Sandpiper, Calidris fuscicollis) had high levels of accuracy assigning samples to known origin (91% of samples correctly assigned), another (Collared Plover, Charadrius collaris) showed low levels of accuracy (52% of samples correctly assigned). Intra-individual variability may account for this difference in efficacy. The prediction model for three species with similar migration and habitat-use patterns performed poorly compared with the model for just one of the species (71% versus 91% of samples correctly assigned). Thus, combining multiple sympatric species may not improve model prediction accuracy. Increasing the number of stable isotopes in the analyses increased the accuracy of assigning shorebirds to their molting origin, but the best combination - involving a subset of all the isotopes analyzed - varied among species.

  11. Dual-isotope technique for determination of in vivo ketone body kinetics

    International Nuclear Information System (INIS)

    Miles, J.M.; Schwenk, W.F.; McClean, K.L.; Haymond, M.W.

    1986-01-01

    Total ketone body specific activity has been widely used in studies of ketone body metabolism to circumvent so-called isotope disequilibrium between the two major ketone body pools, acetoacetate and beta-hydroxybutyrate. Recently, this approach has been criticized on theoretical grounds. In the present studies, [13C]acetoacetate and beta-[14C]hydroxybutyrate were simultaneously infused in nine mongrel dogs before and during an infusion of either unlabeled sodium acetoacetate or unlabeled sodium beta-hydroxybutyrate. Ketone body turnover was determined using total ketone body specific activity, total ketone body moles % enrichment, and an open two-pool model, both before and during the exogenous infusion of unlabeled ketone bodies. Basal ketone body turnover rates were significantly higher using [13C]acetoacetate than with either beta-[14C]hydroxybutyrate alone or the dual-isotope model (3.6 +/- 0.5 vs. 2.2 +/- 0.2 and 2.7 +/- 0.2 mumol X kg-1 X min-1, respectively, P less than 0.05). During exogenous infusion of unlabeled sodium acetoacetate, the dual-isotope model provided the best estimate of ketone body inflow, whereas 14C specific activity underestimated the known rate of acetoacetate infusion by 55% (P less than 0.02). During sodium beta-hydroxybutyrate infusion, [13C]-acetoacetate overestimated ketone body inflow by 55% (P = NS), while better results were obtained with 14C beta-hydroxybutyrate alone and the two-pool model. Ketone body interconversion as estimated by the dual-isotope technique increased markedly during exogenous ketone body infusion. In conclusion, significant errors in estimation of ketone body inflow were made using single-isotope techniques, whereas a dual-isotope model provided reasonably accurate estimates of ketone body inflow during infusion of exogenous acetoacetate and beta-hydroxybutyrate

  12. Analytical techniques for determination of framework oxygen isotope ratio of wairakite

    International Nuclear Information System (INIS)

    Noto, Masami; Kusakabe, Minoru; Uchida, Tetsuo.

    1990-01-01

    Dehydration techniques were developed for the analysis of isotopic ratios of framework oxygen of wairakite, one of calcium zeolites often encountered in geothermal systems. Channel water in wairakite were separated from aluminosilicate framework by dehydration in vacuum at 300 deg, 400 deg, 450 deg, 500 deg, 550 deg, 650 deg, 750 deg, 850 deg, and 950 degC, and by stepwise heating at temperatures from 300 deg to 700 degC. The oxygen isotopic analyses of the separated channel water and the residual aluminosilicate framework of wairakite indicated that dehydration at temperatures higher than 400 degC is accompanied by isotopic exchang between the framework oxygen and dehydrating water vapor. The isotopic exchange during the high temperature dehydration makes the δ 18 O of framework oxygen lower and that of channel water higher than those obtained by dehydration at 300 degC. These results are consistent with dehydration behavior of wairakite under vacuum that the maximum rate of dehydration of channel water is attained at about 400 degC. Consequently it is recommended to dehydrate wairakite at a temperature as low as possible in order to avoid the effect of the isotopic exchange. Time required to attain complete dehydration becomes longer with lowering the temperature of dehydration. To compromise these conflicting effects, the optimum conditions of dehydration have been found that most of the channel water is dehydrated at 300 degC for 24 hours, followed by stepwise heating for additional 17 hours up to 700 degC. We obtained a better than ± 0.1 reproducibility for the framework oxygen isotopic determinations with this technique. (author)

  13. Analytical Methodology for the Determination of Radium Isotopes in Environmental Samples

    International Nuclear Information System (INIS)

    2010-01-01

    Reliable, comparable and 'fit for purpose' results are an essential requirement for any decision based on analytical measurements. For the analyst, the availability of tested and validated analytical procedures is an extremely important tool for production of such analytical measurements. For maximum utility, such procedures should be comprehensive, clearly formulated, and readily available to both the analyst and the customer for reference. Since 2004, the environment programme of the IAEA has included activities aimed at the development of a set of procedures for the determination of radionuclides in terrestrial environmental samples. Measurements of radium isotopes are important for radiological and environmental protection, geochemical and geochronological investigations, hydrology, etc. The suite of isotopes creates and stimulates continuing interest in the development of new methods for determination of radium in various media. In this publication, the four most routinely used analytical methods for radium determination in biological and environmental samples, i.e. alpha spectrometry, gamma spectrometry, liquid scintillation spectrometry and mass spectrometry, are reviewed

  14. Hydrogen isotopic spectral determination in inert gases with the use of light source with contracted discharge

    International Nuclear Information System (INIS)

    Nemets, V.M.; Solov'ev, A.A.

    1981-01-01

    Isotopic-spectral technique for hydrogen determination in helium, neon and argon is developed. It employs a contracted high-frequency discharge as a light source to decrease the distorting effect. of a dummy signal and the ''memory'' effect of the discharge tube. The discharge is realized in a quartz tube approximately 7 mm dia. and gas pressure in it approximately 6x10 4 Pa. The analysis technique comprises sampling of gas, dosed introduction of deuterium into the sample, selection of a mixture portion into the discharge tube, spectroscopic determination of hydrogen isotope ratio and calculation of the sought for hydrogen concentration. The lower boundary of the determined concentrations of hydrogen constitutes 7x10 - 5 , 2x10 - 4 and 4x10 - 4 volumetric per cent in helium, neon, and argon, respectively

  15. Evaporation and abstraction determined from stable isotopes during normal flow on the Gariep River, South Africa

    Science.gov (United States)

    Diamond, Roger E.; Jack, Sam

    2018-04-01

    Changes in the stable isotope composition of water can, with the aid of climatic parameters, be used to calculate the quantity of evaporation from a water body. Previous workers have mostly focused on small, research catchments, with abundant data, but of limited scope. This study aimed to expand such work to a regional or sub-continental scale. The first full length isotope survey of the Gariep River quantifies evaporation on the river and the man-made reservoirs for the first time, and proposes a technique to calculate abstraction from the river. The theoretically determined final isotope composition for an evaporating water body in the given climate lies on the empirically determined local evaporation line, validating the assumptions and inputs to the Craig-Gordon evaporation model that was used. Evaporation from the Gariep River amounts to around 20% of flow, or 40 m3/s, of which about half is due to evaporation from the surface of the Gariep and Vanderkloof Reservoirs, showing the wastefulness of large surface water impoundments. This compares well with previous estimates based on evapotranspiration calculations, and equates to around 1300 GL/a of water, or about the annual water consumption of Johannesburg and Pretoria, where over 10 million people reside. Using similar evaporation calculations and applying existing transpiration estimates to a gauged length of river, the remaining quantity can be attributed to abstraction, amounting to 175 L/s/km in the lower middle reaches of the river. Given that high water demand and climate change are global problems, and with the challenges of maintaining water monitoring networks, stable isotopes are shown to be applicable over regional to national scales for modelling hydrological flows. Stable isotopes provide a complementary method to conventional flow gauging for understanding hydrology and management of large water resources, particularly in arid areas subject to significant evaporation.

  16. Determining the isotopic compositions of uranium and fission products in radioactive environmental microsamples using laser ablation ICP-MS with multiple ion counters

    Energy Technology Data Exchange (ETDEWEB)

    Boulyga, Sergei F.; Prohaska, Thomas [University of Natural Resources and Applied Life Sciences, Department of Chemistry, Division of Analytical Chemistry-VIRIS Laboratory, Vienna (Austria)

    2008-01-15

    This paper presents the application of a multicollector inductively coupled plasma mass spectrometer (MC-ICP-MS) - a Nu Plasma HR - equipped with three ion-counting multipliers and coupled to a laser ablation system (LA) for the rapid and sensitive determination of the {sup 235}U/{sup 238}U, {sup 236}U/{sup 238}U, {sup 145}Nd/{sup 143}Nd, {sup 146}Nd/{sup 143}Nd, {sup 101}Ru/({sup 99}Ru+{sup 99}Tc) and {sup 102}Ru/({sup 99}Ru+{sup 99}Tc) isotope ratios in microsamples collected in the vicinity of Chernobyl. Microsamples with dimensions ranging from a hundred {mu}m to about 1 mm and with surface alpha activities of 3-38 mBq were first identified using nuclear track radiography. U, Nd and Ru isotope systems were then measured sequentially for the same microsample by LA-MC-ICP-MS. The application of a zoom ion optic for aligning the ion beams into the ion counters allows fast switching between different isotope systems, which enables all of the abovementioned isotope ratios to be measured for the same microsample within a total analysis time of 15-20 min (excluding MC-ICP-MS optimization and calibration). The {sup 101}Ru/({sup 99}Ru+{sup 99}Tc) and {sup 102}Ru/({sup 99}Ru+{sup 99}Tc) isotope ratios were measured for four microsamples and were found to be significantly lower than the natural ratios, indicating that the microsamples were contaminated with the corresponding fission products (Ru and Tc). A slight depletion in {sup 146}Nd of about 3-5% was observed in the contaminated samples, but the Nd isotopic ratios measured in the contaminated samples coincided with natural isotopic composition within the measurement uncertainty, as most of the Nd in the analyzed samples originates from the natural soil load of this element. The {sup 235}U/{sup 238}U and {sup 236}U/{sup 238}U isotope ratios were the most sensitive indicators of irradiated uranium. The present work yielded a significant variation in uranium isotope ratios in microsamples, in contrast with previously

  17. Determination of low level of plutonium and uranium isotopes in safeguard swipe sample

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Myung Ho; Park, Jong Ho; Oh, Seong Yong; Lee, Chang Heon; Ahn, Hong Ju; Song, Kyu Seok [Korea Atomic Energy Research Institute, Daejeon (Korea, Republic of)

    2011-10-15

    For the determination of radionuclides, the separation techniques based on the principles of anion exchange, liquid-liquid extraction or column extraction chromatography are frequently used in nuclear analytical applications. Recently, a novel extraction chromatographic resin has been developed by Horwitz and co-workers, which are capable of selective extraction of the actinides. General separation of plutonium and uranium with extraction chromatographic techniques are focused on the environmental or radioactive waste samples. Also, the chemical yields for Pu and U isotopes with extraction chromatographic method sometimes are variable. For effective extraction of Pu isotopes in the very level of plutonium sample with UTEVA resin, the valence adjustment of Pu isotopes in the sample solution requires due to unstability in the oxidation state of Pu isotopes during separation step. Therefore, it is necessary to develop a simple and robust radiochemical separation method for nano- or pico gram amounts of uranium and plutonium in safeguard swipe samples. Chemical yields of plutonium and uranium with extraction chromatographic method of Pu and U upgrades in this study were compared with several separation methods for Pu and U generally used in the radiochemistry field. Also, the redox reactions of hydrogen peroxide with plutonium in the nitric acid media were investigated by UV-Vis-NIR absorption spectroscopy. Based on general extraction chromatography method with UTEVA resin, the separation method of nano- and picogram amounts of uranium and plutonium in safeguard swipe samples was developed in this study

  18. Tracing mercury pathways in Augusta Bay (southern Italy) by total concentration and isotope determination

    International Nuclear Information System (INIS)

    Bonsignore, M.; Tamburrino, S.; Oliveri, E.; Marchetti, A.; Durante, C.; Berni, A.; Quinci, E.; Sprovieri, M.

    2015-01-01

    The mercury (Hg) pollution of sediments is the main carrier of Hg for the biota and, subsequently, for the local fish consumers in Augusta Bay area (SE Sicily, Italy), a coastal marine system affected by relevant sewage from an important chlor-alkali factory. This relationship was revealed by the determination of Mass Dependent (MDF) and Mass Independent Fractionation (MIF) of Hg isotopes in sediment, fish and human hair samples. Sediments showed MDF but no MIF, while fish showed MIF, possibly due to photochemical reduction in the water column and depending on the feeding habitat of the species. Benthic and demersal fish exhibited MDF similar to that of sediments in which anthropogenic Hg was deposited, while pelagic organisms evidenced higher MDF and MIF due to photoreduction. Human hair showed high values of δ 202 Hg (offset of +2.2‰ with respect to the consumed fish) and Δ 199 Hg, both associated to fish consumption. - Highlights: • We report the Hg isotope ratios of sediments, fish and human hair in Augusta Bay. • Hg isotopes show mercury transfers from sediments to benthic and demersal fish. • MIF in fish appears to be driven by effect of photoreduction. • MIF in human hair is inherited by fish consumption. - The mercury (Hg) isotope composition of sediments, fish muscles and human hair has been investigated from the highly polluted Augusta Bay (SE Sicily, Italy)

  19. Determination of integrated neutron flux by the measurement of the isotopic ratios of cadmium and gadolinium

    International Nuclear Information System (INIS)

    Tomiyoshi, Irene Akemy

    1982-01-01

    In this work, the possibility of the indirect determination of the integrated neutron flux, through the change of isotopic ratios of cadmium and gadolinium was investigated. The samples of cadmium we/e gadolinium were irradiated in the IEA-Rl reactor. These elements were chosen because they have high thermal neutron absorption cross section which permit the change in the isotopic composition during a short irradiation time to be measured accurately. The isotopic ratios were measured with a thermionic mass spectrometer the silica-gel technique and arrangement with single filament were used for the cadmium analysis, where as the oxi - reduction technique and arrangement with double filaments were used for gadolinium analysis. The mass fractionation effects for cadmium and gadolinium were corrected respectively by the exponential and potential expansion of the isotopic fractionation factor per atomic mass unit. The flux values supplied by the Centro de Operacao e Utilizacao do Reator de Pesquisas do IPEN were extrapolated. These values and the integrated flux values obtained experimentally were compared. (author)

  20. Determination of the energetics of the UDP-glucose pyrophosphorylase reaction by positional isotope exchange inhibition

    International Nuclear Information System (INIS)

    Hester, L.S.; Raushel, F.M.

    1987-01-01

    A method has been developed for obtaining qualitative information about enzyme-catalyzed reactions by measuring the inhibitory effects of added substrates on positional isotope exchange rates. It has been demonstrated for ordered kinetic mechanisms that an increase in the concentration of the second substrate to add to the enzyme will result in a linear increase in the ratio of the chemical and positional isotope exchange rates. The slopes and intercepts from these plots can be used to determine the partitioning ratios of binary and ternary enzyme complexes. The method has been applied to the reaction catalyzed by UDP-glucose pyrophosphorylase. A positional isotope exchange reaction was measured within oxygen-18-labeled UTP as a function of variable glucose 1-phosphate concentration in the forward reaction. In the reverse reaction, a positional isotope exchange reaction was measured within oxygen-18-labeled UDP-glucose as a function of increasing pyrophosphate concentration. The results have been interpreted to indicate that the interconversion of the ternary central complexes is fast relative to product dissociation in either direction. In the forward direction, the release of UDP-glucose is slower than the release of pyrophosphate. The release of glucose 1-phosphate is slower than the release of UTP in the reverse reaction

  1. An analytical approach to Sr isotope ratio determination in Lambrusco wines for geographical traceability purposes.

    Science.gov (United States)

    Durante, Caterina; Baschieri, Carlo; Bertacchini, Lucia; Bertelli, Davide; Cocchi, Marina; Marchetti, Andrea; Manzini, Daniela; Papotti, Giulia; Sighinolfi, Simona

    2015-04-15

    Geographical origin and authenticity of food are topics of interest for both consumers and producers. Among the different indicators used for traceability studies, (87)Sr/(86)Sr isotopic ratio has provided excellent results. In this study, two analytical approaches for wine sample pre-treatment, microwave and low temperature mineralisation, were investigated to develop accurate and precise analytical method for (87)Sr/(86)Sr determination. The two procedures led to comparable results (paired t-test, with tisotopic values were compared with isotopic data coming from (i) soils of their territory of origin and (ii) wines obtained by same grape varieties cultivated in different districts. The obtained results have shown no significant variability among the different vintages of wines and a perfect agreement between the isotopic range of the soils and wines has been observed. Nevertheless, the investigated indicator was not enough powerful to discriminate between similar products. To this regard, it is worth to note that more soil samples as well as wines coming from different districts will be considered to obtain more trustworthy results. Copyright © 2014 Elsevier Ltd. All rights reserved.

  2. The determination of initial ratio of strontium isotope in rocks and its geological application

    International Nuclear Information System (INIS)

    Ying Junlong; Zhao Puyun; Lin Xiulan

    1989-04-01

    The method to determine the initial ratio of strontium isotopes existed in rocks of poor rubidium and rich strontium and main carrier minerals is introduced. The initial ratio obtained from this method is equivalent to that acquired by Rb-Sr isochrone. Based on this result, information on regional rock genesis and mineralization regularities can be provided. It has great significance in the research on activities of ancient continental margin and material sources as well as their evolution. The migration of rock, and ore-forming materials, matallogenetic mechanism and its distribution in the space and time evolution are studied by using these data. In conclusion, the determination of strontium isotopes has broad prospects in the geological research

  3. Determination of the Geographical Origin of All Commercial Hake Species by Stable Isotope Ratio (SIR) Analysis.

    Science.gov (United States)

    Carrera, Mónica; Gallardo, José M

    2017-02-08

    The determination of the geographical origin of food products is relevant to comply with the legal regulations of traceability, to avoid food fraud, and to guarantee food quality and safety to the consumers. For these reasons, stable isotope ratio (SIR) analysis using an isotope ratio mass spectrometry (IRMS) instrument is one of the most useful techniques for evaluating food traceability and authenticity. The present study was aimed to determine, for the first time, the geographical origin for all commercial fish species belonging to the Merlucciidae family using SIR analysis of carbon (δ 13 C) and nitrogen (δ 15 N). The specific results enabled their clear classification according to the FAO (Food and Agriculture Organization of the United Nations) fishing areas, latitude, and geographical origin in the following six different clusters: European, North African, South African, North American, South American, and Australian hake species.

  4. Factors affecting the determination of the isotopically exchangeable phosphorus in soils

    International Nuclear Information System (INIS)

    Morales, L.E.M.

    1981-06-01

    In order to evaluate the factors that affect the determination of the isotopically exchangeable phosphorus in soils (L value), various greenhouse experiments were carried out. The following factors were considered: carrier level; plant species; harvest time; nitrogen doses; nitrogen sources; culture conditions and soil type. A radioactive solution with an activity level of approximately 10 μCi 32 p/3 kg soil with different carrier levels was located in layers or mixed completely with the soil depending upon the experiment. (author)

  5. Speciative determination of phosphorus in environmental water by the isotope exchange method

    International Nuclear Information System (INIS)

    Ikeda, N.; Yoshikawa, M.; Murakami, S.; Kunika, J.

    1988-01-01

    An isotope exchage method for the speciative determination of phosphorus (PO 4 3- ,PO 3 3- and total P) in natural water samples is proposed by using the exchange system of molybdophosphate in the aqueous phase and tetraphenylarsonium molybdophosphate in the organic phase. In this exchange system, only PO 4 3- exchanges and is determined. When the sample water is treated with Br 2 water in advance, the amount of PO 4 3- +PO 3 3- can be obtained. When the sample is treated with H 2 SO 4 and HNO 3 , the amount of total P can be determined. (author) 4 refs.; 5 tabs

  6. Performance evaluation of nitrogen isotope ratio determination in marine and lacustrine sediments: An inter-laboratory comparison

    NARCIS (Netherlands)

    Bahlmann, E.; Bernasconi, S.M.; Bouillon, S.; Houtekamer, M.J.; Korntheuer, M.; Langenberg, F.; Mayr, C.; Metzke, M.; Middelburg, J.J.; Nagel, B.; Struck, U.; Voß, M.; Emeis, K.C.

    2010-01-01

    Nitrogen isotopes of organic matter are increasingly studied in marine biogeochemistry and geology, plant and animal ecology, and paleoceanography. Here, we present results of an inter-laboratory test on determination of nitrogen isotope ratios in marine and lacustrine sediments. Six different

  7. Improved analytical procedure for the determination of 210Pb and 210Po using alpha-spectrometric isotope dilution

    International Nuclear Information System (INIS)

    Urnezis, P.W.; Holtzman, R.B.

    1981-01-01

    An isotope dilution method has been incorporated into the 210 Pb- 210 Po analysis. A known amount of 209 Po is added to the sample before analysis. Then both 209 Po and 210 Po are deposited on a silver planchet which is assayed in an alpha spectrometer to determine the activities of each isotope. The recoveries generally range from 70% to 90%

  8. Determination of nuclear spins of short-lived isotopes by laser induced fluorescence

    International Nuclear Information System (INIS)

    Buchinger, F.; Dabkiewicz, P.; Kremmling, H.; Kuehl, T.; Mueller, A.C.; Schuessler, H.A.

    1980-01-01

    The spins of several nuclear ground and isomeric states have been measured for a number of mercury isotopes. The fluorescent light from the 6s6p 3 P 1 state is observed at 2537 Angstroem after excitation with the frequency doubled output of a pulsed dye laser. Four different laser induced fluorescence techniques were tested for their applicability: double resonance, Hanle effect, time delayed integral Hanle beats, and time resolved quantum beats. The sensitivity and selectivity of these models are compared with emphasis on the determination of spins of nuclei far from beta-stability, where short half lives and low production yields restrict the number of available atoms. The experiments were carried out on-line with the ISOLDE isotope separator at CERN at densities as low as 10 6 atoms/cm 3 . Results for the very neutron deficient high spin mercury isomers with half lives of several seconds, but also for the ground states of the abundant low spin stable mercury isotopes, are given as examples. The test measurements determined the nuclear spins of the odd sup(185m-191m)Hg isomers to be I = 13/2. (orig.)

  9. Determining Isotopic Composition of Dissolved Nitrate Using Bacterial Denitrification Followed by Laser Spectroscopy

    International Nuclear Information System (INIS)

    Yan Tiezhu; Lee Zhi Yi, Amelia; Heiling, Maria; Weltin, Georg; Toloza, Arsenio; Resch, Christian

    2016-01-01

    Nitrate (NO_3"-) pollution is a prevalent problem that can cause water quality degradation and eutrophication of water bodies. Quantifying the nitrogen and oxygen isotopic composition of nitrates will allow for better identification of their potential sources, which in turn will assist in remediation of contaminated water and the designing of future water management practices. In this research bacterial denitrification followed by laser spectroscopy are used to determine isotopic composition of δ"1"5N and δ"1"8O of dissolved nitrates. The objective of the project is to establish a standard operating procedure (SOP) that outlines the best practices for both methods in sequence and designed to be used as a technical guideline

  10. Determination of spin, magnetic moment and isotopic shift of neutron rich 205Hg by optical pumping

    International Nuclear Information System (INIS)

    Rodriguez, J.; Bonn, J.; Huber, G.; Kluge, H.J.; Otten, E.W.; European Organisation for Nuclear Research, Geneva

    1975-01-01

    Neutron rich 205 Hg(Tsub(1/2) = 5.2 min) was produced and on-line mass separated at the ISOLDE facility at CERN. The polarization achieved by optical pumping via the atomic line (6s 21 S 0 - 6s6p 3 P 1 , lambda = 2,537 A) was monitored by the β decay asymmetry. Hyperfine structure and isotopic shift of the 205 Hg absorption line was determined by Zeeman scanning. In addition a magnetic resoncance was performed on the polarized 205 Hg nuclei in the atomic ground state. The results are: I( 205 Hg) = 1/2 (confirmed); μ(I, 205 Hg) = 0.5915(1)μ(N) (uncorrected for diamagnetism); isotopic shift deltaν(204/205) = ν( 205 Hg) - ν( 204 Hg) = -1.8(1)GHz. μ(I) and IS are discussed briefly in the frame of current literature. (orig.) [de

  11. Radiochemical procedure for the determination of plutonium isotopes in powdered milk

    International Nuclear Information System (INIS)

    Taddei, M.H.T.; Silva, N.C.

    2006-01-01

    A radiochemical procedure for the determination of alpha-emitting isotopes of plutonium in powdered milk is proposed. The procedure involves sample dissolution (by HNO 3 and HClO 4 ), separation by ionic-exchange resin, electrodeposition and alpha-spectroscopy. In order to determine the chemical recovery, 242 Pu was employed as a tracer. A reference material (Marine Sediment IAEA 135) was analyzed to validate such procedure, and to show its reliability. Afterwards, some powdered milk, produced for international trade, was analyzed and chemical recovery was found to be around 95%. (author)

  12. Rapid collection of iron hydroxide for determination of Th isotopes in seawater

    Energy Technology Data Exchange (ETDEWEB)

    Okubo, Ayako, E-mail: okubo.ayako@jaea.go.jp [Japan Atomic Energy Agency, Research Group for Analytical Chemistry (Japan); Obata, Hajime, E-mail: obata@aori.u-tokyo.ac.jp [Atmosphere Ocean Research Institute, The University of Tokyo (Japan); Magara, Masaaki, E-mail: magara.masaaki@jaea.go.jp [Japan Atomic Energy Agency, Research Group for Analytical Chemistry (Japan); Kimura, Takaumi, E-mail: kimura.takaumi@jaea.go.jp [Japan Atomic Energy Agency, Research Group for Analytical Chemistry (Japan); Ogawa, Hiroshi, E-mail: hogawa@aori.u-tokyo.ac.jp [Atmosphere Ocean Research Institute, The University of Tokyo (Japan)

    2013-12-04

    Graphical abstract: -- Highlights: •DIAION CR-20 chelating resin has successfully collected iron-hydroxide with Th isotopes. •Ferric ions in the iron hydroxide were bonded to functional groups of the chelating resin. •The time of preconcentration step was markedly reduced from a few days to 3–4 h. -- Abstract: This work introduces a novel method of recovery of iron hydroxide using a DIAION CR-20 chelating resin column to determine Th isotopes in seawater with a sector field (SF) inductively coupled plasma mass spectrometer (ICP-MS). Thorium isotopes in seawater were co-precipitated with iron hydroxide, and this precipitate was sent to chelating resin column. Ferric ions in the iron hydroxide were bonded to functional groups of the chelating resin directly, resulting in a pH increase of the effluent by release of hydroxide ion from the iron hydroxide. The co-precipitated thorium isotopes were quantitatively collected within the column, which indicated that thorium was retained on the iron hydroxide remaining on the chelating column. The chelating column quantitatively collected {sup 232}Th with iron hydroxide in seawater at flow rates of 20–25 mL min{sup −1}. Based on this flow rate, a 5 L sample was processed within 3–4 h. The >20 h aging of iron hydroxide tends to reduce the recovery of {sup 232}Th. The rapid collection method was successfully applied to the determination of {sup 230}Th and {sup 232}Th in open-ocean seawater samples.

  13. Site-specific and multielement approach to the determination of liquid-vapor isotope fractionation parameters. The case of alcohols

    International Nuclear Information System (INIS)

    Moussa, I.; Naulet, N.; Martin, M.L.; Martin, G.J.

    1990-01-01

    Isotope fractionation phenomena occurring at the natural abundance level in the course of liquid-vapor transformation have been investigated by using the SNIF-NMR method (site-specific natural isotope fractionation studied by NMR) which has a unique capability of providing simultaneous access to fractionation parameters associated with different molecular isotopomers. This new approach has been combined with the determination of overall carbon and hydrogen fractionation effects by isotope ratio mass spectrometry (IRMS). The results of distillation and evaporation experiments of alcohols performed in technical conditions of practical interest have been analyzed according to the Rayleigh-type model. In order to check the performance of the column, unit fractionation factors were measured beforehand for water and for the hydroxylic sites of methanol and ethanol for which liquid-vapor equilibrium constants were already known. Inverse isotope effects are determined in distillation experiments for the overall carbon isotope ratio and for the site-specific hydrogen isotope ratios associated with the methyl and methylene sites of methanol and ethanol. In contrast, normal isotope effects are produced by distillation for the hydroxylic sites and by evaporation for all the isotopic ratios

  14. Applicability of isotopic dilution methods for determination of the zinc supplying capacity of some Indian soils

    International Nuclear Information System (INIS)

    Iyengar, B.R.V.; Deb, D.L.

    1975-01-01

    The applicability of the isotopic dilution methods to determine the zinc supplying capacity of some Indian soils belonging to three soil groups was studied using 65 Zn. In these soils 'L' values determined by the pot culture method and the 'E' values by equilibration in soil suspensions by the carrier free and carrier methods and using chemical extractants DTPA-CaCl 2 -NaOAc and EDTA-NH 4 OAc were compared. The 'L' values were significantly correlated with zinc uptake by maize and also with zinc extracted by a number of chemical extractants. The laboratory determinations 'E' values by isotopic exchange equilibria in soil suspension both with and without carrier zinc led to over estimates and gave grossly exggerated values of 'labile zinc' especially in alkaline and high zinc 'fixing' soils. The 'E' values determined in both DTPA-CaCl 2 -NaOAc and EDTA-NH 4 OAc correlated significantly with zinc uptake by maize. These values agreed well with 'L' values and 'available' zinc determined by chemical soil tests. (author)

  15. Burn-up determination of irradiated thoria samples by isotope dilution-thermal ionisation mass spectrometry

    International Nuclear Information System (INIS)

    Aggarwal, S.K.; Jaison, P.G.; Telmore, V.M.; Shah, R.V.; Sant, V.L.; Sasibhushan, K.; Parab, A.R.; Alamelu, D.

    2010-03-01

    Burn-up was determined experimentally using thermal ionization mass spectrometry for two samples from ThO 2 bundles irradiated in KAPS-2. This involved quantitative dissolution of the irradiated fuel samples followed by separation and determination of Th, U and a stable fission product burn-up monitor in the dissolved fuel solution. Stable fission product 148 Nd was used as a burn-up monitor for determining the number of fissions. Isotope Dilution-Thermal Ionisation Mass Spectrometry (ID-TIMS) using natural U, 229 Th and enriched 142 Nd as spikes was employed for the determination of U, Th and Nd, respectively. Atom % fission values of 1.25 ± 0.03 were obtained for both the samples. 232 U content in 233 U determined by alpha spectrometry was about 500 ppm and this was higher by a factor of 5 compared to the theoretically predicted value by ORIGEN-2 code. (author)

  16. Determination of cadmium, lead and zinc in a candidate reference materials using isotope dilution mass spectrometry

    International Nuclear Information System (INIS)

    Munoz, Luis; Gras, Nuri; Quejido, Alberto; Fernandez, Marta

    2001-01-01

    The growing demands placed on analytical laboratories to ensure the reliability of their results, due to the introduction of systems of quality and to the increasing use of metrology in chemical measurements has led most laboratories to validate their methodologies and to control them statistically. One of the techniques used most often for these purposes is based on the use of reference materials. The proper use of these materials means that laboratory results may be traced to the International System of Units, analytical methodologies can be validated, instruments calibrated and chemical measurements harmonized. One of the biggest challenges in developing reference materials is that of certifying their properties, a process that has been defined as assigning a concentration value that is as close as possible to the true value together with its uncertainty. Organizations that produce reference materials use several options for their certification process, and among these is the use of a primary method. Among the primary methods recognized by the International Office of Weights and Measures is the Isotope Dilution Mass Spectrometry technique. The Chilean Nuclear Energy Commission, through its Reference Materials Program, has prepared a reference material of clam tissue, which has been chemically defined by different analytical methodologies applied in different national and international laboratories. This work describes the methodology developed with the CIEMAT for determining the elements lead, cadmium and zinc in the clam tissue reference material using the primary technique of Isotope Dilution Mass Spectrometry. The calculation is described for obtaining the spike amounts to be added to the sample and the procedure is explained for carrying out the isotopic exchange. The isotopic relationships 204 Pb/ 205 Pb, 111 Cd/ 114 Cd and 66 Zn/ 67 Zn were determined in an atomic emission spectrometer with a plasma source with the following characteristics: plasma

  17. Determination of Light Water Reactor Fuel Burnup with the Isotope Ratio Method

    International Nuclear Information System (INIS)

    Gerlach, David C.; Mitchell, Mark R.; Reid, Bruce D.; Gesh, Christopher J.; Hurley, David E.

    2007-01-01

    For the current project to demonstrate that isotope ratio measurements can be extended to zirconium alloys used in LWR fuel assemblies we report new analyses on irradiated samples obtained from a reactor. Zirconium alloys are used for structural elements of fuel assemblies and for the fuel element cladding. This report covers new measurements done on irradiated and unirradiated zirconium alloys, Unirradiated zircaloy samples serve as reference samples and indicate starting values or natural values for the Ti isotope ratio measured. New measurements of irradiated samples include results for 3 samples provided by AREVA. New results indicate: 1. Titanium isotope ratios were measured again in unirradiated samples to obtain reference or starting values at the same time irradiated samples were analyzed. In particular, 49Ti/48Ti ratios were indistinguishably close to values determined several months earlier and to expected natural values. 2. 49Ti/48Ti ratios were measured in 3 irradiated samples thus far, and demonstrate marked departures from natural or initial ratios, well beyond analytical uncertainty, and the ratios vary with reported fluence values. The irradiated samples appear to have significant surface contamination or radiation damage which required more time for SIMS analyses. 3. Other activated impurity elements still limit the sample size for SIMS analysis of irradiated samples. The sub-samples chosen for SIMS analysis, although smaller than optimal, were still analyzed successfully without violating the conditions of the applicable Radiological Work Permit

  18. Determination of geographic provenance of cotton fibres using multi-isotope profiles and multivariate statistical analysis

    Science.gov (United States)

    Daeid, N. Nic; Meier-Augenstein, W.; Kemp, H. F.

    2012-04-01

    The analysis of cotton fibres can be particularly challenging within a forensic science context where discrimination of one fibre from another is of importance. Normally cotton fibre analysis examines the morphological structure of the recovered material and compares this with that of a known fibre from a particular source of interest. However, the conventional microscopic and chemical analysis of fibres and any associated dyes is generally unsuccessful because of the similar morphology of the fibres. Analysis of the dyes which may have been applied to the cotton fibre can also be undertaken though this can be difficult and unproductive in terms of discriminating one fibre from another. In the study presented here we have explored the potential for Isotope Ratio Mass Spectrometry (IRMS) to be utilised as an additional tool for cotton fibre analysis in an attempt to reveal further discriminatory information. This work has concentrated on un-dyed cotton fibres of known origin in order to expose the potential of the analytical technique. We report the results of a pilot study aimed at testing the hypothesis that multi-element stable isotope analysis of cotton fibres in conjunction with multivariate statistical analysis of the resulting isotopic abundance data using well established chemometric techniques permits sample provenancing based on the determination of where the cotton was grown and as such will facilitate sample discrimination. To date there is no recorded literature of this type of application of IRMS to cotton samples, which may be of forensic science relevance.

  19. Final Progress Report: Isotope Identification Algorithm for Rapid and Accurate Determination of Radioisotopes Feasibility Study

    International Nuclear Information System (INIS)

    Rawool-Sullivan, Mohini; Bounds, John Alan; Brumby, Steven P.; Prasad, Lakshman; Sullivan, John P.

    2012-01-01

    This is the final report of the project titled, 'Isotope Identification Algorithm for Rapid and Accurate Determination of Radioisotopes,' PMIS project number LA10-HUMANID-PD03. The goal of the work was to demonstrate principles of emulating a human analysis approach towards the data collected using radiation isotope identification devices (RIIDs). It summarizes work performed over the FY10 time period. The goal of the work was to demonstrate principles of emulating a human analysis approach towards the data collected using radiation isotope identification devices (RIIDs). Human analysts begin analyzing a spectrum based on features in the spectrum - lines and shapes that are present in a given spectrum. The proposed work was to carry out a feasibility study that will pick out all gamma ray peaks and other features such as Compton edges, bremsstrahlung, presence/absence of shielding and presence of neutrons and escape peaks. Ultimately success of this feasibility study will allow us to collectively explain identified features and form a realistic scenario that produced a given spectrum in the future. We wanted to develop and demonstrate machine learning algorithms that will qualitatively enhance the automated identification capabilities of portable radiological sensors that are currently being used in the field.

  20. Development of pre-concentration procedure for the determination of Hg isotope ratios in seawater samples

    International Nuclear Information System (INIS)

    Štrok, Marko; Hintelmann, Holger; Dimock, Brian

    2014-01-01

    Highlights: • The method for the quantitative pre-concentration of Hg from seawater was developed. • First report of Hg isotope ratios in seawater is presented. • A unique mass independent 200 Hg isotope fractionation was observed. • This fractionation has unique potential to distinguish anthropogenic and natural Hg. - Abstract: Hg concentrations in seawater are usually too low to allow direct (without pre-concentration and removal of salt matrix) measurement of its isotope ratios with multicollector-inductively coupled plasma mass spectrometry (MC-ICP-MS). Therefore, a new method for the pre-concentration of Hg from large volumes of seawater was developed. The final method allows for relatively fast (about 2.5 L h −1 ) and quantitative pre-concentration of Hg from seawater samples with an average Hg recovery of 98 ± 6%. Using this newly developed method we determined Hg isotope ratios in seawater. Reference seawater samples were compared to samples potentially impacted by anthropogenic activity. The results show negative mass dependent fractionation relative to the NIST 3133 Hg standard with δ 202 Hg values in the range from −0.50‰ to −1.50‰. In addition, positive mass independent fractionation of 200 Hg was observed for samples from reference sites, while impacted sites did not show significant Δ 200 Hg values. Although the influence of the impacted sediments is limited to the seawater and particulate matter in very close proximity to the sediment, this observation may raise the possibility of using Δ 200 Hg to distinguish between samples from impacted and reference sites

  1. A review on the determination of isotope ratios of boron with mass spectrometry.

    Science.gov (United States)

    Aggarwal, Suresh Kumar; You, Chen-Feng

    2017-07-01

    The present review discusses different mass spectrometric techniques-viz, thermal ionization mass spectrometry (TIMS), inductively coupled plasma mass spectrometry (ICPMS), and secondary ion mass spectrometry (SIMS)-used to determine 11 B/ 10 B isotope ratio, and concentration of boron required for various applications in earth sciences, marine geochemistry, nuclear technology, environmental, and agriculture sciences, etc. The details of the techniques-P-TIMS, which uses Cs 2 BO 2 + , N-TIMS, which uses BO 2 - , and MC-ICPMS, which uses B + ions for bulk analysis or B - and B + ions for in situ micro-analysis with SIMS-are highlighted. The capabilities, advantages, limitations, and problems in each mass spectrometric technique are summarized. The results of international interlaboratory comparison experiments conducted at different times are summarized. The certified isotopic reference materials available for boron are also listed. Recent developments in laser ablation (LA) ICPMS and QQQ-ICPMS for solids analysis and MS/MS analysis, respectively, are included. The different aspects of sample preparation and analytical chemistry of boron are summarized. Finally, the future requirements of boron isotope ratios for future applications are also given. Presently, MC-ICPMS provides the best precision and accuracy (0.2-0.4‰) on isotope ratio measurements, whereas N-TIMS holds the potential to analyze smallest amount of boron, but has the issue of bias (+2‰ to 4‰) which needs further investigations. © 2016 Wiley Periodicals, Inc. Mass Spec Rev 36:499-519, 2017. © 2016 Wiley Periodicals, Inc.

  2. Sequential Banking.

    OpenAIRE

    Bizer, David S; DeMarzo, Peter M

    1992-01-01

    The authors study environments in which agents may borrow sequentially from more than one leader. Although debt is prioritized, additional lending imposes an externality on prior debt because, with moral hazard, the probability of repayment of prior loans decreases. Equilibrium interest rates are higher than they would be if borrowers could commit to borrow from at most one bank. Even though the loan terms are less favorable than they would be under commitment, the indebtedness of borrowers i...

  3. Determination of uranium and thorium isotopes by solid phase extraction and alpha spectrometry

    International Nuclear Information System (INIS)

    Kuruc, J.; Kovacova, M.; Strisovska, J.; Galanda, D.

    2013-01-01

    The aim of this work was to test the modified method suitable for the separation of isotopes of uranium and thorium samples of rocks, including gold ore and gold concentrate using of extraction chromatography method, after digestion of the sample, concentrating, separate the isotopes of uranium and thorium isotopes to prepare sources for the measurement of alpha spectra. Samples of rocks, gold ore and gold concentrate were digered in microwave decomposition in the environment of hydrogen peroxide and concentrated nitric acid. For the separation of uranium and thorium the vacuum box with cartridges DGA Resin and Resin(R) UTEVA (Triskem International, France) was used. Both sorbents allow separation of uranium from thorium. The results confirmed that the both sorbents give the same results within expanded uncertainty. The mass activity of monitored uranium and thorium radioisotopes was determined by alpha spectrometry method. The yields of separation were determined using uranium-232 as a tracer radionuclide; the activity of 232 U was 0.1438 Bq. Alpha spectra were measured on the Alpha spectrometer EG and G ORTEC 576A with the software MAESTRO, MCA Emulator and Gamma Vision-32 for Windows, USA. Mass activities of radionuclides were converted to mass concentration of isotopes 238 U, 234 U, 232 Th, 230 Th and 228 Th. The highest concentration of 238 U was sampled in granodiorite (Tunnel S-XIV-2, southwards, mining of Cu ore, not working there since 1990), where m( 238 U) = (0.81 ± 0.09) mg kg -1 (DGA Resin) and m( 238 U) = (0.90 ± 0.09) mg kg -1 (UTEVA(R) Resin), as well as m( 232 Th) = (18.8 ± 1.7) mg kg -1 (DGA Resin) and m( 232 Th) = (17.8 ± 1.5) mg kg -1 (UTEVA(R) Resin). In other samples of rocks, gold ore and gold concentrates have specific masses of isotopes of uranium and thorium two-to ten-folds lower. It can be concluded that the rocks, gold ores and concentrates of gold from the 'Rozalia' mine contain lower concentrations of uranium several times against

  4. Comparison of bile acid synthesis determined by isotope dilution versus fecal acidic sterol output in human subjects

    International Nuclear Information System (INIS)

    Duane, W.C.; Holloway, D.E.; Hutton, S.W.; Corcoran, P.J.; Haas, N.A.

    1982-01-01

    Fecal acidic sterol output has been found to be much lower than bile acid synthesis determined by isotope dilution. Because of this confusing discrepancy, we compared these 2 measurements done simultaneously on 13 occasions in 5 normal volunteers. In contrast to previous findings, bile acid synthesis by the Lindstedt isotope dilution method averaged 16.3% lower than synthesis simultaneously determined by fecal acidic sterol output (95% confidence limit for the difference - 22.2 to -10.4%). When one-sample determinations of bile acid pools were substituted for Lindstedt pools, bile acid synthesis by isotope dilution averaged 5.6% higher than synthesis by fecal acidic sterol output (95% confidence limits -4.9 to 16.1%). These data indicate that the 2 methods yield values in reasonably close agreement with one another. If anything, fecal acidic sterol outputs are slightly higher than synthesis by isotope dilution

  5. Final results of the PIDIE intercomparison exercise for the plutonium isotopic determination by gamma-ray spectrometry

    International Nuclear Information System (INIS)

    Morel, J.; Chauvenet, B.; Etcheverry, M.

    1991-01-01

    Final results from the PIDIE intercomparison exercise organised by the ESARDA Working Group on techniques and standards for non-destructive analysis are presented. The aim of this exercise carried out in 1988 was to test the gamma-ray spectroscopy methods used to determine the plutonium isotopic ratios in a large range of isotopic composition, in order to analyse the parameters and the error sources influencing the results. Sets of seven sealed samples of different plutonium isotopic composition were sent to nine participating laboratories. The final results with uncertainty indicators are reported; they are compared with complementary mass-spectrometry determinations. No important bias has been observed from this exercise. Significant improvements in plutonium isotopic determination by gamma-ray spectrometry come from both more elaborate spectrum analysis methods and better equipment

  6. Determination of strontium and lead isotope ratios of grains using high resolution inductively coupled plasma mass spectrometer with single collector

    International Nuclear Information System (INIS)

    Shinozaki, Miyuki; Ariyama, Kaoru; Kawasaki, Akira; Hirata, Takafumi

    2010-01-01

    A method for determining strontium and lead isotope ratios of grains was developed. The samples investigated in this study were rice, barley and wheat. The samples were digested with nitric acid and hydrogen peroxide, and heated in a heating block. Strontium and lead were separated from the matrix by adding an acid digested solution into a column packed with Sr resin, which has selectivity for the absorption of strontium and lead. Strontium and lead isotope ratios were determined using a high-resolution inductively coupled plasma mass spectrometer (HR-ICP-MS) with a single collector. The intraday relative standard deviations of 87 Sr/ 86 Sr and lead isotope ratios ( 204 Pb/ 206 Pb, 207 Pb/ 206 Pb, 208 Pb/ 206 Pb) by HR-ICP-MS measurements were < 0.06% and around 0.1%, respectively. This method enabled us to determine strontium and lead isotope ratios in two days. (author)

  7. Application of ICP-MS and AMS for determination of Pu- and U-isotope ratios for source identification

    Energy Technology Data Exchange (ETDEWEB)

    Skipperud, L. (Norwegian Univ. of Life Sciences, Isotope Lab.. Dept. of Plant and Environmental Sciences, AAs (Norway))

    2010-03-15

    Full text: Anthropogenic plutonium has been introduced into the environment over the past 50 years as the result of the detonation of nuclear weapons and operational releases from the nuclear industry. In the Arctic environment, the main source of plutonium is from atmospheric weapons testing, which have resulted in a relatively uniform, underlying global distribution of plutonium. Plutonium isotope ratios are known to vary with reactor type, nuclear fuel-burn up time, neutron flux, and energy, and for fallout from nuclear detonations, weapon type and yield. Weapons-grade plutonium is characterized by a low content of the 240Pu isotope, with 240Pu/239Pu isotope ratio less than 0.05. In contrast, both global weapons fallout and spent nuclear fuel from civil reactors have higher 240Pu/239Pu isotope ratios (civil nuclear power reactors have 240Pu/239Pu atom ratios of between about 0.2-1). Thus, different sources often exhibit characteristic plutonium isotope ratios and these ratios can be used to identify the origin of contamination, calculate inventories, or follow the migration of contaminated sediments and waters. The measurement of the plutonium-isotope ratios in these studies offers both a means of identifying the origin of radionuclide contamination and the influence of the various nuclear installations on inputs to the Arctic, as well as a potential method for following the movement of water and sediment loads in the rivers. The present paper presents results from determination of plutonium concentrations and isotope ratios in sediment samples collected during various expeditions to the Kara Sea, the Ob and Yenisey estuaries and their river systems and also Pu isotope ratios in the near area of Mayak PA. Weapons-grade plutonium is characterized by a low content of the Pu-240 isotope, with Pu-240/Pu-239 isotope ratio less than 0.05. In contrast, both global weapons fallout and spent nuclear fuel from civil reactors have higher Pu-240/Pu-239 isotope ratios, and

  8. Experimental determination of isotope enrichment factors – bias from mass removal by repetitive sampling

    DEFF Research Database (Denmark)

    Buchner, Daniel; Jin, Biao; Ebert, Karin

    2017-01-01

    to account for mass removal and for volatilization into the headspace. In this study we use both synthetic and experimental data to demonstrate that the determination of ε-values according to current correction methods is prone to considerable systematic errors even in well-designed experimental setups....... Application of inappropriate methods may lead to incorrect and inconsistent ε-values entailing misinterpretations regarding the processes underlying isotope fractionation. In fact, our results suggest that artifacts arising from inappropriate data evaluation might contribute to the variability of published ε...

  9. A Comparison of Marmosa xerophilla home ranges as determined by isotope and live trap methods

    International Nuclear Information System (INIS)

    Thielen D; Arends, A.; Lea, D.

    1995-01-01

    Non breeder females of Marmosa xerophilla home ranges were determined by two methods: The first one, to which we have called isotope marked - localization method (MLR), involve the marked of three individuals with sealed radioactive sources of I-131 of 2 mCi, which were subcutaneously implanted in the back of the animals. During the 40 following days, the individuals were located in their burrows with the help of an Geiger-Muller counter. The vital areas were studied from the polygons that result from the union of the burrows more external points up to [es

  10. A comparison of sequential and information-based methods for determining the co-integration rank in heteroskedastic VAR MODELS

    DEFF Research Database (Denmark)

    Cavaliere, Giuseppe; Angelis, Luca De; Rahbek, Anders

    2015-01-01

    In this article, we investigate the behaviour of a number of methods for estimating the co-integration rank in VAR systems characterized by heteroskedastic innovation processes. In particular, we compare the efficacy of the most widely used information criteria, such as Akaike Information Criterion....... The relative finite-sample properties of the different methods are investigated by means of a Monte Carlo simulation study. For the simulation DGPs considered in the analysis, we find that the BIC-based procedure and the bootstrap sequential test procedure deliver the best overall performance in terms......-based method to over-estimate the co-integration rank in relatively small sample sizes....

  11. Polymeric microchip for the simultaneous determination of anions and cations by hydrodynamic injection using a dual-channel sequential injection microchip electrophoresis system.

    Science.gov (United States)

    Gaudry, Adam J; Nai, Yi Heng; Guijt, Rosanne M; Breadmore, Michael C

    2014-04-01

    A dual-channel sequential injection microchip capillary electrophoresis system with pressure-driven injection is demonstrated for simultaneous separations of anions and cations from a single sample. The poly(methyl methacrylate) (PMMA) microchips feature integral in-plane contactless conductivity detection electrodes. A novel, hydrodynamic "split-injection" method utilizes background electrolyte (BGE) sheathing to gate the sample flows, while control over the injection volume is achieved by balancing hydrodynamic resistances using external hydrodynamic resistors. Injection is realized by a unique flow-through interface, allowing for automated, continuous sampling for sequential injection analysis by microchip electrophoresis. The developed system was very robust, with individual microchips used for up to 2000 analyses with lifetimes limited by irreversible blockages of the microchannels. The unique dual-channel geometry was demonstrated by the simultaneous separation of three cations and three anions in individual microchannels in under 40 s with limits of detection (LODs) ranging from 1.5 to 24 μM. From a series of 100 sequential injections the %RSDs were determined for every fifth run, resulting in %RSDs for migration times that ranged from 0.3 to 0.7 (n = 20) and 2.3 to 4.5 for peak area (n = 20). This system offers low LODs and a high degree of reproducibility and robustness while the hydrodynamic injection eliminates electrokinetic bias during injection, making it attractive for a wide range of rapid, sensitive, and quantitative online analytical applications.

  12. Simulation of the isotopic ratio determination of plutonium by Ge(Li) gamma-ray spectrometry

    International Nuclear Information System (INIS)

    Baba, Hiroshi; Yagi, Hideyuki

    1979-09-01

    A simulation program ''SIMPUG'' was developed for assessing feasibility of the isotopic ratio determination of plutonium by Ge(Li) γ-ray spectrometry. The program consists of (1) construction of the spectrum profiles for eight peak groupings of interest with a given set of isotopic compositions and by the use of the known nuclear data for emitting γ rays and (2) determination of the intensity of each participating nuclide following a presently developed algorithm of spectrum unfolding. Effects of various factors on the reliability of the results were examined with the simulation program. Accuracy of the results was found to be little affected by the change of the detector resolution if the spectrum was taken with sufficient expansion. Counting statistics was concluded to be the most essential factor for the precision of the results, while the aging effect was not found significant. Contamination of fission products beyond a certain level brought about fatal errors in the determined values, particularly in the case of minor components. (author)

  13. Determination of nanogram amounts of iodide by electrochemical isotope dilution analysis

    International Nuclear Information System (INIS)

    Gabrielsson, A.-B.; Beronius, P.

    1976-01-01

    A known quantity of iodide in ethanol as solvent was labelled with 131 I-and subsequently diluted with a predetermined amount of inactive iodide. Specific activities before and after the isotope dilution were established by anodically depositing small fractions of the halide in each sample on rotating silver micro electrodes and determining the activities of the electrodeposits. The lowest concentration of iodide used in any analysis was 1.10 -5 M. Further deposition studies revealed that iodide can be deposited with 1 100% current efficiency on the rotating silver micro electrode for concentration down to 2.4.10 -6 M. Electrodeposition studies for still lower concentrations have not yet been undertaken. These results suggest that amounts of iodide ion down to about 10 ng, and possibly still smaller quantitites, might be determined with the method developed. Amounts from 42 ng to 1 μg can be determined with an error of 2.5%. (T.G.)

  14. Precise determination of sodium in serum by simulated isotope dilution method of inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Yan Ying; Zhang Chuanbao; Zhao Haijian; Chen Wenxiang; Shen Ziyu; Wang Xiaoru; Chen Dengyun

    2007-01-01

    A new precise and accurate method for the determination of sodium in serum by inductively coupled plasma mass spectrometry (ICP-MS) was developed. Since 23 Na is the single isotope element, 27 Al is selected as simulated isotope of Na. Al is spiked into serum samples and Na standard solution. 23 Na/ 27 Al ratio in the Na standard solution is determined to assume the natural Na isotope ratio. The serums samples are digested by purified HNO 3 /H 2 O 2 and diluted to get about 0.6 μg·g -1 Al solutions, and the 23 Na/ 27 Al ratios of the serum samples are obtained to calculate the accurate Na concentrations basing on the isotope dilution method. When the simulated isotope dilution method of ICP-MS is applied and Al is selected as the simulated isotope of Na, the precise and accurate Na concentrations in the serums are determined. The inter-day precision of CV<0.13% for one same serum sample is obtained during 3 days 4 measurements. The spike recoveries are between 99.69% and 100.60% for 4 different serum samples and 3 days multi-measurements. The results of measuring standard reference materials of serum sodium are agree with the certified value. The relative difference between 3 days is 0.22%-0.65%, and the relative difference in one bottle is 0.15%-0.44%. The ICP-MS and Al simulated isotope dilution method is proved to be not only precise and accurate, but also quick and convenient for measuring Na in serum. It is promising to be a reference method for precise determination of Na in serum. Since Al is a low cost isotope dilution reagent, the method is possible to be widely applied for serum Na determination. (authors)

  15. Determining metal assimilation efficiency in aquatic invertebrates using enriched stable metal isotope tracers

    International Nuclear Information System (INIS)

    Croteau, Marie-Noele; Luoma, Samuel N.; Pellet, Bastien

    2007-01-01

    We employ a novel approach that combines pulse-chase feeding and multi-labelled stable isotopes to determine gut passage time (GPT), gut retention time (GRT), food ingestion rate (IR) and assimilation efficiency (AE) of three trace elements for a freshwater gastropod. Lettuce isotopically enriched in 53 Cr, 65 Cu and 106 Cd was fed for 2 h to Lymnaea stagnalis. The release of tracers in feces and water was monitored for 48 h, during which unlabelled lettuce was provided ad libidum. The first defecation of 53 Cr occurred after 5 h of depuration (GPT), whereas 90% of the ingested 53 Cr was recovered in the feces after 22.5 h of depuration (GRT). 53 Chromium was not significantly accumulated in the soft tissues upon exposure. In contrast, 65 Cu and 106 Cd assimilation was detectable for most experimental snails, i.e., 65/63 Cu and 106/114 Cd ratios in exposed snails were higher than those for controls. Food IR during the labelled feeding phase was 0.16 ± 0.07 g g -1 d -1 . IR was inferred from the amount of 53 Cr egested in the feces during depuration and the concentration of 53 Cr in the labelled lettuce. Assimilation efficiencies (±95% CI) determined using mass balance calculations were 84 ± 4% for Cu and 85 ± 3% for Cd. The ratio method yields similar AE estimates. Expanding the application of this novel stable isotope tracer technique to other metals in a wide variety of species will provide unique opportunities to evaluate the interplay between digestive processes and dietary influx of metals. Understanding the biological processes that modulate dietborne metal uptake is crucial to assess the toxicity of dietborne metals

  16. Serum/plasma methylmercury determination by isotope dilution gas chromatography-inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Baxter, Douglas C., E-mail: douglas.baxter@alsglobal.com [ALS Scandinavia AB, Aurorum 10, 977 75 Lulea (Sweden); Faarinen, Mikko [ALS Scandinavia AB, Aurorum 10, 977 75 Lulea (Sweden); Osterlund, Helene; Rodushkin, Ilia [ALS Scandinavia AB, Aurorum 10, 977 75 Lulea (Sweden); Division of Geosciences, Lulea University of Technology, 977 87 Lulea (Sweden); Christensen, Morten [ALS Scandinavia AB, Maskinvaegen 2, 183 53 Taeby (Sweden)

    2011-09-09

    Highlights: {center_dot} We determine methylmercury in serum and plasma using isotope dilution calibration. {center_dot} Separation by gas chromatography and detection by inductively coupled plasma mass spectrometry. {center_dot} Data for 50 specimens provides first reference range for methylmercury in serum. {center_dot} Serum samples shown to be stable for 11 months in refrigerator. - Abstract: A method for the determination of methylmercury in plasma and serum samples was developed. The method uses isotope dilution with {sup 198}Hg-labeled methylmercury, extraction into dichloromethane, back-extraction into water, aqueous-phase ethylation, purge and trap collection, thermal desorption, separation by gas chromatography, and mercury isotope specific detection by inductively coupled plasma mass spectrometry. By spiking 2 mL sample with 1.2 ng tracer, measurements in a concentration interval of (0.007-2.9) {mu}g L{sup -1} could be performed with uncertainty amplification factors <2. A limit of quantification of 0.03 {mu}g L{sup -1} was estimated at 10 times the standard deviation of concentrations measured in preparation blanks. Within- and between-run relative standard deviations were <10% at added concentration levels of 0.14 {mu}g L{sup -1}, 0.35 {mu}g L{sup -1} and 2.8 {mu}g L{sup -1}, with recoveries in the range 82-110%. Application of the method to 50 plasma/serum samples yielded a median (mean; range) concentration of methylmercury of 0.081 (0.091; <0.03-0.19) {mu}g L{sup -1}. This is the first time methylmercury has been directly measured in this kind of specimen, and is therefore the first estimate of a reference range.

  17. Application of the mass spectrometry-isotope dilution technique for the determination of uranium contents in rocks

    International Nuclear Information System (INIS)

    Kakazu, M.H.; Iyer, S.S.

    1980-01-01

    Application of the spectrometric isotope dilution technique for the accurate determination of parts per million range of uranium in rock samples is described. The various aspects of the method like sample dissolution, ion exchange separation, mass spectrometric procedures are discussed. A single filament ionization source was employed for the isotope analysis. A carbon reduction method was used to reduce uranium oxide ions to uranium metal ions. The tracer solution for isotope dilution was prepared from National Bureau of Standards uranium isotopic Standard NBS U-970. Uranium contents are meassured for nine rock samples and the values obtained are compared with the uranium values measured by others workers. Errors caused in the uranium determination due to sample splitting problems as well as the incomplete acid digestion of the samples are discussed. (Author) [pt

  18. Determination of the δ13C (per mille) isotopic rate of the Brazilian beer pilsen type

    International Nuclear Information System (INIS)

    Rossete, Alexssandra L.R.M.; Bendassolli, Jose Albertino; Lopes, Fabio; Martinelli, Luiz Antonio

    2002-01-01

    Beer has been consumed in Brazil since the XIX century. However, at that time, this beverage was imported from England, and the first Brazilian breweries just appeared at the end of the XX century. Basically, beer is made from: malt of barley, Humulus lupulus, water and yeast. In this work, twenty brands of national beer (Pilsen type), and also two different cereals, barley, a C3 metabolism plant, corn, a C4 plant, were analysed to determine their isotope composition δ 13 C (per mille) utilizing a mass spectrometer Delta Plus Finigam and Anca S.L. An aliquot of each sample was transferred using a capillary of glass to a tin capsule contends a small amount of sorbitol. The isotope compositions, δ 13 C, of barley and corn samples determined were -27.2 and -11.5 per mille, respectively. These results were used to calculate the equation of mixture model. Considering the beer samples, the δ 13 C ranged from -18.3 to -23.1 per mille; this result means that the percentage of C3 plant is from 43.3 to 73.9 per mille. In this manner, it is possible to concluded that all beer samples has malted cereals (C4 plant), as far as the low values of C3 plants were presented in these samples as shown through the equation of mixtures model. (author)

  19. Standard test method for radiochemical determination of uranium isotopes in soil by alpha spectrometry

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2011-01-01

    1.1 This test method covers the determination of alpha-emitting uranium isotopes in soil. This test method describes one acceptable approach to the determination of uranium isotopes in soil. 1.2 The test method is designed to analyze 10 g of soil; however, the sample size may be varied to 50 g depending on the activity level. This test method may not be able to completely dissolve all forms of uranium in the soil matrix. Studies have indicated that the use of hydrofluoric acid to dissolve soil has resulted in lower values than results using total dissolution by fusion. 1.3 The lower limit of detection is dependent on count time, sample size, detector, background, and tracer yield. The chemical yield averaged 78 % in a single laboratory evaluation, and 66 % in an interlaboratory collaborative study. 1.4 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only. 1.5 This standard does not purport to address all of the safety concerns, if any, ass...

  20. [Determination of endogenous agmatine in rat plasma by isotope dilution-gas chromatography-mass spectrometry].

    Science.gov (United States)

    Qiu, Zhongli; Lin, Ying; Xiong, Zhili; Xie, Jianwei

    2014-07-01

    A method for the determination of endogenous agmatine in rat plasma was developed by isotope dilution-gas chromatography-negative chemical ionization mass spectrometry (GC-NCI/MS). The plasma samples were analyzed after protein precipitation, evaporation, derivatization by hexafluoroacetone (HFAA), and clean-up on a Florisil SPE column. The GC-MS analysis utilized stable isotope d8-agmatine as internal standard. The samples after treatme were tested by negative chemical ionization with selected ion monitoring (SIM) which was set at m/z 492 (molecular ion of agmatine) and m/z 500 (molecular ion of internal standard). The limit of detection (LOD) of agmatine standard solution was 0.005 7 ng/mL. The calibration curve of the agmatine spiked in rat plasma showed a good linear relationship at the range of 1.14-57.0 ng/mL (r = 0.997). The recoveries of agmatine spiked in rat plasma ranged from 92.3% to 109.8%. Inter-day and intra-day precisions were less than 15%. The average concentration level of agmatine in rat plasma was (22 +/- 9) ng/mL, and there was no significant difference between male and female SD rats (p > 0.05). The method is high sensitive and specific, and can be used for the determination of endogenous agmatine in plasma. It provides a strong support for the subsequent research of agmatine.

  1. Stable Isotope Analysis of Extant Lamnoid Shark Centra: A New Tool in Age Determination?

    Science.gov (United States)

    Labs, J.

    2003-12-01

    The oxygen isotopes of fourteen vertebral centra from ten extant lamnoid sharks (including Carcharodon carcharias [great white], Isurus paucus [longfin mako], and Isurus oxyrinchus [shortfin mako]) were sampled and measured along the growth axis to determine the periodicity of incremental growth represented in the centra. As part of the internal (endochondral) skeleton, shark centra are composed initially of hyaline cartilage, which then secondarily ossifies during ontogeny forming calcified hydroxyapatite bone. The incremental growth of shark centra forms definite growth rings, with darker denser portions being deposited during slower growth times (i.e., winter) and lighter portions being deposited during more rapid growth (i.e., summer). Thus, shark centra, whether they are extant or extinct, are characterized by clearly delineated incremental growth couplets. The problem with this general rule is that there are several factors in which the growth of these couplets can vary depending upon physical environment (including temperature and water depth), food availability, and stress. The challenge for paleobiological interpretations is how to interpret the periodicity of this growth. It can generally be assumed that these bands are annual, but it is uncertain the extent to which exceptions to the rule occur. Stable isotopic analysis provides the potential to independently determine the periodicity of the growth increments and ultimately the ontogenetic age of an individual.

  2. Determination of groundwater characteristics in the Nigde-Misli Plain by means of isotopes

    International Nuclear Information System (INIS)

    Bursali, S.; Ertan, I.; Yalcin, H.; Gunay, G.; Onhon, E.

    1975-06-01

    Nigde-Misli Plain, situated in the Central Anatolia, is 30 km north to Nigde City. The most important part of the plain is Golcuk with a superficial area of 290 sq. kilometers. Ovacik part has a superficial area of 22 sq. kilometers and separately Edikli part with 35 sq. kilometers. The total of the superficial area of the plain is 347 sq. km and its average altitude is 1340 m. The main purpose of this study is to check the sufficiency of the Nigde-Misli aquifer from which all of the wells are fed. Hydrogeological studies of the Nigde-Misli Plain have been completed in order to determine some of the groundwater characteristics. However, it was thought that it would be useful to check and support the hydrogeological conclusions by isotopic methods and to clarify some important points in the groundwater movement for which hydrogeological methods seem to be insufficient. For this purpose, surface water and ground water, precipitation and soil samples have been collected and analysed to determine their stable isotopes and tritium contents. Results have been interpreted in order to answer, as far as it is possible, to the question of the sufficiency of the Nigde-Misli aquifer

  3. Determination of sulfur in steels by isotope dilution mass spectrometry after dissolution with sealed tube

    International Nuclear Information System (INIS)

    Watanabe, Kazuo

    1981-01-01

    The scaled tube dissolution technique was studied for the complete conversion of sulfur in steels to sulfate. Isotope dilution mass spectrometry was used for the determination of sulfur in the sulfate. Sample (0.5 g) was dissolved in nitric acid (7 ml) and hydrochloric acid (3 ml) in a scaled borosilicate glass tube on being heated above 180 0 C overnight. Nitrate ions were removed by repeated evaporation with hydrochloric acid. The residue was dissolved in hydrochloric acid. Sulfate was reduced with a mixture of hydrochloric, hydroiodic and hypophosphorous acids; hydrogen sulfide evolved was absorbed in cadmium acetate solution, then converted to silver sulfide, which was burned to sulfur dioxide in pure oxygen at low pressure, for isotopic analysis. Analytical blank in whole procedure was 0.8 μg of sulfur. This technique was applied to the determination of sulfur in NBS low alloy steels. The principal cause of low values obtained by the open beaker dissolution technique was evaporation losses of sulfur as sulfur dioxide during the dissolution. (author)

  4. Determination of isotopic composition of boron in boron carbide by TIMS and PIGE: an inter-comparison study

    International Nuclear Information System (INIS)

    Sasibhushan, K.; Rao, R.M.; Parab, A.R.; Alamelu, D.; Aggarwal, S.K.; Acharya, R.; Chhillar, S.; Pujari, P.K.

    2015-01-01

    The paper reports a comparison of results on the determination of isotopic composition of boron in boron carbide (B 4 C) samples by Thermal Ionisation Mass Spectrometry (TIMS) and Particle Induced Gamma ray Spectrometry (PIGE). B 4 C samples having varying boron isotopic composition (natural, enriched with respect to 10 B) and their synthetic mixtures) have been analysed by both the techniques. The 10 B atom% was found to be in the range of 20-67%. (author)

  5. An easy method for the determination of Ra isotopes and actinide alpha emitters from the same water sample

    International Nuclear Information System (INIS)

    Moron, M.C.; Garcia-Tenorio, R.; Garcia-Montano, E.; Garcia-Leon, M.; Madurga, G.

    1986-01-01

    Radium isotopes and actinide α emitters are easily determined from the same water sample. The Ra fraction is obtained by coprecipitation with Ba, while a Fe coprecipitation is used for the actinides. Both fractions are measured with a gas-flow proportional counter. Additionally the isotopic Ra composition is obtained by measuring at two or three different times the α activity from the Ra-fraction. The method is applied to rain water and drinking water samples. (author)

  6. Development and validation of an analytical method for the determination of lead isotopic composition using ICP-QMS

    OpenAIRE

    Rodríguez-Salazar, M. T.; Morton Bermea, O.; Hernández-Álvarez, E.; García-Arreola, M. E.; Ortuño-Arzate, M. T.

    2010-01-01

    This work reports a method for the precise and accurate determination of Pb isotope composition in soils and geological matrices by ICP-QMS. Three reference materials (AGV-2, SRM 2709 and JSO-1) were repeatedly measured, using ICP-QMS instruments in order to assess the quality of this analytical procedure. Mass discrimination was evaluated for Pb/Pb with Pb isotope reference material NIST SRM 981, and the correction applied to the above mentioned reference materials to achieve good accuracy o...

  7. Sequential determination of natural ({sup 232}Th, {sup 238}U) and anthropogenic ({sup 137}Cs, {sup 90}Sr, {sup 241}Am, {sup 239+240}Pu) radionuclides in environmental matrix

    Energy Technology Data Exchange (ETDEWEB)

    Michel, H.; Levent, D.; Barci, V.; Barci-Funel, G.; Hurel, C. [Laboratoire de Radiochimie, Sciences Analytiques et Environnement (LRSAE), Universite de Nice Sophia-Antipolis 06108 Nice Cedex (France)

    2008-07-01

    A new sequential method for the determination of both natural (U, Th) and anthropogenic (Sr, Cs, Pu, Am) radionuclides has been developed for application to soil and sediment samples. The procedure was optimised using a reference sediment (IAEA-368) and reference soils (IAEA-375 and IAEA-326). Reference materials were first digested using acids (leaching), 'total' acids on hot plate, and acids in microwave in order to compare the different digestion technique. Then, the separation and purification were made by anion exchange resin and selective extraction chromatography: Transuranic (TRU) and Strontium (SR) resins. Natural and anthropogenic alpha radionuclides were separated by Uranium and Tetravalent Actinide (UTEVA) resin, considering different acid elution medium. Finally, alpha and gamma semiconductor spectrometer and liquid scintillation spectrometer were used to measure radionuclide activities. The results obtained for strontium-90, cesium-137, thorium-232, uranium- 238, plutonium-239+240 and americium-241 isotopes by the proposed method for the reference materials provided excellent agreement with the recommended values and good chemical recoveries. (authors)

  8. Recent developments in automated determinations of trace level concentrations of elements and on-line fractionations schemes exploiting the micro-sequential injection - lab-on-valve approach

    DEFF Research Database (Denmark)

    Hansen, Elo Harald; Miró, Manuel; Long, Xiangbao

    2006-01-01

    The determination of trace level concentrations of elements, such as metal species, in complex matrices by atomic absorption or emission spectrometric methods often require appropriate pretreatments comprising separation of the analyte from interfering constituents and analyte preconcentration...... are presented as based on the exploitation of micro-sequential injection (μSI-LOV) using hydrophobic as well as hydrophilic bead materials. The examples given comprise the presentation of a universal approach for SPE-assays, front-end speciation of Cr(III) and Cr(VI) in a fully automated and enclosed set...

  9. Isotope studies to determine dry deposition of sulfate to deciduous and coniferous trees: Final draft

    International Nuclear Information System (INIS)

    Garten, C.T. Jr.

    1988-01-01

    Experiments have been conducted at two locations near Oak Ridge, Tennessee, with radioactive 35 S (87 day half-life) to examine the cycling behavior of sulfur in yellow poplar (Liriodendron tulipifera), red maple (Acer rubrum), and loblolly pine (Pinus taeda) trees. Some findings pertain to methods development for estimating dry deposition of sulfur to forest canopies and the magnitude of sulfur emissions from natural sources (Task II). We will determine through field studies, the internal cycling, storage, and biogenic emission of sulfur, as traced by 35 SO 4 2- , in environments impacted by atmospheric sulfate deposition; and will determine through isotope dilution studies, the contribution of foliar leaching and dry deposition to net throughfall (NTF) sulfate concentrations beneath deciduous and coniferous trees in such environments. 3 refs., 2 figs., 1 tab

  10. Determination of plutonium isotopes in bilberry using liquid scintillation spectrometry and alpha-particle spectrometry

    International Nuclear Information System (INIS)

    Seferinoğlu, Meryem; Aslan, Nazife; Kurt, Aylin; Erden, Pınar Esra; Mert, Hülya

    2014-01-01

    This paper presents α-particle spectrometry and liquid scintillation spectrometry methods to determine plutonium isotopes in bilberry. The analytical procedure involves sample preparation steps for ashing, digestion of bilberry samples, radiochemical separation of plutonium radioisotopes and their measurement. The validity of the method was checked for coherence using the ζ test, z-test, relative bias and relative uncertainty outlier tests. The results indicated that the recommended procedures for both measurement systems could be successfully applied for the accurate determination of plutonium activities in bilberry samples. - Highlights: • Sample preparation methods for Pu using LSS and alpha spectrometry developed. • Complete separation of plutonium from interfering radionuclides. • Commercial bilberry was spiked with NPL 2011 (AH-B11144) proficiency test sample. • Results were checked using ζ test, z-test, rel. bias and rel. uncert. outlier tests. • Recommended procedures successfully applied to bilberry samples

  11. Determination of isotopic purity in heavy water to suit process requirement (Preprint No. CA-15)

    Energy Technology Data Exchange (ETDEWEB)

    Kanthiah, W S.A.; Srinivasan, K; Usuf Ali, M C.M. [Heavy Water Plant, Tuticorin (India)

    1989-04-01

    In hydrogen/ammonia based heavy water plants, a simple specific gravity determination of heavy water without any purification or thermostating has proved to be simple and easy. The accuracy is found to be well within +- 0.5% in the isotopic purity (I.P) range of 30 to 90% W/W. There are three main methods that can be adopted for determination of I.P in this range: (1)refractometry, (2) infrared spectrophotometry, and (3) pycnometry. Refractrometry requires thermostating and the practical accuracy attainable is +- 1.5% W/W. Infrared spectrophotometer has a reported accuracy/ precision of +- 0.4%. Pycnometric analysis is simple and requires much less expertise and most suited for plant analyses. An accuracy better than +- 0.5% is attained without giving any correction for buoyancy, weighing to accuracy +- 0.1 mg, measuring temperature +- 0.2degC and sample having pH upto 3. (author). 8 annexures.

  12. Development of a flow method for the determination of phosphate in estuarine and freshwaters-Comparison of flow cells in spectrophotometric sequential injection analysis

    International Nuclear Information System (INIS)

    Mesquita, Raquel B.R.; Ferreira, M. Teresa S.O.B.; Toth, Ildiko V.; Bordalo, Adriano A.; McKelvie, Ian D.; Rangel, Antonio O.S.S.

    2011-01-01

    Highlights: → Sequential injection determination of phosphate in estuarine and freshwaters. → Alternative spectrophotometric flow cells are compared. → Minimization of schlieren effect was assessed. → Proposed method can cope with wide salinity ranges. → Multi-reflective cell shows clear advantages. - Abstract: A sequential injection system with dual analytical line was developed and applied in the comparison of two different detection systems viz; a conventional spectrophotometer with a commercial flow cell, and a multi-reflective flow cell coupled with a photometric detector under the same experimental conditions. The study was based on the spectrophotometric determination of phosphate using the molybdenum-blue chemistry. The two alternative flow cells were compared in terms of their response to variation of sample salinity, susceptibility to interferences and to refractive index changes. The developed method was applied to the determination of phosphate in natural waters (estuarine, river, well and ground waters). The achieved detection limit (0.007 μM PO 4 3- ) is consistent with the requirement of the target water samples, and a wide quantification range (0.024-9.5 μM) was achieved using both detection systems.

  13. A Procedure for the Sequential Determination of Radionuclides in Phosphogypsum Liquid Scintillation Counting and Alpha Spectrometry for 210Po, 210Pb, 226Ra, Th and U Radioisotopes

    International Nuclear Information System (INIS)

    2014-01-01

    Since 2004, the Environment Programme of the IAEA has included activities aimed at the development of a set of procedures for the determination of radionuclides in terrestrial environmental samples. Reliable, comparable and 'fit for purpose' results are essential requirements for any decision based on analytical measurements. For the analyst, tested and validated analytical procedures are extremely important tools for the production of such analytical data. For maximum utility, such procedures should be comprehensive, clearly formulated, and readily available to both the analyst and the customer for reference. In this publication, a combined procedure for the sequential determination of 210Po, 210Pb, 226Ra, Th and U radioisotopes in phosphogypsum is described. The method is based on the dissolution of small amounts of phosphogypsum by microwave digestion, followed by sequential separation of 210Po, 210Pb, Th and U radioisotopes by selective extraction chromatography using Sr, TEVA and UTEVA resins. Radium-226 is separated from interfering elements using Ba(Ra)SO4 co-precipitation. Lead-210 is determined by liquid scintillation counting. The alpha source of 210Po is prepared by autodeposition on a silver plate. The alpha sources of Th and U are prepared by electrodeposition on a stainless steel plate. A comprehensive methodology for the calculation of results, including the quantification of measurement uncertainty, was also developed. The procedure is introduced as a recommended procedure and validated in terms of trueness, repeatability and reproducibility in accordance with ISO guidelines

  14. Development of a flow method for the determination of phosphate in estuarine and freshwaters-Comparison of flow cells in spectrophotometric sequential injection analysis

    Energy Technology Data Exchange (ETDEWEB)

    Mesquita, Raquel B.R. [CBQF/Escola Superior de Biotecnologia, Universidade Catolica Portuguesa, R. Dr. Antonio Bernardino de Almeida, 4200-072 Porto (Portugal); Laboratory of Hydrobiology, Institute of Biomedical Sciences Abel Salazar (ICBAS) and Institute of Marine Research (CIIMAR), Universidade do Porto, Lg. Abel Salazar 2, 4099-003 Porto (Portugal); Ferreira, M. Teresa S.O.B. [CBQF/Escola Superior de Biotecnologia, Universidade Catolica Portuguesa, R. Dr. Antonio Bernardino de Almeida, 4200-072 Porto (Portugal); Toth, Ildiko V. [REQUIMTE, Departamento de Quimica, Faculdade de Farmacia, Universidade de Porto, Rua Anibal Cunha, 164, 4050-047 Porto (Portugal); Bordalo, Adriano A. [Laboratory of Hydrobiology, Institute of Biomedical Sciences Abel Salazar (ICBAS) and Institute of Marine Research (CIIMAR), Universidade do Porto, Lg. Abel Salazar 2, 4099-003 Porto (Portugal); McKelvie, Ian D. [School of Chemistry, University of Melbourne, Victoria 3010 (Australia); Rangel, Antonio O.S.S., E-mail: aorangel@esb.ucp.pt [CBQF/Escola Superior de Biotecnologia, Universidade Catolica Portuguesa, R. Dr. Antonio Bernardino de Almeida, 4200-072 Porto (Portugal)

    2011-09-02

    Highlights: {yields} Sequential injection determination of phosphate in estuarine and freshwaters. {yields} Alternative spectrophotometric flow cells are compared. {yields} Minimization of schlieren effect was assessed. {yields} Proposed method can cope with wide salinity ranges. {yields} Multi-reflective cell shows clear advantages. - Abstract: A sequential injection system with dual analytical line was developed and applied in the comparison of two different detection systems viz; a conventional spectrophotometer with a commercial flow cell, and a multi-reflective flow cell coupled with a photometric detector under the same experimental conditions. The study was based on the spectrophotometric determination of phosphate using the molybdenum-blue chemistry. The two alternative flow cells were compared in terms of their response to variation of sample salinity, susceptibility to interferences and to refractive index changes. The developed method was applied to the determination of phosphate in natural waters (estuarine, river, well and ground waters). The achieved detection limit (0.007 {mu}M PO{sub 4}{sup 3-}) is consistent with the requirement of the target water samples, and a wide quantification range (0.024-9.5 {mu}M) was achieved using both detection systems.

  15. Determination of Pu isotopic composition and 241Am by high resolution gamma spectrometry on solid samples

    International Nuclear Information System (INIS)

    Sarkar, Arnab; Paul, Sumana; Aggarwal, Suresh K.; Tomar, Bhupendra S.

    2011-08-01

    The present report gives a detailed account of the development of non-destructive assay technique using high resolution gamma-ray spectrometry (HRGS) for determination of plutonium (Pu) isotopic composition and the 241 Am content in solid Pu samples. Energy range 120-420 keV was used in this study. The methodology involves in situ relative efficiency calibration during the measurement process itself, to reduce the errors and increase the reliability of the method. Twenty solid Pu samples of power reactor and research reactor grade were analyzed by this method and the results were compared with those obtained by thermal ionization mass spectrometry. The accuracy of the final results depends strongly upon the accuracy of the available nuclear data (decay constant, gamma abundance etc.). MATLAB based programme was written to perform the analysis. A counting time of 4 hour was chosen for achieving good statistics on the results for samples having 100-200 mg of Pu. The attainable accuracy is found to be 0.5-1% for the fissile isotopes ( 239 Pu + 241 Pu) and 5-10% for 241 Am content. (author)

  16. Determination of isotopic identity of nitrogen fixed by Frankia associated with the genus Alnus

    International Nuclear Information System (INIS)

    Kurdali, F.; Domenach, A.M.; Daniere, C.; Bardin, R.

    1988-01-01

    To use the 15 N natural abundance method to evaluate the symbiotic nitrogen fixation by actinorhizal trees, it is necessary to determine the isotopic identity of assimilated nitrogen from two sources: the soil and the air. This study reports an isotopic value of fixed nitrogen by two alder species (Alnus Incana(L.) Moench and Alnus glutinosa(L.) Gaertn.) growing on nitrogen-free medium in greenhouse experiments. The δ 15 N value of the aerial parts was -2. This value was stable with time and did not depend on the Frankia strains used. This value could be used to estimate the nitrogen fixation in the natural ecosystem. Other parameters such as the mobilization of nitrogen reserves and the choice of the reference plant must be investigated to apply this method. The nodules of these two alder species were enriched in 15 N relative to the rest of the plant but there was no relationship between symbiotic effectiveness of Frankia strains and 15 N enrichment of nodules. On the other hand, for naturally growing trees, an enrichment in 15 N was found primarily in the vesicles of nodules that are the sites of nitrogen fixation. 37 refs., 4 figs., 3 tabs. (author)

  17. Gas chromatographic/mass spectrometric determination of carbon isotope composition in unpurified samples: methamphetamine example.

    Science.gov (United States)

    Low, I A; Liu, R H; Legendre, M G; Piotrowski, E G; Furner, R L

    1986-10-01

    A gas chromatograph/quadrupole mass spectrometer system, operated in electron impact/selected ion monitoring mode, is used to determine the intensity ratio of the m/z 59 and the m/z 58 ions of the [C3H8N]+ fragment derived from methamphetamine samples synthesized with varying amounts of 13C-labeled methylamine. Crude products are introduced into the gas chromatograph without prior cleanup. The ratios measured were in excellent agreement with those calculated. A change in 0.25% use of 13C-methylamine is sufficient for product differentiation. The feasibility of using isotope labeling and subsequent mass spectrometric isotope ratio measurement as the basis of a compound tracing mechanism is discussed. Specifically, if methamphetamine samples manufactured from legal sources are asked to incorporate distinct 13C compositions, their sources can be traced when samples are diverted into illegal channels. Samples derived from illicit preparations can also be traced if the manufacturers of a precursor (methylamine in this case) incorporate distinct 13C compositions in their products.

  18. Determination of isoniazid concentration in rabbit vertebrae by isotope tracing technique in conjunction with HPLC.

    Science.gov (United States)

    Liu, Peng; Fu, Zhaozong; Jiang, Jianming; Yuan, Liang; Lin, Zhen

    2013-09-01

    Medications compounded with isoniazid (INH) are usually applied to surgical sites at the completion of surgery to locally kill postoperative residual tubercle bacilli. However, the distribution and elimination of INH in the vertebrae in vivo are not known. In this study, isotope tracing was used in conjunction with high-pressure liquid chromatography (HPLC) to address this. INH and technetium-99 m-labeled INH were applied to the vertebrae of rabbits. After 2 and 6 h, osseous tissues containing INH, as determined by radionuclide imaging, were collected for detection with HPLC. The results showed that INH mainly stayed around the vertebrae 6 h after its application and did not permeate widely into the blood or other organs, except for the kidneys. The standard deviations of INH concentrations in the technetium-99 m-INH group were approximately four-fold smaller than those in the INH group. This method of coupling isotope tracing and HPLC can effectively limit experimental error during sample collection, allowing accurate and reliable identification of the concentration levels of INH in osseous tissues in vivo. Copyright © 2013 John Wiley & Sons, Ltd.

  19. Normality test for determining the correction factor of isotopic composition in PWR spent fuel

    International Nuclear Information System (INIS)

    Lee, Y. H.; Shin, H. S.; Noh, S. K.; Seo, K. S.

    2001-01-01

    Normality test has been carried out for the ratios of the measured-to-calculated isotopic compositions in PWR spent fuel, using Shapiro-Wilk W, Lilliefors D, Cramer-von Mises and Anderson-Darling. All 38 istopices have been evaluated by means of the 1.5xIQR rule and then outliers have been discarded. As result, it seems that only 20 nuclides are satisfied with the normality at significance level 5 %. 18 Nuclides(samples) including U-235 have higher significance probability(p-value) than 25 % in W-test and p-values obtained by other three tests exceed the upper limit. Besides, in 6 nuclides including Pu-239, it seems that the p-values are between 5 % and 25 % in W test. From these results, in order to predict the isotopic compositions in the conservative point of view, it is decided that the correction factors for the nuclides are determined at the 95/95 probability and confidence level by using tolerance limit-methods with the assumption that only 18 nuclides are satisfied with thr normality

  20. Development of pre-concentration procedure for the determination of Hg isotope ratios in seawater samples.

    Science.gov (United States)

    Štrok, Marko; Hintelmann, Holger; Dimock, Brian

    2014-12-03

    Hg concentrations in seawater are usually too low to allow direct (without pre-concentration and removal of salt matrix) measurement of its isotope ratios with multicollector-inductively coupled plasma mass spectrometry (MC-ICP-MS). Therefore, a new method for the pre-concentration of Hg from large volumes of seawater was developed. The final method allows for relatively fast (about 2.5Lh(-1)) and quantitative pre-concentration of Hg from seawater samples with an average Hg recovery of 98±6%. Using this newly developed method we determined Hg isotope ratios in seawater. Reference seawater samples were compared to samples potentially impacted by anthropogenic activity. The results show negative mass dependent fractionation relative to the NIST 3133 Hg standard with δ(202)Hg values in the range from -0.50‰ to -1.50‰. In addition, positive mass independent fractionation of (200)Hg was observed for samples from reference sites, while impacted sites did not show significant Δ(200)Hg values. Although the influence of the impacted sediments is limited to the seawater and particulate matter in very close proximity to the sediment, this observation may raise the possibility of using Δ(200)Hg to distinguish between samples from impacted and reference sites. Copyright © 2014 Elsevier B.V. All rights reserved.

  1. Quantitative determination of nitrogen biological fixation by the N-15 isotopic method

    International Nuclear Information System (INIS)

    Basantes, Emilio; Trivelin, Paulo; Mui Tsai, Siu

    1993-01-01

    In order to quantify the biological nitrogen fixation (BNF) and to evaluate the mycorrhiza effect in the BNF, an experiment was carried on by applying 1 5 N -ammonium sulphate and mycorrhiza fungi to the soil. The treatments included legumes: mucuna negra(Stizolobium atterrinum Piper et Tracv) and caupi (Vigna unguiculoata L. Walp). Two control plants: non nodulating soybean (Glycine max L.Merril) and rice (Oryza sativa), were used for measuring the fixed N in the legumes by isotope dilution method. Both legumes and control plants assimmilated the same ammounts of nitrogen from the soil and fertilizer. The greater N content in the legumnes was determined as coming from the fixed nitrogen. Rice and non nodulating soybean showed to be good controls for measuring biological nitrogen fixation using isotopic dilution method. The values of fixed nitrogen for legumes calculated using rice as control plant were slightly greater than those with non nodulating soybean, nevertheless there were no significant statistical differences between the values. The mucuna fixed more N than caupi in both mycorrhiza treatments (76.7, 66.6 and 56. 7 per cent of N fixed, respectively). The mycorrhiza increased dry matter yield (13.84 per cent), accumulation of N in the plant(14.85 per cent N) and the biological N fixation (16.06 per cent N-fixed) in caupi

  2. Solvent extraction of elemental sulfur from coal and a determination of its source using stable sulfur isotopes

    Energy Technology Data Exchange (ETDEWEB)

    Hackley, K.C.; Buchanan, D.H.; Coombs, K.; Chaven, C.; Kruse, C.W. (Eastern Illinois University, Charleston, IL (USA). Chemistry Dept.)

    1990-01-01

    Hot tetrachloroethene (perchloroethylen PCE) extracts significant amounts of elemental sulfur (S{sup o}) from weathered coals but not from pristine coals. The objective of this study was to determine whether S{sup o} extracted by PCE is an oxidation product of pyrite or whether it originates in some way from unstable, organically-bound sulfur. The isotopic composition of the PCE-extracted S{sup o} was compared to the isotopic compositions of the pyritic and the organic sulfur in a coal. The S{sup o} was shown to have an isotopic signature similar to the pyritic sulfur. Additionally, the isotopic differences observed between the pyritic, S{sup o} and sulfatic sulfur were consistent with bacterial mediated oxidation of sulfide sulfur (pyrite) as the source of both the sulfatic and elemental sulfur. 21 refs., 2 tabs.

  3. Comparison of total body water determinations in lactating women by anthropometry, water displacement, and deuterium isotope dilution

    International Nuclear Information System (INIS)

    Wong, W.; Butte, N.; Lee, L.; Garza, C.; Klein, P.

    1986-01-01

    To expand the limited data on the total body water in lactating women, the authors have determined total body water contents, in eight subjects from anthropometric measurements, water displacement, and isotope dilution of deuterium oxide. On the day of the study, their skinfold thicknesses were measured over the biceps and triceps muscles and at the suprailiac and subscapular areas. Their body densities were measured by water displacement. Deuterium oxide was administered orally at 100 mg/kg of body weight. One predose milk sample was collected from each subject. The milk samples were defatted by centrifugation and the milk water was reduced to hydrogen gas for hydrogen isotope ratio measurements by gas-isotope-ratio mass spectrometry. The results indicated that total body water in lactating women estimated from anthropometric measurements was 49.7 +/- 3.3% of body weight, by water displacement was 54.9 +/- 7.2%, and by isotope dilution was 50.8 +/- 3.7%

  4. Determination of the isotopic coefficient for x2N using a dimensional analysis of the Schroedinger equation

    International Nuclear Information System (INIS)

    Pali, R.; Coss, R. de; Mustre de Leon, J.

    1999-01-01

    The adimensionalization of equations which govern the dynamics of a physical system can be very useful when studying the qualitative behavior of any variable involved in those equations. In a dynamic system like a particle moving in an effective potential, the isotopic coefficient measure the degree of anharmonicity of the potential. In general each eigenstate has a different coefficient. In this work, we determined the isotopic coefficients for potentials of the form V(x) ∝ x 2N (N=1,2,3,...) through the adimensionalization process of the Schroedinger equation. We found an analytic expression for the isotopic coefficient which depends only of N but not on the eigenstate. The isotopic coefficient value starts at 1/2 for N=1 (harmonic potential) and gradually converges to 1.0 when N increments. This reflects the fact that the potential is more anharmonic for increasing N. (Author)

  5. A new sniffer probe for the determination of hydrogen isotope ratios in the W7-AS stellarator

    Science.gov (United States)

    Zebisch, P.; Taglauer, E.

    1999-07-01

    An improved sniffer probe was constructed for measurements of the hydrogen isotope ratio and impurities in the plasma edge of the W7-AS stellarator. Details of the new design and the probe performance are presented. The new design allows changing the head without breaking the vacuum in the torus. It has a high mechanical stability, effective screening of the magnetic field and high sensitivity. The gas dynamic properties of the probe are analyzed using transmission line calculus, resulting in a rise time of 114 ms for hydrogen. During the 1997 spring measurement campaign, H/D isotope ratio measurements were carried through showing considerable outgassing of the walls during and after the discharge. He glow discharges reduce the isotope ratio drastically. Results from a typical experiment day are presented together with the analytic procedure for determining the isotope ratio in both the plasma edge and in the neutral gas region between the plasma and the vessel walls.

  6. Solvent extraction of elemental sulfur from coal and a determination of its source using stable sulfur isotopes

    Science.gov (United States)

    Hackley, Keith C.; Buchanan, D.H.; Coombs, K.; Chaven, C.; Kruse, C.W.

    1990-01-01

    Hot tetrachloroethene (perchloroethylene, PCE) extracts significant amounts of elemental sulfur (So) from weathered coals but not from pristine coals. The objective of this study was to determine whether So extracted by PCE is an oxidation product of pyrite or whether it originates in some way from unstable, organically-bound sulfur. The isotopic composition of the PCE-extracted So was compared to the isotopic compositions of the pyritic and the organic sulfur in a coal. The So was shown to have an isotopic signature similar to the pyritic sulfur. Additionally, the isotopic differences observed between the pyritic, So and sulfatic sulfur were consistent with bacterial mediated oxidation of sulfide sulfur (pyrite) as the source of both the sulfatic and elemental sulfur. ?? 1990.

  7. Application of isotope dilution for the determination of thorium in biological samples by inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Igarashi, Yasuhito; Shiraishi, Kunio; Takaku, Yuichi; Masuda, Kimihiko; Seki, Riki; Yamamoto, Masayoshi.

    1992-01-01

    The applicability of isotope dilution-inductively coupled plasma mass spectrometry (ID-ICP-MS) was examined for Th in biological samples. A naturally occurring isotope of Th(Th-230) was used as the spiking isotope. The concentration of Th-230 in the final sample solution was about 50 - 60 pg/ml; an isotope ratio of 232/230 could be measured with a relative standard deviation of less than 2%. The error magnification depended on the amount of Th-232 being concomitant with the Th-230. Though it was shown that one ng of Th-232 could be determined with reasonable precision with a tracer of the present purity, more care should be taken to reduce any source of systematic error. (author)

  8. Determination of dasatinib in the tablet dosage form by ultra high performance liquid chromatography, capillary zone electrophoresis, and sequential injection analysis.

    Science.gov (United States)

    Gonzalez, Aroa Garcia; Taraba, Lukáš; Hraníček, Jakub; Kozlík, Petr; Coufal, Pavel

    2017-01-01

    Dasatinib is a novel oral prescription drug proposed for treating adult patients with chronic myeloid leukemia. Three analytical methods, namely ultra high performance liquid chromatography, capillary zone electrophoresis, and sequential injection analysis, were developed, validated, and compared for determination of the drug in the tablet dosage form. The total analysis time of optimized ultra high performance liquid chromatography and capillary zone electrophoresis methods was 2.0 and 2.2 min, respectively. Direct ultraviolet detection with detection wavelength of 322 nm was employed in both cases. The optimized sequential injection analysis method was based on spectrophotometric detection of dasatinib after a simple colorimetric reaction with folin ciocalteau reagent forming a blue-colored complex with an absorbance maximum at 745 nm. The total analysis time was 2.5 min. The ultra high performance liquid chromatography method provided the lowest detection and quantitation limits and the most precise and accurate results. All three newly developed methods were demonstrated to be specific, linear, sensitive, precise, and accurate, providing results satisfactorily meeting the requirements of the pharmaceutical industry, and can be employed for the routine determination of the active pharmaceutical ingredient in the tablet dosage form. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Immersed single-drop microextraction interfaced with sequential injection analysis for determination of Cr(VI) in natural waters by electrothermal-atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Pena, Francisco; Lavilla, Isela; Bendicho, Carlos

    2008-01-01

    Single-drop microextraction (SDME) and sequential injection analysis have been hyphenated for ultratrace metal determination by Electrothermal-Atomic Absorption Spectrometry (ETAAS). The novel method was targeted on extraction of the Cr(VI)-APDC chelate and encompasses the potential of SDME as a miniaturized and virtually solvent-free preconcentration technique, the ability of sequential injection analysis to handle samples and the versatility of furnace autosamplers for introducing microliter samples in ETAAS. The variables influencing the microextraction of Cr(VI) onto an organic solvent drop, i.e., type of organic solvent, microextraction time, stirring rate of the sample solution, drop volume, immersion depth of the drop, salting-out effect, temperature of the sample, concentration of the complexing agent and pH of the sample solution were fully investigated. For a 5 and 20 min microextraction time, the preconcentration factors were 20 and 70, respectively. The detection limit was 0.02 μg/L of Cr(VI) and the repeatability expressed as relative standard deviation was 7%. The SDME-SIA-ETAAS technique was validated against BCR CRM 544 (lyophilized solution) and applied to ultrasensitive determination of Cr(VI) in natural waters

  10. Immersed single-drop microextraction interfaced with sequential injection analysis for determination of Cr(VI) in natural waters by electrothermal-atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Pena, Francisco; Lavilla, Isela [Departamento de Quimica Analitica y Alimentaria, Area de Quimica Analitica, Facultad de Quimica, Universidad de Vigo, Campus As Lagoas-Marcosende, s/n, 36310 Vigo (Spain); Bendicho, Carlos [Departamento de Quimica Analitica y Alimentaria, Area de Quimica Analitica, Facultad de Quimica, Universidad de Vigo, Campus As Lagoas-Marcosende, s/n, 36310 Vigo (Spain)], E-mail: bendicho@uvigo.es

    2008-04-15

    Single-drop microextraction (SDME) and sequential injection analysis have been hyphenated for ultratrace metal determination by Electrothermal-Atomic Absorption Spectrometry (ETAAS). The novel method was targeted on extraction of the Cr(VI)-APDC chelate and encompasses the potential of SDME as a miniaturized and virtually solvent-free preconcentration technique, the ability of sequential injection analysis to handle samples and the versatility of furnace autosamplers for introducing microliter samples in ETAAS. The variables influencing the microextraction of Cr(VI) onto an organic solvent drop, i.e., type of organic solvent, microextraction time, stirring rate of the sample solution, drop volume, immersion depth of the drop, salting-out effect, temperature of the sample, concentration of the complexing agent and pH of the sample solution were fully investigated. For a 5 and 20 min microextraction time, the preconcentration factors were 20 and 70, respectively. The detection limit was 0.02 {mu}g/L of Cr(VI) and the repeatability expressed as relative standard deviation was 7%. The SDME-SIA-ETAAS technique was validated against BCR CRM 544 (lyophilized solution) and applied to ultrasensitive determination of Cr(VI) in natural waters.

  11. Determination of the theoretical feasibility for the transmutation of europium isotopes from high flux isotope reactor control cylinders

    International Nuclear Information System (INIS)

    Elam, K.R.; Reich, W.J.

    1995-09-01

    The High Flux Isotope Reactor (HFIR) at the Oak Ridge National Laboratory (ORNL) is a 100 MWth light-water research reactor designed and built in the 1960s primarily for the production of transuranic isotopes. The HFIR is equipped with two concentric cylindrical blade assemblies, known as control cylinders, that are used to control reactor power. These control cylinders, which become highly radioactive from neutron exposure, are periodically replaced as part of the normal operation of the reactor. The highly radioactive region of the control cylinders is composed of europium oxide in an aluminum matrix. The spent HFIR control cylinders have historically been emplaced in the ORNL Waste Area Grouping (WAG) 6. The control cylinders pose a potential radiological hazard due to the long lived radiotoxic europium isotopes 152 Eu, 154 Eu, and 155 Eu. In a 1991 health evaluation of WAG 6 (ERD 1991) it was shown that these cylinders were a major component of the total radioactivity in WAG 6 and posed a potential exposure hazard to the public in some of the postulated assessment scenarios. These health evaluations, though preliminary and conservative in nature, illustrate the incentive to investigate methods for permanent destruction of the europium radionuclides. When the cost of removing the control cylinders from WAG 6, performing chemical separations and irradiating the material in HFIR are factored in, the option of leaving the control cylinders in place for decay must be considered. Other options, such as construction of an engineered barrier around the disposal silos to reduce the chance of migration, should also be analyzed

  12. Stable isotope ratio determination of the origin of vanillin in vanilla extracts and its relationship to vanillin/potassium ratios

    International Nuclear Information System (INIS)

    Martin, G.E.; Alfonso, F.C.; Figert, D.M.; Burggraff, J.M.

    1981-01-01

    A method is described for isolating vanillin from vanilla extract, followed by stable isotope ratio analysis to determine the amount of natural vanillin contained in adulterated vanilla extracts. After the potassium content is determined, the percent Madagascar and/or Java vanilla beans incorporated into the extract may then be approximated from the vanillin/potassium ratio

  13. Sequential automated fusion/extraction chromatography methodology for the dissolution of uranium in environmental samples for mass spectrometric determination

    Energy Technology Data Exchange (ETDEWEB)

    Milliard, Alex; Durand-Jezequel, Myriam [Laboratoire de Radioecologie, Departement de chimie, Universite Laval, 1045 Avenue de la Medecine, Quebec, QC, G1V 0A6 (Canada); Lariviere, Dominic, E-mail: dominic.lariviere@chm.ulaval.ca [Laboratoire de Radioecologie, Departement de chimie, Universite Laval, 1045 Avenue de la Medecine, Quebec, QC, G1V 0A6 (Canada)

    2011-01-17

    An improved methodology has been developed, based on dissolution by automated fusion followed by extraction chromatography for the detection and quantification of uranium in environmental matrices by mass spectrometry. A rapid fusion protocol (<8 min) was investigated for the complete dissolution of various samples. It could be preceded, if required, by an effective ashing procedure using the M4 fluxer and a newly designed platinum lid. Complete dissolution of the sample was observed and measured using standard reference materials (SRMs) and experimental data show no evidence of cross-contamination of crucibles when LiBO{sub 2}/LiBr melts were used. The use of a M4 fusion unit also improved repeatability in sample preparation over muffle furnace fusion. Instrumental issues originating from the presence of high salt concentrations in the digestate after lithium metaborate fusion was also mitigated using an extraction chromatography (EXC) protocol aimed at removing lithium and interfering matrix constituants prior to the elution of uranium. The sequential methodology, which can be performed simultaneously on three samples, requires less than 20 min per sample for fusion and separation. It was successfully coupled to inductively coupled plasma mass spectrometry (ICP-MS) achieving detection limits below 100 pg kg{sup -1} for 5-300 mg of sample.

  14. Development of a sequential injection-square wave voltammetry method for determination of paraquat in water samples employing the hanging mercury drop electrode.

    Science.gov (United States)

    dos Santos, Luciana B O; Infante, Carlos M C; Masini, Jorge C

    2010-03-01

    This work describes the development and optimization of a sequential injection method to automate the determination of paraquat by square-wave voltammetry employing a hanging mercury drop electrode. Automation by sequential injection enhanced the sampling throughput, improving the sensitivity and precision of the measurements as a consequence of the highly reproducible and efficient conditions of mass transport of the analyte toward the electrode surface. For instance, 212 analyses can be made per hour if the sample/standard solution is prepared off-line and the sequential injection system is used just to inject the solution towards the flow cell. In-line sample conditioning reduces the sampling frequency to 44 h(-1). Experiments were performed in 0.10 M NaCl, which was the carrier solution, using a frequency of 200 Hz, a pulse height of 25 mV, a potential step of 2 mV, and a flow rate of 100 µL s(-1). For a concentration range between 0.010 and 0.25 mg L(-1), the current (i(p), µA) read at the potential corresponding to the peak maximum fitted the following linear equation with the paraquat concentration (mg L(-1)): i(p) = (-20.5 ± 0.3)C (paraquat) - (0.02 ± 0.03). The limits of detection and quantification were 2.0 and 7.0 µg L(-1), respectively. The accuracy of the method was evaluated by recovery studies using spiked water samples that were also analyzed by molecular absorption spectrophotometry after reduction of paraquat with sodium dithionite in an alkaline medium. No evidence of statistically significant differences between the two methods was observed at the 95% confidence level.

  15. Development of a mass spectrometrical isotope dilution analysis for determination of trace iodine levels and its application for food samples

    International Nuclear Information System (INIS)

    Schindlmeier, W.

    1984-01-01

    A mass spectrometrical isotope dilution procedure for the determination of trace amounts of iodine in various materials was developed using 129 I as indicator isotope, based on the determination of the 129 I/ 127 I isotope relationship. Negative thermionization was used as ionization method. The analysis procedure, which worked with a standard deviation of between 0,1 and 10% (depending on material tested), was used to determine the iodine level of table salt - both iodized and normal salt (3-6 ppm and less than 0,006 ppm respectively), and food samples with an organic matrix. For comparison the iodine levels were also measured with an iodine-selective electrode. Special preparation and separation procedures were done to suit the sample material. A comparison of the levels of iodine concentration in various powdered milks which were measured by international collaborators using varying methods shows the superior reproducibility of the MS-IDA. (RB) [de

  16. Multisample conversion of water to hydrogen by zinc for stable isotope determination

    Science.gov (United States)

    Kendall, C.; Coplen, T.B.

    1985-01-01

    Two techniques for the conversion of water to hydrogen for stable isotope ratio determination have been developed that are especially suited for automated multisample analysis. Both procedures involve reaction of zinc shot with a water sample at 450 ??C. in one method designed for water samples in bottles, the water is put in capillaries and is reduced by zinc in reaction vessels; overall savings in sample preparation labor of 75% have been realized over the standard uranium reduction technique. The second technique is for waters evolved under vacuum and is a sealed-tube method employing 9 mm o.d. quartz tubing. Problems inherent with zinc reduction include surface inhomogeneity of the zinc and exchange of hydrogen both with the zinc and with the glass walls of the vessels. For best results, water/zinc and water/glass surface area ratios of vessels should be kept as large as possible.

  17. Atmospheric dinitrogen fixation in the flooded rhizosphere as determined by the N-15 isotope technique

    International Nuclear Information System (INIS)

    Yoshida, Tomio; Yoneyama, Tadakatsu.

    1980-01-01

    Atmospheric nitrogen fixation in the rice rhizosphere was determined under in situ conditions of growing flooded rice using the N-15 isotope method. The whole plant growing in a pot at a reproductive stage was placed in a specially designed glass container and exposed to a 15 N 2 atmosphere. The amounts of total nitrogen fixed in the rice rhizosphere under the experimental conditions were 1366, 592, 878, and 698 μg per pot containing 0.4 kg of soil during 15 N 2 exposure for 7 to 13 days in the four experiments conducted in this study. It was also found that the nitrogen fixed in the rice rhizosphere was translocated into other plant parts. Nineteen to 25% of the total atmospheric nitrogen fixed in the rice rhizosphere was found in the roots, leaves and stems, and ears of the rice plants during the 15 N 2 exposure period. (author)

  18. Determination of the four natural Ra isotopes in thermal waters by gamma-ray spectrometry

    International Nuclear Information System (INIS)

    Condomines, M.; Rihs, S.; Lloret, E.; Seidel, J.L.

    2010-01-01

    Our method for the simultaneous determination of the four natural Ra isotopes ( 226 Ra, 228 Ra, 224 Ra and 223 Ra) in thermal waters involves a separation of Ra on a selective filter (3 M EMPORE TM Radium Rad disk), and a single counting using a broad-energy HPGe detector (BE Ge manufactured by CANBERRA TM ). The calculation of 223 Ra and 228 Ra activities requires interference and cascade summing corrections. The 226 Ra activities in CO 2 -rich thermal waters of the Lodeve Basin (South of France) range from 530 to 2240 mBq/l. The low ( 228 Ra/ 226 Ra) activity ratios (0.19-0.29) suggest that Ra is mostly derived from the aquifer carbonates. The short-lived 224 Ra and 223 Ra are probably added to the water through recoil or desorption processes from Th-enriched coatings on the fracture walls.

  19. Determination of the isotopic composition of atmospheric methane and its application in the Antarctic

    Science.gov (United States)

    Lowe, David C.; Brenninkmeijer, Carl A. M.; Tyler, Stanley C.; Dlugkencky, Edward J.

    1991-01-01

    A procedure for establishing the C-13/C-12 ratio and the C-14 abundance in the atmospheric methane is discussed. The method involves air sample collection, measurement of the methane mixing ratio by gas chromotography followed by quantitative conversion of the methane in the air samples to CO2 and H2O, and analysis of the resulting CO2 for the C-13/C-12 ratio by stable isotope ratio mass spectrometry and measurement of C-14 content by accelerator mass spectrometry. The carbon isotropic composition of methane in air collected at Baring Head, New Zealand, and in air collected on aircraft flights between New Zealand and Antarctica is determined by the method, and no gradient in the composition between Baring Head and the South Pole station is found. As the technique is refined, and more data is gathered, small seasonal and long-term variations in C-13 are expected to be resolved.

  20. Total cholesterol in serum determined by isotope dilution/mass spectrometry, with liquid-chromatographic separation

    International Nuclear Information System (INIS)

    Takatsu, Akiko; Nishi, Sueo

    1988-01-01

    We describe an accurate, precise method for determination of total serum cholesterol by isotope dilution/mass spectrometry (IDMS) with liquid chromatographic separation. After adding [3,4- 13 C] cholesterol to serum and hydrolyzing the cholesterol esters, we extract the total cholesterol. High-performance liquid chromatography (HPLC) is used to separate the extracted cholesterol for measurement by electron-impact mass spectrometry with use of a direct-insertion device. To evaluate the specificity and the accuracy of this method, we also studied the conventional IDMS method, which involves converting cholesterol to the trimethylsilyl ether and assay by gas chromatography-mass spectrometry with use of a capillary column. The coefficient of variation for the HPLC method was a little larger than for the conventional method, but mean values by each method agreed within 1% for all sera tested. (author)

  1. The determination of blood volume in horses using stable isotope 50Cr

    International Nuclear Information System (INIS)

    Ito, Nobuhiko; Kunugiyama, Iwao; Tanaka, Masayoshi; Inoue, Megumi; Furukawa, Yoshinori; Hiraga, Atsushi; Yamanobe, Akira; Kubo, Katsuyoshi.

    1991-01-01

    A method using stable isotope 50 Cr was presented to determine equine blood volumes accurately in the field. The erythrocyte labelled with 50 Cr was injected intravenously, then small amount of blood was collected at regular intervals, and the erythrocyte volume was measured from dilution rate of 50 Cr. A blood volume was calculated from the erythrocyte volume and the packed cell volume (PCV). The present results suggested that the optimum time of collecting blood at rest was 2 h after injection of tagged blood. The red cell volumes and the total blood volumes of fifteen thoroughbred horses measured by the 50 Cr method were 46.6±9.9 and 133±17 ml/kg body weight, respectively. The mean red cell volume of stallion was larger than mare (t-test, p<0.05), and three was no significant difference in the blood volume. (author)

  2. The determination of blood volume in horses using stable isotope sup 50 Cr

    Energy Technology Data Exchange (ETDEWEB)

    Ito, Nobuhiko; Kunugiyama, Iwao; Tanaka, Masayoshi; Inoue, Megumi; Furukawa, Yoshinori (Kitasato Univ., Towada, Aomori (Japan). School of Veterinary Medicine and Animal Sciences); Hiraga, Atsushi; Yamanobe, Akira; Kubo, Katsuyoshi

    1991-05-01

    A method using stable isotope {sup 50}Cr was presented to determine equine blood volumes accurately in the field. The erythrocyte labelled with {sup 50}Cr was injected intravenously, then small amount of blood was collected at regular intervals, and the erythrocyte volume was measured from dilution rate of {sup 50}Cr. A blood volume was calculated from the erythrocyte volume and the packed cell volume (PCV). The present results suggested that the optimum time of collecting blood at rest was 2 h after injection of tagged blood. The red cell volumes and the total blood volumes of fifteen thoroughbred horses measured by the {sup 50}Cr method were 46.6+-9.9 and 133+-17 ml/kg body weight, respectively. The mean red cell volume of stallion was larger than mare (t-test, p<0.05), and three was no significant difference in the blood volume. (author).

  3. Method for determination of radioactive iodine isotopes in environmental objects and biologic materials

    International Nuclear Information System (INIS)

    Dubynin, O.D.; Pogodin, R.I.

    1981-01-01

    The method proposed for determination of radioactive iodine isotopes content in environmental objects and biologic materials is based on the extraction of iodine with carbon tetrachloride and subsequent precipitation of bismuthyl iodine (BiOI) in perchloric medium. Sample preparation for analysis is carried out using conventional alkaline ashing methods. Quantitative iodine separation is hampered if macroquantities of Cl - , Br - , SO 4 2 - , SO 8 2 - , Cr 2 O 7 2 - and other ions are present in the solution. Iodine extraction is carried out before its precipitation. Separated iodine preparation activity is measured using scintillation (NaI) Tl gamma spectrometer. The method's sensitivity when measuring iodine-131 preparations makes up 0.07 Bq per 1 sample with the error +-25 %

  4. Reduction of determinate errors in mass bias-corrected isotope ratios measured using a multi-collector plasma mass spectrometer

    International Nuclear Information System (INIS)

    Doherty, W.

    2015-01-01

    A nebulizer-centric instrument response function model of the plasma mass spectrometer was combined with a signal drift model, and the result was used to identify the causes of the non-spectroscopic determinate errors remaining in mass bias-corrected Pb isotope ratios (Tl as internal standard) measured using a multi-collector plasma mass spectrometer. Model calculations, confirmed by measurement, show that the detectable time-dependent errors are a result of the combined effect of signal drift and differences in the coordinates of the Pb and Tl response function maxima (horizontal offset effect). If there are no horizontal offsets, then the mass bias-corrected isotope ratios are approximately constant in time. In the absence of signal drift, the response surface curvature and horizontal offset effects are responsible for proportional errors in the mass bias-corrected isotope ratios. The proportional errors will be different for different analyte isotope ratios and different at every instrument operating point. Consequently, mass bias coefficients calculated using different isotope ratios are not necessarily equal. The error analysis based on the combined model provides strong justification for recommending a three step correction procedure (mass bias correction, drift correction and a proportional error correction, in that order) for isotope ratio measurements using a multi-collector plasma mass spectrometer

  5. Comparison of IRMS and NMR spectrometry for the determination of intramolecular 13C isotope composition: application to ethanol.

    Science.gov (United States)

    Gilbert, Alexis; Hattori, Ryota; Silvestre, Virginie; Wasano, Nariaki; Akoka, Serge; Hirano, Satoshi; Yamada, Keita; Yoshida, Naohiro; Remaud, Gérald S

    2012-09-15

    Isotopic (13)C NMR is a relatively recent technique which allows the determination of intramolecular (13)C isotope composition at natural abundance. It has been used in various scientific fields such as authentication, counterfeiting or plant metabolism. Although its precision has already been evaluated, the determination of its trueness remains still challenging. To deal with that issue, a comparison with another normalized technique must be achieved. In this work, we compare the intramolecular (13)C isotope distribution of ethanol from different origins obtained using both Isotope Ratio Mass Spectrometry (IRMS) and Nuclear Magnetic Resonance (NMR) spectrometry techniques. The IRMS approach consists of the oxidation of ethanol to acetic acid followed by the degradation of the latter for the analysis of each fragments formed. We show here that the oxidation of ethanol to acetic acid does not bring any significant error on the determination of the site-specific δ(13)C (δ(13)C(i)) of ethanol using the IRMS approach. The difference between the data obtained for 16 samples from different origins using IRMS and NMR approaches is not statistically significant and remains below 0.3‰. These results are encouraging for the future studies using isotopic NMR, especially in combination with the IRMS approach. Copyright © 2012. Published by Elsevier B.V.

  6. Improved radiocarbon analyses of modern human hair to determine the year-of-death by cross-flow nanofiltered amino acids: common contaminants, implications for isotopic analysis, and recommendations.

    Science.gov (United States)

    Santos, Guaciara M; De La Torre, Hector A Martinez; Boudin, Mathieu; Bonafini, Marco; Saverwyns, Steven

    2015-10-15

    In forensic investigation, radiocarbon ((14)C) measurements of human tissues (i.e., nails and hair) can help determine the year-of-death. However, the frequent use of cosmetics can bias hair (14)C results as well as stable isotope values. Evidence shows that hair exogenous impurities percolate beyond the cuticle layer, and therefore conventional pretreatments are ineffective in removing them. We conducted isotopic analysis ((14)C, δ(13)C, δ(15)N and C/N) of conventionally treated and cross-flow nanofiltered amino acid (CFNAA)-treated samples (scalp- and body-hair) from a single female subject using fingernails as a reference. The subject studied frequently applies a permanent dark-brown dye kit to her scalp-hair and uses other care products for daily cleansing. We also performed pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) analyses of CFNAA-treated scalp-hair to identify contaminant remnants that could possibly interfere with isotopic analyses. The conventionally treated scalp- and body-hair showed (14)C offsets of ~21‰ and ~9‰, respectively. These offsets confirm the contamination by petrochemicals in modern human hair. A single CFNAA extraction reduced those offsets by ~34%. No significant improvement was observed when sequential extractions were performed, as it appears that the procedure introduced some foreign contaminants. A chromatogram of the CFNAA scalp-hair pyrolysis products showed the presence of petroleum and plant/animal compound residues, which can bias isotopic analyses. We have demonstrated that CFNAA extractions can partially remove cosmetic contaminants embedded in human hair. We conclude that fingernails are still the best source of keratin protein for year-of-death determinations and isotopic analysis, with body-hair and/or scalp-hair coupled with CFNAA extraction a close second. Copyright © 2015 John Wiley & Sons, Ltd.

  7. Isotope dilution ICP-MS with laser-assisted sample introduction for direct determination of sulfur in petroleum products

    Energy Technology Data Exchange (ETDEWEB)

    Boulyga, Sergei F.; Heilmann, Jens; Heumann, Klaus G. [Johannes Gutenberg-University Mainz (Germany). Institute of Inorganic Chemistry and Analytical Chemistry

    2005-08-01

    Inductively coupled plasma isotope dilution mass spectrometry (ICP-IDMS) with direct laser-assisted introduction of isotope-diluted samples into the plasma, using a laser ablation system with high ablation rates, was developed for accurate sulfur determinations in different petroleum products such as 'sulfur-free' premium gasoline, diesel fuel, and heating oil. Two certified gas oil reference materials were analyzed for method validation. Two different {sup 34}S-enriched spike compounds, namely, elementary sulfur dissolved in xylene and dibenzothiophene in hexane, were synthesized and tested for their usefulness in this isotope dilution technique. The isotope-diluted sample was adsorbed on a filter-paper-like material, which was fixed in a special holder for irradiation by the laser beam. Under these conditions no time-dependent spike/analyte fractionation was only observed for the dibenzothiophene spike during the laser ablation process, which means that the measured {sup 34}S/{sup 32}S isotope ratio of the isotope-diluted sample remained constant - a necessary precondition for accurate results with the isotope dilution technique. A comparison of LA-ICP-IDMS results with the certified values of the gas oil reference materials and with results obtained from ICP-IDMS analyses with wet sample digestion demonstrated the accuracy of the new LA-ICP-IDMS method in the concentration range of 9.2 {mu}g g{sup -1} ('sulfur-free' premium gasoline) to 10.4 mg g{sup -1} (gas oil reference material BCR 107). The detection limit for sulfur by LA-ICP-IDMS is 0.04 {mu}g g{sup -1} and the analysis time is only about 10 min, which therefore also qualifies this method for accurate determinations of low sulfur contents in petroleum products on a routine level. (orig.)

  8. Isotope dilution ICP-MS with laser-assisted sample introduction for direct determination of sulfur in petroleum products.

    Science.gov (United States)

    Boulyga, Sergei F; Heilmann, Jens; Heumann, Klaus G

    2005-08-01

    Inductively coupled plasma isotope dilution mass spectrometry (ICP-IDMS) with direct laser-assisted introduction of isotope-diluted samples into the plasma, using a laser ablation system with high ablation rates, was developed for accurate sulfur determinations in different petroleum products such as 'sulfur-free' premium gasoline, diesel fuel, and heating oil. Two certified gas oil reference materials were analyzed for method validation. Two different 34S-enriched spike compounds, namely, elementary sulfur dissolved in xylene and dibenzothiophene in hexane, were synthesized and tested for their usefulness in this isotope dilution technique. The isotope-diluted sample was adsorbed on a filter-paper-like material, which was fixed in a special holder for irradiation by the laser beam. Under these conditions no time-dependent spike/analyte fractionation was only observed for the dibenzothiophene spike during the laser ablation process, which means that the measured 34S/32S isotope ratio of the isotope-diluted sample remained constant-a necessary precondition for accurate results with the isotope dilution technique. A comparison of LA-ICP-IDMS results with the certified values of the gas oil reference materials and with results obtained from ICP-IDMS analyses with wet sample digestion demonstrated the accuracy of the new LA-ICP-IDMS method in the concentration range of 9.2 microg g(-1) ('sulfur-free' premium gasoline) to 10.4 mg g(-1) (gas oil reference material BCR 107). The detection limit for sulfur by LA-ICP-IDMS is 0.04 microg g(-1) and the analysis time is only about 10 min, which therefore also qualifies this method for accurate determinations of low sulfur contents in petroleum products on a routine level.

  9. Determination of iodine in oyster tissue by isotope dilution laser resonance ionization mass spectrometry

    International Nuclear Information System (INIS)

    Fassett, J.D.; Murphy, T.J.

    1990-01-01

    The technique of laser resonance ionization mass spectrometry has been combined with isotope dilution analysis to determine iodine in oyster tissue. The long-lived radioisotope, 129I, was used to spike the samples. Samples were equilibrated with the 129I, wet ashed under controlled conditions, and iodine separated by coprecipitation with silver chloride. The analyte was dried as silver ammonium iodide upon a tantalum filament from which iodine was thermally desorbed in the resonance ionization mass spectrometry instrument. A single-color, two-photon resonant plus one-photon ionization scheme was used to form positive iodine ions. Long-lived iodine signals were achieved from 100 ng of iodine. The precision of 127I/129I measurement has been evaluated by replicate determinations of the spike, the spike calibration samples, and the oyster tissue samples and was 1.0%. Measurement precision among samples was 1.9% for the spike calibration and 1.4% for the oyster tissue. The concentration of iodine determined in SRM 1566a, Oyster Tissue, was 4.44 micrograms/g with an estimate of the overall uncertainty for the analysis of +/- 0.12 microgram/g

  10. Use of isotopic sulfur to determine whitebark pine consumption by Yellowstone bears: a reassessment

    Science.gov (United States)

    Schwartz, Charles C.; Teisberg, Justin E.; Fortin, Jennifer K.; Haroldson, Mark A.; Servheen, Christopher; Robbins, Charles T.; van Manen, Frank T.

    2014-01-01

    Use of naturally occurring stable isotopes to estimate assimilated diet of bears is one of the single greatest breakthroughs in nutritional ecology during the past 20 years. Previous research in the Greater Yellowstone Ecosystem (GYE), USA, established a positive relationship between the stable isotope of sulfur (δ34S) and consumption of whitebark pine (Pinus albicaulis) seeds. That work combined a limited sample of hair, blood clots, and serum. Here we use a much larger sample to reassess those findings. We contrasted δ34S values in spring hair and serum with abundance of seeds of whitebark pine in samples collected from grizzly (Ursus arctos) and American black bears (U. americanus) in the GYE during 2000–2010. Although we found a positive relationship between δ34S values in spring hair and pine seed abundance for grizzly bears, the coefficients of determination were small (R2 ≤ 0.097); we failed to find a similar relationship with black bears. Values of δ34S in spring hair were larger in black bears and δ34S values in serum of grizzly bears were lowest in September and October, a time when we expect δ34S to peak if whitebark pine seeds were the sole source of high δ34S. The relationship between δ34S in bear tissue and the consumption of whitebark pine seeds, as originally reported, may not be as clean a method as proposed. Data we present here suggest other foods have high values of δ34S, and there is spatial heterogeneity affecting the δ34S values in whitebark pine, which must be addressed.

  11. Application and evaluation of the mass spectrometric isotope dilution technique in the determination of rare earths in geological materials

    International Nuclear Information System (INIS)

    Moraes, N.M.P. de.

    1988-01-01

    Establishment of the experimental procedures employed in the rare earth element determination of geological samples by mass spectrometric isotope dilution analysis is discussed in the present work. The procedures involve preparation and calibration of the isotope tracers isotope dilution, dissolution in a teflon pressure vessel, chemical separation and isotope analysis using a fully automated Micromass VG ISOTOPES model 354 thermal ionization mass spectrometer. For the initial chemical separation of total rare earths the cationic resin was employed and HC1 and HNO 3 acids as eluents. In the second step rare earths elements were separated into individual (La, Ce and Nd) and subgroups (Sm-Eu-Gd, Yb-Er-Dy) fractions using the same cationic resin and α-HIBA as eluent. Nine elements La, Ce, Nd, Sm, Eu, Gd, Dy, Er and Yb are determined by this method in the ''United States Geological Survey'' (USGS) standard samples GSP-1, AGV-1 and G-2, with an overall precision of +- 1 to 2% and an accuracy of 5%. The concentration of rare earth element determined in the standard sample PCC-1 showed that the total analytical blanks are in submicrogram levels. The concentration of rare earth elements in the same USGS standard samples were also determined by Instrumental neutron activation analysis, neutron activation analysis with chemical separation before irradiation and inductively coupled argon plasma spectroscopy. The chemical procedures employed for these methods are the same as that used for mass spectrometric isotope dilution. Based on the results obtained, each method was evaluated pointing out their merits and defects. The study clearly showed that the chemical procedure employed for all these techniques was satisfactory. (author) [pt

  12. Fast sequential multi-element determination of major and minor elements in environmental samples and drinking waters by high-resolution continuum source flame atomic absorption spectrometry.

    Science.gov (United States)

    Gómez-Nieto, Beatriz; Gismera, Ma Jesús; Sevilla, Ma Teresa; Procopio, Jesús R

    2015-01-07

    The fast sequential multi-element determination of 11 elements present at different concentration levels in environmental samples and drinking waters has been investigated using high-resolution continuum source flame atomic absorption spectrometry. The main lines for Cu (324.754 nm), Zn (213.857 nm), Cd (228.802 nm), Ni (232.003 nm) and Pb (217.001 nm), main and secondary absorption lines for Mn (279.482 and 279.827 nm), Fe (248.327, 248.514 and 302.064 nm) and Ca (422.673 and 239.856 nm), secondary lines with different sensitivities for Na (589.592 and 330.237 nm) and K (769.897 and 404.414 nm) and a secondary line for Mg (202.582 nm) have been chosen to perform the analysis. A flow injection system has been used for sample introduction so sample consumption has been reduced up to less than 1 mL per element, measured in triplicate. Furthermore, the use of multiplets for Fe and the side pixel registration approach for Mg have been studied in order to reduce sensitivity and extend the linear working range. The figures of merit have been calculated and the proposed method was applied to determine these elements in a pine needles reference material (SRM 1575a), drinking and natural waters and soil extracts. Recoveries of analytes added at different concentration levels to water samples and extracts of soils were within 88-115% interval. In this way, the fast sequential multi-element determination of major and minor elements can be carried out, in triplicate, with successful results without requiring additional dilutions of samples or several different strategies for sample preparation using about 8-9 mL of sample. Copyright © 2014 Elsevier B.V. All rights reserved.

  13. Determination of the separation factor of uranium isotopes by gaseous diffusion; Determination des facteurs de separation des isotopes de l'uranium par diffusion gazeuse

    Energy Technology Data Exchange (ETDEWEB)

    Bilous, O; Counas, G [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

    1958-07-01

    A 12-stage pilot separation cascade with a low output has been constructed to measure the separation factor of uranium isotopes by gaseous diffusion. The report describes some of the separation results obtained, and also provides information on the time necessary for equilibrium to be established and on the influence of various perturbations on the pressure profile in the cascade. (author) [French] Une cascade pilote de 12 etages de separation a faible debit a ete construite pour mesurer le facteur de separation des isotopes de l'uranium par diffusion gazeuse. Le rapport decrit certains des resultats de separation obtenus et fournit egalement des donnees sur les temps de mise en equilibre et l'influence de diverses perturbations sur le profil des pressions dans la cascade. (auteur)

  14. Determination of total cyanide in soil by isotope dilution GC/MS following pentafluorobenzyl derivatization

    Energy Technology Data Exchange (ETDEWEB)

    Campanella, Beatrice, E-mail: beatrice.campanella@pi.iccom.cnr.it [Università di Pisa, Dipartimento di Chimica e Chimica Industriale, via Moruzzi 13, 56124 Pisa (Italy); Consiglio Nazionale delle Ricerche (CNR), Istituto di Chimica dei Composti Organometallici, UOS di Pisa, via Moruzzi 1, 56124 Pisa (Italy); Biancalana, Lorenzo [Università di Pisa, Dipartimento di Chimica e Chimica Industriale, via Moruzzi 13, 56124 Pisa (Italy); D' Ulivo, Lucia [National Research Council of Canada, 1200 Montreal Road, Ottawa, ON K1A 0R6 (Canada); Onor, Massimo; Bramanti, Emilia [Consiglio Nazionale delle Ricerche (CNR), Istituto di Chimica dei Composti Organometallici, UOS di Pisa, via Moruzzi 1, 56124 Pisa (Italy); Mester, Zoltan; Pagliano, Enea [National Research Council of Canada, 1200 Montreal Road, Ottawa, ON K1A 0R6 (Canada)

    2017-04-08

    The high toxicity of cyanide, along with its widespread industrial use, has fuelled interest in the development of analytical methods for its determination in complex matrices. In this study, we propose a novel approach for the measurement of total cyanide in soil samples based on single-step derivatization with pentafluorobenzyl bromide (F{sub 5}Bn−Br) followed by quantitation with gas chromatography mass spectrometry in negative chemical ionization mode. The reaction between CN{sup −} and F{sub 5}Bn−Br resulted in the identification of several derivatives such as F{sub 5}Bn−CN, (F{sub 5}Bn)(F{sub 5}Ph)CH−CN, and (F{sub 5}Bn){sub 2}(F{sub 5}Ph)C−CN. The relative proportion between such compounds was dependent on experimental conditions. When a 100 μL aliquot of an alkaline-aqueous extract was reacted with 700 μL of 1.3% F{sub 5}Bn−Br in acetone, the tri-alkylated derivative was the most abundant. In such conditions a detection limit of 0.5 ng/g of CN{sup −} was attained. Soil samples were initially spiked with an alkaline solution of K{sup 13}C{sup 15}N internal standard and suspended in 7.5% aqueous NaOH. Determination of total cyanide was achieved by digestion of the alkaline extract with H{sub 3}PO{sub 4} to produce HCN which was then trapped in 0.1% NaOH in a sealed double vial system, followed by reaction with F{sub 5}Bn−Br. Isotope dilution calibration was chosen for quantitation, and the validity of the novel method was demonstrated by analysis of soil Certified Reference Materials (CRMs) and by spike recovery tests. - Highlights: • A cost-effective, fast and simple method for determination of total cyanide in soil is presented. • A new micro-distillation strategy was developed overcoming the problems of a conventional distillation. • Negative chemical ionization-mass spectrometer has been exploited to obtain a high sensitivity and specificity. • High accuracy was attained for the analysis of certified reference materials with

  15. NMR spectroscopic determination of an equilibrium isotope effect on the hydration of cobalt(II)

    International Nuclear Information System (INIS)

    Evilia, R.F.; Saunders, M.

    1985-01-01

    A recently reported NMR method for the measurement of deuterium equilibrium isotope effects is applied to the hydration of the paramagnetic cobalt(II) ion. An isotope effect of about 1.3% is measured. A substantial difference between the intrinsic shift of H 2 O and D 2 O when coordinated to cobalt is also measured

  16. Determination of lead isotopes in Arctic and Antarctic snow and ice

    International Nuclear Information System (INIS)

    Rosman, K.J.R.; Chisholm, W.

    1994-01-01

    The development of high sensitivity mass spectrometry to measure Pb isotopes in Arctic and Antarctic snow and ice has provided a powerful tool for identifying sources of global Pb pollution. The combination of isotope abundance information with concentration measurements adds another dimension to analytical chemistry. (authors). 11 refs., 4 figs

  17. Determination of uranium in urine - Measurement of isotope ratios and quantification by use of inductively coupled plasma mass spectrometry

    NARCIS (Netherlands)

    Krystek, Petra; Ritsema, R.

    2002-01-01

    For analysis of uranium in urine determination of the isotope ratio and quantification were investigated by high-resolution inductively coupled plasma mass spectrometry (HR ICP-MS). The instrument used (ThermoFinniganMAT ELEMENT2) is a single-collector MS and, therefore, a stable sample-introduction

  18. Determination of total selenium and Se-77 in isotopically enriched human samples by ICP-dynamic reaction cell-MS

    DEFF Research Database (Denmark)

    Sloth, Jens Jørgen; Larsen, Erik Huusfeldt; Bügel, Susanne H.

    2003-01-01

    and the digested faecal samples were diluted using an aqueous diluent containing 0.5% Triton X-100, 2% nitric acid and 3% methanol. Selenium was detected as Se-76, Se-77 and Se-80 by ICP- DRC- MS. Selenium originating from the natural isotope abundance yeast and other selenium sources from the diet was determined...

  19. Direct determination of mercury in cosmetic samples by isotope dilution inductively coupled plasma mass spectrometry after dissolution with formic acid

    Energy Technology Data Exchange (ETDEWEB)

    Gao, Ying; Shi, Zeming; Zong, Qinxia; Wu, Peng; Su, Jing [Sichuan Provincial Key Laboratory of Nuclear Technology in Geology, College of Nuclear Technology and Automation Engineering, Chengdu University of Technology, Chengdu 610059 (China); Liu, Rui, E-mail: liur.ray@gmail.com [Mineral Resources Chemistry Key Laboratory of Sichuan Higher Education Institutions, College of Materials and Chemistry and Chemical Engineering, Chengdu University of Technology, Chengdu 610059 (China)

    2014-02-17

    Graphical abstract: -- Highlights: •Simple, sensitive, and accurate method is established for mercury determination in cosmetics. •The sample preparation procedure is highly simplified. •Isotope dilution efficiently eliminates matrix effect. •First report of using formic acid based method in combination with PVG-ID-ICP MS for mercury quantitation in cosmetics. -- Abstract: A new method was proposed for the accurate determination of mercury in cosmetic samples based on isotopic dilution (ID)-photochemical vapor generation (PVG)-inductively coupled plasma mass spectrometry (ICP MS) measurement. Cosmetic samples were directly dissolved in formic acid solution and subsequently subjected to PVG for the reduction of mercury into vapor species following by ICP MS detection. Therefore, the risks of analyte contamination and loss were avoided. Highly enriched {sup 201}Hg isotopic spike is added to cosmetics and the isotope ratios of {sup 201}Hg/{sup 202}Hg were measured for the quantitation of mercury. With ID calibration, the influences originating from sample matrixes for the determination of mercury in cosmetic samples have been efficiently eliminated. The effects of several experimental parameters, such as the concentration of the formic acid, and the flow rates of carrier gas and sample were investigated. The method provided good reproducibility and the detection limits were found to be 0.6 pg mL{sup −1}. Finally, the developed method was successfully applied for the determination of mercury in six cosmetic samples and a spike test was performed to verify the accuracy of the method.

  20. The determination of environmental levels of uranium and thorium series isotopes and 137Cs in aquatic and terrestrial samples

    International Nuclear Information System (INIS)

    Wilkinson, P.

    1985-01-01

    This publication details the analytical methods used at the Freshwater Institute for the radiochemical analysis of aquatic and terrestrial samples. Sample collection methods are described with emphasis on water sampling. A detailed 'Calculations' section contains the mathematical formulae used to determine the absolute activity of each isotope analyzed. 25 refs

  1. Determination of isotope fractionation effect using a double spike (242Pu+240Pu) during the mass spectrometric analysis of plutonium

    International Nuclear Information System (INIS)

    Chitambar, S.A.; Parab, A.R.; Khodade, P.S.; Jain, H.C.

    1986-01-01

    Isotope fractionation effect during the mass spectrometric analysis of plutonium has been investigated using a double spike ( 242 Pu+ 240 Pu) and the determination of concentration of plutonium in dissolver solution of irradiated fuel is reported. (author). 6 refs., 2 tables

  2. Determination of the geographic origin of rice by chemometrics with strontium and lead isotope ratios and multielement concentrations.

    Science.gov (United States)

    Ariyama, Kaoru; Shinozaki, Miyuki; Kawasaki, Akira

    2012-02-22

    The objective of this study was to develop a technique for determining the country of origin of rice in the Japanese market. The rice samples included a total of 350 products grown in Japan (n = 200), the United States (n = 50), China (n = 50), and Thailand (n = 50). In this study, (87)Sr/(86)Sr and Pb isotope ((204)Pb, (206)Pb, (207)Pb, and (208)Pb) ratios and multielement concentrations (Al, Fe, Co, Ni, Cu, Rb, Sr, and Ba) were determined by high-resolution inductively coupled plasma mass spectrometry. By combining three chemometric techniques based on different principles and determination criteria, the countries of origin of rice were determined. The predictions made by 10-fold cross-validation were around 97% accurate. The presented method demonstrated the effectiveness of determining the geographic origin of an agricultural product by combining several chemometric techniques using heavy element isotope ratios and multielement concentrations.

  3. Determination of isotopic purity in heavy water to suit process requirement (Preprint No. CA-15)

    International Nuclear Information System (INIS)

    Kanthiah, W.S.A.; Srinivasan, K.; Usuf Ali, M.C.M.

    1989-04-01

    In hydrogen/ammonia based heavy water plants, a simple specific gravity determination of heavy water without any purification or thermostating has proved to be simple and easy. The accuracy is found to be well within ± 0.5% in the isotopic purity (I.P) range of 30 to 90% W/W. There are three main methods that can be adopted for determination of I.P in this range: (1)refractometry, (2) infrared spectrophotometry, and (3) pycnometry. Refractrometry requires thermostating and the practical accuracy attainable is ± 1.5% W/W. Infrared spectrophotometer has a reported accuracy/ precision of ± 0.4%. Pycnometric analysis is simple and requires much less expertise and most suited for plant analyses. An accuracy better than ± 0.5% is attained without giving any correction for buoyancy, weighing to accuracy ± 0.1 mg, measuring temperature ± 0.2degC and sample having pH upto 3. (author). 8 annexures

  4. Urinary oxalate excretion, as determined by isotope dilution and indirect colorimetry

    International Nuclear Information System (INIS)

    Prenen, J.A.C.; Boer, P.; Leersum, L. van; Oldenburg, S.J.; Endeman, H.J.

    1983-01-01

    A simple and reliable method for the determination of urinary oxalate excretion is described. Urinary oxalate is precipitated with calcium chloride, and the oxalate content of the precipitate is measured by an indirect colorimetric method developed by Neas and Guyon in 1972. For single urine samples, a correction is made for the incompleteness of the precipitation of calcium oxalate by isotope dilution. The range of normal values (5% limits) determined in 52 normal subjects was 0.121-0.325 mmol.24 h - 1 .m - 2 for a 1-day collection period and 0.145-0.301 mmol. 24 h - 1 .m - 2 for a 3-day collection period. The within-assay CV of a control urine with a low oxalate concentration was 9% (n=7) and the between-assay CV for the same control urine was 12% (n=6). When the values obtained for oxalate excretion were normalized to body surface area, there was no significant difference between males and females; the main source of variation was the intra-individual variation. (Auth.)

  5. Determination of vitamin B12 (cobalamine) absorption by means of a simple double-isotope technique

    International Nuclear Information System (INIS)

    Hippe, E.; Brynskov, J.; Gimsing, P.; Hjelt, K.

    1986-01-01

    The background, practical instruction and clinical results of a simplified method of determining the absorption of cobalamine (vitamin B 12 ) are presented. The simultaneous administration of 57 CO-CN-cobalamine, a non-absorbable marker ( 51 CrCl 3 ), and red carmine tablets enable quantitative assessments of the cobalamine absorption by collection of a small red feaces sample. In contrast to the classical Schilling-test, this vitamin B 12 absorption test (B 12 -ABS-test) or faeces-spot-test is, independent of fasting, flushing dose, renal function and diurnal urinary collection. This is documented in a series of clinical studies. The B 12 -ABS-test provides accurate and precise results compared to the reference method (whole-body-counting). The Schilling test, on the contrary, gives approximately 50% false low values in a reference group of elderly hospitalized patients. A modification of the B 12 -ABS-test, has been used to determine the cobalamine absorption in children, and a set of age-related reference intervals have been established, together with quantitative measurements of the cobalamine absorption in children with small bowel diseases. Based on several years of practical experience, we recommend replacement of the Schilling test by this simple double-isotope technique. (author)

  6. Determination of benzene in different food matrices by distillation and isotope dilution HS-GC/MS

    International Nuclear Information System (INIS)

    Medeiros Vinci, Raquel; Canfyn, Michael; De Meulenaer, Bruno; Schaetzen, Thibault de; Van Overmeire, Ilse; De Beer, Jacques; Van Loco, Joris

    2010-01-01

    Benzene is classified by the IARC as carcinogenic to humans. Several sources may contribute for the occurrence of benzene in foods, such as, environmental contamination and the reaction of benzoate salts with ascorbic acid (naturally present or added as food additives). Matrix effect on benzene recovery (e.g. in fatty foods) and artefactual benzene formation from benzoate during analysis in the presence of ascorbate are some of the challenges presented when determining benzene in a wide range of foodstuffs. Design of experiment (DOE) was used to determine the most important variables in benzene recovery from headspace GC/MS. Based on the results of the DOE, a versatile method for the extraction of benzene from all kind of food commodities was developed. The method which consisted of distillation and isotope dilution HS-GC/MS was in-house validated. Artefactual benzene was prevented by addition of a borate buffer solution (pH 11) under distillation conditions. The method presented in this study allows the use of a matrix-independent calibration with detection limits below the legal limit established by the European Council for benzene in drinking water (1 μg L -1 ).

  7. Determination of Dibutyltin in Sediments Using Isotope Dilution Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry

    International Nuclear Information System (INIS)

    Yim, Yong Hyeon; Park, Ji Youn; Han, Myung Sub; Park, Mi Kyung; Kim, Byung Joo; Lim, Young Ran; Hwang, Eui Jin; So, Hun Young

    2005-01-01

    A method is described for the determination of dibutyltin (DBT) in sediment by isotope dilution using liquid chromatography inductively-coupled plasma/mass spectrometry (LC-ICP/MS). To achieve the highest accuracy and precision, special attentions are paid in optimization and evaluation of overall processes of the analysis including extraction of analytes, characterization of the standards used for calibration and LC-ICP/MS conditions. An approach for characterization of natural abundance DBT standard has been developed by combining inductively-coupled plasma/optical emission spectrometry (ICP/OES) and LC-ICP/MS for the total Sn assay and the analysis of Sn species present as impurities, respectively. An excellent LC condition for separation of organotin species was found, which is suitable for simultaneous DBT and tributyltin (TBT) analysis as well as impurity analysis of DBT standards. Microwave extraction condition was also optimized for high efficiency while preventing species transformation. The present method determines the amount contents of DBT in sediments with expanded uncertainty of less than 5% and its result shows high degree of equivalence with reference values of an international inter-comparison and a certified reference material (CRM) within stated uncertainties

  8. Determination of Dibutyltin in Sediments Using Isotope Dilution Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Yim, Yong Hyeon; Park, Ji Youn; Han, Myung Sub; Park, Mi Kyung; Kim, Byung Joo; Lim, Young Ran; Hwang, Eui Jin; So, Hun Young [Korea Research Institute of Standards and Science, Daejeon (Korea, Republic of)

    2005-03-15

    A method is described for the determination of dibutyltin (DBT) in sediment by isotope dilution using liquid chromatography inductively-coupled plasma/mass spectrometry (LC-ICP/MS). To achieve the highest accuracy and precision, special attentions are paid in optimization and evaluation of overall processes of the analysis including extraction of analytes, characterization of the standards used for calibration and LC-ICP/MS conditions. An approach for characterization of natural abundance DBT standard has been developed by combining inductively-coupled plasma/optical emission spectrometry (ICP/OES) and LC-ICP/MS for the total Sn assay and the analysis of Sn species present as impurities, respectively. An excellent LC condition for separation of organotin species was found, which is suitable for simultaneous DBT and tributyltin (TBT) analysis as well as impurity analysis of DBT standards. Microwave extraction condition was also optimized for high efficiency while preventing species transformation. The present method determines the amount contents of DBT in sediments with expanded uncertainty of less than 5% and its result shows high degree of equivalence with reference values of an international inter-comparison and a certified reference material (CRM) within stated uncertainties.

  9. Determination of benzene in different food matrices by distillation and isotope dilution HS-GC/MS

    Energy Technology Data Exchange (ETDEWEB)

    Medeiros Vinci, Raquel [Department of Food Safety and Food Quality, Faculty of Bioscience Engineering, Ghent University, Coupure Links 653, B-9000 Ghent (Belgium); Canfyn, Michael [Food, Medicines and Consumer Safety, Scientific Institute of Public Health, Rue Juliette Wytsmanstraat 14, 1050 Brussels (Belgium); De Meulenaer, Bruno [Department of Food Safety and Food Quality, Faculty of Bioscience Engineering, Ghent University, Coupure Links 653, B-9000 Ghent (Belgium); Schaetzen, Thibault de; Van Overmeire, Ilse; De Beer, Jacques [Food, Medicines and Consumer Safety, Scientific Institute of Public Health, Rue Juliette Wytsmanstraat 14, 1050 Brussels (Belgium); Van Loco, Joris, E-mail: Joris.VanLoco@iph.fgov.BE [Food, Medicines and Consumer Safety, Scientific Institute of Public Health, Rue Juliette Wytsmanstraat 14, 1050 Brussels (Belgium)

    2010-07-05

    Benzene is classified by the IARC as carcinogenic to humans. Several sources may contribute for the occurrence of benzene in foods, such as, environmental contamination and the reaction of benzoate salts with ascorbic acid (naturally present or added as food additives). Matrix effect on benzene recovery (e.g. in fatty foods) and artefactual benzene formation from benzoate during analysis in the presence of ascorbate are some of the challenges presented when determining benzene in a wide range of foodstuffs. Design of experiment (DOE) was used to determine the most important variables in benzene recovery from headspace GC/MS. Based on the results of the DOE, a versatile method for the extraction of benzene from all kind of food commodities was developed. The method which consisted of distillation and isotope dilution HS-GC/MS was in-house validated. Artefactual benzene was prevented by addition of a borate buffer solution (pH 11) under distillation conditions. The method presented in this study allows the use of a matrix-independent calibration with detection limits below the legal limit established by the European Council for benzene in drinking water (1 {mu}g L{sup -1}).

  10. Utilization of radioanalytical methods for the determination of isotopes of U, Pu and Am in activated charcoal from IEA-R1 reactor

    Energy Technology Data Exchange (ETDEWEB)

    Geraldo, Bianca; Marumo, Julio T., E-mail: bgeraldo@ipen.br, E-mail: jtmarumo@ipen.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil); Taddei, Maria Helena T., E-mail: mhtaddei@cnen.gov.br [Laboratorio de Pocos de Caldas (LAPOC/CNEN-MG), Pocos de Caldas, MG (Brazil)

    2013-07-01

    Activated charcoal is a radioactive waste arising from the water purification system of the nuclear research reactor. The management of this waste includes its characterization in order to identify and quantify the existing radionuclides, including those known as 'difficult-to-measure radionuclides' (RDM). The analysis of these RDM usually involves complex radiochemical costly and time consuming procedures for the purification and separation of them. The objective of this work was to define a methodology of sequential analysis of isotopes of U, Pu and Am, present in activated charcoal, evaluating chemical recovery, analysis time, quantity of radioactive waste generated and cost. Ion exchange and the chromatographic extraction methodologies were compared. Both methods showed high chemical recoveries, ranged from 74 and 100% for U, 76 and 100% for Pu and 87 and 100% for Am, demonstrating that these methods provide accurate and reliable results. However, chromatographic extraction method is more suitable for the determination of the radionuclides because it generates the smaller volume of waste and is more cost-effectively. (author)

  11. Utilization of radioanalytical methods for the determination of isotopes of U, Pu and Am in activated charcoal from IEA-R1 reactor

    International Nuclear Information System (INIS)

    Geraldo, Bianca; Marumo, Julio T.; Taddei, Maria Helena T.

    2013-01-01

    Activated charcoal is a radioactive waste arising from the water purification system of the nuclear research reactor. The management of this waste includes its characterization in order to identify and quantify the existing radionuclides, including those known as 'difficult-to-measure radionuclides' (RDM). The analysis of these RDM usually involves complex radiochemical costly and time consuming procedures for the purification and separation of them. The objective of this work was to define a methodology of sequential analysis of isotopes of U, Pu and Am, present in activated charcoal, evaluating chemical recovery, analysis time, quantity of radioactive waste generated and cost. Ion exchange and the chromatographic extraction methodologies were compared. Both methods showed high chemical recoveries, ranged from 74 and 100% for U, 76 and 100% for Pu and 87 and 100% for Am, demonstrating that these methods provide accurate and reliable results. However, chromatographic extraction method is more suitable for the determination of the radionuclides because it generates the smaller volume of waste and is more cost-effectively. (author)

  12. Determination of the nuclear electric charge distribution of samarium isotopes 144, 148, 150, 152, 154 by the muonic atom method

    International Nuclear Information System (INIS)

    Barreau, Pierre.

    1977-01-01

    The theory of the nucleus-negative muon system in the case of electrical interactions is discussed. The interactions of muons with the samarium isotopes 152, 154, 144, 148, 150 are investigated. After a description of the experimental device, from muon beam production to data acquisition (detection of the gamma spectra), the results are analyzed and the nuclear charge distribution parameters determined: for each isotope the absolute value of c (half-density radius) and t (skin thickness); for 152 Sm and 154 Sm the parameter β 2 (quadrupolar defomation). Nuclear polarization was accounted for throughout the analysis [fr

  13. Determination of isotopic ratios of osmium and ruthenium in meteorites by pretreatment and radiochemical neutron activation analysis

    International Nuclear Information System (INIS)

    Chinfang Chai; Yongzhong Liu; Xueying Mao

    1996-01-01

    The isotopic abundance ratios of 190 Os/ 184 Os and 96 Ru/ 102 Ru for the metal phases of the Jilin and Taonan stone meteorites were determined by pretreatment and radiochemical neutron activation analysis. All experimental factors affecting Os and Ru isotopic ratios were discussed, including sampling, standard, irradiation, separation and counting. The statistical errors of measurements for the 199 Os/ 184 Os ratio can be controlled within 1%. The experimental results indicate that the statistically significant anomalies of the 190 Os/ 184 Os and 96 Ru/ 102 Ru ratios have not been found relative to the terrestrial Os and Ru standards. (author). 6 refs., 1 fig., 5 tabs

  14. Height determination at the transfer unit in isotopic distillation of hydrogen on type B7 ordered column packing

    International Nuclear Information System (INIS)

    Pop, F.; Croitoru, C.; Peculea, M.

    2001-01-01

    Owing to the low pressure drop implied by ordered column packings these are often utilized for vacuum distillations and separation of mixtures in which the important component occurs at a very low concentration, as for instance is the case of water, deuterium or oxygen isotopic distillation. The paper presents a model for determination of the height of transfer unit (HTU) in the hydrogen isotopic distillation installation, equipped with ordered column packing of B7 type. The computed values for HUT based on the analogy between heat, moment and mass transfer, were compared with the experimental data

  15. Online induction heating for determination of isotope composition of woody stem water with laser spectrometry: A methods assessment

    Science.gov (United States)

    Lazarus, Brynne E.; Germino, Matthew; Vander Veen, Jessica L.

    2016-01-01

    Application of stable isotopes of water to studies of plant–soil interactions often requires a substantial preparatory step of extracting water from samples without fractionating isotopes. Online heating is an emerging approach for this need, but is relatively untested and major questions of how to best deliver standards and assess interference by organics have not been evaluated. We examined these issues in our application of measuring woody stem xylem of sagebrush using a Picarro laser spectrometer with online induction heating. We determined (1) effects of cryogenic compared to induction-heating extraction, (2) effects of delivery of standards on filter media compared to on woody stem sections, and (3) spectral interference from organic compounds for these approaches (and developed a technique to do so). Our results suggest that matching sample and standard media improves accuracy, but that isotopic values differ with the extraction method in ways that are not due to spectral interference from organics.

  16. Determination of lead isotopic composition of airborne particulate matter by ICPMS: implications for lead atmospheric emissions in Canada

    International Nuclear Information System (INIS)

    Celo, V.; Dabek-Zlotorzynska, E.

    2009-01-01

    Full text: Quadrupole ICPMS was used for determination of trace metal concentrations and lead isotopic composition in fine particulate matter (PM 2.5 ) collected at selected sites within the Canadian National Air Pollution Surveillance network, from February 2005 to February 2007. High enrichment factors indicated that lead is mostly of anthropogenic origin and consequently, the lead isotopic composition is directly related to that of pollution sources. The 206 Pb/ 207 Pb and 208 Pb/ 207 Pb ratios were measured and the results were compared to the isotopic signatures of lead from different sources. Various approaches were used to assess the impact of relevant sources and the meteorological conditions in the occurrence and distribution of lead in Canadian atmospheric aerosols. (author)

  17. Development of a portable mass spectrometric system for determination of isotopic composition of solid uranium samples using fluorine volatilization

    Science.gov (United States)

    Loge, G.

    1994-09-01

    Using hardware and materials supplied by LANL, a prototype quadrupole mass spectrometer system designed for portable field analysis of isotopic composition of solid uranium samples was assembled and tested. The system contained the capability for fluorine volatilization of solid uranium samples with gas introduction, which was successfully tested and demonstrated using 100 mg samples of U3O8. Determination of precision and accuracy for measuring isotopic composition was performed using isotopic standards. Use with soil samples containing uranium were also attempted. Silicates in the soil forming SiF4 were found to be a kinetic bottleneck to the formation of UF6. This could be avoided by performing some sort of chemical separation as a pre-treatment step, which was demonstrated using nitric acid.

  18. Use of radioanalytical methods for determination of uranium, neptunium, plutonium, americium and curium isotopes in radioactive wastes; Utilizacao de metodos radioanaliticos para a determinacao de isotopos de uranio, plutonio, americio e curio em rejeitos radioativos

    Energy Technology Data Exchange (ETDEWEB)

    Geraldo, Bianca

    2012-07-01

    Activated charcoal is a common type of radioactive waste that contains high concentrations of fission and activation products. The management of this waste includes its characterization aiming the determination and quantification of the specific radionuclides including those known as Difficult-to-Measure Radionuclides (RDM). The analysis of the RDM's generally involves complex radiochemical analysis for purification and separation of the radionuclides, which are expensive and time-consuming. The objective of this work was to define a methodology for sequential analysis of the isotopes of uranium, neptunium, plutonium, americium and curium present in a type of radioactive waste, evaluating chemical yield, analysis of time spent, amount of secondary waste generated and cost. Three methodologies were compared and validated that employ ion exchange (TI + EC), extraction chromatography (EC) and extraction with polymers (ECP). The waste chosen was the activated charcoal from the purification system of primary circuit water cooling the reactor IEA-R1. The charcoal samples were dissolved by acid digestion followed by purification and separation of isotopes with ion exchange resins, extraction and chromatographic extraction polymers. Isotopes were analyzed on an alpha spectrometer, equipped with surface barrier detectors. The chemical yields were satisfactory for the methods TI + EC and EC. ECP method was comparable with those methods only for uranium. Statistical analysis as well the analysis of time spent, amount of secondary waste generated and cost revealed that EC method is the most effective for identifying and quantifying U, Np, Pu, Am and Cm present in charcoal. (author)

  19. Optimization and application of ICPMS with dynamic reaction cell for precise determination of 44Ca/40Ca isotope ratios.

    Science.gov (United States)

    Boulyga, Sergei F; Klötzli, Urs; Stingeder, Gerhard; Prohaska, Thomas

    2007-10-15

    An inductively coupled plasma mass spectrometer with dynamic reaction cell (ICP-DRC-MS) was optimized for determining (44)Ca/(40)Ca isotope ratios in aqueous solutions with respect to (i) repeatability, (ii) robustness, and (iii) stability. Ammonia as reaction gas allowed both the removal of (40)Ar+ interference on (40)Ca+ and collisional damping of ion density fluctuations of an ion beam extracted from an ICP. The effect of laboratory conditions as well as ICP-DRC-MS parameters such a nebulizer gas flow rate, rf power, lens potential, dwell time, or DRC parameters on precision and mass bias was studied. Precision (calculated using the "unbiased" or "n - 1" method) of a single isotope ratio measurement of a 60 ng g(-1) calcium solution (analysis time of 6 min) is routinely achievable in the range of 0.03-0.05%, which corresponded to the standard error of the mean value (n = 6) of 0.012-0.020%. These experimentally observed RSDs were close to theoretical precision values given by counting statistics. Accuracy of measured isotope ratios was assessed by comparative measurements of the same samples by ICP-DRC-MS and thermal ionization mass spectrometry (TIMS) by using isotope dilution with a (43)Ca-(48)Ca double spike. The analysis time in both cases was 1 h per analysis (10 blocks, each 6 min). The delta(44)Ca values measured by TIMS and ICP-DRC-MS with double-spike calibration in two samples (Ca ICP standard solution and digested NIST 1486 bone meal) coincided within the obtained precision. Although the applied isotope dilution with (43)Ca-(48)Ca double-spike compensates for time-dependent deviations of mass bias and allows achieving accurate results, this approach makes it necessary to measure an additional isotope pair, reducing the overall analysis time per isotope or increasing the total analysis time. Further development of external calibration by using a bracketing method would allow a wider use of ICP-DRC-MS for routine calcium isotopic measurements, but it

  20. Determination of isotope ratio of elements by mass distribution in molecules of varied chemical compounds

    International Nuclear Information System (INIS)

    Gladkikh, I.S.; Babichev, A.P.

    1999-01-01

    The procedure and program for calculation of isotope ratio of elements involving in the compound being studied using data of mass spectrometry were elaborated. The methods developed for the O 2 , SiH 4 , Cd(CH 3 ) 2 molecules were demonstrated for the illustration. The results of calculation provide support for the efficiency of the program and satisfactory reliability of the results during calculation of the isotope and complex compound concentrations. The program may be used for the estimation of the degree of nonequilibrium isotope distributions, it may indicate on the errors of the mass spectroscopy results [ru

  1. Voltammetric behaviour at gold electrodes immersed in the BCR sequential extraction scheme media Application of underpotential deposition-stripping voltammetry to determination of copper in soil extracts

    Energy Technology Data Exchange (ETDEWEB)

    Beni, Valerio; Newton, Hazel V.; Arrigan, Damien W.M.; Hill, Martin; Lane, William A.; Mathewson, Alan

    2004-01-30

    The development of mercury-free electroanalytical systems for in-field analysis of pollutants requires a foundation on the electrochemical behaviour of the chosen electrode material in the target sample matrices. In this work, the behaviour of gold working electrodes in the media employed in the BCR sequential extraction protocol, for the fractionation of metals in solid environmental matrices, is reported. All three of the BCR sequential extraction media are redox active, on the basis of acidity and oxygen content as well as the inherent reducing or oxidising nature of some of the reagents employed: 0.11 M acetic acid, 0.1 M hydroxylammonium chloride (adjusted to pH 2) and 1 M ammonium acetate (adjusted to pH 2) with added trace hydrogen peroxide. The available potential ranges together with the demonstrated detection of target metals in these media are presented. Stripping voltammetry of copper or lead in the BCR extract media solutions reveal a multi-peak behaviour due to the stripping of both bulk metal and underpotential metal deposits. A procedure based on underpotential deposition-stripping voltammetry (UPD-SV) was evaluated for application to determination of copper in 0.11 M acetic acid soil extracts. A preliminary screening step in which different deposition times are applied to the sample enables a deposition time commensurate with UPD-SV to be selected so that no bulk deposition or stripping occurs thus simplifying the shape and features of the resulting voltammograms. Choice of the suitable deposition time is then followed by standards addition calibration. The method was validated by the analysis of a number of BCR 0.11 M acetic acid soil extracts. Good agreement was obtained been the UPD-SV method and atomic spectroscopic results.

  2. Voltammetric behaviour at gold electrodes immersed in the BCR sequential extraction scheme media Application of underpotential deposition-stripping voltammetry to determination of copper in soil extracts

    International Nuclear Information System (INIS)

    Beni, Valerio; Newton, Hazel V.; Arrigan, Damien W.M.; Hill, Martin; Lane, William A.; Mathewson, Alan

    2004-01-01

    The development of mercury-free electroanalytical systems for in-field analysis of pollutants requires a foundation on the electrochemical behaviour of the chosen electrode material in the target sample matrices. In this work, the behaviour of gold working electrodes in the media employed in the BCR sequential extraction protocol, for the fractionation of metals in solid environmental matrices, is reported. All three of the BCR sequential extraction media are redox active, on the basis of acidity and oxygen content as well as the inherent reducing or oxidising nature of some of the reagents employed: 0.11 M acetic acid, 0.1 M hydroxylammonium chloride (adjusted to pH 2) and 1 M ammonium acetate (adjusted to pH 2) with added trace hydrogen peroxide. The available potential ranges together with the demonstrated detection of target metals in these media are presented. Stripping voltammetry of copper or lead in the BCR extract media solutions reveal a multi-peak behaviour due to the stripping of both bulk metal and underpotential metal deposits. A procedure based on underpotential deposition-stripping voltammetry (UPD-SV) was evaluated for application to determination of copper in 0.11 M acetic acid soil extracts. A preliminary screening step in which different deposition times are applied to the sample enables a deposition time commensurate with UPD-SV to be selected so that no bulk deposition or stripping occurs thus simplifying the shape and features of the resulting voltammograms. Choice of the suitable deposition time is then followed by standards addition calibration. The method was validated by the analysis of a number of BCR 0.11 M acetic acid soil extracts. Good agreement was obtained been the UPD-SV method and atomic spectroscopic results

  3. Expression of multidrug resistance genes MVP, MDR1, and MRP1 determined sequentially before, during, and after hyperthermic isolated limb perfusion of soft tissue sarcoma and melanoma patients.

    Science.gov (United States)

    Stein, Ulrike; Jürchott, Karsten; Schläfke, Matthias; Hohenberger, Peter

    2002-08-01

    Isolated, hyperthermic limb perfusion (ILP) with recombinant human tumor necrosis factor alpha and melphalan is a highly effective treatment for advanced soft tissue sarcoma (STS) and locoregional metastatic malignant melanoma. Multidrug resistance (MDR)-associated genes are known to be inducible by heat and drugs; expression levels of the major vault protein (MVP), MDR1, and MDR-associated protein 1 (MRP1) were determined sequentially before, during, and after ILP of patients. Twenty-one STS or malignant melanoma patients were treated by ILP. Tumor tissue temperatures were recorded continuously and ranged from 33.4 degrees C initially to peak values of 40.4 degrees C during ILP. Serial true-cut biopsy specimens from tumor tissues were routinely microdissected. Expression analyses for MDR genes were performed by real-time reverse transcriptase polymerase chain reaction and immunohistochemistry. In 83% of the patients, MVP expression was induced during hyperthermic ILP. MVP-mRNA inductions often paralleled the increase in temperature during ILP. Increased MVP protein expressions either were observed simultaneously with the MVP-mRNA induction or were delayed until after the induction at the transcriptional level. Inductions of MDR1 and MRP1 were observed in only 13% and 27% of the specimens analyzed. Temperatures and drugs applied preferentially led to an induction of MVP and were not sufficient to induce MDR1 and MRP1 in the majority of tumors. This study is the first to analyze the expression of MDR-associated genes sequentially during ILP of patients and demonstrates that treatment might lead to increased levels of MVP, whereas enhanced levels of MDR1 and MRP1 remain rare events.

  4. Intrinsic ratios of glucose, fructose, glycerol and ethanol 13C/12C isotopic ratio determined by HPLC-co-IRMS: toward determining constants for wine authentication.

    Science.gov (United States)

    Guyon, François; Gaillard, Laetitia; Salagoïty, Marie-Hélène; Médina, Bernard

    2011-09-01

    High-performance liquid chromatography linked to isotope ratio mass spectrometry (HPLC-co-IRMS) via a Liquiface© interface has been used to simultaneously determine (13)C isotope ratios of glucose (G), fructose (F), glycerol (Gly) and ethanol (Eth) in sweet and semi-sweet wines. The data has been used the study of wine authenticity. For this purpose, 20 authentic wines from various French production areas and various vintages have been analyzed after dilution in pure water from 20 to 200 times according to sugar content. If the (13)C isotope ratios vary according to the production area and the vintage, it appears that internal ratios of (13)C isotope ratios (R((13)C)) of the four compounds studied can be considered as a constant. Thus, ratios of isotope ratios are found to be 1.00 ± 0.04 and 1.02 ± 0.08 for R((13)C(G/F)) and R((13)C(Gly/Eth)), respectively. Moreover, R((13)C(Eth/Sugar)) is found to be 1.15 ± 0.10 and 1.16 ± 0.08 for R((13)C(Gly/Sugar)). Additions of glucose, fructose and glycerol to a reference wine show a variation of the R((13)C) value for a single product addition as low as 2.5 g/L(-1). Eighteen commercial wines and 17 concentrated musts have been analyzed. Three wine samples are suspicious as the R((13)C) values are out of range indicating a sweetening treatment. Moreover, concentrated must analysis shows that (13)C isotope ratio can be also used directly to determine the authenticity of the matrix.

  5. LC/MS Method for the Determination of Stable Isotope Labeled Promethazine in Human Plasma

    Science.gov (United States)

    Zuwei, Wang; Boyd, Jason; Berens, Kurt L.; Putcha, Lakshmi

    2004-01-01

    Promethazine (PMZ) is taken by astronauts orally (PO), intramuscularly (IM) or rectally (PR) for space motion sickness. LC/MS method was developed with off-line solid phase extraction to measure plasma concentrations of PMZ given as stable isotope-labeled (SIL) formulations by the three different routes of administration simultaneously. Samples (0.5ml) were loaded on to Waters Oasis HLB co-polymer cartridges and eluted with 1.0 mL methanol. HPLC separation of the eluted sample was performed using an Agilent Zorbax SB-CN column (50 x 2.1 mm) at a flow rate of 0.2 mL/min for 6 min. Acetonitrile/ ammonium acetate (30 mM) in water (3:2, v/v), pH 5.6 plus or minus 0.1, was used as the mobile phase for separation. Concentrations of PMZ, PMZ-d4 and PMZ-d7 and chlorpromazine (internal standard) were determined using a Micromass ZMD single quadrupole mass spectrometer with Electrospray Ionization (ESI). ESI mass spectra were acquired in positive ion mode with selected ion monitoring of [M+ H]dot plus. The method is rapid, reproducible and the assay specific parameters are listed in a table. A novel, sensitive and specific method for the measurement of PMZ and SIL PMZ in human plasma is reported.

  6. Construction of CARS Spectroscopy for Determination of Isotope shift of Hydrogen H2, D2

    International Nuclear Information System (INIS)

    Zidan, M. D.; Jazmati, A.; Manni, A.

    2007-01-01

    Coherent anti-Stokes Raman scattering (CARS) spectrometer has been built. It consists of Raman cell, which is filled with a H2 gas at 5 atm pressure, and a frequency-doubled Nd:YAG laser-pumped dye laser. The two beams are focused by means of a bi-convex 400 mm lens into the Raman cell. The anti-Stokes signal (CARS beam) is generated due to four-wave mixing process. The anti-Stokes signal is directed to a monochrometer entrance slit by prism to be detected by a photomultiplier, which is connected to a computer. The dye laser frequency has to be tuned to satisfy the energy difference between the V 1 beam (Nd:YAG laser beam) and the V 2 beam (the Stokes beam or the dye laser beam) that exactly corresponds to a vibrational or a rotational Raman resonance (E 2 -E 1 ) in the hydrogen molecule, then the anti-Stokes signal ( V 3 ) is generated. The spectra of the anti-Stokes signal has been recorded to determine the isotope shift between H 2 , and D 2 , which is 1161 cm -1 .

  7. Application of environmental isotopes to determine the cause of rising water levels in Lake Beseka, Ethiopia

    International Nuclear Information System (INIS)

    Zemedagegnehu, E.; Travi, Y.; Aggarwal, P.

    1999-01-01

    Water level in Lake Beskea, located in the Ethiopian Rift Valley, has been rising continuously for the last about 30 years. The surface area of the lake has increased from about 6 Km 2 to the present 40 Km 2 and has posed serious problems for environmental management, including inundation of grazing and cultivated lands and, potentially, railway tracks. Historically, the lake received recharge from precipitation, surface runoff in the catchment, groundwater discharge, surface runoff from nearby thermal springs. As the lake levels have risen, the thermal springs are now submerged. An increase in the discharge form these thermal springs may be the original cause of lake water rise, or they may have been submerged as a result of the rising water level. An initial study conducted in the 1970s attributed the rising lake levels to increased runoff from adjoining irrigated areas. However, stricter controls on irrigation runoff failed to check the rising lake levels. A multi-disciplinary study, including geophysical, hydrological, geochemical, isotopic, and modeling techniques was then initiated to determine the cause(s) of lake level rise. Results of piezometric and geophysical surveys indicate that the principal cause of rising water levels may be the increased inflow from submerged springs in the southwestern portion of the lake

  8. Determination of management by labor competencies in the production process of the Isotope Center

    International Nuclear Information System (INIS)

    Pérez Centurión, Yoneiki; Fernández Rodríguez, Rosio

    2016-01-01

    The present research is carried out in the Center of Isotopes (CENTIS) belonging to the Agency of Nuclear Energy and Advanced Technologies of the Ministry of Science, Technology and Environment of Cuba (CITMA). Its mission is to develop, produce, and supply radiopharmaceuticals, clinical diagnostics and scientific and technical health services in the national and international markets. Based on a diagnosis of the organization through the GRH-DPC model, it was determined that the main problem is the Deficient Management of Human Resources, highlighting as main cause that the labor competencies are not identified at any of its three levels . As a result of this analysis the need to establish a procedure to carry out the process of identification and validation of the competency system, as well as the design of the profile of positions by competencies of the entity. For the development of this work, different tools and techniques were used in the field of research such as: bibliographical analysis, brainstorming, expert method, statistical tools, cause and effect diagram, SWOT matrix, flow diagram, among others. The main result of the research is the identification of the organization's distinctive competencies, those of the key production processes of 99 Mo-99mTc Generators and the profiles of the positions of the Production Management linked to the selected subprocesses.

  9. Isotope dilution analysis for the determination of zinc in blood samples of diabetic patients

    International Nuclear Information System (INIS)

    Garg, A.N.; Kumar, A.; Maheshwari, G.; Sharma, S.

    2005-01-01

    Isotope dilution analysis (IDA) based on solvent extraction has been developed for the determination of zinc in the blood of diabetic patients and healthy adults as controls. The method using 65 Zn as a tracer is based on the formation of a red colored complex with dithizone in chloroform which is measured by counting of the 1115 keV γ-rays by gamma-ray spectrometry. Various extraction parameters such as pH, nature of solvent and amount of reagent were optimized. Zinc concentration in diabetic patients (n = 10) was found in a much wider range (1.5-157 μg/ml) compared to those in healthy adults (3.1-95.9 μg/ml for n = 5). t-Test of data shows 80-90% confidence limits. A comparison of mean values, 28.5 ± 48.5 μg/ml for diabetics and 33.1 ± 34.5 μg/ml for controls shows 13.9% lower zinc concentration in diabetics. No correlation was found with eating (vegetarian/nonvegetarian)/drinking or smoking habits, but in general, females showed somewhat lower concentration compared to those in males though population size in each case was very small. (author)

  10. Determination of uranium and thorium isotopes and polonium in sediment profiles from Baixada Santista, SP

    International Nuclear Information System (INIS)

    Ramos, Guilherme da Franca

    2010-01-01

    The objective of the present work is to determine the activity concentration of uranium and thorium isotopes and polonium in estuarine sediments from Baixada Santista. The area comprehends nine cities in the Brazilian coast (Bertioga, Guaruja, Santos, Sao Vicente, Cubatao, Praia Grande, Mongagua, Itanhaem and Peruibe). It is one of the most important industrial areas in Brazil due to the large number of industries operating in Cubatao, such as steel, petrochemical and fertilizer industries. That, together with a large population, causes a negative impact on the marine biota. In the present work 10 profiles of sediment cores, with depth varying from 41 to 98 cm, were analyzed. The cores were obtained from Santos, Cubatao, Sao Vicente and Bertioga. The cores were sliced every 2 cm and were treated with both physical and chemical processes, including drying, grinding and sieving. The samples were dissolved by acid digestion, till total dissolution and destruction of organic matter. After the acid digestion, the samples were filtered and evaporated till dryness. The radiochemical techniques used to separate the radionuclides and to prepare the final source for alpha counting were ion exchange chromatography and spontaneous deposition for polonium and electrodeposition for U and Th. The final sources were counted in a surface barrier alpha spectrometer. Values obtained for the radionuclides analyzed were similar to the activity concentrations of sediments in non polluted areas, with the exception of a few samples that showed anthropic influence. (author)

  11. Signatures of nitrogen stable isotope and determination of organic food authentication

    International Nuclear Information System (INIS)

    Yuan Yuwei; Zhang Zhiheng; Yang Guiling; Wang Qiang

    2009-01-01

    Chemical fertilizers were not permitted to be applied in organic agricultural production, so fertilizer as one of agricultural inputs is an important regulatory aspect in the organic food accreditation. Natural stable isotope abundances δ 15 N from different nitrogenous fertilizers are different, the same as in the agricultural products. Natural abundances δ 15 N in the agricultural products using organic fertilizer is higher than those in the products without using any fertilizer, while it is the lowest in the products using chemical nitrogenous fertilizer. Natural abundances δ 15 N are also affected by the ways of fertilizer treatment, the types of the crops and the growth stages as well as the different parts of crops. Generally, natural abundances of δ 15 N are preferred to trace nitrogenous fertilizer for the vegetables with shorter growing period, but not for the crops with longer growing period or nitrogen fixation. The techniques to trace the nitrogen abundances of δ 15 N in the crops play a positive role, which is useful for the determination of organic food authentication, perfecting the system of quality and supervision and protecting public health, therefore it has a theoretical and applied value. (authors)

  12. Determination of inositol 1,4,5-trisphosphate levels in Dictyostelium by isotope dilution assay

    International Nuclear Information System (INIS)

    Van Haastert, P.J.

    1989-01-01

    A commercial isotope dilution assay was used for the determination of Ins(1,4,5)P3 levels in the microorganism Dictyostelium discoideum. Cross-reactivity in the assay was detected with extracts from cells and the medium. The compound which induced this cross-reactivity was tentatively identified as Ins(1,4,5)P3 by (i) codegradation with authentic [ 32 P]Ins(1,4,5)P3 by three specific Ins(1,4,5)P3 phosphatases, and (ii) co-chromatography with authentic [ 32 P]Ins(1,4,5)P3 on HPLC columns. The cellular concentration was estimated as 165 +/- 42 pmol/10(8) cells, yielding a mean intracellular Ins(1,4,5)P3 concentration of 3.3 microM. Dictyostelium cells secrete large amounts of Ins(1,4,5)P3 at a rate of about 10% of the cellular content per minute, yielding about 0.13 microM extracellular Ins(1,4,5)P3 after 15 min in a suspension of 10(8) cells/ml. The chemoattractant cAMP induced a transient increase of the Ins(1,4,5)P3 concentration; the data suggest an intracacellular rise from 3.3 to 5.5 microM with a maximum at 6 s after stimulation

  13. Daily cortisol production rate in man determined by stable isotope dilution/mass spectrometry

    International Nuclear Information System (INIS)

    Esteban, N.V.; Loughlin, T.; Yergey, A.L.; Zawadzki, J.K.; Booth, J.D.; Winterer, J.C.; Loriaux, D.L.

    1991-01-01

    Growth retardation as well as the development of Cushingoid features in adrenally insufficient patients treated with the currently accepted replacement dose of cortisol (33-41 mumol/day.m2; 12-15 mg/m2.day) prompted us to reevaluate the cortisol production rate (FPR) in normal subjects and patients with Cushing's syndrome, using a recently developed thermospray liquid chromatography-mass spectrometry method. The stable isotope [9,12,12-2H3]cortisol was infused continuously for 31 h at about 5% of the anticipated FPR. Blood samples were obtained at 20-min intervals for 24 h, spun, and pooled in 4-h groups. Tracer dilution in plasma was determined by liquid chromatography/mass spectrometry. The method was validated with controlled infusions in 6 patients with adrenal insufficiency. Results from 12 normal volunteers revealed a FPR of 27.3 +/- 7.5 mumol/day (9.9 +/- 2.7 mg/day) or 15.7 mumol/day.m2; 5.7 mg/m2. day. A previously unreported circadian variation in FPR was observed. Patients with Cushing's syndrome demonstrated unequivocal elevation of FPR and cortisol concentration correlated during each sample period in normal volunteers, indicating that cortisol secretion, rather than metabolism, is mainly responsible for changes in plasma cortisol. Our data suggest that the FPR in normal subjects may be lower than previously believed

  14. Evaluation of a novel PTFE material for use as a means for separation and preconcentration of trace levels of metal ions in sequential injection (SI) and sequential injection lab-on-valve (SI-LOV) systems. Determination of cadmium (II) with detection by electrothermal atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Long, Xiangbao; Chomchoei, Roongrat; Hansen, Elo Harald

    2004-01-01

    with an external packed column and in a sequential injection lab-on-valve (SI-LOV) system. Employed for the determination of cadmium(II), complexed with diethyldithiophosphate (DDPA), and detection by electrothermal atomic absorption spectrometry (ETAAS), its performance was compared to that of a previously used...

  15. The use of stable isotopes for Cr(VI) determination in silty-clay soil solution.

    Science.gov (United States)

    Zuliani, Tea; Sčančar, Janez; Milačič, Radmila

    2013-09-01

    In assessing the environmental hazard of Cr(VI) present in soil, exchangeable Cr(VI) is important, since it can be easily washed out from the upper part of the soil into subsurface soil, surface and ground water, and taken up by plants. The aim of this study was to evaluate the degree of species interconversion that may occur during the extraction of exchangeable Cr(VI) from silty-clay soil with phosphate buffer in order to establish an extraction method that would be effective, accurate and with minimal or no species interconversions. The Cr(VI) concentration in soil extracts was determined by speciated isotope dilution inductively coupled plasma mass spectrometry (SID-ICP-MS). The study was performed on soil samples from a field treated with tannery waste for 17 years. Samples were spiked by enriched stable isotopic solutions of (50)Cr(VI) and (53)Cr(III) that were added to phosphate buffers (0.1 M KH2PO4-K2HPO4 (pH 7.2) and/or 0.1 M K2HPO4 (pH 8)). To optimize extraction, mechanical shaking and/or ultrasound-assisted extraction were compared. The separation and detection of Cr species was performed by high-performance liquid chromatography (HPLC) ICP-MS. When mechanical shaking was applied, 90 % reduction of Cr(VI) was induced by extraction with 0.1 M KH2PO4-K2HPO4, while with 0.1 M K2HPO4 reduction was around 40 %. To shorten the extraction time and the possibility of species interconversions, ultrasound-assisted extraction was further applied only with 0.1 M K2HPO4. For total extraction of exchangeable Cr(VI) with a maximum 10 % reduction of Cr(VI), five consecutive ultrasound-assisted extractions were needed.

  16. Determination of carbon isotope ratios for honey samples by means of a liquid chromatography/isotope ratio mass spectrometry system coupled with a post-column pump.

    Science.gov (United States)

    Kawashima, Hiroto; Suto, Momoka; Suto, Nana

    2018-05-20

    Liquid chromatography/isotope ratio mass spectrometry (LC/IRMS) has been used to authenticate and trace products such as honey, wine, and lemon juice, and compounds such as caffeine and pesticides. However, LC/IRMS has several disadvantages, including the high cost of the CO 2 membrane and blocking by solidified sodium persulfate. Here, we developed an improved system for determining carbon isotope ratios by LC/IRMS. The main improvement was the use of a post-column pump. Using the improved system, we determined δ 13 C values for glucose with high accuracy and precision (0.1‰ and 0.1‰, respectively; n = 3). The glucose, fructose, disaccharide, trisaccharide, and organic acid constituents of the honey samples were analyzed by LC/IRMS. The δ 13 C values for glucose, fructose, disaccharides, trisaccharides, and organic acids ranged from -27.0 to -24.2‰, -26.8 to -24.0‰, -28.8 to -24.0‰, -27.8 to -22.8‰, and -30.6 to -27.4‰, respectively. The analysis time was 1/3-1/2 the times required for analysis by previously reported methods. The column flow rate could be arbitrarily adjusted with the post-column pump. We applied the improved method to 26 commercial honey samples. Our results can be expected to be useful for other researchers who use LC/IRMS. This article is protected by copyright. All rights reserved.

  17. Cryogenic separation of an oxygen-argon mixture in natural air samples for the determination of isotope and molecular ratios.

    Science.gov (United States)

    Keedakkadan, Habeeb Rahman; Abe, Osamu

    2015-04-30

    The separation and purification of oxygen-argon mixtures are critical in the high-precision analysis of Δ(17) O and δ(O2 /Ar) for geochemical applications. At present, chromatographic methods are used for the separation and purification of oxygen-argon mixtures or pure oxygen, but these methods require the use of high-purity helium as a carrier gas. Considerable interest has been expressed in the development of a helium-free cryogenic separation of oxygen-argon mixtures in natural air samples. The precise and simplified cryogenic separation of oxygen-argon mixtures from natural air samples presented here was made possible using a single 5A (30/60 mesh) molecular sieve column. The method involves the trapping of eluted gases using molecular sieves at liquid nitrogen temperature, which is associated with isotopic fractionation. We tested the proposed method for the determination of isotopic fractionations during the gas exchange between water and atmospheric air at equilibrium. The dependency of fractionation was studied at different water temperatures and for different methods of equilibration (bubbling and stirring). Isotopic and molecular fractionations during gas desorption from molecular sieves were studied for different amounts and types of molecular sieves. Repeated measurements of atmospheric air yielded a reproducibility (±SD) of 0.021 ‰, 0.044 ‰, 15 per meg and 1.9 ‰ for δ(17) O, δ(18) O, Δ(17) O and δ(O2 /Ar) values, respectively. We applied the method to determine equilibrium isotope fractionation during gas exchange between air and water. Consistent δ(18) O and Δ(17) O results were obtained with the latest two studies, whereas there was a significant difference in δ(18) O values between seawater and deionized water. We have revised a helium-free, cryogenic separation of oxygen-argon mixtures in natural air samples for isotopic and molecular ratio analysis. The use of a single 13X (1/8" pellet) molecular sieve yielded the smallest isotopic

  18. A Procedure for the Sequential Determination of Radionuclides in Environmental Samples. Liquid Scintillation Counting and Alpha Spectrometry for 90Sr, 241Am and Pu Radioisotopes

    International Nuclear Information System (INIS)

    2014-01-01

    Since 2004, IAEA activities related to the terrestrial environment have aimed at the development of a set of procedures to determine radionuclides in environmental samples. Reliable, comparable and ‘fit for purpose’ results are an essential requirement for any decision based on analytical measurements. For the analyst, tested and validated analytical procedures are extremely important tools for the production of analytical data. For maximum utility, such procedures should be comprehensive, clearly formulated and readily available for reference to both the analyst and the customer. This publication describes a combined procedure for the sequential determination of 90 Sr, 241 Am and Pu radioisotopes in environmental samples. The method is based on the chemical separation of strontium, americium and plutonium using ion exchange chromatography, extraction chromatography and precipitation followed by alpha spectrometric and liquid scintillation counting detection. The method was tested and validated in terms of repeatability and trueness in accordance with International Organization for Standardization (ISO) guidelines using reference materials and proficiency test samples. Reproducibility tests were performed later at the IAEA Terrestrial Environment Laboratory. The calculations of the massic activity, uncertainty budget, decision threshold and detection limit are also described in this publication. The procedure is introduced for the determination of 90 Sr, 241 Am and Pu radioisotopes in environmental samples such as soil, sediment, air filter and vegetation samples. It is expected to be of general use to a wide range of laboratories, including the Analytical Laboratories for the Measurement of Environmental Radioactivity (ALMERA) network for routine environmental monitoring purposes

  19. Determination of Unknown Neutron Cross Sections for the Production of Medical Isotopes

    Energy Technology Data Exchange (ETDEWEB)

    Stephen E. Binney

    2004-04-09

    Calculational assessment and experimental verification of certain neutron cross sections that are related to widely needed new medical isotopes. Experiments were performed at the Oregon State University TRIGA Reactor and the High Flux Irradiation Reactor at Oak Ridge National Laboratory.

  20. Use of stable isotope analysis to determine of the timing of ontogenic habitat shifts

    Data.gov (United States)

    National Oceanic and Atmospheric Administration, Department of Commerce — SAIP funding for stable isotope research was provided in FY11 and FY13; the FY11 funding was for loggerhead turtles (described below) as opposed to green turtles in...

  1. Analytical procedures for determining Pb and Sr isotopic compositions in water samples by ID-TIMS

    Directory of Open Access Journals (Sweden)

    Veridiana Martins

    2008-01-01

    Full Text Available Few articles deal with lead and strontium isotopic analysis of water samples. The aim of this study was to define the chemical procedures for Pb and Sr isotopic analyses of groundwater samples from an urban sedimentary aquifer. Thirty lead and fourteen strontium isotopic analyses were performed to test different analytical procedures. Pb and Sr isotopic ratios as well as Sr concentration did not vary using different chemical procedures. However, the Pb concentrations were very dependent on the different procedures. Therefore, the choice of the best analytical procedure was based on the Pb results, which indicated a higher reproducibility from samples that had been filtered and acidified before the evaporation, had their residues totally dissolved, and were purified by ion chromatography using the Biorad® column. Our results showed no changes in Pb ratios with the storage time.

  2. Determination of groundwater characteristics and water budget in the Edremit Plain by means of isotopes

    International Nuclear Information System (INIS)

    Onhon, E.

    1983-08-01

    Detailed field investigations with environmental isotopes (O-18, D, T, C-14 and C-13) have been conducted to study the replenishment process and flow dynamics of groundwater system in Edremit plain, which is an area of 200 m 2 size located in the eastern part of Turkey. Along with conventional hydrogeological and hydrochemical data collected from the study area, results of environmental isotopic analyses performed on water samples systematically collected from the area, enabled to delineate the source and origin of recharge to the shallow groundwater aquifers and as well provided information on various dynamic parameters of groundwater flow. In addition to basic flow dynamic characteristics of the shallow aquifer in the study area, environmental isotopes were used to investigate the hydraulic interconnections between deeper thermal groundwater system and the upper shallow aquifers. Results of all the environmental isotopic analyses and their interpretation are given

  3. Determination of uranium in urine - measurement of isotope ratios and quantification by use of inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Krystek, P.; Ritsema, R.

    2002-01-01

    For analysis of uranium in urine determination of the isotope ratio and quantification were investigated by high-resolution inductively coupled plasma mass spectrometry (HR ICP-MS). The instrument used (ThermoFinniganMAT ELEMENT2) is a single-collector MS and, therefore, a stable sample-introduction system was chosen. The methodical set-up was optimized to achieve the best precision for both the isotope ratio and the total uranium concentration in the urine matrix.Three spiked urine samples from an European interlaboratory comparison were analyzed to determine the 235 U/ 238 U isotope ratio. The ratio was found to be in the range 0.002116 to 0.007222, the latter being the natural uranium isotope ratio. The first ratio indicates the abundance of depleted uranium.The effect of storage conditions and the stability for the matrix urine were investigated by using ''real-life'' urine samples from unexposed persons in the Netherlands. For samples stored under refrigeration and acidified the results (range 0.8 to 5.3 ng L -1 U) were in the normal fluctuation range whereas a decrease in uranium concentration was observed for samples stored at room temperature without acidification. (orig.)

  4. Mass spectrometric determination of magnesium isotopic ratios and its corrections for electron multiplier discrimination and mass fractionation

    International Nuclear Information System (INIS)

    Deng Zhongguo

    1989-01-01

    The mass spectrometric determination of magnesium isotopic ratios by the use of uranyl nitrate added to magnesium samples to act as a binding agent is reported. Prebaking empty filaments and preheating filaments with deposited magnesium samples on its surface in a vacuum are employed to reduce the Na signal from the thenium-ribbon. Methods for correcting magnesium isotopic ratios for electron multiplier discrimination and mass fractionation are described in detail. The results of the determination of natural magnesium isotopic ratios are 25 Mg/ 24 Mg = 0.12660 (1±0.01%) and 26 Mg/ 24 Mg = 0.13938 (1±0.10%). The magnesium isotopic ratios of rich - 26 Mg-2 sample and rich- 25 Mg-1 sample are 24 Mg/ 26 Mg = 0.003463 (1±0.2%), 25 Mg/ 26 Mg = 0.001656 (±0.2%) and 24 Mg/ 25 Mg = 0.006716 (1±0.2%), 26 Mg/ 25 Mg = 0.007264 (1±0.2%) respectively

  5. Simultaneous determination of 14N and 15N isotopes in opium by proton induced γ-ray emission technique

    International Nuclear Information System (INIS)

    Pritty Rao; Reddy, G.L.N.; Vikram Kumar, S.; Ramana, J.V.; Raju, V.S.; Sanjiv Kumar

    2012-01-01

    The paper describes the simultaneous determination of 14 N and 15 N isotopes in opium by proton induced γ-ray emission (PIGE) technique. The isotopic ratio of 14 N and 15 N is a useful parameter for assigning provenance of (seized) illicit drugs. The measurement, non-destructive in nature, is performed on pellets made up of opium powders and is based on the prompt detection of 2.313 and 4.4 MeV γ-rays emanating from 14 N(p,p'γ) 14 N and 15 N(p,αγ) 12 C nuclear reactions respectively, induced simultaneously by 3.6-3.8 MeV proton beam. Positive as well as negative deviations from the natural isotopic abundance (99.63:0.37) were observed in the samples. The precision of the measurements is about 4%. The methodology provides an easy and rapid approach to determine the isotopic ratio of 14 N and 15 N and has been used for the first time in the analysis of opium. (author)

  6. Application of SAIL phenylalanine and tyrosine with alternative isotope-labeling patterns for protein structure determination

    Energy Technology Data Exchange (ETDEWEB)

    Takeda, Mitsuhiro [Nagoya University, Structural Biology Research Center, Graduate School of Science (Japan); Ono, Akira M.; Terauchi, Tsutomu [SAIL Technologies Co., Inc. (Japan); Kainosho, Masatsune, E-mail: kainosho@nmr.chem.metro-u.ac.j [Nagoya University, Structural Biology Research Center, Graduate School of Science (Japan)

    2010-01-15

    The extensive collection of NOE constraint data involving the aromatic ring signals is essential for accurate protein structure determination, although it is often hampered in practice by the pervasive signal overlapping and tight spin couplings for aromatic rings. We have prepared various types of stereo-array isotope labeled phenylalanines ({epsilon}- and {zeta}-SAIL Phe) and tyrosine ({epsilon}-SAIL Tyr) to overcome these problems (Torizawa et al. 2005), and proven that these SAIL amino acids provide dramatic spectral simplification and sensitivity enhancement for the aromatic ring NMR signals. In addition to these SAIL aromatic amino acids, we recently synthesized {delta}-SAIL Phe and {delta}-SAIL Tyr, which allow us to observe and assign {delta}-{sup 13}C/{sup 1}H signals very efficiently. Each of the various types of SAIL Phe and SAIL Tyr yields well-resolved resonances for the {delta}-, {epsilon}- or {zeta}-{sup 13}C/{sup 1}H signals, respectively, which can readily be assigned by simple and robust pulse sequences. Since the {delta}-, {epsilon}-, and {zeta}-proton signals of Phe/Tyr residues give rise to complementary NOE constraints, the concomitant use of various types of SAIL-Phe and SAIL-Tyr would generate more accurate protein structures, as compared to those obtained by using conventional uniformly {sup 13}C, {sup 15}N-double labeled proteins. We illustrated this with the case of an 18.2 kDa protein, Escherichia coli peptidyl-prolyl cis-trans isomerase b (EPPIb), and concluded that the combined use of {zeta}-SAIL Phe and {epsilon}-SAIL Tyr would be practically the best choice for protein structural determinations.

  7. Application of SAIL phenylalanine and tyrosine with alternative isotope-labeling patterns for protein structure determination.

    Science.gov (United States)

    Takeda, Mitsuhiro; Ono, Akira M; Terauchi, Tsutomu; Kainosho, Masatsune

    2010-01-01

    The extensive collection of NOE constraint data involving the aromatic ring signals is essential for accurate protein structure determination, although it is often hampered in practice by the pervasive signal overlapping and tight spin couplings for aromatic rings. We have prepared various types of stereo-array isotope labeled phenylalanines (epsilon- and zeta-SAIL Phe) and tyrosine (epsilon-SAIL Tyr) to overcome these problems (Torizawa et al. 2005), and proven that these SAIL amino acids provide dramatic spectral simplification and sensitivity enhancement for the aromatic ring NMR signals. In addition to these SAIL aromatic amino acids, we recently synthesized delta-SAIL Phe and delta-SAIL Tyr, which allow us to observe and assign delta-(13)C/(1)H signals very efficiently. Each of the various types of SAIL Phe and SAIL Tyr yields well-resolved resonances for the delta-, epsilon- or zeta-(13)C/(1)H signals, respectively, which can readily be assigned by simple and robust pulse sequences. Since the delta-, epsilon-, and zeta-proton signals of Phe/Tyr residues give rise to complementary NOE constraints, the concomitant use of various types of SAIL-Phe and SAIL-Tyr would generate more accurate protein structures, as compared to those obtained by using conventional uniformly (13)C, (15)N-double labeled proteins. We illustrated this with the case of an 18.2 kDa protein, Escherichia coli peptidyl-prolyl cis-trans isomerase b (EPPIb), and concluded that the combined use of zeta-SAIL Phe and epsilon-SAIL Tyr would be practically the best choice for protein structural determinations.

  8. Application of SAIL phenylalanine and tyrosine with alternative isotope-labeling patterns for protein structure determination

    International Nuclear Information System (INIS)

    Takeda, Mitsuhiro; Ono, Akira M.; Terauchi, Tsutomu; Kainosho, Masatsune

    2010-01-01

    The extensive collection of NOE constraint data involving the aromatic ring signals is essential for accurate protein structure determination, although it is often hampered in practice by the pervasive signal overlapping and tight spin couplings for aromatic rings. We have prepared various types of stereo-array isotope labeled phenylalanines (ε- and ζ-SAIL Phe) and tyrosine (ε-SAIL Tyr) to overcome these problems (Torizawa et al. 2005), and proven that these SAIL amino acids provide dramatic spectral simplification and sensitivity enhancement for the aromatic ring NMR signals. In addition to these SAIL aromatic amino acids, we recently synthesized δ-SAIL Phe and δ-SAIL Tyr, which allow us to observe and assign δ- 13 C/ 1 H signals very efficiently. Each of the various types of SAIL Phe and SAIL Tyr yields well-resolved resonances for the δ-, ε- or ζ- 13 C/ 1 H signals, respectively, which can readily be assigned by simple and robust pulse sequences. Since the δ-, ε-, and ζ-proton signals of Phe/Tyr residues give rise to complementary NOE constraints, the concomitant use of various types of SAIL-Phe and SAIL-Tyr would generate more accurate protein structures, as compared to those obtained by using conventional uniformly 13 C, 15 N-double labeled proteins. We illustrated this with the case of an 18.2 kDa protein, Escherichia coli peptidyl-prolyl cis-trans isomerase b (EPPIb), and concluded that the combined use of ζ-SAIL Phe and ε-SAIL Tyr would be practically the best choice for protein structural determinations.

  9. Comparison of isotope dilution and excretion methods for determining the half-life of ascorbic acid in the guinea pig

    International Nuclear Information System (INIS)

    Kipp, D.E.; Rivers, J.M.

    1984-01-01

    The half-life of ascorbic acid (AA) in guinea pigs was investigated by the isotope dilution and excretion methods. The dilution method measures [1-14C]AA disappearance from the plasma, whereas the excretion method measures the elimination of [1-14C]AA and the metabolites from the body. Two groups of animals underwent both isotope studies in reverse order. Animals were conditioned to the experimental procedures and fed 2.5 mg AA/100 g body weight orally to maintain a daily intake of the vitamin independent of food consumption. The two isotope procedures imposed similar stress on the animals, as determined by plasma cortisol levels and body weight changes. The AA half-life calculations of the rapidly exchangeable pool by the isotope dilution method yielded values of 1.23 and 0.34 hours for the two groups, respectively. The half-life of the slowly exchangeable pool for the two groups was 60.2 and 65.8 hours, respectively. The half-life of AA in the rapidly exchangeable pool, as measured by the excretion studies, was 4.57-8.75 hours. For the slowly exchangeable pool, it was 146-149 hours. The longer half-life of both pools obtained with the excretion method indicates that the isotope is disappearing from the plasma more rapidly than it is being excreted. This suggests that a portion of the [1-14C]AA leaving the plasma is removed to a body pool that is not sampled by the isotope excretion method

  10. Construction of a two-photon-laser spectrometer and determination of the hyperfine splitting and isotopic shift of barium

    International Nuclear Information System (INIS)

    Jitschin, W.

    1977-01-01

    A sensitive two-photon-laser spectrometer was constructed, that allowed to measure atomic states with an energy from 31 000 up to 37500 cm -1 with about 2 MHz resolution. The large energy range and the high resolution were reached by using a wide-wavelength tunable, narrow-band dye-laser. With this spectrometer transitions could be detected at barium from the electron ground-state 6s 2 1 S 0 to 10 upper states in the 5 most common isotopes 138 Ba, 137 Ba, 136 Ba, 135 Ba and 134 Ba. The transitions could be measured precisely. It was possible to derive lower limits of the life-time of these states from the widths of the recorded resonance lines (typically several nsec), that should in fact not be smaller than the actual lifetimes. From the measured hyper-fine splitting of the 6 transitions with angular momentum J = 2 at the oddnumbered isotopes 137 Ba and 135 Ba the parameters of the hyper-fine splitting could be determined. Hereby an accuracy of about IMH 2 could be reached at the A-factor and about 5MHz at the B-factor. At the measured transitions the isotopic shifts of the particular isotope could be determined with an accuracy of a few MHz. There was only a simple theory of the isotopic shift with only few parameters worked out for the theoretical interpretation of the measured data, that describes the data even at the experimentally reached high accuracy. Two parameters of this theory depending only from atomic nucleus properties, could be determined with a 0.5 % error. (orig./WB) [de

  11. Determination of isotopic composition of uranium in microparticles by secondary ion mass spectrometry

    International Nuclear Information System (INIS)

    Veniaminov, N.N.; Kolesnikov, O.N.; Stebel'kov, V.A.

    1992-01-01

    Aerosol particles including uranium in their composition are specific atmospheric polutants. Uranium is used as nuclear fuel in atomic power stations and in spacecraft power units, and also as a component of nuclear warheads. In order to monitor the discharge of uranium-containing aerosol particles to the atmosphere, they must first be identified. As an example, one may cite an investigation of the elemental composition and radioactivity of particles formed in the accident at the Chernobyl atomic power station. One of the most informative indicators of the origin of uranium-containing aerosol particles is the isotopic composition of the uranium. Secondary ion mass spectrometry (SIMS) offers unique possibilities for the measurement of isotope ratios in individual microscopic objects. At the same time, a measurement of isotope ratios of sulfur in microsection of galenite PbS 2 has shown that the application of SIMS for these purposes is seriously limited by the difference in yield of secondary ions for isotopes with different masses. These discrimination effects, in the case of light elements such as boron, may result in distortion of the isotope ratios by several percent. In the case of heavy elements, however, the effect is less significant, amounting to about 0.5% for lead isotopes. 13 refs., 3 figs., 1 tab

  12. Sequential determination of nickel and cadmium in tobacco, molasses and refill solutions for e-cigarettes samples by molecular fluorescence.

    Science.gov (United States)

    Talio, María Carolina; Alesso, Magdalena; Acosta, Mariano; Wills, Verónica S; Fernández, Liliana P

    2017-11-01

    In this work, a new procedure was developed for separation and preconcentration of nickel(II) and cadmium(II) in several and varied tobacco samples. Tobacco samples were selected considering the main products consumed by segments of the population, in particular the age (youth) and lifestyle of the consumer. To guarantee representative samples, a randomized strategy of sampling was used. In the first step, a chemofiltration on nylon membrane is carried out employing eosin (Eo) and carbon nanotubes dispersed in sodium dodecylsulfate (SDS) solution (phosphate buffer pH 7). In this condition, Ni(II) was selectively retained on the solid support. After that, the filtrate liquid with Cd(II) was re-conditioned with acetic acid /acetate buffer solution (pH 5) and followed by detection. A spectrofluorimetric determination of both metals was carried out, on the solid support and the filtered aqueous solution, for Ni(II) and Cd(II), respectively. The solid surface fluorescence (SSF) determination was performed at λ em = 545nm (λ ex = 515nm) for Ni(II)-Eo complex and the fluorescence of Cd(II)-Eo was quantified in aqueous solution using λ em = 565nm (λ ex = 540nm). The calibration graphs resulted linear in a range of 0.058-29.35μgL -1 for Ni(II) and 0.124-56.20μgL -1 for Cd(II), with detection limits of 0.019 and 0.041μgL -1 (S/N = 3). The developed methodology shows good sensitivity and adequate selectivity, and it was successfully applied to the determination of trace amounts of nickel and cadmium present in tobacco samples (refill solutions for e-cigarettes, snuff used in narguille (molasses) and traditional tobacco) with satisfactory results. The new methodology was validated by ICP-MS with adequate agreement. The proposed methodology represents a novel fluorescence application to Ni(II) and Cd(II) quantification with sensitivity and accuracy similar to atomic spectroscopies, introducing for the first time the quenching effect on SSF. Copyright © 2017 Elsevier B

  13. Sequential determination of arsenic, selenium, antimony, and tellurium in foods via rapid hydride evolution and atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Fiorino, J.A.; Jones, J.W.; Capar, S.G.

    1976-01-01

    Analysis of acid digests of foods for As, Se, Sb, and Te was semiautomated. Hydrides generated by controlled addition of base stabilized NaBH 4 solution to acid digests are transported directly into a shielded, hydrogen (nitrogen diluted), entrained-air flame for atomic absorption spectrophotometric determination of the individual elements. The detection limits, based on 1 g of digested sample, are approximately 10 to 20 ng/g for all four elements. Measurement precision is 1 to 2 percent relative standard deviation for each element measured at 0.10 μg. A comparison is made of results of analysis of lyophilized fish tissues for As and Se by instrumental neutron activation (INAA), hydride generation with atomic absorption spectrometry, fluorometry, and spectrophotometry. NBS standard reference materials (orchard leaves and bovine liver) analyzed for As, Se, and Sb by this method show excellent agreement with certified values and with independent NAA values

  14. Determining origin in a migratory marine vertebrate: a novel method to integrate stable isotopes and satellite tracking

    Science.gov (United States)

    Vander Zanden, Hannah B.; Tucker, Anton D.; Hart, Kristen M.; Lamont, Margaret M.; Fujisaki, Ikuko; Addison, David S.; Mansfield, Katherine L.; Phillips, Katrina F.; Wunder, Michael B.; Bowen, Gabriel J.; Pajuelo, Mariela; Bolten, Alan B.; Bjorndal, Karen A.

    2015-01-01

    Stable isotope analysis is a useful tool to track animal movements in both terrestrial and marine environments. These intrinsic markers are assimilated through the diet and may exhibit spatial gradients as a result of biogeochemical processes at the base of the food web. In the marine environment, maps to predict the spatial distribution of stable isotopes are limited, and thus determining geographic origin has been reliant upon integrating satellite telemetry and stable isotope data. Migratory sea turtles regularly move between foraging and reproductive areas. Whereas most nesting populations can be easily accessed and regularly monitored, little is known about the demographic trends in foraging populations. The purpose of the present study was to examine migration patterns of loggerhead nesting aggregations in the Gulf of Mexico (GoM), where sea turtles have been historically understudied. Two methods of geographic assignment using stable isotope values in known-origin samples from satellite telemetry were compared: 1) a nominal approach through discriminant analysis and 2) a novel continuous-surface approach using bivariate carbon and nitrogen isoscapes (isotopic landscapes) developed for this study. Tissue samples for stable isotope analysis were obtained from 60 satellite-tracked individuals at five nesting beaches within the GoM. Both methodological approaches for assignment resulted in high accuracy of foraging area determination, though each has advantages and disadvantages. The nominal approach is more appropriate when defined boundaries are necessary, but up to 42% of the individuals could not be considered in this approach. All individuals can be included in the continuous-surface approach, and individual results can be aggregated to identify geographic hotspots of foraging area use, though the accuracy rate was lower than nominal assignment. The methodological validation provides a foundation for future sea turtle studies in the region to inexpensively

  15. Liquid and gas chromatography coupled to isotope ratio mass spectrometry for the determination of 13C-valine isotopic ratios in complex biological samples

    NARCIS (Netherlands)

    Godin, Jean-Philippe; Breuillé, Denis; Obled, Christiane; Papet, Isabelle; Schierbeek, Henk; Hopfgartner, Gérard; Fay, Laurent-Bernard

    2008-01-01

    On-line gas chromatography-combustion-isotope ratio mass spectrometry (GC-C-IRMS) is commonly used to measure isotopic ratios at natural abundance as well as for tracer studies in nutritional and medical research. However, high-precision (13)C isotopic enrichment can also be measured by liquid

  16. Method development for the determination of arsenic by sequential injection/anodic stripping voltammetry using long-lasting gold-modified screen-printed carbon electrode.

    Science.gov (United States)

    Punrat, Eakkasit; Chuanuwatanakul, Suchada; Kaneta, Takashi; Motomizu, Shoji; Chailapakul, Orawon

    2013-11-15

    An automated method has been developed for determining the concentration of inorganic arsenic. The technique uses sequential injection/anodic stripping voltammetry with a long-lasting gold-modified screen-printed carbon electrode. The long-lasting gold electrode was electrochemically deposited onto a screen-printed carbon electrode at a potential of -0.5 V vs. Ag/AgCl in a supporting electrolyte solution of 1M hydrochloric acid. Under optimal conditions and the applied potentials, the electrode demonstrated that it can be used for a long time without a renewal process. The linear range for the determination of arsenic(III) was 1-100 μg L(-1), and the limit of detection (LOD) in standard solutions was as low as 0.03 μg L(-1) for a deposition time of 120 s and sample volume of 1 mL. This method was used to determine the concentration of arsenic(III) in water samples with satisfactory results. The LOD in real samples was found to be 0.5 μg L(-1). In addition, speciation between arsenic(III) and arsenic(V) has been achieved with the proposed method using deposition potentials of -0.5 V and -1.5 V for the determination of the arsenic(III) concentration and the total arsenic concentration, respectively; the results were acceptable. The proposed method is an automated system that offers a less expensive alternative for determining trace amounts of inorganic arsenic. © 2013 Elsevier B.V. All rights reserved.

  17. Automated magnetic sorbent extraction based on octadecylsilane functionalized maghemite magnetic particles in a sequential injection system coupled with electrothermal atomic absorption spectrometry for metal determination.

    Science.gov (United States)

    Giakisikli, Georgia; Anthemidis, Aristidis N

    2013-06-15

    A new automatic sequential injection (SI) system for on-line magnetic sorbent extraction coupled with electrothermal atomic absorption spectrometry (ETAAS) has been successfully developed for metal determination. In this work, we reported effective on-line immobilization of magnetic silica particles into a microcolumn by the external force of two strong neodymium iron boron (NdFeB) magnets across it, avoiding the use of frits. Octadecylsilane functionalized maghemite magnetic particles were used as sorbent material. The potentials of the system were demonstrated for trace cadmium determination in water samples. The method was based on the on-line complex formation with diethyldithiocarbamate (DDTC), retention of Cd-DDTC on the surface of the MPs and elution with isobutyl methyl ketone (IBMK). The formation mechanism of the magnetic solid phase packed column and all critical parameters (chemical, flow, graphite furnace) influencing the performance of the system were optimized and offered good analytical characteristics. For 5 mL sample volume, a detection limit of 3 ng L(-1), a relative standard deviation of 3.9% at 50 ng L(-1) level (n=11) and a linear range of 9-350 ng L(-1) were obtained. The column remained stable for more than 600 cycles keeping the cost down in routine analysis. The proposed method was evaluated by analyzing certified reference materials and natural waters. Copyright © 2013 Elsevier B.V. All rights reserved.

  18. Determination of essential elements in beverages, herbal infusions and dietary supplements using a new straightforward sequential approach based on flame atomic absorption spectrometry.

    Science.gov (United States)

    Gómez-Nieto, Beatriz; Gismera, Mª Jesús; Sevilla, Mª Teresa; Procopio, Jesús R

    2017-03-15

    A simple method based on FAAS was developed for the sequential multi-element determination of Cu, Zn, Mn, Mg and Si in beverages and food supplements with successful results. The main absorption lines for Cu, Zn and Si and secondary lines for Mn and Mg were selected to carry out the measurements. The sample introduction was performed using a flow injection system. Using the choice of the absorption line wings, the upper limit of the linear range increased up to 110mgL -1 for Mg, 200mgL -1 for Si and 13mgL -1 for Zn. The determination of the five elements was carried out, in triplicate, without the need of additional sample dilutions and/or re-measurements, using less than 3.5mL of sample to perform the complete analysis. The LODs were 0.008mgL -1 for Cu, 0.017mgL -1 for Zn, 0.011mgL -1 for Mn, 0.16mgL -1 for Si and 0.11mgL -1 for Mg. Copyright © 2016 Elsevier Ltd. All rights reserved.

  19. Determination of stable isotope ratio of lead in airborne particulate matter by ICP-MS

    International Nuclear Information System (INIS)

    Mukai, Hitoshi; Ambe, Yoshinari

    1990-01-01

    ICP-MS was applied to the measurement of stable isotope ratios of lead, which are used as an indicator of the source of lead in airborne particulate matter. For the measurement of lead isotopes ratios, the influences of machine conditions, lead concentration and matrix elements to the precision and accuracy of the measurements were studied. At a scanning mode, dwell time of 40∼160 μs gave the best precision to the isotope ratio measurements; about 0.3 % of R.S.D. for 206 Pb/ 207 Pb and 206 Pb/ 208 Pb, 0.6 % for 206 Pb/ 204 Pb. Precision of the measurement was better at a high concentration of lead in sample solution. The observed value of 206 Pb/ 207 Pb ratio was not affected by the lead concentration, but in the cases of 206 Pb/ 204 Pb and 206 Pb/ 208 Pb, about 1 % of the value changed in the observed ratios with the lead concentration of 100∼500 μg/l. Six matrix elements (Na, K, Ca, Mg, Al, Fe) did not affect the observed isotope ratios up to 200 mg/l. The lead isotope ratios of reference materials {Urban Particulates (NIST) and Vehicle Exhausted Particulates (NIES)} were measured by using two kinds of sample; crude sample and lead-isolated sample from matrix elements by anodic deposition. Both cases gave the same isotope ratio values, therefore, lead isotope ratios in airborne particulate samples can be measured by ICP-MS without any separation of lead from matrix elements. (author)

  20. Determination of endogenous manganese excretion in broiler chicks by an isotope-dilution method

    International Nuclear Information System (INIS)

    Weigand, E.; Kirchgessner, M.; Kilic, A.

    1988-01-01

    A tracer study with broiler chicks was conducted to determine endogenous Mn excretion in response to graded levels of dietary Mn supply by the isotope-dilution method. Starting with 46 day-old chicks, low-Mn diets were fed for 12 days before 8 chicks were slaughtered for assessing the intial Mn status and 38 chicks each were given an intramuscular injection of 555 kBq 54 Mn. Four groups of six birds each were fed, one bird per cage, diets containing 2.8, 9.1, 25.8, and 59.7 ppm Mn for 16 days before slaughter and carcass analyses. Two groups of 7 birds were fed the diets with 9.1 and 25.8 ppm Mn for 8 days. Mn supply significantly affected 54 Mn excretion activity of distribution among various body organs, especially the liver. The specific activity of Mn in excreta and in whole-body declined exponentially with time and differed between groups. Endogenous Mn in excreta was estimated on the basis that the specific activity of excreta Mn from day 9 to 12 and day 13 to 16 was reflected, on the average, by that of liver Mn on day 10 and 14, respectively. It averaged in the order of increasing Mn supply 12.5 vs. 12.0; 7.7 vs. 8.5; 3.9 vs. 4.3, and 2.0 vs. 2.3% of total excreta Mn. Total Mn excretion from day 9 to 16 averaged 88.9, 95.0, 97.9. and 98.9% of Mn intake. (author)

  1. Determining the sources of calcium for migratory songbirds using stable strontium isotopes.

    Science.gov (United States)

    Blum, Joel D; Taliaferro, E Hank; Holmes, Richard T

    2001-02-01

    We investigated natural variations in the stable isotopic composition of strontium (a surrogate for calcium) in the bones of a single species of breeding migratory songbird, as well as in their eggshells, egg contents, and food sources. We use this information to determine the sources of calcium to these migratory songbirds and their offspring. Samples were collected from two locations in the northeastern USA (Hubbard Brook, NH, and Downer Forest, VT.) that differed in soil geochemistry. The mean 87 Sr/ 86 Sr ratios of food items (caterpillars and snails), eggshells, and egg contents were indistinguishable within each site, but significantly different between the two sites. Mean 87 Sr/ 86 Sr ratios for the bones of adult females were significantly different between the two sites, but values were significantly lower than those of food items and eggshells at each site. Two of four adult individuals studied at each site had 87 Sr/ 86 Sr ratios lower than the entire range of values for local food sources. Mixing calculations indicate that up to 60% of skeletal strontium and calcium was derived from foods consumed in the winter grounds where lower 87 Sr/ 86 Sr ratios predominate. At each study site, the 87 Sr/ 86 Sr ratio of eggshells differed significantly between clutches, but the mean clutch 87 Sr/ 86 Sr ratios were unrelated to the skeletal 87 Sr/ 86 Sr ratio of the laying adult. These findings suggest that strontium (and hence calcium) for eggshell production in this species is derived predominantly from local food sources in breeding areas. Thus, reductions in available calcium in northern temperate ecosystems due to the influences of acid deposition could be potentially harmful to this and other species of migratory bird.

  2. Determination of the isotopic composition of neutron irradiated nuclear fuel materials by MCNPX

    International Nuclear Information System (INIS)

    Cerba, S.; Necas, V.

    2012-01-01

    The aim of this study was to examine whether the MCNPX code can provide acceptable results in fuel depletion calculation. There sets of cross section libraries have been process with the NJOY code on the basis of three different cross section evaluations. These libraries had been validated and the statistical evaluation of the results showed that all three sets had been processed correctly and they are applicable for the burnup calculation. To verify the burnup capabilities of the MCNPX code the third case of the IV-B phase of the OECD NEA Burnup credit benchmark has been chosen, which is a code to code validation. The main task was to compare the k and the isotope concentrations at 4 burnup steps. The comparison of the calculation results clearly showed that the results obtained by MCNPX were in the range of other codes used in nuclear research. There were some discrepancies between the calculated and the benchmark data, but it was not possible to definitely conclude whether they were caused by the accuracy of the program or not. On the one hand, the results showed that some discrepancies may have been caused by the different cross section evaluations used in the calculation. On the other hand we cannot determine, how accurate the results from the other codes were; thus the deviations that at the first glance seemed to be high might not have necessarily meant inaccuracies in the calculation. Despite the fact that the MCNPX code is still in development, we can conclude that the code is capable of obtaining relevant results. (authors)

  3. Determination of nitrate pollution sources in the Marano Lagoon (Italy) by using a combined approach of hydrochemical and isotopic techniques

    Energy Technology Data Exchange (ETDEWEB)

    Saccon, Pierpaolo; Leis, Albrecht [JOANNEUM RESEARCH Forschungsgesellschaft mbH, Institute for Water, Energy and Sustainability, 8010 Graz (Austria); Marca, Alina; Kaiser, Jan; Campisi, Laura [School of Environmental Sciences, University of East Anglia, NR4 7TJ Norwich (United Kingdom); Boettcher, Michael E.; Escher, Peter [Leibniz Institute for Baltic Sea Research (IOW), Geochemistry and Isotope Geochemistry Group, D-18119 Rostock (Germany); Savarino, Joel; Erbland, Joseph [UJF-Grenoble 1/CNRS-INSU, Laboratoire de Glaciologie et Geophysique de l' Environnement (LGGE) UMR 5183 (France); Eisenhauer, Anton [GEOMAR, Helmholtz Zentrum fuer Ozean Forschung Kiel, Wischhofstr. 1-3, 24148 Kiel (Germany)

    2013-07-01

    Due to increased pollution by nitrate from intensive agricultural and other anthropogenic activities the Marano lagoon (northeast Italy) and part of its catchment area have been investigated, applying a combined approach of hydrochemical and isotopic techniques. Thus, to identify and characterize the potential multiple-sources of nitrate pollution the isotopic compositions of nitrate (δ{sup 15}N, δ{sup 18}O, and Δ{sup 17}O), boron (δ{sup 11}B), water (δ{sup 2}H and δ{sup 18}O), and sulphate (δ{sup 34}S and δ{sup 18}O), as well as the chemical composition of different water types have been determined. In the monitoring program water samples from the lagoon, its tributary rivers, the groundwater upwelling line, groundwater, sewage, and open sea on a quarterly interval from 2009 to 2010 have been collected and analyzed. Coupling isotopic and hydrochemical results indicate that the nitrate load in the lagoon was not only derived from agriculture activities but also from other sources such as urban wastewaters, in situ nitrification, and atmospheric deposition. However, none of the samples showed the isotopic characteristics of synthetic fertilizers. (authors)

  4. Development of a Method to Isolate Glutamic Acid from Foodstuffs for a Precise Determination of Their Stable Carbon Isotope Ratio.

    Science.gov (United States)

    Kobayashi, Kazuhiro; Tanaka, Masaharu; Yatsukawa, Yoichi; Tanabe, Soichi; Tanaka, Mitsuru; Ohkouchi, Naohiko

    2018-01-01

    Recent growing health awareness is leading to increasingly conscious decisions by consumers regarding the production and traceability of food. Stable isotopic compositions provide useful information for tracing the origin of foodstuffs and processes of food production. Plants exhibit different ratios of stable carbon isotopes (δ 13 C) because they utilized different photosynthetic (carbon fixation) pathways and grow in various environments. The origins of glutamic acid in foodstuffs can be differentiated on the basis of these photosynthetic characteristics. Here, we have developed a method to isolate glutamic acid in foodstuffs for determining the δ 13 C value by elemental analyzer-isotope-ratio mass spectrometry (EA/IRMS) without unintended isotopic fractionation. Briefly, following acid-hydrolysis, samples were defatted and passed through activated carbon and a cation-exchange column. Then, glutamic acid was isolated using preparative HPLC. This method is applicable to measuring, with a low standard deviation, the δ 13 C values of glutamic acid from foodstuffs derived from C3 and C4 plants and marine algae.

  5. Using Gas Chromatography/Isotope Ratio Mass Spectrometry to Determine the Fractionation Factor for H2 Production by Hydrogenases

    International Nuclear Information System (INIS)

    Yang, Hui; Ghandi, H.; Shi, Liang; Kreuzer, Helen W.; Ostrom, Nathaniel; Hegg, Eric L.

    2012-01-01

    Hydrogenases catalyze the reversible formation of H2, and they are key enzymes in the biological cycling of H2. H isotopes should be a very useful tool in quantifying proton trafficking in biological H2 production processes, but there are several obstacles that have thus far limited the use of this tool. In this manuscript, we describe a new method that overcomes some of these barriers and is specifically designed to measure isotopic fractionation during enzyme-catalyzed H2 evolution. A key feature of this technique is that purified hydrogenases are employed, allowing precise control over the reaction conditions and therefore a high level of precision. A custom-designed high-throughput gas chromatography-isotope ratio mass spectrometer is employed to measure the isotope ratio of the H2. Using this method, we determined that the fractionation factor of H2 production by the (NiFe)-hydrogenase from Desulfivibrio fructosovran is 0.27. This result indicates that, as expected, protons are highly favored over deuterons during H2 evolution. Potential applications of this new method are discussed.

  6. Determination of boron isotope ratios by high-resolution continuum source molecular absorption spectrometry using graphite furnace vaporizers

    Science.gov (United States)

    Abad, Carlos; Florek, Stefan; Becker-Ross, Helmut; Huang, Mao-Dong; Heinrich, Hans-Joachim; Recknagel, Sebastian; Vogl, Jochen; Jakubowski, Norbert; Panne, Ulrich

    2017-10-01

    Boron isotope amount ratios n(10B)/n(11B) have been determined by monitoring the absorption spectrum of boron monohydride (BH) in a graphite furnace using high-resolution continuum source molecular absorption spectrometry (HR-CS-MAS). Bands (0 → 0) and (1 → 1) for the electronic transition X1Σ+ → A1Π were evaluated around wavelengths 433.1 nm and 437.1 nm respectively. Clean and free of memory effect molecular spectra of BH were recorded. In order to eliminate the memory effect of boron, a combination of 2% (v/v) hydrogen gas in argon and 1% trifluoromethane in argon, an acid solution of calcium chloride and mannitol as chemical modifiers was used. Partial least square regression (PLS) for analysis of samples and reference materials were applied. For this, a spectral library with different isotopes ratios for PLS regression was built. Results obtained around the 433.1 nm and 437.1 nm spectral regions are metrologically compatible with those reported by mass spectrometric methods. Moreover, for the evaluated region of 437 nm, an accuracy of 0.15‰ is obtained as the average deviation from the isotope reference materials. Expanded uncertainties with a coverage factor of k = 2 range between 0.15 and 0.44‰. This accuracy and precision are compatible with those obtained by mass spectrometry for boron isotope ratio measurements.

  7. Use of Isotopic Data to Determine Influence of Seasonal Effects in Rivers

    Energy Technology Data Exchange (ETDEWEB)

    Michel, R. L. [US Geological Survey, Menlo Park, CA (United States); Aggarwal, P. K.; Araguas Araguas, L.; Newman, B.; Kurttas, T. [International Atomic Energy Agency, Vienna (Austria)

    2013-07-15

    In 2002 the International atomic energy agency and its Member states initiated a programme for the collection and measurement of isotopes (stable isotopes of water and tritium) in river waters. The purpose of this programme is to establish a long term database (GNIR) similar to the global database currently available for precipitation. These isotopic data provide a baseline for studying parameters in hydrologic basins that can be used to monitor any changes in the basin response due to shifts in future climatic or land use factors. Below, selected {sup 18}O and tritium data sets where measurements from several years of routine sampling are available are analysed. A ratio of the average monthly isotopic concentration divided by the average yearly concentration is used to normalize data and makes it possible to compare data from different sites. In general, high flow periods are strongly influenced by younger water whereas baseflow is primarily composed of water of greater age (probably decadal). Using this approach and flow rates, it should be possible to estimate the isotopic concentrations of baseflow. This data set will make it possible to track changes in baseflow concentrations occurring due to future changes in climate or land use. (author)

  8. Isotopic Determination of Nuclear Materials Using Nuclear Fission Track Registration Technique and Thermal Ionization Mass Spectrometric Technique

    International Nuclear Information System (INIS)

    Jeon, Young Sin; Pyo, Hyeong Yeol; Park, Yong Joon; Song, Kyu Seok; Kim, Won Ho; Jee, Kwang Yong

    2007-05-01

    It is very important to develope the technology for the determination of isotopic ratios of hot particles( 234 U, 235 U, 236 U etc.) detected from swipe samples of various nuclear facilities. This technology is highly competitive internationally and has to be established independently as long as our government maintains atomic energy and treats nuclear materials. In this text, sample pretreatment procedure, gamma-ray counting, alpha or fission track techniques, isotopic analysis of U and Pu, background problems and detection limits for mass determination, and their application to the real swipe sample were described with detailed procedure. This technology would contribute to the Korean economy's high growth rate as well as to superiority of government's leading research and development programs if successfully established

  9. Determination of rare-earth elements in rocks by isotope-excited X-ray fluorescence spectrometry

    DEFF Research Database (Denmark)

    Kunzendorf, Helmar; Wollenberg, H.A.

    1970-01-01

    Isotope-excited X-ray fluorescence spectrometry furnishes a rapid determination of rare-earth elements in unprepared rock samples. The samples are excited by 241Am γ-rays, generating X-ray spectra on a multichannel pulse-height analyser. Gaussian peaks of the Kα and Kβ X-ray energies are treated ......-ray spectrometric scan of a longitudinally sliced drill core showed a close correlation between rare-earth abundances and appropriate minerals.......Isotope-excited X-ray fluorescence spectrometry furnishes a rapid determination of rare-earth elements in unprepared rock samples. The samples are excited by 241Am γ-rays, generating X-ray spectra on a multichannel pulse-height analyser. Gaussian peaks of the Kα and Kβ X-ray energies are treated...

  10. On-line liquid phase micro-extraction based on drop-in-plug sequential injection lab-at-valve platform for metal determination

    Energy Technology Data Exchange (ETDEWEB)

    Mitani, Constantina [Laboratory of Analytical Chemistry, Department of Chemistry, Aristotle University, Thessaloniki 54124 (Greece); Anthemidis, Aristidis N., E-mail: anthemid@chem.auth.gr [Laboratory of Analytical Chemistry, Department of Chemistry, Aristotle University, Thessaloniki 54124 (Greece)

    2013-04-10

    Highlights: ► Drop-in-plug micro-extraction based on SI-LAV platform for metal preconcentration. ► Automatic liquid phase micro-extraction coupled with FAAS. ► Organic solvents with density higher than water are used. ► Lead determination in environmental water and urine samples. -- Abstract: A novel automatic on-line liquid phase micro-extraction method based on drop-in-plug sequential injection lab-at-valve (LAV) platform was proposed for metal preconcentration and determination. A flow-through micro-extraction chamber mounted at the selection valve was adopted without the need of sophisticated lab-on-valve components. Coupled to flame atomic absorption spectrometry (FAAS), the potential of this lab-at-valve scheme is demonstrated for trace lead determination in environmental and biological water samples. A hydrophobic complex of lead with ammonium pyrrolidine dithiocarbamate (APDC) was formed on-line and subsequently extracted into an 80 μL plug of chloroform. The extraction procedure was performed by forming micro-droplets of aqueous phase into the plug of the extractant. All critical parameters that affect the efficiency of the system were studied and optimized. The proposed method offered good performance characteristics and high preconcentration ratios. For 10 mL sample consumption an enhancement factor of 125 was obtained. The detection limit was 1.8 μg L{sup −1} and the precision expressed as relative standard deviation (RSD) at 50.0 μg L{sup −1} of lead was 2.9%. The proposed method was evaluated by analyzing certified reference materials and applied for lead determination in natural waters and urine samples.

  11. Determination of rare-earth elements in rocks by isotope-excited X-ray fluorescence spectrometry

    DEFF Research Database (Denmark)

    Kunzendorf, Helmar; Wollenberg, H.A.

    1970-01-01

    Isotope-excited X-ray fluorescence spectrometry furnishes a rapid determination of rare-earth elements in unprepared rock samples. The samples are excited by 241Am γ-rays, generating X-ray spectra on a multichannel pulse-height analyser. Gaussian peaks of the Kα and Kβ X-ray energies are treated......-ray spectrometric scan of a longitudinally sliced drill core showed a close correlation between rare-earth abundances and appropriate minerals....

  12. Determination of the isotopic ratio 235U/238U in UF6 using quadrupole mass spectrometry

    International Nuclear Information System (INIS)

    Kusahara, Helena Sueco

    1979-01-01

    In this work measurements of isotope ratios 235 U / 23 '8U in uranium hexafluoride are carried out using a quadrupole mass spectrometer. The operational parameters, which affect the final precision of the results, are standardized. Optimized procedures for the preparation of uranium hexafluoride samples by fluorination of uranium oxides using cobalt trifluoride method are established. Careful attention is given to the process of purification of uranium hexafluoride samples by fractional distillation. Adequate statistical methods for analysing the results obtained for single ratio measurements as well as the ratio ' of isotopic ratios of sample and standard ar.e developed. A precision of about 10 -4 for single ratio measurements and accuracy of about 0,3% for the ratio of sample and standard ratios are obtained. These results agree with the values which have been obtained using magnetic mass spectrometers. The procedures and methods established in this work can be employed in the systematic uranium isotope analysis in UF 6 form. (author)

  13. The use of isotopic correlation technique for determination of sup(241)Am and sup(243)Am concentration in nuclear irradiated fuels

    International Nuclear Information System (INIS)

    Souza Sarkis, J.E. de.

    1990-01-01

    In the last years the isotopic correlation technique is emerging as a powerful tool for the determination of concentration and isotopic composition of heavy nuclides in the nuclear fuel cycle. Accordingly, this technique has gained significant importance for the safeguard of the nuclear materials as well as for the accounting and build up of actinides elements in the irradiated nuclear fuels. In this work 42 isotopic correlations between the nuclides sup(241)Am and sup(243)Am and post irradiation isotopic data of 7 samples from fuel element BE-124 and 1 sample from fuel element BE-120 from the Obrigheim pressurized water nuclear power reactor, Federal Republic of Germany, were proposed. These isotopic correlations allowed to estimate the isotopic concentrations of sup(241)Am and sup(243)Am with an average deviation, relative to the experimental data obtained from isotopic dilution mass spectrometry technique, of 10%. These results are more precise than those found using the computer code ORIGEN 2 demonstrating the great potential of this technique for the determination of isotopic concentration and build up of those nuclides in irradiated nuclear fuels. The analytical and other experimental aspects of the post irradiation isotopic analysis of nuclear fuels are also discussed. (author)

  14. To problem of experimental determination of parameters of μ-atom charge-exchange process of hydrogen isotopes on He nuclei

    International Nuclear Information System (INIS)

    Bystritskij, V.M.; Stolupin, V.A.

    1990-01-01

    The kinetics of μ-atomic and μ-molecular processes occuring in hydrogen isotopes-helium mixture is observed. The expressions are obtained to determine the parameters of a process of the muon transition from hydrogen isotope μ atoms to helium nuclei with the use of different experimental methods. 18 refs.; 3 figs.; 1 tab

  15. Introduction and optimization of methods for isotopic determination of thorium and uranium via α-spectroscopy and their applications in analysis of water from Morro do Ferro, Brazil

    International Nuclear Information System (INIS)

    Vale, M.G.R.

    1982-01-01

    Methods for isotopic determination of thorium and uranium via α-spectroscopy, using a surface barrier detector, are described. The methods were applied in surface waters, borehole water, sediments and minerals from Morro do Ferro (MG), Brazil. Results and analysis by different techniques are compared and some discussions concerning to Th-concentration levels and anomalous isotopic and nuclidic ratios are presented. (Author) [pt

  16. Determining synthesis rates of individual proteins in zebrafish (Danio rerio) with low levels of a stable isotope labelled amino acid.

    Science.gov (United States)

    Geary, Bethany; Magee, Kieran; Cash, Phillip; Young, Iain S; Whitfield, Phillip D; Doherty, Mary K

    2016-05-01

    The zebrafish is a powerful model organism for the analysis of human cardiovascular development and disease. Understanding these processes at the protein level not only requires changes in protein concentration to be determined but also the rate at which these changes occur on a protein-by-protein basis. The ability to measure protein synthesis and degradation rates on a proteome-wide scale, using stable isotope labelling in conjunction with mass spectrometry is now a well-established experimental approach. With the advent of more selective and sensitive mass spectrometers, it is possible to accurately measure lower levels of stable isotope incorporation, even when sample is limited. In order to challenge the sensitivity of this approach, we successfully determined the synthesis rates of over 600 proteins from the cardiac muscle of the zebrafish using a diet where either 30% or 50% of the L-leucine was replaced with a stable isotope labelled analogue ([(2) H7 ]L-leucine]. It was possible to extract sufficient protein from individual zebrafish hearts to determine the incorporation rate of the label into hundreds of proteins simultaneously, with the two labelling regimens showing a good correlation of synthesis rates. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Determination of trace metal ions via on-line separation and preconcentration by means of chelating Sepharose beads in a sequential injection lab-on-valve (SI-LOV) system coupled to electrothermal atomic absorption spectrometric detection

    DEFF Research Database (Denmark)

    Long, Xiangbao; Hansen, Elo Harald; Miró, Manuel

    2005-01-01

    The analytical performance of an on-line sequential injection lab-on-valve (SI-LOV) system using chelating Sepharose beads as sorbent material for the determination of ultra trace levels of Cd(II), Pb(II) and Ni(II) by electrothermal atomic absorption spectrometry (ETAAS) is described and discussed...

  18. The use of natural radioactive Isotopes in the determination of pollution sources of AL-Kabir AL-Shimali river

    International Nuclear Information System (INIS)

    Al-Masri, M. S.; Shwiekani, R.; Mamish, S.

    2012-01-01

    In the present research, variations of concentration levels of some natural radioactive isotopes (226 Ra, 210 Po,210 Pb, U and Th isotopes) and some trace elements (Cu, Zn, Pb, Cd) in water and sediments of AL-Kabir AL-Shimali river during the period of 2009-2010 have been studied. The samples were collected along the river from the asphalt factory to the end of the mouth of the river in the Mediterranean Sea. Results showed that concentrations of natural radioactive isotopes have been increased slightly in water and sediments of the river after the asphalt factory and after the factories area, while the concentrations of Rn in the river's water were low along the river except the waters of October 16, Lake Dam that reached a value of 341 mBq/l. These high concentrations in water and sediments of the AL-Kabir AL-Shimali River were due to discharges from the asphalt factory and other factories known to contain natural radioactive isotopes, indicating the possibility of using these isotopes in the determination of pollution sources of AL-Kabir AL-Shimali River. However, the measured concentrations are relatively low compared to the values reported in the world due to river water flow that dilute concentrations of these elements. On the other hand, measurements of trace elements (Cu,Zn,Pb,Cd) showed low concentrations in the waters of the river, with some increases in the concentrations in river sediments after the asphalt factory and the factories area , indicating the contribution of the factories outlets in this increase. The results were compared with the results of previous studies conducted on the Euphrates and the Orontes, where the comparison showed lower values in the AL-Kabir AL-Shimali river environment. (author)

  19. The use of natural radioactive isotopes in the determination of pollution sources of Al-Kabir Al-Shimali river

    International Nuclear Information System (INIS)

    ALmasri, M.; Shweikani, R.; Mamish, S.; Al-Haleem, M.A.; Al-Shamali, K.; Jerby, B.

    2010-10-01

    In the present research, variations of concentration levels of some natural radioactive isotopes ( 226 Ra, 210 Po, 210 Pb, U and Th isotopes) and some trace elements (Cu, Zn, Pb, Cd) in water and sediments of Al-Kabir Al-Shimali river during the period of 2009-2010 have been studied. The samples were collected along the river from the asphalt factory to the end of the mouth of the river in the Mediterranean Sea. Results showed that concentrations of natural radioactive isotopes have been increased slightly in water and sediments of the river after the asphalt factory and after the factories area, while the concentrations of Rn in the river's water were low along the river except the waters of October 16, Lake Dam that reached a value of 341mBq/l. These high concentrations in water and sediments of the Al-Kabir Al-Shimali River were due to discharges from the asphalt factory and other factories known to contain natural radioactive isotopes, indicating the possibility of using these isotopes in the determination of pollution sources of Al-Kabir Al-Shimali River. However, the measured concentrations are relatively low compared to the values reported in the world due to river water flow that dilute concentrations of these elements. On the other hand, measurements of trace elements (Cu,Zn,Pb,Cd) showed low concentrations in the waters of the river, with some increases in the concentrations in river sediments after the asphalt factory and the factories area , indicating the contribution of the factories outlets in this increase. The results were compared with the results of previous studies conducted on the Euphrates and the Orontes, where the comparison showed lower values in the Al-Kabir Al-Shimali river environment.(author)

  20. Determination of dissolved inorganic carbon (DIC) and dissolved organic carbon (DOC) in freshwaters by sequential injection spectrophotometry with on-line UV photo-oxidation

    International Nuclear Information System (INIS)

    Tue-Ngeun, Orawan; Sandford, Richard C.; Jakmunee, Jaroon; Grudpan, Kate; McKelvie, Ian D.; Worsfold, Paul J.

    2005-01-01

    An automated sequential injection (SI) method for the determination of dissolved inorganic carbon (DIC) and dissolved organic carbon (DOC) in freshwaters is presented. For DIC measurement on-line sample acidification (sulphuric acid, pH 2 which subsequently diffused through a PTFE membrane into a basic, cresol red acceptor stream. The CO 2 increased the concentration of the acidic form of the cresol red indicator, with a resultant decrease in absorbance at 570 nm being directly proportional to DIC concentration. DIC + DOC was determined after on-line sample irradiation (15 W low power UV lamp) coupled with acid-peroxydisulfate digestion, with the subsequent detection of CO 2 as described above. DOC was determined by subtraction of DIC from (DIC + DOC). Analytical figures of merit were linear ranges of 0.05-5.0 mg C L -1 for both DIC and DIC + DOC, with typical R.S.D.s of less than 7% (0.05 mg C L -1 -5.3% for DIC and 6.6% for DIC + DOC; 4.0 mg C L -1 -2.6% for DIC and 2.4% for DIC + DOC, n = 3) and an LOD (blank + 3S.D.) of 0.05 mg C L -1 . Sample throughput for the automated system was 8 h -1 for DIC and DOC with low reagent consumption (acid/peroxydisulfate 200 μL per DIC + DOC analysis). A range of model carbon compounds and Tamar River (Plymouth, UK) samples were analysed for DIC and DOC and the results showed good agreement with a high temperature catalytic oxidation (HTCO) reference method (t-test, P = 0.05)

  1. Determination of dissolved inorganic carbon (DIC) and dissolved organic carbon (DOC) in freshwaters by sequential injection spectrophotometry with on-line UV photo-oxidation

    Energy Technology Data Exchange (ETDEWEB)

    Tue-Ngeun, Orawan [Department of Chemistry, Faculty of Science, Chiang Mai University, Chiang Mai 50200 (Thailand); Sandford, Richard C. [School of Earth, Ocean and Environmental Sciences, University of Plymouth, Drakes Circus, Plymouth PL4 8AA (United Kingdom)]. E-mail: rsandford@plymouth.ac.uk; Jakmunee, Jaroon [Department of Chemistry, Faculty of Science, Chiang Mai University, Chiang Mai 50200 (Thailand); Grudpan, Kate [Department of Chemistry, Faculty of Science, Chiang Mai University, Chiang Mai 50200 (Thailand); McKelvie, Ian D. [Water Studies Centre, School of Chemistry, Monash University, P.O. Box 23, Clayton Campus, Vic. 3800 (Australia); Worsfold, Paul J. [School of Earth, Ocean and Environmental Sciences, University of Plymouth, Drakes Circus, Plymouth PL4 8AA (United Kingdom)

    2005-12-04

    An automated sequential injection (SI) method for the determination of dissolved inorganic carbon (DIC) and dissolved organic carbon (DOC) in freshwaters is presented. For DIC measurement on-line sample acidification (sulphuric acid, pH < 2), converted DIC to CO{sub 2} which subsequently diffused through a PTFE membrane into a basic, cresol red acceptor stream. The CO{sub 2} increased the concentration of the acidic form of the cresol red indicator, with a resultant decrease in absorbance at 570 nm being directly proportional to DIC concentration. DIC + DOC was determined after on-line sample irradiation (15 W low power UV lamp) coupled with acid-peroxydisulfate digestion, with the subsequent detection of CO{sub 2} as described above. DOC was determined by subtraction of DIC from (DIC + DOC). Analytical figures of merit were linear ranges of 0.05-5.0 mg C L{sup -1} for both DIC and DIC + DOC, with typical R.S.D.s of less than 7% (0.05 mg C L{sup -1}-5.3% for DIC and 6.6% for DIC + DOC; 4.0 mg C L{sup -1}-2.6% for DIC and 2.4% for DIC + DOC, n = 3) and an LOD (blank + 3S.D.) of 0.05 mg C L{sup -1}. Sample throughput for the automated system was 8 h{sup -1} for DIC and DOC with low reagent consumption (acid/peroxydisulfate 200 {mu}L per DIC + DOC analysis). A range of model carbon compounds and Tamar River (Plymouth, UK) samples were analysed for DIC and DOC and the results showed good agreement with a high temperature catalytic oxidation (HTCO) reference method (t-test, P = 0.05)

  2. On-line dynamic fractionation and automatic determination of inorganic phosphorous in environmental solid substrates exploiting sequential injection microcolumn extraction and flow injection analysi

    DEFF Research Database (Denmark)

    Buanuam, Janya; Miró, Manuel; Hansen, Elo Harald

    2006-01-01

    Sequential injection microcolumn extraction (SI-MCE) based on the implementation of a soil containing microcartridge as external reactor in a sequential injection network is, for the first time, proposed for dynamic fractionation of macronutrients in environmental solids, as exemplified by the pa......Sequential injection microcolumn extraction (SI-MCE) based on the implementation of a soil containing microcartridge as external reactor in a sequential injection network is, for the first time, proposed for dynamic fractionation of macronutrients in environmental solids, as exemplified...... by the partitioning of inorganic phosphorous in agricultural soils. The on-line fractionation method capitalises on the accurate metering and sequential exposure of the various extractants to the solid sample by application of programmable flow as precisely coordinated by a syringe pump. Three different soil phase...... associations for phosphorus, that is, exchangeable, Al- and Fe-bound and Ca-bound fractions, were elucidated by accommodation in the flow manifold of the 3 steps of the Hietjles-Litjkema (HL) scheme involving the use of 1.0 M NH4Cl, 0.1 M NaOH and 0.5 M HCl, respectively, as sequential leaching reagents...

  3. Power of isotopic fine structure for unambiguous determination of metabolite elemental compositions: In silico evaluation and metabolomic application

    International Nuclear Information System (INIS)

    Nagao, Tatsuhiko; Yukihira, Daichi; Fujimura, Yoshinori; Saito, Kazunori; Takahashi, Katsutoshi; Miura, Daisuke; Wariishi, Hiroyuki

    2014-01-01

    Graphical abstract: - Highlights: • We developed a method to determine elemental composition of metabolites. • The method was based on mass spectral data and empirical constraints. • In the validation study, the method succeeded for 70% of detected peaks. - Abstract: In mass spectrometry (MS)-based metabolomics studies, reference-free identification of metabolites is still a challenging issue. Previously, we demonstrated that the elemental composition (EC) of metabolites could be unambiguously determined using isotopic fine structure, observed by ultrahigh resolution MS, which provided the relative isotopic abundance (RIA) of 13 C, 15 N, 18 O, and 34 S. Herein, we evaluated the efficacy of the RIA for determining ECs based on the MS peaks of 20,258 known metabolites. The metabolites were simulated with a ≤25% error in the isotopic peak area to investigate how the error size effect affected the rate of unambiguous determination of the ECs. The simulation indicated that, in combination with reported constraint rules, the RIA led to unambiguous determination of the ECs for more than 90% of the tested metabolites. It was noteworthy that, in positive ion mode, the process could distinguish alkali metal-adduct ions ([M + Na] + and [M + K] + ). However, a significant degradation of the EC determination performance was observed when the method was applied to real metabolomic data (mouse liver extracts analyzed by infusion ESI), because of the influence of noise and bias on the RIA. To achieve ideal performance, as indicated in the simulation, we developed an additional method to compensate for bias on the measured ion intensities. The method improved the performance of the calculation, permitting determination of ECs for 72% of the observed peaks. The proposed method is considered a useful starting point for high-throughput identification of metabolites in metabolomic research

  4. Determination of 239Pu/240Pu isotopic ratio by high resolution alpha-particle spectrometry

    International Nuclear Information System (INIS)

    Amoudry, F.; Burger, P.

    1983-05-01

    The development of passivated ion-implanted silicon detectors and of very thin alpha-particle sources improves the resolution of alpha-particle spectra and allows to separate energy pics up to now unseparate. The 239 Pu/ 240 Pu isotopic ratio of a mixture has been measured using the alpha spectrometry deconvolution code DEMO [fr

  5. Isotopic dependence of the fragments' internal temperatures determined from multifragment emission

    Science.gov (United States)

    Souza, S. R.; Donangelo, R.

    2018-05-01

    The internal temperatures of fragments produced by an excited nuclear source are investigated by using the microcanonical version of the statistical multifragmentation model, with discrete energy. We focus on the fragments' properties at the breakup stage, before they have time to deexcite by particle emission. Since the adopted model provides the excitation energy distribution of these primordial fragments, it allows one to calculate the temperatures of different isotope families and to make inferences about the sensitivity to their isospin composition. It is found that, due to the functional form of the nuclear density of states and the excitation energy distribution of the fragments, proton-rich isotopes are hotter than neutron-rich isotopes. This property has been taken to be an indication of earlier emission of the former from a source that cools down as it expands and emits fragments. Although this scenario is incompatible with the prompt breakup of a thermally equilibrated source, our results reveal that the latter framework also provides the same qualitative features just mentioned. Therefore they suggest that this property cannot be taken as evidence for nonequilibrium emission. We also found that this sensitivity to the isotopic composition of the fragments depends on the isospin composition of the source, and that it is weakened as the excitation energy of the source increases.

  6. Determination of the separation factor of uranium isotopes by gaseous diffusion

    International Nuclear Information System (INIS)

    Bilous, O.; Counas, G.

    1958-01-01

    A 12-stage pilot separation cascade with a low output has been constructed to measure the separation factor of uranium isotopes by gaseous diffusion. The report describes some of the separation results obtained, and also provides information on the time necessary for equilibrium to be established and on the influence of various perturbations on the pressure profile in the cascade. (author) [fr

  7. 99 Tc NMR determination of the oxygen isotope content in 18 O-enriched water.

    Science.gov (United States)

    Tarasov, Valerii P; Kirakosyan, Gayana А; German, Konstantin E

    2018-03-01

    99 Tc NMR has been suggested as an original method of evaluating the content of oxygen isotopes in oxygen-18-enriched water, a precursor for the production of radioisotope fluorine-18 used in positron emission tomography. To this end, solutions of NH 4 TcO 4 or NaTcO 4 (up to 0.28 mol/L) with natural abundance of oxygen isotopes in virgin or recycled 18 O-enriched water have been studied by 99 Tc NMR. The method is based on 16 O/ 17 O/ 18 O intrinsic isotope effects in the 99 Tc NMR chemical shifts, and the statistical distribution of oxygen isotopes in the coordination sphere of TcO 4 - and makes it possible to quantify the composition of enriched water by measuring the relative intensities of the 99 Tc NMR signals of the Tc 16 O 4-n 18 O n - isotopologues. Because the oxygen exchange between TcO 4 - and enriched water in neutral and alkaline solutions is characterized by slow kinetics, gaseous HCl was bubbled through a solution for a few seconds to achieve the equilibrium distribution of oxygen isotopes in the Tc coordination sphere without distortion of the oxygen composition of the water. Pertechnetate ion was selected as a probe due to its high stability in solutions and the significant 99 Tc NMR shift induced by a single 16 O→ 18 O substitution (-0.43 ± 0.01 ppm) in TcO 4 - and spin coupling constant 1 J( 99 Tc- 17 O) (131.46 Hz) favourable for the observation of individual signals of Tc 16 O 4-n 18 O n - isotopologues. Copyright © 2017 John Wiley & Sons, Ltd.

  8. Direct determination of halogens in powdered geological and environmental samples using isotope dilution laser ablation ICP-MS

    Science.gov (United States)

    Boulyga, Sergei F.; Heumann, Klaus G.

    2005-04-01

    Laser ablation inductively coupled plasma isotope dilution mass spectrometry (LA-ICP-IDMS) with a special laser ablation system for bulk analyses (LINA-Spark(TM)-Atomiser) was applied for direct determinations of chlorine, bromine, and iodine in rock and sediment samples. Special attention was focused on possible inter-halogen fractionations and analyte/spike isotope fractionations by using LA-ICP-MS and LA-ICP-IDMS, respectively. A variation of Br/Cl and I/Cl element intensity ratios by a factor of 1.3-3 was observed when changing the nebulizer gas flow rate in the range of 0.84-1.0 L min-1 and the laser power density in the range of 2-10 GW cm-2, respectively. When using an internal standard for halogen quantification in LA-ICP-MS, this inter-element fractionation can cause systematic errors, which can be avoided by applying the isotope dilution technique. However, at high laser power densities (>5.7 GW cm-2 for iodine and >4.0 GW cm-2 for bromine and chlorine) the corresponding measured isotope ratio of the isotope-diluted sample deviates significantly from the target value. Under optimised conditions concentrations in the range of 30 [mu]g g-1-16 × 103 [mu]g g-1 for chlorine, <2-140 [mu]g g-1 for bromine, and <0.1-31 [mu]g g-1 for iodine were determined by LA-ICP-IDMS in two sediment reference materials (SRM 1646, SRM 2704) and three rock reference samples (GS-N, Granite; BX-N, Bauxite; DT-N, Disthene), which have not been certified for these halogens. The sediment results agree well within the given uncertainties with indicative values by different methods and the results of the rock samples with those obtained by negative thermal ionisation isotope dilution mass spectrometry. The detection limits of LA-ICP-IDMS are 8 [mu]g g-1 for chlorine, 1.7 [mu]g g-1 for bromine, and 0.1 [mu]g g-1 for iodine.

  9. Isotope dilution alpha spectrometry for the determination of plutonium concentration in irradiated fuel dissolver solution : IDAS and R-IDAS

    International Nuclear Information System (INIS)

    Ramaniah, M.V.; Jain, H.C.; Aggarwal, S.K.; Chitambar, S.A.; Kavimandan, V.D.; Almaula, A.I.; Shah, P.M.; Parab, A.R.; Sant, V.L.

    1980-01-01

    The report presents a new technique, Isotope Dilution Alpha Spectrometry (IDAS) and Reverse Isotope Dilution Alpha Spectrometry (R-IDAS) for determining the concentration of plutonium in the irradiated fuel dissolver solution. The method exploits sup(238)Pu in IDAS and sup(239)Pu in R-IDAS as a spike and provides an alternative method to Isotope Dilution Mass Spectrometry (IDMS) which requires enriched sup(242)Pu as a spike. Depending upon the burn-up of the fuel, sup(238)Pu or sup(239)Pu is used as a spike to change the sup(238)Pu/(sup(239)Pu+sup(240)Pu)α activity ratio in the sample by a factor of 10. This change is determined by α-spectrometry on electrodeposited sources using a solid state silicon surface barrier detector coupled to a multichannel analyser. The validity of a simple method based on the geometric progression (G.P.) decrease for the far tail of the spectrum to correct for the tail contribution of sup(238)Pu peak (5.50 MeV) to the low energy sup(239)Pu + sup(240)Pu peak (5.17 MeV) is established. Results for the plutonium concentration on different irradiated fuel dissolver solutions with burn-uo ranging from J,000 to 100,000 MWD/TU are presented and compared with those obtained by IDMS. The values obtained by IDAS or R-IDAS and IDMS agree within 0.5%. (auth.)

  10. Determination of Cd and Pb in human blood by isotope dilution inductively coupled plasma mass spectrometry : International comparison

    International Nuclear Information System (INIS)

    Park, Chang Joon; Suh, Jeong Ki; Lee, Sang Hwa

    1996-01-01

    Inorganic analytical laboratory of Korea Research Institute of Standards and Science participated in an interlaboratory comparison program operated by Quebec Toxicology Centre of Canada in 1994 and again in 1995. The objective of this program is to enable participating laboratories to assess reproducibility and accuracy of their analytical results for trace toxic elements in human biological fluids. This laboratory determined Cd and Pb concentrations in 3 levels of human blood samples by isotope dilution inductively coupled plasma mass spectrometry. 0.5 mL of blood sample is added to the digestion bomb together with 2 mL of nitric acid and enriched spike isotopes and then decomposed in the microwave digestion system. The decomposed sample is diluted to 10 mL and nebulized into ICP-MS. The Cd and Pb values reported by all participating laboratories are presented and compared. The values reported by this laboratory are within the acceptable range of target values. (author)

  11. Determination of trace heavy metals in herbs by sequential injection analysis-anodic stripping voltammetry using screen-printed carbon nanotubes electrodes

    International Nuclear Information System (INIS)

    Injang, Uthaitip; Noyrod, Peeyanun; Siangproh, Weena; Dungchai, Wijitar; Motomizu, Shoji; Chailapakul, Orawon

    2010-01-01

    A method for the simultaneous determination of Pb(II), Cd(II), and Zn(II) at low μg L -1 concentration levels by sequential injection analysis-anodic stripping voltammetry (SIA-ASV) using screen-printed carbon nanotubes electrodes (SPCNTE) was developed. A bismuth film was prepared by in situ plating of bismuth on the screen-printed carbon nanotubes electrode. Operational parameters such as ratio of carbon nanotubes to carbon ink, bismuth concentration, deposition time and flow rate during preconcentration step were optimized. Under the optimal conditions, the linear ranges were found to be 2-100 μg L -1 for Pb(II) and Cd(II), and 12-100 μg L -1 for Zn(II). The limits of detection (S bl /S = 3) were 0.2 μg L -1 for Pb(II), 0.8 μg L -1 for Cd(II) and 11 μg L -1 for Zn(II). The measurement frequency was found to be 10-15 stripping cycle h -1 . The present method offers high sensitivity and high throughput for on-line monitoring of trace heavy metals. The practical utility of our method was also demonstrated with the determination of Pb(II), Cd(II), and Zn(II) by spiking procedure in herb samples. Our methodology produced results that were correlated with ICP-AES data. Therefore, we propose a method that can be used for the automatic and sensitive evaluation of heavy metals contaminated in herb items.

  12. The metabolic network of Clostridium acetobutylicum: Comparison of the approximate Bayesian computation via sequential Monte Carlo (ABC-SMC) and profile likelihood estimation (PLE) methods for determinability analysis.

    Science.gov (United States)

    Thorn, Graeme J; King, John R

    2016-01-01

    The Gram-positive bacterium Clostridium acetobutylicum is an anaerobic endospore-forming species which produces acetone, butanol and ethanol via the acetone-butanol (AB) fermentation process, leading to biofuels including butanol. In previous work we looked to estimate the parameters in an ordinary differential equation model of the glucose metabolism network using data from pH-controlled continuous culture experiments. Here we combine two approaches, namely the approximate Bayesian computation via an existing sequential Monte Carlo (ABC-SMC) method (to compute credible intervals for the parameters), and the profile likelihood estimation (PLE) (to improve the calculation of confidence intervals for the same parameters), the parameters in both cases being derived from experimental data from forward shift experiments. We also apply the ABC-SMC method to investigate which of the models introduced previously (one non-sporulation and four sporulation models) have the greatest strength of evidence. We find that the joint approximate posterior distribution of the parameters determines the same parameters as previously, including all of the basal and increased enzyme production rates and enzyme reaction activity parameters, as well as the Michaelis-Menten kinetic parameters for glucose ingestion, while other parameters are not as well-determined, particularly those connected with the internal metabolites acetyl-CoA, acetoacetyl-CoA and butyryl-CoA. We also find that the approximate posterior is strongly non-Gaussian, indicating that our previous assumption of elliptical contours of the distribution is not valid, which has the effect of reducing the numbers of pairs of parameters that are (linearly) correlated with each other. Calculations of confidence intervals using the PLE method back this up. Finally, we find that all five of our models are equally likely, given the data available at present. Copyright © 2015 Elsevier Inc. All rights reserved.

  13. Determination of platinum-group elements in the geological standard reference materials by isotope dilution-ICPMS

    Energy Technology Data Exchange (ETDEWEB)

    Mingyue, Hu; Hongliao, He [National Research Center for Geoanalysis, Beijing (China)

    2005-10-15

    Platinum group elements (PGEs) includes platinum, palladium, iridium, osmium, rhodium and ruthenium. It has very high economic and scientific value in the field of geoscience and environmental science. But the analysis data referred by the different lab are very disperse because of the difficulty of the determination of PGEs. It makes very difficult to fix the value of the PGEs in the standard reference materials. In the article, the values of the PGEs in the standard reference materials of ocean sediment are determined by isotope dilution technique and dependable values of these elements are provided. (authors)

  14. Determination of platinum-group elements in the geological standard reference materials by isotope dilution-ICPMS

    International Nuclear Information System (INIS)

    Hu Mingyue; He Hongliao

    2005-01-01

    Platinum group elements (PGEs) includes platinum, palladium, iridium, osmium, rhodium and ruthenium. It has very high economic and scientific value in the field of geoscience and environmental science. But the analysis data referred by the different lab are very disperse because of the difficulty of the determination of PGEs. It makes very difficult to fix the value of the PGEs in the standard reference materials. In the article, the values of the PGEs in the standard reference materials of ocean sediment are determined by isotope dilution technique and dependable values of these elements are provided. (authors)

  15. Determination of the residence time of rain water in some hydrographic basins by means of stable isotopes

    International Nuclear Information System (INIS)

    Goncalves, A.R.L.

    1979-10-01

    Samples of rain-and river water, monthly collected during one year from ten stations of the Amazon basin analysed in their 18 O and D content. The residence time of rain water for each station was determined using the values of Δ 18 O(%o) and ΔD(%). The values of Δ 18 O(%o) were correlated with the precipitation ones (mm) in order to determine the occurence of 'amount effect' in the stations. An analysis of samples was done along the Amazon River for simple observation of the 'isotopic fractionation' phenomenon the values of Δ 18 O(%o). (Author) [pt

  16. Application of PCA-LDA method to determine the geographical origin of tea based on determination of stable isotopes and multi-elements

    International Nuclear Information System (INIS)

    Yuan Yuwei; Zhang Yongzhi; Yang Guiling; Zhang Zhiheng; Fu Haiyan; Han Wenyan; Li Shufang

    2013-01-01

    The ratio of stable isotope and concentration of multi-element in tea was determinated with isotope ratio mass spectrometry (IRMS) and inductively coupled plasma mass spectrometry (ICP-MS). Pattern recognition techniques with principal component analysis (PCA) and linear discriminant analysis (LDA) were used to classify the geographical origins of tea from Fujian, Shandong and Zhejiang province, and Yuyao, Jinhua and Xihu region of Zhejiang. The results showed the values of δ"1"5N, δ"1"3C, δD, δ"1"8O and the ratios of "2"0"6Pb/"2"0"7Pb, "2"0"8Pb/"2"0"6Pb and "8"7Sr/"8"6Sr in tea samples were different from different origins. There was also large variable for the concentrations of 27 mineral elements, such as Li, Be, Na and so on, with a specific character of origin. The method of PCA could be used to classify the geographical origin of tea from different origins but with a cross in the scatter plot. However, PCA combining with LDA could gave correct assignation percentages of 99% for the tea samples among Fujian, Shandong and Zhejiang provinces, and 87% for the tea samples among Yuyao, Jinhua and Xihu region of Zhejiang. These results revealed that it was possible and feasible to classify the geographical origin of tea by the method of PCA-LDA based on the determination of isotopes and multi-elements. (authors)

  17. New determination of the vapour pressures of the isotopes of neon; Nouvelles determinations des tensions de vapeur des isotopes du neon

    Energy Technology Data Exchange (ETDEWEB)

    Roth, R [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

    1960-03-15

    We have undertaken an experimental reinvestigation of the vapor pressures of the neon isotopes over the temperature range 16.30-30.1 deg. K. Measurements were made by differential manometry in a Giauque-Johnston type cryostat modified for temperature stability. The New sample contained 99.9 % Ne{sup 20} and the Ne{sup 22} sample contained 72,2 % Ne{sup 22}. Extrapolation to pure Ne{sup 20} and Ne{sup 22} can be made with sufficient accuracy by the use of Raoult's law. Our results are in substantial agreement with those of Keesom and Haantjes. At 20 deg. K, where the scatter in our data is an order of magnitude smaller than in the data of Keesom and Haantjes, we find In P{sub Ne{sup 2}{sup 0}}/P{sub Ne{sup 2}{sup 2}} is 6 % larger than the smoothed line given by them. For solid neon, our data can be represented to a high accuracy by a Debye harmonic lattice with {theta}{sub D} (Ne{sup 20}) = 74.6 deg. K. The result may be compared with the value obtained by Henshaw from the Debye-Waller temperature factor, {theta}{sub D} = 73 deg. K, and with the recent calculation of the zero point energy of Ne by Bernardes, from which he obtains {theta}{sub D} 8E{sub {theta}}/9R = 73 deg.. K. (author) [French] On a construit un appareillage dont le principe est derive de celui des instruments decrits par GIAUQUE et EGAN ou par H.L. JOHNSTON qui a permis d'etendre le domaine des mesures de tension de vapeur des isotopes du Neon entre 16,30 et 32 deg. K environ. Le rapport des pressions extremes atteintes est ainsi multiplie par plus de 40 pour le neon ordinaire qui servait de reference et de thermometre. L'appareil, adapte en particulier au travail sous pressions elevees, permet, de plus, de travailler sur de relativement petites quantites totales de gaz - environ 500 cm{sup 3} suffisent dans l'intervalle de pression evoque. La stabilite de temperature obtenue peut etre tres bonne surtout lorsque l'on travaille dans la phase liquide; dans ce cas, les variations totales de

  18. New determination of the vapour pressures of the isotopes of neon; Nouvelles determinations des tensions de vapeur des isotopes du neon

    Energy Technology Data Exchange (ETDEWEB)

    Roth, R. [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

    1960-03-15

    We have undertaken an experimental reinvestigation of the vapor pressures of the neon isotopes over the temperature range 16.30-30.1 deg. K. Measurements were made by differential manometry in a Giauque-Johnston type cryostat modified for temperature stability. The New sample contained 99.9 % Ne{sup 20} and the Ne{sup 22} sample contained 72,2 % Ne{sup 22}. Extrapolation to pure Ne{sup 20} and Ne{sup 22} can be made with sufficient accuracy by the use of Raoult's law. Our results are in substantial agreement with those of Keesom and Haantjes. At 20 deg. K, where the scatter in our data is an order of magnitude smaller than in the data of Keesom and Haantjes, we find In P{sub Ne{sup 2}{sup 0}}/P{sub Ne{sup 2}{sup 2}} is 6 % larger than the smoothed line given by them. For solid neon, our data can be represented to a high accuracy by a Debye harmonic lattice with {theta}{sub D} (Ne{sup 20}) = 74.6 deg. K. The result may be compared with the value obtained by Henshaw from the Debye-Waller temperature factor, {theta}{sub D} = 73 deg. K, and with the recent calculation of the zero point energy of Ne by Bernardes, from which he obtains {theta}{sub D} 8E{sub {theta}}/9R = 73 deg.. K. (author) [French] On a construit un appareillage dont le principe est derive de celui des instruments decrits par GIAUQUE et EGAN ou par H.L. JOHNSTON qui a permis d'etendre le domaine des mesures de tension de vapeur des isotopes du Neon entre 16,30 et 32 deg. K environ. Le rapport des pressions extremes atteintes est ainsi multiplie par plus de 40 pour le neon ordinaire qui servait de reference et de thermometre. L'appareil, adapte en particulier au travail sous pressions elevees, permet, de plus, de travailler sur de relativement petites quantites totales de gaz - environ 500 cm{sup 3} suffisent dans l'intervalle de pression evoque. La stabilite de temperature obtenue peut etre tres bonne surtout lorsque l'on travaille dans la phase liquide; dans ce cas, les

  19. Selective isotope determination of lanthanum by diode-laser-initiated resonance-ionization mass spectrometry

    International Nuclear Information System (INIS)

    Young, J.P.; Shaw, R.W.

    1995-01-01

    A diode-laser step has been incorporated into a resonance-ionization mass spectrometry optical excitation process to enhance the isotopic selectivity of the technique. Lanthanum isotope ratio enhancements as high as 10 3 were achieved by use of a single-frequency cw diode laser tuned to excite the first step of a three-step excitation--ionization optical process; the subsequent steps were excited by use of a pulsed dye laser. Applying the same optical technique, we measured atomic hyperfine constants for the high-lying even-parity 4 D 5/2 state of lanthanum at 30 354 cm --1 . The general utility of this spectral approach is discussed

  20. Determination of total uranium by mass spectrometry utilizing the isotopic dilution technique

    International Nuclear Information System (INIS)

    Cretella, R.F.; Noutary, C.J.; Servant, R.E.

    1981-01-01

    The isotopic dilution associated to mass spectrometry is a high-sensitivity technique that allows to work with microquantities of the sample, making it possible to analize the content in highly radioactive solutions with excellent accuracy and minimum risk. The proposed technique is described and its results are discussed through the analysis of: 1) A synthetic sample that simulates dissolved spent fuel elements; 2) Uranium dioxide of nuclear purity and 3) Uranium concentrate. 233 U(ORNL) was employed as a tracer and a Nuclide 12-90-SU mass spectrometer of simple magnetic focus as measurement instrument. The accuracy reached in the analyses is better than 0.5% with a reliability of 95%. The analysis of the errors shows that their main contributing source are the errors in the measurement of the isotopic ratios. (M.E.L.) [es

  1. Reverse isotope dilution method for determining benzene and metabolites in tissues

    International Nuclear Information System (INIS)

    Bechtold, W.E.; Sabourin, P.J.; Henderson, R.F.

    1988-01-01

    A method utilizing reverse isotope dilution for the analysis of benzene and its organic soluble metabolites in tissues of rats and mice is presented. Tissues from rats and mice that had been exposed to radiolabeled benzene were extracted with ethyl acetate containing known, excess quantities of unlabeled benzene and metabolites. Butylated hydroxytoluene was added as an antioxidant. The ethyl acetate extracts were analyzed with semipreparative reversed-phase HPLC. Isolated peaks were collected and analyzed for radioactivity (by liquid scintillation spectrometry) and for mass (by UV absorption). The total amount of each compound present was calculated from the mass dilution of the radiolabeled isotope. This method has the advantages of high sensitivity, because of the high specific activity of benzene, and relative stability of the analyses, because of the addition of large amounts of unlabeled carrier analogue

  2. Method for determination of stable carbon isotope ratio of methylnitrophenols in atmospheric particulate matter

    Directory of Open Access Journals (Sweden)

    S. Moukhtar

    2011-11-01

    Full Text Available A technique for the measurement of the stable isotope ratio of methylnitrophenols in atmospheric particulate matter is presented. Atmospheric samples from rural and suburban areas were collected for evaluation of the procedure. Particulate matter was collected on quartz fibre filters using dichotomous high volume air samplers. Methylnitrophenols were extracted from the filters using acetonitrile. The sample was then purified using a combination of high-performance liquid chromatography and solid phase extraction. The final solution was then divided into two aliquots. To one aliquot, a derivatising agent, Bis(trimethylsilyltrifluoroacetamide, was added for Gas Chromatography-Mass Spectrometry analysis. The second half of the sample was stored in a refrigerator. For samples with concentrations exceeding 1 ng μl−1, the second half of the sample was used for measurement of stable carbon isotope ratios by Gas Chromatography-Isotope Ratio Mass Spectrometry.

    The procedure described in this paper provides a method for the analysis of methylnitrophenols in atmospheric particulate matter at concentrations as low as 0.3 pg m−3 and for stable isotope ratios with an accuracy of better than ±0.5‰ for concentrations exceeding 100 pg m−3.

    In all atmospheric particulate matter samples analysed, 2-methyl-4-nitrophenol was found to be the most abundant methylnitrophenol, with concentrations ranging from the low pg m−3 range in rural areas to more than 200 pg m−3 in some samples from a suburban location.

  3. An evaluation of water isotope collection for determining evapotranspiration in seasonal wetlands.

    Science.gov (United States)

    Bernier, T.; Root, T.

    2015-12-01

    The use of isotope hydrology has become a successful tool for water resource investigations. The complex task of defining interactions between groundwater, surface water, and atmospheric water vapor continue to remain a challenge. Evapotranspiration is still a dominant source of uncertainty for water resources management, especially in the face of climate change. The development of cavity ring-down spectroscopy has provided a valuable tool that makes it possible to quantify evaporation and transpiration using isotopic mass balance techniques. However, these techniques require collection of vapor at both the evaporation and transpiration fronts as well as directly above the canopy. Obtaining these representative samples is difficult. We are unaware of other attempts to use these techniques in seasonal swamps, such as the Florida Everglades, where collection of representative end members is complicated by seasonally inundated conditions. The purpose of the research presented here is to test different methods of collecting the necessary representative samples in variably inundated environments. Our tests are being conducting in a controlled setting to allow us to validate our isotope-derived estimates of evaporation and transpiration against conventional water balances. This paper will present the preliminary results of our first series of tests.

  4. Trophic structure of a coastal fish community determined with diet and stable isotope analyses.

    Science.gov (United States)

    Malek, A J; Collie, J S; Taylor, D L

    2016-09-01

    A combination of dietary guild analysis and nitrogen (δ(15) N) and carbon (δ(13) C) stable-isotope analysis was used to assess the trophic structure of the fish community in Rhode Island and Block Island Sounds, an area off southern New England identified for offshore wind energy development. In the autumn of 2009, 2010 and 2011, stomach and tissue samples were taken from 20 fish and invertebrate species for analysis of diet composition and δ(15) N and δ(13) C signatures. The food chain in Rhode Island and Block Island Sounds comprises approximately four trophic levels within which the fish community is divided into distinct dietary guilds, including planktivores, benthivores, crustacivores and piscivores. Within these guilds, inter-species isotopic and dietary overlap is high, suggesting that resource partitioning or competitive interactions play a major role in structuring the fish community. Carbon isotopes indicate that most fishes are supported by pelagic phytoplankton, although there is evidence that benthic production also plays a role, particularly for obligate benthivores such as skates Leucoraja spp. This type of analysis is useful for developing an ecosystem-based approach to management, as it identifies species that act as direct links to basal resources as well as species groups that share trophic roles. © 2016 The Fisheries Society of the British Isles.

  5. Development of a simplified methodology for the isotopic determination of fuel spent in Light Water Reactors

    International Nuclear Information System (INIS)

    Hernandez N, H.; Francois L, J.L.

    2005-01-01

    The present work presents a simplified methodology to quantify the isotopic content of the spent fuel of light water reactors; their application is it specific to the Laguna Verde Nucleo electric Central by means of a balance cycle of 18 months. The methodology is divided in two parts: the first one consists on the development of a model of a simplified cell, for the isotopic quantification of the irradiated fuel. With this model the burnt one is simulated 48,000 MWD/TU of the fuel in the core of the reactor, taking like base one fuel assemble type 10x10 and using a two-dimensional simulator for a fuel cell of a light water reactor (CPM-3). The second part of the methodology is based on the creation from an isotopic decay model through an algorithm in C++ (decay) to evaluate the amount, by decay of the radionuclides, after having been irradiated the fuel until the time in which the reprocessing is made. Finally the method used for the quantification of the kilograms of uranium and obtained plutonium of a normalized quantity (1000 kg) of fuel irradiated in a reactor is presented. These results will allow later on to make analysis of the final disposition of the irradiated fuel. (Author)

  6. Determination of phosphorus in urban sewage sludge using the isotopic exchange kinetics method

    International Nuclear Information System (INIS)

    Rojas de Tramontini, Susana; Barbaro, Nestor O.; Lopez, Silvia C.

    1999-01-01

    The aim of this work was to assess the differences among soil available P, the use by the plants of sludge P, and of a water soluble fertilizer (Ca(H 2 PO 4 ) 2 ) P, using isotopic exchange kinetics methods. The sludge was provided by the Sewage Sludge Treatment Plant of Tucuman City, Argentina. The isotopic exchange kinetics experiment, in which the fate of carrier free 32 PO 4 added to the soil solution at a steady state was studied, gives information on soil P exchangeability. The experiment was carried out in the laboratory, where sewage sludge and water soluble fertilizer were added to soil samples taken at a depth of 0-25 and 25-40 cm. Changes in the soil P isotopically exchangeable within 1 minute measurements in the soil with sludge and in the soil with water soluble fertilizer showed that the 0-25 cm deep soil samples had a low P sorption capacity (r1 /R values were low). The sludge had high total and organic P, but the P in the soil solution was lower than the P provided by the water soluble fertilizer. Therefore, despite its higher total P content, this sludge contained slow available forms of P

  7. Optimisation and application of ICP-MS and alpha-spectrometry for determination of isotopic ratios of depleted uranium and plutonium in samples collected in Kosovo

    OpenAIRE

    Boulyga, S. F.; Testa, C.; Desideri, D.; Becker, J. S.

    2001-01-01

    The determination of environmental contamination with natural and artificial actinide isotopes and evaluation of their source requires precise isotopic determination of actinides, above all uranium and plutonium. This can be achieved by alpha spectrometry or by inductively coupled plasma mass spectrometry (ICP-MS) after chemical separation of actinides. The performance of a sector-field ICP-MS (ICP-SFMS) coupled to a low-flow micronebulizer with a membrane desolvation unit, "Aridus'', was stu...

  8. Exploiting dynamic reaction cell inductively coupled plasma mass spectrometry (DRC-ICP-MS) for sequential determination of trace elements in blood using a dilute-and-shoot procedure

    International Nuclear Information System (INIS)

    Lemos Batista, Bruno; Lisboa Rodrigues, Jairo; Andrade Nunes, Juliana; Oliveira Souza, Vanessa Cristina de; Barbosa, Fernando

    2009-01-01

    Inductively coupled plasma mass spectrometry with quadrupole (q-ICP-MS) and dynamic reaction cell (DRC-ICP-MS) were evaluated for sequential determination of As, Cd, Co, Cr, Cu, Mn, Pb, Se, Tl, V and Zn in blood. The method requires as little as 100 μL of blood. Prior to analysis, samples (100 μL) were diluted 1:50 in a solution containing 0.01% (v/v) Triton X-100 and 0.5% (v/v) nitric acid. The use of the DRC was only mandatory for Cr, Cu, V and Zn. For the other elements the equipment may be operated in a standard mode (q-ICP-MS). Ammonia was used as reaction gas. Selection of best flow rate of ammonium gas and optimization of the quadrupole dynamic band-pass tuning parameter (RPq) were carried out, using a ovine base blood for Cr and V and a synthetic matrix solution (SMS) for Zn and Cu diluted 1:50 and spiked to contain 1 μg L -1 of each element. Method detection limits (3 s) for 75 As, 114 Cd, 59 Co, 51 Cr, 63 Cu 55 Mn, 208 Pb, 82 Se, 205 Tl, 51 V, and 64 Zn were 14.0, 3.0, 11.0, 7.0, 280, 9.0, 3.0, 264, 0.7, 6.0 and 800 ng L -1 , respectively. Method validation was accomplished by the analysis of blood Reference Materials produced by the L'Institut National de Sante Publique du Quebec (Canada).

  9. Sequential injection chromatography with post-column reaction/derivatization for the determination of transition metal cations in natural water samples.

    Science.gov (United States)

    Horstkotte, Burkhard; Jarošová, Patrícia; Chocholouš, Petr; Sklenářová, Hana; Solich, Petr

    2015-05-01

    In this work, the applicability of Sequential Injection Chromatography for the determination of transition metals in water is evaluated for the separation of copper(II), zinc(II), and iron(II) cations. Separations were performed using a Dionex IonPAC™ guard column (50mm×2mm i.d., 9 µm). Mobile phase composition and post-column reaction were optimized by modified SIMPLEX method with subsequent study of the concentration of each component. The mobile phase consisted of 2,6-pyridinedicarboxylic acid as analyte-selective compound, sodium sulfate, and formic acid/sodium formate buffer. Post-column addition of 4-(2-pyridylazo)resorcinol was carried out for spectrophotometric detection of the analytes׳ complexes at 530nm. Approaches to achieve higher robustness, baseline stability, and detection sensitivity by on-column stacking of the analytes and initial gradient implementation as well as air-cushion pressure damping for post-column reagent addition were studied. The method allowed the rapid separation of copper(II), zinc(II), and iron(II) within 6.5min including pump refilling and aspiration of sample and 1mmol HNO3 for analyte stacking on the separation column. High sensitivity was achieved applying an injection volume of up to 90µL. A signal repeatability of<2% RSD of peak height was found. Analyte recovery evaluated by spiking of different natural water samples was well suited for routine analysis with sub-micromolar limits of detection. Copyright © 2015 Elsevier B.V. All rights reserved.

  10. Sequential determination of fat- and water-soluble vitamins in Rhodiola imbricata root from trans-Himalaya with rapid resolution liquid chromatography/tandem mass spectrometry.

    Science.gov (United States)

    Tayade, Amol B; Dhar, Priyanka; Kumar, Jatinder; Sharma, Manu; Chaurasia, Om P; Srivastava, Ravi B

    2013-07-30

    A rapid method was developed to determine both types of vitamins in Rhodiola imbricata root for the accurate quantification of free vitamin forms. Rapid resolution liquid chromatography/tandem mass spectrometry (RRLC-MS/MS) with electrospray ionization (ESI) source operating in multiple reactions monitoring (MRM) mode was optimized for the sequential analysis of nine water-soluble vitamins (B1, B2, two B3 vitamins, B5, B6, B7, B9, and B12) and six fat-soluble vitamins (A, E, D2, D3, K1, and K2). Both types of vitamins were separated by ion-suppression reversed-phase liquid chromatography with gradient elution within 30 min and detected in positive ion mode. Deviations in the intra- and inter-day precision were always below 0.6% and 0.3% for recoveries and retention time. Intra- and inter-day relative standard deviation (RSD) values of retention time for water- and fat-soluble vitamin were ranged between 0.02-0.20% and 0.01-0.15%, respectively. The mean recoveries were ranged between 88.95 and 107.07%. Sensitivity and specificity of this method allowed the limits of detection (LOD) and limits of quantitation (LOQ) of the analytes at ppb levels. The linear range was achieved for fat- and water-soluble vitamins at 100-1000 ppb and 10-100 ppb. Vitamin B-complex and vitamin E were detected as the principle vitamins in the root of this adaptogen which would be of great interest to develop novel foods from the Indian trans-Himalaya. Copyright © 2013 Elsevier B.V. All rights reserved.

  11. Fast determination of trace elements in organic fertilizers using a cup-horn reactor for ultrasound-assisted extraction and fast sequential flame atomic absorption spectrometry.

    Science.gov (United States)

    Teixeira, Leonel Silva; Vieira, Heulla Pereira; Windmöller, Cláudia Carvalhinho; Nascentes, Clésia Cristina

    2014-02-01

    A fast and accurate method based on ultrasound-assisted extraction in a cup-horn sonoreactor was developed to determine the total content of Cd, Co, Cr, Cu, Mn, Ni, Pb and Zn in organic fertilizers by fast sequential flame atomic absorption spectrometry (FS FAAS). Multivariate optimization was used to establish the optimal conditions for the extraction procedure. An aliquot containing approximately 120 mg of the sample was added to a 500 µL volume of an acid mixture (HNO3/HCl/HF, 5:3:3, v/v/v). After a few minutes, 500 µL of deionized water was added and eight samples were simultaneously sonicated for 10 min at 50% amplitude, allowing a sample throughput of 32 extractions per hour. The performance of the method was evaluated with a certified reference material of sewage sludge (CRM 029). The precision, expressed as the relative standard deviation, ranged from 0.58% to 5.6%. The recoveries of analytes were found to 100%, 109%, 96%, 92%, 101%, 104% and 102% for Cd, Cr, Cu, Mn, Ni, Pb and Zn, respectively. The linearity, limit of detection and limit of quantification were calculated and the values obtained were adequate for the quality control of organic fertilizers. The method was applied to the analysis of several commercial organic fertilizers and organic wastes used as fertilizers, and the results were compared with those obtained using the microwave digestion procedure. A good agreement was found between the results obtained by microwave and ultrasound procedures with recoveries ranging from 80.4% to 117%. Two organic waste samples were not in accordance with the Brazilian legislation regarding the acceptable levels of contaminants. © 2013 Published by Elsevier B.V.

  12. Determination of urea kinetics by isotope dilution with [C-13]urea and gas chromatography isotope ratio mass spectrometry (GC-IRMS) analysis

    NARCIS (Netherlands)

    Kloppenburg, Wybe; Wolthers, BG; Stellaard, F; Elzinga, H; Tepper, T; deJong, PE; Huisman, RM

    1. Stable urea isotopes can be used to study urea kinetics in humans, The use of stable urea isotopes far studying urea kinetic parameters in humans on a large scale is hampered by the high costs of the labelled material, We devised a urea dilution for measurement of the distribution volume,

  13. Determination of 240Pu/239Pu isotope ratios in Kara Sea and Novaya Zemlya sediments using accelerator mass spectrometry

    International Nuclear Information System (INIS)

    Oughton, D.H.; Skipperud, L.; Salbu, B.; Fifield, L.K.; Cresswell, R.C.; Day, J.P.

    1999-01-01

    Accelerator mass spectrometry (AMS) has been used to determine Pu activity concentrations and 240 Pu/ 239 Pu isotope ratios in sediments from the Kara Sea and radioactive waste dumping sites at Novaya Zemlya. Measured 239,240 Pu activities ranged from 0.06 - 9.8 Bq/kg dry weight, 240 Pu/ 239 Pu atom ratios ranged from 0.13 to 0.28, and 238 Pu/ 239,240 Pu activity ratios from 0.02 to 0.6. Perturbations from global fallout isotope ratios were evident at three sites: the Yenisey Estuary and Abrosimov Fjords where 240 Pu/ 239 Pu ratios were lower (0.13-0.14); and Stepovogo Fjord sediments where ratios were higher (up to 0.28) than fallout ratios. Based on procedural blanks, detection limits for AMS were below 1 fg Pu and the method showed good precision for isotope ratio measurements, minimal matrix, interference and memory effects. For high level samples, comparison between alpha spectrometry and AMS gave good agreement for measurement of 239,240 Pu activity concentrations. (author)

  14. Preliminary Study: Application of Off-Axis ICOS to Determine Stable Carbon Isotope in Dissolved Inorganic Carbon

    Science.gov (United States)

    Kim, Y. T.; Lee, J. M.; Hwang, J. H.; Piao, J.; Woo, N. C.

    2015-12-01

    CO2 is one of the major causes for global climate change. Because stable carbon isotope ratio is used to trace carbon source, several analytical techniques likes IRMS (Isotope Ratio Mass Spectrometry) and LAS (Laser Absorption Spectrometry) were extensively used. Off-axis ICOS, a kind of LAS, has merits on long-term stability and field application, therefore it is widely being used in CCS (Carbon Capture and Storage) field. The aim of this study is to extend the application scope of OA-ICOS to determine dissolved inorganic carbon (DIC). Because OA-ICOS showed dependence of δ13C on CO2 concentration, data processing is required. We tested CO2 Carbon Isotope Analyzer (CCIA-36-EP, Los Gatos Research) with both reference gas (δ13C= -28.28‰) and aqueous solutions prepared by dissolving sodium bicarbonate standards (δ13C= -12.26‰ and +3.96‰). The differences of δ13C between reference and measurement values are plotted by CO2 concentrations, then compared. At first, we checked the similarity between our curve pattern for reference gas and Guillon's research (δ13C= -43.99‰) by other Analyzer. To analyze aqueous samples, more errors can be caused than gas analysis. The carbon isotope fractionation occurs during dissolving standard reagents and extracting DIC as CO2 gas form. This effect is mixed with CO2 concentration dependence effect, therefore the curve patterns are different with that for reference gas. Our experiments are done for various δ13C values. It could be an important point to use OA-ICOS to analyze DIC, too.

  15. Determination of symbiotic nitrogen fixation by labelling the soil atmosphere with sup(15)N sub(2) at low isotope enrichment

    International Nuclear Information System (INIS)

    Trivelin, P.C.O.

    1982-01-01

    A direct method to determine the total symbiotic nitrogen fixation during the leguminous plants cycles has been, developed, by labelling the soil atmosphere with sup(15)N sub(2) at low isotope enrichment, of about 1 atom % excess. The soil explored by the root system of leguminous plants was confined by means of a chamber in the field and by sealed pots in greenhouse experiments in order to maintain the soil air labelled with sup(15)N sub(2). The average sup(15)N concentration in the soil atmosphere, necessary to calculate dinitrogen fixation, was obtained by integration of the exponential functions of isotope dilution. Those functions were obtained by periodic sampling and analysis of the N sub(2) in the soil atmosphere. The field experiment with labelled atmosphere was carried out from the 22 sup(nd) to the 31 sup(st) day of the bean crop cycle and 5.5 mg N/plant (24% of total plant N) was derived from fixation. In pot experiments, under greenhouse conditions, integrated determination of fixation was made in Phaseolus beans (from the 19 sup(th) to the 67 sup(th) day from planting) and in soybeans (from the 24 sup(th) to the 70 sup(th) day from planting). The soil atmosphere was labelled with sup(15)N sub(2) in both cases. Average fixation obtained for Phaseolus beans was 80 mg N/plant (65% of total plant N) and for soybeans 265 mg N/plant (71% of total plant N). Evaluation of the basic concept of the isotope dilution method to determine nitrogen fixation in pots experiments, as proposed by Fried and Middelboe (1977) has also been made in the present paper. Simultaneous determinations of fixation in soybeans, using the isotope dilution method of Fried and Middelboe, natural variation of the sup(15)N/ sup(14)N ratios, and total-N differences, indicated the same results for pot experiments, harvested at the end of the plant cycle. (author)

  16. Precise determination of the neutron scattering length of lead isotopes 204Pb,207Pb and 208Pb by neutron interferometry

    International Nuclear Information System (INIS)

    Ioffe, A.; Ermakov, O.; Karpikhin, I.; Krupchitsky, P.; Mikula, P.; Lukas, P.; Vrana, M.

    2000-01-01

    The neutron scattering length of lead isotopes 204 Pb, 207 Pb and 208 Pb are determined by a set of neutron interferometry experiments. The obtained values b (208) =9.494(30) fm, b (207) =9.286(16) fm, b (204) =10.893(78) fm have much higher accuracy then current table data. Together with the precise value of b for natural lead, these results represent a complete set of data and allow one to calculate b (206) =9.221(69) fm, which is in the very good agreement with the present day experimental value. (orig.)

  17. Simultaneous determination of the intravenous and oral pharmacokinetic parameters of D,L-verapamil using stable isotope-labelled verapamil.

    Science.gov (United States)

    Eichelbaum, M; Somogyi, A; von Unruh, G E; Dengler, H J

    1981-01-01

    Following i.v. administration, the plasma concentration-time curve of verapamil could best be described by either a mono- or biexponential equation. Total plasma clearance (1.26 1/min) approached liver blood flow (1.51/min), so it can be concluded that its clearance is liver blood flow-dependent. Although absorption was almost complete after oral administration, absolute bioavailability (20%) was low, due to extensive hepatic first-pass metabolism. The approach using stable isotope-labelled and unlabelled drug permits simultaneous administration by the intravascular and extravascular routes, thus allowing determination of absolute bioavailability in a single experiment.

  18. LA-MC-ICPMS Determination of Copper Isotope Ratios in Turquoise from the Southwestern United States.

    Science.gov (United States)

    Evans, M. J.; Fayek, M.; Riciputi, L.; Anovitz, L.; Hull, S.; Mathien, F. J.; Milford, H.

    2004-12-01

    Hydrothermal circulation driven by igneous intrusion led to the deposition of turquoise throughout the southwestern United States and Mesoamerica. The genesis of these copper-ore deposits is unclear; conflicting hypotheses call on ascent of magmatic waters (hypogene) or descent and recirculation of meteroric waters (supergene). Copper isotope analyses were performed by laser-ablation multi-collector ICPMS to survey turquoise deposits from AZ, NV, CA, NM, and CO. The turquoise have [Cu] from 0.1 to 10 wt% and are all found in near-surface alteration zones. Analyses of individual turquoise grains are reproducible to better than 0.4\\permil \\delta65Cu (1\\sigma) (relative to NBS-976). \\delta65Cu values show significant variation (ca. 10\\permil) between the deposits, equal to the total range reported for continental ores and both hypogene and supergene deposits. The variability between deposits may reflect differences in source Cu isotopic composition or more likely, hydrothermal processes during leaching and deposition. The mining and trade of turquoise played an important role in early social and economic development between Mesoamerica and N. America. Copper isotopes will improve differentiation between turquoise source areas, aiding archaeological and cultural studies of trade between and within Mesoamerica and the SW USA. Research sponsored by NSF-BCS (Archaeology) grant #0312088 to Fayek and the Office of Basic Energy Sciences, U.S. Department of Energy, under contract with Oak Ridge National Laboratory, managed by UT-Battelle, LLC. The submitted manuscript has been authored by a contractor of the U.S. Government under contract No. DE-AC05-00OR22725. Accordingly, the U.S. Government retains a nonexclusive, royalty-free license to publish or reproduce the published form of this contribution, or allow others to do so, for U.S. Government purposes.

  19. Exploiting flow injection and sequential injection for trace metal determinations in conjunction with detection by electrothermal atomic absorption spectrometry and inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Hansen, Elo Harald

    and selectivity. Either in order to separate/preconcentrate the analyte material, or because of the presence of potentially interfering matrix constituents. Such pretreatments are advantageously performed in flow injection (FI) or sequential injection (SI) manifolds, where all appropriate unit operations can...

  20. Determination of half life of tellurium isotopes: a proposal for the teaching of nuclear physics

    International Nuclear Information System (INIS)

    Ruivo, Julio C.; Zamboni, Cibele B.; Batista, Wagner F.

    2013-01-01

    This work aimed at the development of courseware for teaching nuclear physics, using experimental data of half-life measurement (T1/2) of Tellurium isotopes (A=127 and 131). The choice of Tellurium was established for providing nuclear data, which are fundamental in related investigations of nuclear structure and its use in various areas such as geochemistry, chemical and pharmaceutical industries, astrophysics etc. For evaluation of the proposal performance, the material was made available, bringing a lot of information about nuclear safety, production and storage of radioactive material and concepts of radioactive decay, subatomic particles, emission of gamma radiation, half-life, etc.

  1. Determination of half life of tellurium isotopes: a proposal for the teaching of nuclear physics

    Energy Technology Data Exchange (ETDEWEB)

    Ruivo, Julio C.; Zamboni, Cibele B.; Batista, Wagner F., E-mail: julio.ruivo.costa@usp.br, E-mail: czamboni@ipen.br, E-mail: fisicawagner@gmail.com [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

    2013-07-01

    This work aimed at the development of courseware for teaching nuclear physics, using experimental data of half-life measurement (T1/2) of Tellurium isotopes (A=127 and 131). The choice of Tellurium was established for providing nuclear data, which are fundamental in related investigations of nuclear structure and its use in various areas such as geochemistry, chemical and pharmaceutical industries, astrophysics etc. For evaluation of the proposal performance, the material was made available, bringing a lot of information about nuclear safety, production and storage of radioactive material and concepts of radioactive decay, subatomic particles, emission of gamma radiation, half-life, etc.

  2. Determination of 90Sr and Pu isotopes in contaminated groundwater samples by inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Zoriy, Miroslav V.; Ostapczuk, Peter; Halicz, Ludwik; Hille, Ralf; Becker, J. Sabine

    2005-04-01

    A sensitive analytical method for determining the artificial radionuclides 90Sr, 239Pu and 240Pu at the ultratrace level in groundwater samples from the Semipalatinsk Test Site area in Kazakhstan by double-focusing sector field inductively coupled plasma mass spectrometry (ICP-SFMS) was developed. In order to avoid possible isobaric interferences at m/z 90 for 90Sr determination (e.g. 90Zr+, 40Ar50Cr+, 36Ar54Fe+, 58Ni16O2+, 180Hf2+, etc.), the measurements were performed at medium mass resolution under cold plasma conditions. Pu was separated from uranium by means of extraction chromatography using Eichrom TEVA resin with a recovery of 83%. The limits of detection for 90Sr, 239Pu and 240Pu in water samples were determined as 11, 0.12 and 0.1 fg ml-1, respectively. Concentrations of 90Sr and 239Pu in contaminated groundwater samples ranged from 18 to 32 and from 28 to 856 fg ml-1, respectively. The 240Pu/239Pu isotopic ratio in groundwater samples was measured as 0.17. This isotope ratio indicates that the most probable source of contamination of the investigated groundwater samples was the nuclear weapons tests at the Semipalatinsk Test Site conducted by the USSR in the 1960s.

  3. Determination of total and isotopic uranium by inductively coupled plasma-mass spectrometry at the Fernald Environmental Management Project

    International Nuclear Information System (INIS)

    Miller, F.L.; Bolin, R.N.; Feller, M.T.; Danahy, R.J.

    1995-01-01

    At the Fernald Environmental Management Project (FEMP) in southwestern Ohio, ICP-mass spectrometry (ICP-MS), with sample introduction by peristaltic pumping, is used to determine total and isotopic uranium (U-234, U-235, U-236 and U-238) in soil samples. These analyses are conducted in support of the environmental cleanup of the FEMP site. Various aspects of the sample preparation and instrumental analysis will be discussed. Initial sample preparation consists of oven drying to determine moisture content, and grinding and rolling to homogenize the sample. This is followed by a nitric/hydrofluoric acid digestion to bring the uranium in the sample into solution. Bismuth is added to the sample prior to digestion to monitor for losses. The total uranium (U-238) content of this solution and the U 235 /U 238 ratio are measured on the first pass through the ICP-MS. To determine the concentration of the less abundant U 234 and U 236 isotopes, the digestate is further concentrated by using Eichrom TRU-Spec extraction columns before the second pass through the ICP-MS. Quality controls for both the sample preparation and instrumental protocols will also be discussed. Finally, an explanation of the calculations used to report the data in either weight percent or activity units will be given

  4. Expanded uncertainty associated with determination of isotope enrichment factors: Comparison of two point calculation and Rayleigh-plot.

    Science.gov (United States)

    Julien, Maxime; Gilbert, Alexis; Yamada, Keita; Robins, Richard J; Höhener, Patrick; Yoshida, Naohiro; Remaud, Gérald S

    2018-01-01

    The enrichment factor (ε) is a common way to express Isotope Effects (IEs) associated with a phenomenon. Many studies determine ε using a Rayleigh-plot, which needs multiple data points. More recent articles describe an alternative method using the Rayleigh equation that allows the determination of ε using only one experimental point, but this method is often subject to controversy. However, a calculation method using two points (one experimental point and one at t 0 ) should lead to the same results because the calculation is derived from the Rayleigh equation. But, it is frequently asked "what is the valid domain of use of this two point calculation?" The primary aim of the present work is a systematic comparison of results obtained with these two methodologies and the determination of the conditions required for the valid calculation of ε. In order to evaluate the efficiency of the two approaches, the expanded uncertainty (U) associated with determining ε has been calculated using experimental data from three published articles. The second objective of the present work is to describe how to determine the expanded uncertainty (U) associated with determining ε. Comparative methodologies using both Rayleigh-plot and two point calculation are detailed and it is clearly demonstrated that calculation of ε using a single data point can give the same result as a Rayleigh-plot provided one strict condition is respected: that the experimental value is measured at a small fraction of unreacted substrate (f < 30%). This study will help stable isotope users to present their results in a more rigorous expression: ε ± U and therefore to define better the significance of an experimental results prior interpretation. Capsule: Enrichment factor can be determined through two different methods and the calculation of associated expanded uncertainty allows checking its significance. Copyright © 2017 Elsevier B.V. All rights reserved.

  5. Accurate experimental determination of the isotope effects on the triple point temperature of water. I. Dependence on the "2H abundance

    International Nuclear Information System (INIS)

    Faghihi, V.; Aerts-Bijma, A.T.; Jansen, H.G.; Spriensma, J.J.; Meijer, H.A.J.; Peruzzi, A.; Geel, J. van

    2015-01-01

    Variation in the isotopic composition of water is one of the major contributors to uncertainty in the realization of the triple point of water (TPW). Although the dependence of the TPW on the isotopic composition of the water has been known for years, there is still a lack of a detailed and accurate experimental determination of the values for the correction constants. This paper is the first of two articles (Part I and Part II) that address quantification of isotope abundance effects on the triple point temperature of water. In this paper, we describe our experimental assessment of the "2H isotope effect. We manufactured five triple point cells with prepared water mixtures with a range of "2H isotopic abundances encompassing widely the natural abundance range, while the "1"8O and "1"7O isotopic abundance were kept approximately constant and the "1"8O - "1"7O ratio was close to the Meijer-Li relationship for natural waters. The selected range of "2H isotopic abundances led to cells that realised TPW temperatures between approximately -140 μK to + 2500 μK with respect to the TPW temperature as realized by VSMOW (Vienna Standard Mean Ocean Water). Our experiment led to determination of the value for the δ"2H correction parameter of A_2_H = 673 μK/(per thousand deviation of δ"2H from VSMOW) with a combined uncertainty of 4 μK (k = 1, or 1 s). (authors)

  6. Uranium determination in sea water using the isotopic dilution technique and HR-ICPMS

    International Nuclear Information System (INIS)

    Pereira, Marcio Henrique da Costa; Sarkis, Jorge Eduardo de Souza; Hortellani, Marcos Antonio; Nascimento, Marcos R.L.

    2009-01-01

    In this work, the uranium total and the isotopic composition in seawater were calculated using the isotopic dilution applied to the mass spectrometry. The used tracer was a 233 U solution . Near 99 % of the present salts in the matrix were separated by evaporation up to the saturation point. The uranium present in aqueous phase was separated from the matrix through the ion exchange chromatography using the strong Dowex 1 x 8 200-400 mesh anionic resin in chloridric medium 12 M. The analyses were performed in a high resolution mass spectrometer with plasma inductively coupled source. The method validation was done using the seawater standard CASS-4 (Near shore Seawater Reference Material for Trace metals) produced by the NRC C. The procedure allowed to obtain the fractions exempt of salts, having as consequence a greater stability in the analytical signal, and a rise in the instrumental revenue for a great number of samples. The uranium found in the samples was present in levels considered naturals and were obtained with a precision near 2 %

  7. Metal Content and Stable Isotope Determination in Some Commercial Beers from Romanian Markets

    Directory of Open Access Journals (Sweden)

    Cezara Voica

    2015-01-01

    Full Text Available Characterization of beer samples is of interest because their compositions affect the taste and stability of beer and, also, consumer health. In this work, the characterizations of 20 Romanian beers were performed by mean of Inductively Coupled Plasma Mass Spectrometry (ICP-MS and Isotope Ratio Mass Spectrometry (IRMS in order to trace heavy metals and isotopic content of them. Major, minor, and trace metals are important in beer fermentation since they supply the appropriate environment for yeast growth and influence yeast metabolism. Beside this, the presence of the C4 plants in the brewing process was followed. Our study has shown that the analyzed beers indicated the presence of different plant types used in brewing: C3, C3-C4 mixtures, and also C4, depending on producers. Also the trace metal content of each sample is presented and discussed in this study. A comparison of the beers quality manufactured by the same producer but bottled in different type of packaging like glass, dose, or PET was made; our results show that no compositional differences among the same beer type exist.

  8. The Potential for Zinc Stable Isotope Techniques and Modelling to Determine Optimal Zinc Supplementation

    Directory of Open Access Journals (Sweden)

    Cuong D. Tran

    2015-05-01

    Full Text Available It is well recognised that zinc deficiency is a major global public health issue, particularly in young children in low-income countries with diarrhoea and environmental enteropathy. Zinc supplementation is regarded as a powerful tool to correct zinc deficiency as well as to treat a variety of physiologic and pathologic conditions. However, the dose and frequency of its use as well as the choice of zinc salt are not clearly defined regardless of whether it is used to treat a disease or correct a nutritional deficiency. We discuss the application of zinc stable isotope tracer techniques to assess zinc physiology, metabolism and homeostasis and how these can address knowledge gaps in zinc supplementation pharmacokinetics. This may help to resolve optimal dose, frequency, length of administration, timing of delivery to food intake and choice of zinc compound. It appears that long-term preventive supplementation can be administered much less frequently than daily but more research needs to be undertaken to better understand how best to intervene with zinc in children at risk of zinc deficiency. Stable isotope techniques, linked with saturation response and compartmental modelling, also have the potential to assist in the continued search for simple markers of zinc status in health, malnutrition and disease.

  9. Determination of stable and radioactive isotopes in rain water in Sahel in 1975 and 1976

    International Nuclear Information System (INIS)

    Baudet, J.; Abi, B.

    1979-01-01

    The problem of desertification in Africa incites to materialize the circuit of the water vapour between its main source, the Gulf of Guinea, and its precipitation site. Some rainwater samples have been collected in Ouagadougou in 1975 and 1976 during the rainy season. The dosage of the stable isotopes D and O 18 and radioactive isotope T shows that in 1975, a year with a general rain deficit, the rain was formed in a continental air mass. On the contrary, in 1976, a year with excess rain, the rain was formed in a maritime air mass. A study of the wind flows at 600, 900, 1500 and 2100 m shows that in 1975 the monsoon penetration is limited to the bottom of the Gulf of Guinea facing Cameroons, while in 1976 it entered the African Continent through the whole Gulf Coast, from Senegal to Cameroons. In 1976, the monsoon went up in latitude 3 0 to 5 0 more to the north than in 1975 [fr

  10. Determination of the origin and texture of marble artifacts using stable isotopes

    Science.gov (United States)

    Dotsika, E.; Poutoukis, D.; Zisi, N.; Psomiadis, D.

    2009-04-01

    For the characterization of marble and the identification of the origin of marble artifacts, samples from several ancient monuments of Greece were analyzed using several techniques: stable isotopes of carbonates (13C, 18O), XRD analysis and optical microscopy, from which information can be obtained on the origin and texture of the marble used for the production of the artifacts. The full range of grain sizes and isotopic signatures that occur in a lot of different quarries has been measured and presented. In a δ13C versus δ18O diagram, the fields corresponding to all known ancient quarries (from Penteli, Cyclades, especially Naxos (Mela, Apol, Apir, Senax), Keros, Paros (Parlak, Parlyc) and Asia Minor (Prokon)) are reported. The plots representing the analyzed samples are also shown on the same diagram. The final results of the study indicate the origin of the carbonate material of the artefacts from each of the ancient monument. In cases that the samples plot on overlapping areas, a further study is proposed, using the maximum grain size of the material.

  11. The Potential for Zinc Stable Isotope Techniques and Modelling to Determine Optimal Zinc Supplementation

    Science.gov (United States)

    Tran, Cuong D.; Gopalsamy, Geetha L.; Mortimer, Elissa K.; Young, Graeme P.

    2015-01-01

    It is well recognised that zinc deficiency is a major global public health issue, particularly in young children in low-income countries with diarrhoea and environmental enteropathy. Zinc supplementation is regarded as a powerful tool to correct zinc deficiency as well as to treat a variety of physiologic and pathologic conditions. However, the dose and frequency of its use as well as the choice of zinc salt are not clearly defined regardless of whether it is used to treat a disease or correct a nutritional deficiency. We discuss the application of zinc stable isotope tracer techniques to assess zinc physiology, metabolism and homeostasis and how these can address knowledge gaps in zinc supplementation pharmacokinetics. This may help to resolve optimal dose, frequency, length of administration, timing of delivery to food intake and choice of zinc compound. It appears that long-term preventive supplementation can be administered much less frequently than daily but more research needs to be undertaken to better understand how best to intervene with zinc in children at risk of zinc deficiency. Stable isotope techniques, linked with saturation response and compartmental modelling, also have the potential to assist in the continued search for simple markers of zinc status in health, malnutrition and disease. PMID:26035248

  12. A new method of accurate determination of isotopic composition and concentration of strontium in a spike solution used for geochronological works

    International Nuclear Information System (INIS)

    Yanagi, Takeru

    1990-01-01

    A new method of accurate determination of isotopic composition and concentration of a strontium-84 spike solution was devised for simultaneous determination of strontium contents and isotopic compositions in rocks and minerals by measuring strontium isotopic ratios in spiked samples. In this method, the isotopic composition of strontium in the spike were determined so as to minimize the sum of squares of deviations of spike strontium-84 concentrations which were calculated from measured isotopic ratios of strontium in five different mixtures of the spike and the standard solution. The method can eliminate all mass discriminations occurred during the measurements on a surface ionization mass spectrometer. The results were tested by measuring 87 Sr/ 86 Sr ratios of Eimer and Amend SrCO 3 and JB-1 geochemical reference material, and by determining the strontium content in JB-1. The measurements of strontium isotope ratios in spiked samples give average values of 0.708007±0.000052 and 0.70417±0.00004 for 87 Sr/ 86 Sr ratios of E and A SrCO 3 and JB-1, respectively. The strontium content in JB-1 was estimated at 457.1±1.3 ppm. These values are very close to reported respective values. (author)

  13. Determination of isotope ratios of metals (and metalloids) by means of inductively coupled plasma-mass spectrometry for provenancing purposes - A review

    International Nuclear Information System (INIS)

    Balcaen, L.; Moens, L.; Vanhaecke, F.

    2010-01-01

    Since considerable time, isotopic analysis of different elements present in a sample, material or object (such as the 'light' elements H, C, N, O and S and 'heavy' elements, such as Sr and Pb), has been used in provenancing studies, as several factors - defined by 'the environment' or origin of the sample - can lead to measurable differences in their isotopic composition. For the light elements, traditionally, (gas source) isotope ratio mass spectrometry (IR-MS) is used, while for a long period of time, thermal ionization mass spectrometry (TIMS) was considered as the only technique capable of detecting subtle variations in the isotopic composition of the 'heavier' elements. However, since the introduction of the first inductively coupled plasma mass spectrometers (ICP-MS), considerable attention has been devoted to the development of methodologies and strategies to perform isotopic analysis by means of ICP-MS. While the relatively modest isotope ratio precision offered by single-collector ICP-MS may already be fit-for-purpose under some circumstances, especially the introduction of multi-collector ICP-MS instruments, equipped with an array of Faraday detectors instead of a single electron multiplier, has lead to tremendous improvements in the field of isotopic analysis. As a result, MC-ICP-MS can be seen as a very strong competitor of TIMS nowadays, while it even provides information on the small isotopic variations shown by some elements, that are not or hardly accessible by means of TIMS (e.g., elements with a high ionization energy). Owing to these new instrumental developments, the application field of isotopic analysis by means of ICP-MS is continuously growing, also in the field of provenance determination. This paper is intended as a review of the developments in and the recent applications of isotopic analysis by means of ICP-MS in this specific research field.

  14. Determination of tungsten in high-alloy steels and heat resisting alloys by isotope dilution-spark source mass spectrometry

    International Nuclear Information System (INIS)

    Saito, Morimasa; Yamada, Kei; Okochi, Haruno; Hirose, Fumio

    1983-01-01

    Tungsten in high-alloy steels and heat-resisting alloys was determined by isotope dilution method combined with spark source mass spectrometry by using 183 W enriched tungsten. The spike solution was prepared by fusing tungsten trioxide in sodium carbonate. A high-alloy steel sample was dissolved in the mixture of sulfuric acid and phosphoric acid together with the spike solution; a sample of heat resisting alloy was similarly dissolved in the mixture of hydrochloric acid, nitric acid, sulfuric acid, and phosphoric acid. The solution was evaporated to give dense white fumes. Tungsten was separated from the residue by a conventional cinchonine salt-precipitation method. The salt was ignited, and the residue was mixed with graphite powder and pressed into electrodes. The isotope 183 W and 184 W were measured. The method was applied to the determination of tungsten in JSS and NBS standard high-alloy steels and JAERI standard nickel- and NBS standard cobalt-base heat resisting alloys containing more than 0.05% tungsten. The results were obtained with satisfactory precision and accuracy. However, the results obtained for JSS standard high- speed steels containing molybdenum tended to be significantly lower than the certified values. (author)

  15. A comparison between isotopic and different methods for determining urea fertilizer use efficiency under trickle figuration on tomato

    International Nuclear Information System (INIS)

    Mousavi Shalmani, M.A.; Sagheb, N.; Rafii, H.; Hobbi, M.S.; Khorosani, A.

    2002-01-01

    In order to study the fertilizer use efficiency by two different methods, an experimental design was conducted in Randomized Complete Block (RBC) with four replications and treatments in the plots with 35 square meter, area. 1200 seedlings of tomato (variety of early Urbana V.F.) were planted on June 3. 1996 at the distances of 50 cm apart. Fertilization and irrigation were performed by two fertilizer pumps (one for P and K and the other for N). The treatments of N 0 , N 1 , N 2 and N 3 received 0, 287.5, 575 and 862.5 kg N/ha respectively. The 14 N/ 15 N isotopic ratio of nitrogen gas was determined by the use of emission spectrometer and the fertilizer use efficiency was determined by using nuclear chemical equations. Because of the shortage of micro nutrients in soil and unbalanced quantity of N,P and K as fertilizers the results have shown a large amount of free radicals (NH 4 , NO 3 ) remained in the soil. This disturbed the balance between absorption of nitrogen from its different sources in the soil. Therefor, the share of fertilizer increased and in this condition, the priming effects were seen and different methods showed lower amounts of fertilizer use efficiency in comparison with the isotopic method

  16. Determination of mixing characteristics of the river Kabul and the river Indus using physico-chemical and stable isotope parameters

    International Nuclear Information System (INIS)

    Qureshi, R.M.; Hussain, Q.M.; Sajjad, M.I.; Hussain, S.D.; Latif, Z.

    1990-11-01

    This report presents a comparative study on the usefulness of stable isotope parameters (hydrogen and oxygen) versus the physico-chemical parameters (electrical conductivity, temperature, pH value) of water to determine the extent of mixing of the river Kabul with the river Indus near Attock. In view of the sampling techniques employed in the present investigations, electrical conductivity and temperature are found to be the best field parameters for a quick estimate of mixing path length. However, the stable isotopes of the water molecule, due to their greater sensitivity and measuring accuracy, provide a better scenario of mixing characteristics as compared to the physico-chemical parameters. It appears that under normal flow condition, it takes about 5 km channel distance for complete mixing of the Kabul river water in the Indus river channel. A computer code MIXABC is developed to determine the percentage contribution of one river water along a mixing channel in the other river. Details of the source programs are presented. The code can be used on any IBM-compatible microsystem. (author)

  17. Determination of low-level Radium isotope activities in fresh waters by gamma spectrometry

    International Nuclear Information System (INIS)

    Molina Porras, Arnold; Condomines, Michel; Seidel, Jean Luc

    2017-01-01

    A new portable sampling system was developed to extract Radium isotopes from large volumes (up to 300 L) of fresh surface- and ground-waters of low Ra-activities (<5 mBq/L). Ra is quantitatively adsorbed on a small amount (6.5 g) of MnO_2-coated acrylic fibers, which are then dried and burned at 600 °C in the laboratory. The resulting Mn-oxide powder (about 2 cm"3 when compacted) is then analyzed through gamma-ray spectrometry which allows measurement of the whole Ra quartet ("2"2"6Ra, "2"2"8Ra, "2"2"4Ra and "2"2"3Ra) in a single counting of a few days. The usual relative standard combined uncertainties (1σ) are 2–3% for "2"2"6Ra, "2"2"8Ra and "2"2"4Ra; and less than 10% for "2"2"3Ra. This method was applied to the analysis of Ra in karstic waters of the Lez aquifer, and surface- and ground-waters of the upper and middle Vidourle watershed (South of France). The analyzed waters have relatively low "2"2"6Ra activities (1–4 mBq/L) in both cases, regardless of the contrasted geology (Mesozoic limestone vs crystalline Variscan basement), but clearly distinct ("2"2"8Ra/"2"2"6Ra) ratios in agreement with the differences in Th/U ratios of the two drained areas. Short-lived Ra isotopes ("2"2"4Ra and "2"2"3Ra) appear to be mainly influenced by near-surface desorption/recoil processes for most of the sampling sites. - Highlights: • New portable system for sampling fresh- and ground-waters of low Ra activities. • Simultaneous measurement of all four radium isotopes through gamma-spectrometry. • Relative uncertainties are 2% to 3% for "2"2"6Ra, "2"2"8Ra and "2"2"4Ra; and <10 % for "2"2"3Ra. • ("2"2"8Ra/"2"2"6Ra) ratios are valuable tracers of water origin in karstic aquifers.

  18. Determination of 129I/127I isotope ratios in liquid solutions and environmental soil samples by ICP-MS with hexapole collision cell

    OpenAIRE

    Izmer, A. V.; Boulyga, S. F.; Becker, J. S.

    2003-01-01

    The determination of I-129 in environmental samples at ultratrace levels is very difficult by ICP-MS due to a high noise caused by Xe impurities in argon plasma gas (interference of Xe-129(+)), possible (IH2+)-I-127 interference and an insufficient abundance ratio sensitivity of the ICP mass spectrometer for I-129/I-127 isotope ratio measurement. A sensitive, powerful and fast analytical technique for iodine isotope ratio measurements in aqueous solutions and contaminated soil samples directl...

  19. Determination of micro-quantities of several elements in soil solution by isotope dilution and activation analyses

    International Nuclear Information System (INIS)

    Cho, C.M.; Axmann, H.

    1965-01-01

    Determination of small quantities of plant nutrients in the soil solution of flooded rice soils is a difficult problem. The concentrations of Mn, Fe and P, for example, in some soil solutions are so small that no chemical method gives any accurate result. Neutron activation analysis was reported to give a much lower limit of detectability for several elements, while for elements with low-induced activity after neutron irradiation, substoichiometric isotopic dilution analysis was applied. One of the advantages of neutron activation analysis lies in the fact that simultaneous activation of every inducible element in a sample takes place. This gives an opportunity to determine many elements by one sample preparation and irradiation. This, however, is not a simple task since identification of the activated products and their quantitative estimation becomes very difficult. Certain operations of separation must be carried out before activity measurements. Ion-exchange resin columns and chemical separation following the addition of carriers were successfully used for the determination of many elements after neutron irradiation. These procedures, however, cannot be directly applied to the determination of the elements of agronomic interest. A procedure was developed to determine several elements of agronomic interest. Times of irradiation and cooling, quick separation by ion-exchange columns, together with chemical precipitation for β-emitters of relatively long half-lives, were all combined to get the maximum benefit from neutron activation analysis. For Fe, for which no satisfactory neutron activation analysis has yet been developed, a modified substoichiometric double isotope dilution procedure is applied

  20. Possibility of determination of the Galaxy age by the method of uranium - thorium isotopic relations

    International Nuclear Information System (INIS)

    Lyutostanskij, Yu.S.; Malevannyj, S.V.; Panov, I.V.; Chechetkin, V.M.

    1988-01-01

    Calculations concerning the formation of heavy elements in an astrophysical fast nuclear process characteristics of the Supernova explosions are carried out in the kinetic model of nucleosynthesis. The age of the Galaxy T G has been calculated making use of the method of uranium-thorium isotopic relations supplemented with the data on 244 Pu abundance in meteorites. T G is shown to be strongly dependent upon the calculation method applied to production of nuclei in r process, upon the data on neutron-rich nuclei and as well upon the external conditions, i.e. the density and temperature in the explosing star. The possibility of nucleosynthesis takes place due to close Supernova explosion, which enriched the chemical content of earth matter with heavy elements is analyzed. The range of allowed values of parameters of the theory of nucleosynthesis is studied

  1. Differential Isotope Labeling of Glycopeptides for Accurate Determination of Differences in Site-Specific Glycosylation.

    Science.gov (United States)

    Pabst, Martin; Benešová, Iva; Fagerer, Stephan R; Jacobsen, Mathias; Eyer, Klaus; Schmidt, Gregor; Steinhoff, Robert; Krismer, Jasmin; Wahl, Fabian; Preisler, Jan; Zenobi, Renato

    2016-01-04

    We introduce a stable isotope labeling approach for glycopeptides that allows a specific glycosylation site in a protein to be quantitatively evaluated using mass spectrometry. Succinic anhydride is used to specifically label primary amino groups of the peptide portion of the glycopeptides. The heavy form (D4(13)C4) provides an 8 Da mass increment over the light natural form (H4(12)C4), allowing simultaneous analysis and direct comparison of two glycopeptide profiles in a single MS scan. We have optimized a protocol for an in-solution trypsin digestion, a one-pot labeling procedure, and a post-labeling solid-phase extraction to obtain purified and labeled glycopeptides. We provide the first demonstration of this approach by comparing IgG1 Fc glycopeptides from polyclonal IgG samples with respect to their galactosylation and sialylation patterns using MALDI MS and LC-ESI-MS.

  2. Use of AERIN code for determining internal doses of transuranic isotopes

    International Nuclear Information System (INIS)

    King, W.C.

    1980-01-01

    The AERIN computer code is a mathematical expression of the ICRP Lung Model. The code was developed at the Lawrence Livermore National Laboratory to compute the body organ burdens and absorbed radiation doses resulting from the inhalation of transuranic isotopes and to predict the amount of activity excreted in the urine and feces as a function of time. Over forty cases of internal exposure have been studied using the AERIN code. The code, as modified, has proven to be extremely versatile. The case studies presented demonstrate the excellent correlation that can be obtained between code predictions and observed bioassay data. In one case study a discrepancy was observed between an in vivo count of the whole body and the application of the code using urine and fecal data as input. The discrepancy was resolved by in vivo skull counts that showed the code had predicted the correct skeletal burden

  3. Accurate determination and certification of bromine in plastic by isotope dilution inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Ohata, Masaki, E-mail: m-oohata@aist.go.jp; Miura, Tsutomu

    2014-07-21

    Highlights: • Accurate analytical method of Br in plastic was studied by isotope dilution ICPMS. • A microwave acid digestion using quartz vessel was suitable for Br analysis. • Sample dilution by NH{sub 3} solution could remove memory effect for ICPMS measurement. • The analytical result of the ID-ICPMS showed consistency with that of INAA. • The ID-ICPMS developed could apply to certification of Br in candidate plastic CRM. - Abstract: The accurate analytical method of bromine (Br) in plastic was developed by an isotope dilution inductively coupled plasma mass spectrometry (ID-ICPMS). The figures of merit of microwave acid digestion procedures using polytetrafluoroethylene (PTFE) or quartz vessels were studied and the latter one was suitable for Br analysis since its material was free from Br contamination. The sample dilution procedures using Milli-Q water or ammonium (NH{sub 3}) solution were also studied to remove memory effect for ICPMS measurement. Although severe memory effect was observed on Milli-Q water dilution, NH{sub 3} solution could remove it successfully. The accuracy of the ID-ICPMS was validated by a certified reference material (CRM) as well as the comparison with the analytical result obtained by an instrumental neutron activation analysis (INAA) as different analytical method. From these results, the ID-ICPMS developed in the present study could be evaluated as accurate analytical method of Br in plastic materials and it could apply to certification of Br in candidate plastic CRM with respect to such regulations related to RoHS (restriction of the use of hazardous substances in electrical and electronics equipment) directive.

  4. Accurate determination and certification of bromine in plastic by isotope dilution inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Ohata, Masaki; Miura, Tsutomu

    2014-01-01

    Highlights: • Accurate analytical method of Br in plastic was studied by isotope dilution ICPMS. • A microwave acid digestion using quartz vessel was suitable for Br analysis. • Sample dilution by NH 3 solution could remove memory effect for ICPMS measurement. • The analytical result of the ID-ICPMS showed consistency with that of INAA. • The ID-ICPMS developed could apply to certification of Br in candidate plastic CRM. - Abstract: The accurate analytical method of bromine (Br) in plastic was developed by an isotope dilution inductively coupled plasma mass spectrometry (ID-ICPMS). The figures of merit of microwave acid digestion procedures using polytetrafluoroethylene (PTFE) or quartz vessels were studied and the latter one was suitable for Br analysis since its material was free from Br contamination. The sample dilution procedures using Milli-Q water or ammonium (NH 3 ) solution were also studied to remove memory effect for ICPMS measurement. Although severe memory effect was observed on Milli-Q water dilution, NH 3 solution could remove it successfully. The accuracy of the ID-ICPMS was validated by a certified reference material (CRM) as well as the comparison with the analytical result obtained by an instrumental neutron activation analysis (INAA) as different analytical method. From these results, the ID-ICPMS developed in the present study could be evaluated as accurate analytical method of Br in plastic materials and it could apply to certification of Br in candidate plastic CRM with respect to such regulations related to RoHS (restriction of the use of hazardous substances in electrical and electronics equipment) directive

  5. Determination of serum calcium levels by 42Ca isotope dilution inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Han, Bingqing; Ge, Menglei; Zhao, Haijian; Yan, Ying; Zeng, Jie; Zhang, Tianjiao; Zhou, Weiyan; Zhang, Jiangtao; Wang, Jing; Zhang, Chuanbao

    2017-11-27

    Serum calcium level is an important clinical index that reflects pathophysiological states. However, detection accuracy in laboratory tests is not ideal; as such, a high accuracy method is needed. We developed a reference method for measuring serum calcium levels by isotope dilution inductively coupled plasma mass spectrometry (ID ICP-MS), using 42Ca as the enriched isotope. Serum was digested with 69% ultrapure nitric acid and diluted to a suitable concentration. The 44Ca/42Ca ratio was detected in H2 mode; spike concentration was calibrated by reverse IDMS using standard reference material (SRM) 3109a, and sample concentration was measured by a bracketing procedure. We compared the performance of ID ICP-MS with those of three other reference methods in China using the same serum and aqueous samples. The relative expanded uncertainty of the sample concentration was 0.414% (k=2). The range of repeatability (within-run imprecision), intermediate imprecision (between-run imprecision), and intra-laboratory imprecision were 0.12%-0.19%, 0.07%-0.09%, and 0.16%-0.17%, respectively, for two of the serum samples. SRM909bI, SRM909bII, SRM909c, and GBW09152 were found to be within the certified value interval, with mean relative bias values of 0.29%, -0.02%, 0.10%, and -0.19%, respectively. The range of recovery was 99.87%-100.37%. Results obtained by ID ICP-MS showed a better accuracy than and were highly correlated with those of other reference methods. ID ICP-MS is a simple and accurate candidate reference method for serum calcium measurement and can be used to establish and improve serum calcium reference system in China.

  6. A determination of elementary separation factors of isotopes 235U and 238U in the ionic exchange process and of eluents in the water-glycerine system

    International Nuclear Information System (INIS)

    Murgulescu, S.E.

    1977-01-01

    In the experiments focused on uranium isotope separation by ion and chemical exchange, the water-glycerine system was employed. The principle of the method consists in shifting a uranium band along an ion-exchange resin column by means of an eluent. The isotope effect of reactions determining the band heading into the column where complex bands between the metal ion and the ligand form and break up under the resin influence, is determined by the difference in affinity between the two isotopes as against the eluent. The isotope effect in question determines a unit deviation of the equilibrium constant for the classical isotope exchange reaction. Starting from the experimental results obtained, it was concluded that the ion and chemical exchange between the IV and VI valence forms of uranium can be applied to isotope separation in terms of the separation unit. As against the methods that have been applied at present (gaseous scattering, hydro-extracting and the nozzle method), for which every new stage corresponds to a separation elementary factor, several separation elementary factors can be cumulated into a single stage in a chemical and ion exchange unit, by the optimization of the shifting band and length. (author)

  7. Determination of mercury in coal by isotope dilution cold-vapor generation inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Long, S.E.; Kelly, W.R.

    2002-04-01

    A method based on isotope dilution cold-vapor inductively coupled plasma mass spectrometry (ID-CV-ICPMS) has been developed for high-accuracy determinations of mercury in bituminous and sub-bituminous coals. A closed-system digestion process employing a Carius tube is used to completely oxidize the coal matrix and chemically equilibrate the mercury in the sample with a Hg-201 isotopic spike. The digestates are diluted with high-purity quartz-distilled water, and the mercury is released as a vapor by reduction with tin chloride. Measurements of Hg-201/Hg-202 isotope ratios are made using a quadrupole ICPMS system in time-resolved analysis mode. The new method has some significant advantages over existing methods. The instrument detection limit is less than 1 pg/mL. The average blank (n = 17) is 30 pg, which is roughly 1 order of magnitude lower than the equivalent microwave digestion procedure. The detection limit in coal is blank limited and is similar to 40 pg/g. Memory effects are very low. The relative reproducibility of the analytical measurements is similar to 0.5% for mercury concentrations in the range 10-150 ng/g. The method has been used to measure mercury concentrations in six coal reference materials, SRM 1632b (77.4 ng/g), SRM 1632c (94.3 ng/g), BCR 40 (433.2 ng/g), BCR 180 (125.0 ng/g), BCR 181 (135.8 ng/g), and SARM 20 (252.6 ng/g), as well as a coal fly ash, SRM 1633b (143.1 ng/g). The method is equally applicable to other types of fossil fuels including both crude and refined oils.

  8. Limitation of secondary electron multiplier non-linearity on accurate U-Th isotopic determination by MC-ICP-MS

    Science.gov (United States)

    Shen, C.; Wu, C.; Gallet, S.; Cheng, H.; Edwards, R.; Hsieh, Y.; Lin, K.

    2008-12-01

    Contemporary multicollector-inductively coupled plasma mass spectrometry (MC-ICP-MS) with discrete dynode secondary electron multipliers (SEMs) can offer U-Th isotopic determinations with subpermil-permil- level precision in femtogram quantities. However, accurate isotopic measurement requires fully understanding SEM mass and intensity biases. In additional to dead-time effect, Richter et al (2001, Int. J. Mass Spectrom., 206, 105-127) reported a nonlinearity on SEMs produced by ETP and MasCom for count rates > 20 thousand counts per second (cps). We evaluated the possible biases for ion beams of 500- 1,600,000 cps on a latest MasCom SEM, SEV TE-Z/17, with more effective ion optical acceptance area (>50%) and better peak shape than previous models, used in a MC-ICP-MS, Thermo Fisher NEPTUNE. With the retarding potential quadruple lens (RPQ) turned off, ion beam intensity can be biased by only dead- time effect, which can be precisely corrected online or offline. With the RPQ on, two additional biases, an exponential-like increase of ion beam intensity from 100-100,000 s cps and an apparent dead-time effect (-2 to 2 ns) at high count rates, are observed. They are likely caused by the slightly defocused ions with a wide kinetic energy spread of ~5 eV, 10 times worse than that with thermal source, passing through the RPQ lens to the SEM, which is installed behind the focal plane. Fortunately, the two biases, which are stable during the daily measurements with the same settings of inlet system, source lenses, zoom optics, and RPQ, can be corrected effectively offline to earn accurate U-Th isotopic measurement.

  9. Sub-stoichiometric isotope dilution analysis method for the determination of iodine in common salts using iodine-131 tracer

    International Nuclear Information System (INIS)

    Singh, Vivek; Garg, A.N.

    1994-01-01

    A sub-stoichiometric isotope dilution analysis (SIDA) method was developed for the determination of iodine in different brands of common salts. An aqueous salt solution containing 131 I tracer and NaI as carrier is oxidized by tartaric acid and KIO 3 and the liberated iodine is extracted with CCl 4 . To the extract an aqueous solution of AgNO 3 is added in substoichiometric amount to obtain a colloidal solution of AgI. On adding sodium thiosulfate solution, the NaI so formed passes into aqueous solution, which is then counted. Several different brands of salt were analysed. The method is especially suitable for the determination of microgram amounts of iodide in the presence of excess of chloride. (Author)

  10. Determination of fission products and actinides by inductively coupled plasma-mass spectrometry using isotope dilution analysis. A study of random and systematic errors

    International Nuclear Information System (INIS)

    Ignacio Garcia Alonso, Jose

    1995-01-01

    The theory of the propagation of errors (random and systematic) for isotope dilution analysis (IDA) has been applied to the analysis of fission products and actinide elements by inductively coupled plasma-mass spectrometry (ICP-MS). Systematic errors in ID-ICP-MS arising from mass-discrimination (mass bias), detector non-linearity and isobaric interferences in the measured isotopes have to be corrected for in order to achieve accurate results. The mass bias factor and the detector dead-time can be determined by using natural elements with well-defined isotope abundances. A combined method for the simultaneous determination of both factors is proposed. On the other hand, isobaric interferences for some fission products and actinides cannot be eliminated using mathematical corrections (due to the unknown isotope abundances in the sample) and a chemical separation is necessary. The theory for random error propagation in IDA has been applied to the determination of non-natural elements by ICP-MS taking into account all possible sources of uncertainty with pulse counting detection. For the analysis of fission products, the selection of the right spike isotope composition and spike to sample ratio can be performed by applying conventional random propagation theory. However, it has been observed that, in the experimental determination of the isotope abundances of the fission product elements to be determined, the correction for mass-discrimination and the correction for detector dead-time losses contribute to the total random uncertainty. For the instrument used in the experimental part of this study, it was found that the random uncertainty on the measured isotope ratios followed Poisson statistics for low counting rates whereas, for high counting rates, source instability was the main source of error

  11. The application of scanning electron microscopy to the determination of elemental and isotopic composition in individual actinide particles

    International Nuclear Information System (INIS)

    Vatter, I.; Cattle, G.; Tushingham, J.

    2000-01-01

    Techniques for the determination of both elemental and isotopic composition of actinides within single particles are required by the IAEA in support of their environmental safeguards programme. SEM and SIMS are valuable techniques for the measurement of elemental and isotopic composition, respectively, on the particle scale. The potential for effective combination of SEM and SIMS has been investigated at Harwell Laboratory. In trials, copper finder grids have been successfully used to enable re-identification of particles between SEM and SIMS instruments. Use of the grids enables rapid relocation of particles pre-selected by SEM for SIMS measurement. The work has highlighted a possible matrix effect in plutonium measurement that results in variable sensitivity dependent on the presence of other elements (including uranium). This effect would limit the use of SIMS to obtain elemental ratios, and highlights the requirement to use both SEM and SIMS to gain full and accurate information. The possible use of autoradiography as an adjunct to SEM has been investigated. In principle, autoradiography could be used to identify higher enrichments of uranium and enable pre-selection of particles for SIMS measurement. During trials, practical problems have been encountered which have demonstrated this particular approach to be unsuitable. (author)

  12. An analytical procedure for determination of sulphur species and isotopes in boreal acid sulphate soils and sediments

    Directory of Open Access Journals (Sweden)

    K. BACKLUND

    2008-12-01

    Full Text Available An analytical scheme suitable for boreal acid sulphate (AS soils and sediments was developed on the basis of existing methods. The presented procedure can be used to quantify and discriminate among acid volatile sulphide, cold chromium reducible sulphur, hot chromium reducible sulphur, elemental sulphur, sulphate sulphur, organic sulphur, total reducible sulphur and total sulphur. The sulphur fractions are recovered as either Ag2S or BaSO4 precipitates and can further be used for isotope analysis. Overlaps between sulphur species are common during speciation, and must be minimized. Some of these overlaps are caused by poor sampling and storage, inappropriate conditions during the distillation, or natural variations in the sample (e.g. Fe3+ interference and grain size. The procedural impact was determined by conducting tests on both artificial and natural samples containing one or several sulphur species. The method is applied on reduced sediment from an AS soil locality (Överpurmo and a brackish lake (Larsmo Lake in western Finland and the results, including S-isotopes, are discussed.;

  13. Determination of biomass of mango (Mangifera indica L.) trees by non-destructive method using principle of isotope dilution

    International Nuclear Information System (INIS)

    Kotur, S.C.; Keshava Murthy, S.V.

    2003-01-01

    Biomass of 4-year old trees alphonso mango was estimated by injecting of carrier-free 32 P into the trunk followed by radio-assay of the isotope after a complete dilution of 32 P in the tree, being 3 months after injection. The isotopically calculated plant volume (59 903-68 981 cc plant -1 ) and biomass (31.70 - 36.23 kg plant -1 ) showed good agreement but generally overestimated both by about 23% compared to the actual values determined physically (43 720-60 693 cc plant -1 and 22.88-34.78 kg plant -1 , respectively). Application of the technique in a set of another four 15-year old mango trees yielded volume estimates of 1, 70, 749-1 75 835 cc plant -1 (mean=1, 75 835±1.12%) and biomass estimates of 73.0 - 87.4 kg plant -1 (mean=80.45±6.8%). The technique is of promise in fertilizer use efficiency and nutrient dynamics studies in tree crops. (author)

  14. Isotopic determinations of carbon and oxygen in the metasedimentary rocks of the Rio Pardo group-Bahia State, Brazil

    International Nuclear Information System (INIS)

    Costa Pinto, N.M.A.C.

    1977-01-01

    Determination of the carbon and oxygen isotopic compositions were made on approximately 100 samples of Late Precambrian metasedimentary rocks of the Rio Pardo Group from Southern Bahia. The results obtained show that carbon varies from δ 13 =C=5,73 per mille to δ 13 C=+9,00 per mille, and oxygen from δ 18 O=-1,87 per mille to δ 18 O=-19,67 per mille relative to PBD. The interpretations lead to some conclusions which confirm the validity the isotopic technique as auxiliary instrument in the study of geological problems. These include: 1) the evidence of a marine transgression during the Camaca sedimentation; 2) the probability that the dolomitic metalimestones of the Agua Preta formation belong to the Serra do Paraiso formation; 3) the assignment of the dolomitic metalismestones, which occur in Itiroro and which had been previously grouped with the crystalline basement rocks, to the Serra do Paraiso formation; 4) the removal of the marble from Serra do Paraiso formation and re-signment to the basement rocks, and finally; 5) the sedimentary evolution of the Rio Pardo Group from a typical fresh-water to a marine environment. (Author) [pt

  15. Determination of Trace Iron in Red Wine by Isotope Dilution Mass Spectrometry Using Multiple-Collector Inductively Coupled Plasma Mass Spectrometry

    International Nuclear Information System (INIS)

    Zhou Tao; Wang Jun; Lu Hai; Zhou Yuanjing; Li Haifeng

    2009-01-01

    This paper introduces determination of trace iron in red wine certified reference material by isotope dilution mass spectrometry (IDMS) method using a multiplecollector inductively coupled plasma mass spectrometry, equipped with a hexapole collision cell. The measurement procedure of iron isotopic abundance ratios was deeply researched. Reduced polyatomic ion interferences to iron isotopes ion by collision reaction using Ar and H 2 gas, high precise isotopic abundance ratios were achieved. Two relative measurement methods (ICP-MS and ICP-OES) were used to analyze trace iron in red wine. The results are compared with IDMS results, which indicate that they are accordant. The uncertainty analyses include each uncertainty factor in whole experiment and the uncertainty of used certified reference material and it shows that the procedure blank is not neglectable to detect limit and precision of the method. The establishment of IDMS method for analysis of trace iron in red wine supports the certification of certified reference materials. (authors)

  16. Determination of sulfur isotopic composition for the study of iron sulfides origin, biotic or abiotic, in anoxic corrosion

    International Nuclear Information System (INIS)

    Grousset, Sophie

    2016-01-01

    The first goal of this project was to develop a methodology based on the study of the sulfur isotopic composition enabling the determination of iron sulfides origin, biotic or abiotic, within the corrosion products layers (CPL). Then, the aim was to apply this methodology to real corrosion systems in order to determine the mechanisms of iron sulfides formation. Sulfur isotopic analyses methodologies, adapted to micrometric iron sulfides layers observed in real corrosion systems, were developed in nanoSIMS and ToF-SIMS. The study of iron sulfides formed in anoxic carbonated medium with or without sulphate-reducing bacteria validated the use of these methods for the determination of iron sulfides origin. The application of these methods coupled with the precise characterization of irons sulfides formed in the real corrosion systems show two kind of corrosion pattern. In pattern 1, the iron sulfides are localized in the external part of the CPL. They result from the Fe 2+ migration from the metal surface to areas rich in biotic S 2- . In this pattern, corrosion rates are lower than 20 μm/year for laboratory systems, and lower than 5 μm/year for archaeological objects. In pattern 2, the large presence of conductive phases in the CPL results in the delocalization of electrons, and so a disequilibrium of the charges at the metal's surface. That leads to the migration of biotic S 2- in the CPL till the metal where they precipitate in iron sulphides. This pattern shows high corrosion rates (∼100 μm/an) that might be resulting from the accumulation of bio-corrosion and chloride corrosion mechanisms. (author) [fr

  17. Determination of uranium and thorium isotopes in soil samples by coprecipitation

    International Nuclear Information System (INIS)

    Ngo Quang Huy; Trinh Thi Bich; Nguyen Van Suc

    2012-01-01

    The paper presents a procedure to prepare soil samples for U and Th isotope measurement by alpha-spectrometry after coprecipitation with LaF 3 . In this procedure the reduction of U(VI) to U(IV) was performed by Zn metal in 4M HCl solution. The recoveries of chemical separation equal to ε U-chemistry = 78±4% for uranium and ε Th-chemistry = 82±4% for thorium. Canberra alpha-spectrometer was used with PIPS detectors of A-1200-37-AM Model of 1200 mm 2 active area. The counting efficiency of the measuring system equals to ε counting = 18% and the total efficiencies were ε U = ε counting - ε U-chemistry = 14.0 ± 0.7% for uranium and ε Th = ε counting - ε Th-chemistry = 14.7 ± 0.7% for thorium. The recoveries of chemical separation were rather high (about 80%), that leads to the use of a small weight of soil sample (about 0.5 g). The efficiencies were also stable, that allows analyzing the soil sample without using radiotracers. They are advantages of the sample preparation procedure of this work. (author)

  18. Consequences of shoaling of the Central American Seaway determined from modeling Nd isotopes

    Science.gov (United States)

    Sepulchre, P.; Arsouze, T.; Donnadieu, Y.; Dutay, J.-C.; Jaramillo, C.; Le Bras, J.; Martin, E.; Montes, C.; Waite, A. J.

    2014-03-01

    The Central American Seaway played a pivotal role in shaping global climate throughout the late Cenozoic. Recent geological surveys have provided new constraints on timing of the seaway shoaling, while neodymium isotopic (ɛNd) data measured on fossil teeth, debris, and ferromanganese crusts have helped define the history of water masses in the region. Here we provide the first 3-D simulations of ɛNd responses to the shoaling seaway. Our model suggests that a narrow and shallow seaway is sufficient to affect interoceanic circulation, that inflow/outflow balance between the Caribbean and the Antilles responds nonlinearly to sill depth, and that a seaway narrower than 400 km is consistent with an active Atlantic meridional overturning circulation during the late Miocene. Simulated ɛNd values in the Caribbean confirm that inputs from radiogenic Pacific waters in the Caribbean decrease as the seaway shoals. Despite model limitations, a comparison between our results and ɛNd values recorded in the Caribbean helps constrain the depth of the Central American Seaway through time, and we infer that a depth between 50 and 200 m could have been reached 10 Ma ago.

  19. New determination of the vapour pressures of the isotopes of neon

    International Nuclear Information System (INIS)

    Roth, R.

    1960-03-01

    We have undertaken an experimental reinvestigation of the vapor pressures of the neon isotopes over the temperature range 16.30-30.1 deg. K. Measurements were made by differential manometry in a Giauque-Johnston type cryostat modified for temperature stability. The New sample contained 99.9 % Ne 20 and the Ne 22 sample contained 72,2 % Ne 22 . Extrapolation to pure Ne 20 and Ne 22 can be made with sufficient accuracy by the use of Raoult's law. Our results are in substantial agreement with those of Keesom and Haantjes. At 20 deg. K, where the scatter in our data is an order of magnitude smaller than in the data of Keesom and Haantjes, we find In P Ne 20 /P Ne 22 is 6 % larger than the smoothed line given by them. For solid neon, our data can be represented to a high accuracy by a Debye harmonic lattice with θ D (Ne 20 ) = 74.6 deg. K. The result may be compared with the value obtained by Henshaw from the Debye-Waller temperature factor, θ D = 73 deg. K, and with the recent calculation of the zero point energy of Ne by Bernardes, from which he obtains θ D 8E θ /9R = 73 deg.. K. (author) [fr

  20. Quantitative determination of cyclobutane thymine dimers in DNA by stable isotope-dilution mass spectrometry

    International Nuclear Information System (INIS)

    Podmore, I.D.; Cooke, M.S.; Herbert, K.E.; Lunec, J.

    1996-01-01

    In order to understand the role of UV-induced DNA lesions in biological processes such as mutagenesis and carcinogenesis, it is essential to detect and quantify DNA damage in cells. In this paper we present a novel and both highly selective and sensitive assay using capillary gas chromatography (GC) combined with mass spectrometry (MS) for the detection and accurate quantitation of a major product of UV-induced DNA damage (cis-syb cyclobutadithymine). Quantitation of the cyclobutane thymine dimer was achieved by the use of an internal standard in the form of a stable 2 H-labeled analogue. Both isotopically labeled and nonlabeled dimers were prepared directly from their corresponding monomers. Each was identified as their trimethylsilyl ether derivative by GC-MS. Calibration plots were obtained for known quantities of both nonlabeled and analyte and internal standard. Quantitation of cis-syn cyclobutadithymine was demonstrated in DNA exposed to UVC radiation over a dose range of 0 3500 J m -2 . Under the conditions used, the limit of detection was found to be 20-50 fmol on column (equivalent to 0.002-0.005 nmol dimer per mg DNA). The results of the present study indicate that capillary GC-MS is an ideally suited technique for selective and sensitive quantification of cis-syn cyclobutadithymine in DNA and hence UV-induced DNA damage. (author)

  1. Selectively dispersed isotope labeling for protein structure determination by magic angle spinning NMR

    Energy Technology Data Exchange (ETDEWEB)

    Eddy, Matthew T. [Massachusetts Institute of Technology, Department of Chemistry (United States); Belenky, Marina [Brandeis University, Department of Chemistry (United States); Sivertsen, Astrid C. [Massachusetts Institute of Technology, Francis Bitter Magnet Laboratory (United States); Griffin, Robert G. [Massachusetts Institute of Technology, Department of Chemistry (United States); Herzfeld, Judith, E-mail: herzfeld@brandeis.edu [Brandeis University, Department of Chemistry (United States)

    2013-10-15

    The power of nuclear magnetic resonance spectroscopy derives from its site-specific access to chemical, structural and dynamic information. However, the corresponding multiplicity of interactions can be difficult to tease apart. Complimentary approaches involve spectral editing on the one hand and selective isotope substitution on the other. Here we present a new 'redox' approach to the latter: acetate is chosen as the sole carbon source for the extreme oxidation numbers of its two carbons. Consistent with conventional anabolic pathways for the amino acids, [1-{sup 13}C] acetate does not label {alpha} carbons, labels other aliphatic carbons and the aromatic carbons very selectively, and labels the carboxyl carbons heavily. The benefits of this labeling scheme are exemplified by magic angle spinning spectra of microcrystalline immunoglobulin binding protein G (GB1): the elimination of most J-couplings and one- and two-bond dipolar couplings provides narrow signals and long-range, intra- and inter-residue, recoupling essential for distance constraints. Inverse redox labeling, from [2-{sup 13}C] acetate, is also expected to be useful: although it retains one-bond couplings in the sidechains, the removal of CA-CO coupling in the backbone should improve the resolution of NCACX spectra.

  2. On-line ion exchange preconcentration in a sequential injection lab-on-valve microsystem incorporating a renewable column with ETAAS for the trace-level determination of bismuth in urine and river sediment

    DEFF Research Database (Denmark)

    Wang, Jianhua; Hansen, Elo Harald

    2001-01-01

    A sequential injection system for on-line ion-exchange separation and preconcentration of trace-level amounts of metal ions with ensuing detection by electrothermal atomic absorption spectrometry (ETAAS) is described. Based on the use of a renewable microcolumn incorporated within an integrated l.......3% for the determination of 2.0 mug/l Bi (n = 7). The procedure was validated by determination of bismuth in a certified reference material CRM 320 (river sediment), and by bismuth spike recoveries in two human urine samples....

  3. Hydrogen isotope determination by TC/EA technique in application to volcanic glass as a window into secondary hydration

    Science.gov (United States)

    Martin, Erwan; Bindeman, Ilya; Balan, Etienne; Palandri, Jim; Seligman, Angela; Villemant, Benoit

    2017-12-01

    The use of volcanic glass as recorder of paleoenvironmental conditions has existed for 30 years. In this paper we investigate the methodological aspects of the determination of water content, isotopic composition, and water speciation in volcanic glass using the High Temperature Conversion/Elemental Analyzer (TCEA) mass spectrometer system on milligram quantities of glass concentrates. It is shown here that the precision and the reproducibility of this method is comparable to off-line conventional methods that require 100 times greater amount of material (δD ± 3‰; [H2O]tot ± 10relative% if 1 wt%) but is quicker and permits easy replication. This method extracts 100% of the water as verified by FTIR measurements. Finally, this study confirms the interest of DRIFT spectroscopy in the NIR range for the study of porous samples such as volcanic pumices and tephra, to determine the water speciation (H2O/OH). It may complement conventional FTIR transmission measurements in the MIR or NIR range that usually require homogeneous transparent sections or high degree of sample dilution in a non-absorbing matrix. Using these methods, we attempt to discriminate residual magmatic from secondary meteoric water in volcanic glass. Using mafic to differentiated samples from different geological settings and different climatic conditions, we show that the H-isotope composition and water content of volcanic glass alone are not always sufficient to provide clear distinction between magmatic and meteoric origin. However if the magma is known to have a δD between - 90‰ and - 40‰ (- 60‰ for MORB mantle source), it is quite easy to resolve the δD evolution during magmatic degassing from post-depositional rehydration by meteoric water with δD - 20‰. Water speciation measurements may provide additional information. In most cases, isotopic and total water measurements should be complemented by characterization of water speciation. During magmatic degassing (from 6 wt% to 0.1 wt

  4. Understanding the role of fog in forest hydrology: Stable isotopes as tools for determining input and partitioning of cloud water in montane forests

    Science.gov (United States)

    Scholl, M.; Eugster, W.; Burkard, R.

    2011-01-01

    Understanding the hydrology of tropical montane cloud forests (TMCF) has become essential as deforestation of mountain areas proceeds at an increased rate worldwide. Passive and active cloud-water collectors, throughfall and stemflow collectors, visibility or droplet size measurements, and micrometeorological sensors are typically used to measure the fog water inputs to ecosystems. In addition, stable isotopes may be used as a natural tracer for fog and rain. Previous studies have shown that the isotopic signature of fog tends to be more enriched in the heavier isotopes 2H and 18O than that of rain, due to differences in condensation temperature and history. Differences between fog and rain isotopes are largest when rain is from synoptic-scale storms, and fog or orographic cloud water is generated locally. Smaller isotopic differences have been observed between rain and fog on mountains with orographic clouds, but only a few studies have been conducted. Quantifying fog deposition using isotope methods is more difficult in forests receiving mixed precipitation, because of limitations in the ability of sampling equipment to separate fog from rain, and because fog and rain may, under some conditions, have similar isotopic composition. This article describes the various types of fog most relevant to montane cloud forests and the importance of fog water deposition in the hydrologic budget. A brief overview of isotope hydrology provides the background needed to understand isotope applications in cloud forests. A summary of previous work explains isotopic differences between rain and fog in different environments, and how monitoring the isotopic signature of surface water, soil water and tree xylem water can yield estimates of the contribution of fog water to streamflow, groundwater recharge and transpiration. Next, instrumentation to measure fog and rain, and methods to determine isotopic concentrations in plant and soil water are discussed. The article concludes with

  5. Determination of vanadium, manganese and tungsten in steels with an 241 Am-Be isotopic neutron source

    International Nuclear Information System (INIS)

    Galdino, S.M.L.

    1985-09-01

    A non-destructive neutron activation method was developed for determination of vanadium, manganese, and tungsten in alloy-steel, with the aid of an Am-Be 1,85x10 11 Bq(5Ci) isotopic neutron source, employing NaI (T1) detector well type 2x2 in. The 51 V (n,γ) 52 V, 55 Mn (n,γ) 56 Mn, and 186 W (n,γ) 187 W nuclear reactions are induced in steel samples subject to activation by thermal neutron. After irradiation, the activity of the samples was measured by γ-spectrometry under the 1434 KeV 52 V, 847KeV 56 Mn, and 686 KeV 187 W photopeaks. Possible interferences due to other radionuclides activity were investigated by determining the 52 V, 56 Mn, and 187 W half-lifes. The time of analysis for vanadium determination was 11 min, with 1,5% of precision and 3,4% of average absolute deviation. The time of analysis for manganese determination was 22,8 min with 4,0% of precision and 3,4% of average absolute deviation. The time of analysis for tungsten determination was 44,62 min with 3,8% of precision and 3,1% of average absolute deviation. The activation analysis method is adequated for steel quality control in industry. (Author) [pt

  6. Multi-element determination in environmental samples by mass spectrometric isotope dilution analysis using thermal ionization. Pt. 2

    International Nuclear Information System (INIS)

    Hilpert, K.; Waidmann, E.

    1988-01-01

    An analytical procedure for the multi-element analysis of the elements Fe, Ni, Cu, Zn, Ga, Rb, Sr, Cd, Ba, Tl, and Pb in pine needles by mass spectrometric isotope dilution analysis using thermal ionization has been reported in Part I of this paper. This procedure is now transferred to the non-vegetable material 'Oyster Tissue' (Standard Reference Material 1566, National Bureau of Standards, USA). By a modification of the analytical procedure, it was possible to determine Cr in this material in addition to the aforementioned elements. No concentrations are certified for the elements Ga, Ba and Tl analyzed in this work. The concentrations of the remaining elements obtained by the multi-element analysis agree well with those certified. (orig.)

  7. Application of in situ current normalized PIGE method for determination of total boron and its isotopic composition

    International Nuclear Information System (INIS)

    Chhillar, Sumit; Acharya, R.; Sodaye, S.; Pujari, P.K.

    2014-01-01

    A particle induced gamma-ray emission (PIGE) method using proton beam has been standardized for determination of isotopic composition of natural boron and enriched boron samples. Target pellets of boron standard and samples were prepared in cellulose matrix. The prompt gamma rays of 429 keV, 718 keV and 2125 keV were measured from 10 B(p,αγ) 7 Be, 10 B(p, p'γ) 10 B and 11 B(p, p'γ) 11 B nuclear reactions, respectively. For normalizing the beam current variations in situ current normalization method was used. Validation of method was carried out using synthetic samples of boron carbide, borax, borazine and lithium metaborate in cellulose matrix. (author)

  8. Determination of radium and uranium isotopes in natural waters by sorption on hydrous manganese dioxide followed by alpha-spectrometry

    International Nuclear Information System (INIS)

    Bojanowski, R.; Radecki, Z.; Burns, K.

    2005-01-01

    Water samples, spiked with 133 Ba and 232 U radiotracers, are scavenged for radium and uranium isotopes using hydrous manganese dioxide which is produced in-situ, by reacting manganese (+2) and permanganate ions at pH 8-9. The precipitate is solubilized with ascorbic and acetic acids and the resulting solution filtered through a glass fibre filter GF/F to remove particulate matter. The radium is co-precipitated with barium ions by the addition of a saturated Na 2 SO 4 solution where a small amount of BaSO 4 suspension is introduced to initiate crystallization. The micro precipitate containing the radium is collected on a 0.1 membrane filter and the filtrate saved for follow-up uranium analysis. The 226 Ra on the filter is determined by alpha-spectrometry and its recovery is assessed by measuring the 133 Ba on the same filter using gamma-spectrometry. The filtrate containing uranium is passed through a Dowex AG 1 x 4 ion-exchange resin in the SO 4 2- form which retains uranium while other ions are eluted by dilute (0.25M) sulphuric acid. Uranium is eluted from the column by distilled water, electrodeposited on a silver disc and the uranium isotopes and their recovery are determined by alpha-spectrometry. The method was tested on a variety of natural and spiked water samples with known concentrations of 226 Ra and 238 U and was found to yield accurate results within ±10% RSD of the target values. (author)

  9. Geochemical and isotopic determination of deep groundwater contributions and salinity to the shallow groundwater and surface water systems, Mesilla Basin, New Mexico, Texas, and Mexico

    Science.gov (United States)

    Robertson, A.; Carroll, K. C.; Kubicki, C.; Purtshert, R.

    2017-12-01

    The Mesilla Basin/Conejos-Médanos aquifer system, extending from southern New Mexico to Chihuahua, Mexico, is a priority transboundary aquifer under the 2006 United States­-Mexico Transboundary Aquifer Assessment Act. Declining water levels, deteriorating water quality, and increasing groundwater use by municipal, industrial, and agricultural users on both sides of the international border raise concerns about long-term aquifer sustainability. Relative contributions of present-day and "paleo" recharge to sustainable fresh groundwater yields has not been determined and evidence suggests that a large source of salinity at the distal end of the Mesilla Basin is saline discharge from deep groundwater flow. The magnitude and distribution of those deep saline flow paths are not determined. The contribution of deep groundwater to discharge and salinity in the shallow groundwater and surface water of the Mesilla Basin will be determined by collecting discrete groundwater samples and analyzing for aqueous geochemical and isotopic tracers, as well as the radioisotopes of argon and krypton. Analytes include major ions, trace elements, the stable isotopes of water, strontium and boron isotopes, uranium isotopes, the carbon isotopes of dissolved inorganic carbon, noble gas concentrations and helium isotope ratios. Dissolved gases are extracted and captured from groundwater wells using membrane contactors in a process known as ultra-trace sampling. Gas samples are analyzed for radioisotope ratios of krypton by the ATTA method and argon by low-level counting. Effectiveness of the ultra-trace sampling device and method was evaluated by comparing results of tritium concentrations to the krypton-85 content. Good agreement between the analyses, especially in samples with undetectable tritium, indicates that the ultra-trace procedure is effective and confirms that introduction of atmospheric air has not occurred. The geochemistry data indicate a complex system of geochemical

  10. Determining the speciation of Zn in soils around the sediment ponds of chemical plants by XRD and XAFS spectroscopy and sequential extraction.

    Science.gov (United States)

    Minkina, Tatiana; Nevidomskaya, Dina; Bauer, Tatiana; Shuvaeva, Victoria; Soldatov, Alexander; Mandzhieva, Saglara; Zubavichus, Yan; Trigub, Alexander

    2018-09-01

    For a correct assessment of risk of polluted soil, it is crucial to establish the speciation and mobility of the contaminants. The aim of this study was to investigate the speciation and transformation of Zn in strongly technogenically transformed contaminated Spolic Technosols for a long time in territory of sludge collectors by combining analytical techniques and synchrotron techniques. Sequential fractionation of Zn compounds in studied soils revealed increasing metal mobility. Phyllosilicates and Fe and Mn hydroxides were the main stabilizers of Zn mobility. A high degree of transformation was identified for the composition of the mineral phase in Spolic Technosols by X-ray powder diffraction. Technogenic phases (Zn-containing authigenic minerals) were revealed in Spolic Technosols samples through the analysis of their Zn K-edge EXAFS and XANES spectra. In one of the samples Zn local environment was formed by predominantly oxygen atoms, and in the other one mixed ZnS and ZnO bonding was found. Zn speciation in the studied technogenically transformed soils was due to the composition of pollutants contaminating the floodplain landscapes for a long time, and, second, this is the combination of physicochemical properties controlling the buffer properties of investigated soils. X-ray spectroscopic and X-ray powder diffraction analyses combined with sequential extraction assays is an effective tool to check the affinity of the soil components for heavy metal cations. Copyright © 2018 Elsevier B.V. All rights reserved.

  11. Sequential charged particle reaction

    International Nuclear Information System (INIS)

    Hori, Jun-ichi; Ochiai, Kentaro; Sato, Satoshi; Yamauchi, Michinori; Nishitani, Takeo

    2004-01-01

    The effective cross sections for producing the sequential reaction products in F82H, pure vanadium and LiF with respect to the 14.9-MeV neutron were obtained and compared with the estimation ones. Since the sequential reactions depend on the secondary charged particles behavior, the effective cross sections are corresponding to the target nuclei and the material composition. The effective cross sections were also estimated by using the EAF-libraries and compared with the experimental ones. There were large discrepancies between estimated and experimental values. Additionally, we showed the contribution of the sequential reaction on the induced activity and dose rate in the boundary region with water. From the present study, it has been clarified that the sequential reactions are of great importance to evaluate the dose rates around the surface of cooling pipe and the activated corrosion products. (author)

  12. Sm isotope composition and Sm/Eu ratio determination in an irradiated 153Eu sample by ion exchange chromatography-quadrupole inductively coupled plasma mass spectrometry combined with double spike isotope dilution technique

    International Nuclear Information System (INIS)

    Bourgeois, M.; Isnard, H.; Gourgiotis, A.; Stadelmann, G.; Gautier, C.; Mialle, S.; Nonell, A.; Chartier, F.

    2011-01-01

    Within the framework of the research undertaken by the French Atomic Energy Commission on transmutation of long-lived radionuclides, targets of highly enriched actinides and fission products were irradiated in the fast neutron reactor Phenix. Precise and accurate measurements of the isotopic and elemental composition of the enriched elements are therefore required. In order to obtain the uncertainties of several per mil and to reduce handling time and exposure to analyst on radioactive material, the on-line coupling of ion exchange chromatography with quadrupole inductively coupled plasma mass spectrometry has been associated with the technique of the double spike isotope dilution. We present in this paper the results obtained on an irradiated sample of Europium oxide powder (enriched at 99.13% in 153 Eu). After irradiation of around 5 mg of Eu 2 O 3 powder the theoretical calculations predict the formation of several micrograms of gadolinium and samarium isotopes. In relation to the very high activity of the sample after irradiation and the very low quantity of Sm formed, the on-line ion exchange chromatography separation of Gd, Sm and Eu before Sm isotope ratio measurements has been developed for the quantification of the 152 Sm/ 153 Eu ratio. These on-line measurements were associated with the double spike isotope dilution technique after calibration of a 147 Sm/ 151 Eu spike solution. The external reproducibility of Sm isotopic ratios was determined to be around 0.5% (2 σ) resulting in a final uncertainty on the 152 Sm/ 153 Eu ratio of around 1% (2 σ). These on-line measurements present therefore a robust and high-throughput alternative to the thermal-ionisation mass spectrometry technique used so far in combination with off-line chromatographic separation, particularly in nuclear applications where characterisation of high activity sample solutions is required. (authors)

  13. Determination of niobium in rocks by an isotope dilution spectrophotometric method

    Science.gov (United States)

    Greenland, L.P.; Campbell, E.Y.

    1970-01-01

    Rocks and minerals are fused with sodium peroxide in the presence of carrierfree 95Nb. The fusion cake is leached with water and the precipitate dissolved in hydrofluoric-sulfuric acid mixture. Niobium is extracted into methyl isobutyl ketone and further purified by ion exchange. The amount of niobium is determined spectrophotometrically with 4-(2-pyridylazo)-resorcinol, and the chemical yield of the separations determined by counting 95Nb. This procedure is faster and less sensitive to interferences than previously proposed methods for determining niobium in rocks.The high purity of the separated niobium makes the method applicable to nearly all matrices. ?? 1970.

  14. The HP 9825 A program for the determination of an isotope half-life

    International Nuclear Information System (INIS)

    Jujuratisbela, Uju.

    1980-01-01

    Determination of half life of gold 198, indium 116, manganese 56, copper 64 are presented, using least squares method in HP 9825 A. This method is more accurate and needs less time than graphic method. (author tr.)

  15. Accurate determination of selected pesticides in soya beans by liquid chromatography coupled to isotope dilution mass spectrometry.

    Science.gov (United States)

    Huertas Pérez, J F; Sejerøe-Olsen, B; Fernández Alba, A R; Schimmel, H; Dabrio, M

    2015-05-01

    A sensitive, accurate and simple liquid chromatography coupled with mass spectrometry method for the determination of 10 selected pesticides in soya beans has been developed and validated. The method is intended for use during the characterization of selected pesticides in a reference material. In this process, high accuracy and appropriate uncertainty levels associated to the analytical measurements are of utmost importance. The analytical procedure is based on sample extraction by the use of a modified QuEChERS (quick, easy, cheap, effective, rugged, safe) extraction and subsequent clean-up of the extract with C18, PSA and Florisil. Analytes were separated on a C18 column using gradient elution with water-methanol/2.5 mM ammonium acetate mobile phase, and finally identified and quantified by triple quadrupole mass spectrometry in the multiple reaction monitoring mode (MRM). Reliable and accurate quantification of the analytes was achieved by means of stable isotope-labelled analogues employed as internal standards (IS) and calibration with pure substance solutions containing both, the isotopically labelled and native compounds. Exceptions were made for thiodicarb and malaoxon where the isotopically labelled congeners were not commercially available at the time of analysis. For the quantification of those compounds methomyl-(13)C2(15)N and malathion-D10 were used respectively. The method was validated according to the general principles covered by DG SANCO guidelines. However, validation criteria were set more stringently. Mean recoveries were in the range of 86-103% with RSDs lower than 8.1%. Repeatability and intermediate precision were in the range of 3.9-7.6% and 1.9-8.7% respectively. LODs were theoretically estimated and experimentally confirmed to be in the range 0.001-0.005 mg kg(-1) in the matrix, while LOQs established as the lowest spiking mass fractionation level were in the range 0.01-0.05 mg kg(-1). The method reliably identifies and quantifies the

  16. Accurate experimental determination of the isotope effects on the triple point temperature of water. I. Dependence on the 2H abundance

    Science.gov (United States)

    Faghihi, V.; Peruzzi, A.; Aerts-Bijma, A. T.; Jansen, H. G.; Spriensma, J. J.; van Geel, J.; Meijer, H. A. J.

    2015-12-01

    Variation in the isotopic composition of water is one of the major contributors to uncertainty in the realization of the triple point of water (TPW). Although the dependence of the TPW on the isotopic composition of the water has been known for years, there is still a lack of a detailed and accurate experimental determination of the values for the correction constants. This paper is the first of two articles (Part I and Part II) that address quantification of isotope abundance effects on the triple point temperature of water. In this paper, we describe our experimental assessment of the 2H isotope effect. We manufactured five triple point cells with prepared water mixtures with a range of 2H isotopic abundances encompassing widely the natural abundance range, while the 18O and 17O isotopic abundance were kept approximately constant and the 18O  -  17O ratio was close to the Meijer-Li relationship for natural waters. The selected range of 2H isotopic abundances led to cells that realised TPW temperatures between approximately  -140 μK to  +2500 μK with respect to the TPW temperature as realized by VSMOW (Vienna Standard Mean Ocean Water). Our experiment led to determination of the value for the δ2H correction parameter of A2H  =  673 μK / (‰ deviation of δ2H from VSMOW) with a combined uncertainty of 4 μK (k  =  1, or 1σ).

  17. Determination of gas recovery efficiency at two Danish landfills by performing downwind methane measurements and stable carbon isotopic analysis

    DEFF Research Database (Denmark)

    Fathi Aghdam, Ehsan; Fredenslund, Anders Michael; Chanton, Jeffrey

    2018-01-01

    In this study, the total methane (CH4) generation rate and gas recovery efficiency at two Danish landfills were determined by field measurements. The landfills are located close to each other and are connected to the same gas collection system. The tracer gas dispersion method was used...... for quantification of CH4 emissions from the landfills, while the CH4 oxidation efficiency in the landfill cover layers was determined by stable carbon isotopic technique. The total CH4 generation rate was estimated by a first-order decay model (Afvalzorg) and was compared with the total CH4 generation rate...... determined by field measurements. CH4 emissions from the two landfills combined ranged from 29.1 to 49.6 kg CH4/h. The CH4 oxidation efficiency was 6–37%, with an average of 18% corresponding to an average CH4 oxidation rate of 8.1 kg CH4/h. The calculated gas recovery efficiency was 59–76%, indicating...

  18. Determination of the mechanism of demethylenation of (methylenedioxy)phenyl compounds by cytochrome P450 using deuterium isotope effects

    International Nuclear Information System (INIS)

    Fukuto, J.M.; Kumagai, Y.; Cho, A.K.

    1991-01-01

    The mechanism of demethylenation of (methylenedioxy)benzene (MDB), (methylenedioxy)amphetamine (MDA), and (methylenedioxy)methamphetamine (MDMA) by purified rabbit liver cytochrome P450IIB4 has been investigated by using deuterium isotope effects. A comparison of the magnitude and direction of the observed kinetic isotope effects indicates that the three compounds are demethylenated by different mechanisms. The different mechanisms of demethylenation have been proposed on the basis of comparisons of the observed biochemical isotope effects with the isotope effects from purely chemical systems

  19. Understanding N timing in corn yield and fertilizer N recovery: An insight from an isotopic labeled-N determination

    Science.gov (United States)

    de Almeida, Rodrigo Estevam Munhoz; Pierozan Junior, Clovis; Lago, Bruno Cocco; Trivelin, Paulo Cesar Ocheuze

    2018-01-01

    Early fertilizer nitrogen (N) application on cover crops or their residues during the off-season is a practice adopted in Brazil subtropical conditions under no-tillage corn (Zea mays L.) systems. However, the effect of early N application on yield, plant N content, and N recovery efficiency (NRE) for corn is not yet well documented. Five fertilizer N timings in an oat-corn system were evaluated in two studies utilizing an isotopic-labeled N determination, 15N isotope. The N fertilization timings were: (i) oat tillering, (ii) 15 days before corn planting time, over the oat residues, (iii) at corn planting time, (iv) in-season at the three-leaf growth stage (V3), and (v) in-season split application at V3 and six-leaf (V6) growth stages. Based on the statistical analysis, the N fertilization timings were separated into three groups: 1) N-OATS, designated to N applied at oat; 2) N-PLANT, referred to pre-plant and planting N applications; and 3) N-CORN, designated to in-season corn N applications. Corn yield was not affected by the N fertilization timing. However, the N-CORN N fertilization timings enhanced NRE by 17% and 35% and final N recovery system (plant plus soil) by 16% and 24% all relative to N-OATS and N-PLANT groups, respectively. Overall, N-OATS resulted in the largest N derived from fertilizer (NDFF) amount in the deeper soil layer, in overall a delta of 10 kg N ha-1 relative to the rest of the groups. Notwithstanding corn yield was not affected, early N fertilization under subtropical conditions is not a viable option since NRE was diminished and the non-recovery N increased relative to the in-season N applications. PMID:29462178

  20. Determination of ultratrace levels of tributyltin in waters by isotope dilution and gas chromatography coupled to tandem mass spectrometry.

    Science.gov (United States)

    Rodríguez-Cea, Andrés; Rodríguez-González, Pablo; Font Cardona, Nuria; Aranda Mares, José Luís; Ballester Nebot, Salomé; García Alonso, J Ignacio

    2015-12-18

    The current EU legislation lays down the Environmental Quality Standards (EQS) of 45 priority substances in surface water bodies. In particular, the concentration of tributyltin (TBT) must not exceed 0.2ngL(-1) and analytical methodologies with a Limit of Quantification (LOQ) equal or below 0.06ngL(-1) are urged to be developed. This work presents a procedure for the determination of ultratrace levels of TBT in water samples by Isotope Dilution and GC-MS/MS operating in Selected Reaction Monitoring (SRM) mode which meets current EU requirements. The method requires the monitorization of five consecutive transitions (287>175 to 291>179) for the sensitive and selective detection of TBT. The measured isotopic distribution of TBT fragment ions was in agreement with the theoretical values computed by a polynomial expansion algorithm. The combined use of Tandem Mass Spectrometry, a sample volume of 250mL, the preconcentration of 1mL of organic phase to 30μL and an injection volume of 25μL by Programmed Temperature Vaporization provided a LOQ of 0.0426ngL(-1) for TBT (calculated as ten times the standard deviation of nine independent blanks). The recovery for TBT calculated in Milli-Q water at the EQS level was 106.3±4%. A similar procedure was also developed for the quantification of dibutyltin (DBT) and monobutyltin (MBT) in water samples showing satisfactory results. The method was finally implemented in a routine testing laboratory to demonstrate its applicability to real samples obtaining quantitative recoveries for TBT at the EQS level in mineral water, river water and seawater. Copyright © 2015 Elsevier B.V. All rights reserved.

  1. Understanding N timing in corn yield and fertilizer N recovery: An insight from an isotopic labeled-N determination.

    Science.gov (United States)

    Maciel de Oliveira, Silas; Almeida, Rodrigo Estevam Munhoz de; Ciampitti, Ignacio A; Pierozan Junior, Clovis; Lago, Bruno Cocco; Trivelin, Paulo Cesar Ocheuze; Favarin, José Laércio

    2018-01-01

    Early fertilizer nitrogen (N) application on cover crops or their residues during the off-season is a practice adopted in Brazil subtropical conditions under no-tillage corn (Zea mays L.) systems. However, the effect of early N application on yield, plant N content, and N recovery efficiency (NRE) for corn is not yet well documented. Five fertilizer N timings in an oat-corn system were evaluated in two studies utilizing an isotopic-labeled N determination, 15N isotope. The N fertilization timings were: (i) oat tillering, (ii) 15 days before corn planting time, over the oat residues, (iii) at corn planting time, (iv) in-season at the three-leaf growth stage (V3), and (v) in-season split application at V3 and six-leaf (V6) growth stages. Based on the statistical analysis, the N fertilization timings were separated into three groups: 1) N-OATS, designated to N applied at oat; 2) N-PLANT, referred to pre-plant and planting N applications; and 3) N-CORN, designated to in-season corn N applications. Corn yield was not affected by the N fertilization timing. However, the N-CORN N fertilization timings enhanced NRE by 17% and 35% and final N recovery system (plant plus soil) by 16% and 24% all relative to N-OATS and N-PLANT groups, respectively. Overall, N-OATS resulted in the largest N derived from fertilizer (NDFF) amount in the deeper soil layer, in overall a delta of 10 kg N ha-1 relative to the rest of the groups. Notwithstanding corn yield was not affected, early N fertilization under subtropical conditions is not a viable option since NRE was diminished and the non-recovery N increased relative to the in-season N applications.

  2. Double-label autoradiographic deoxyglucose method for sequential measurement of regional cerebral glucose utilization

    Energy Technology Data Exchange (ETDEWEB)

    Redies, C; Diksic, M; Evans, A C; Gjedde, A; Yamamoto, Y L

    1987-08-01

    A new double-label autoradiographic glucose analog method for the sequential measurement of altered regional cerebral metabolic rates for glucose in the same animal is presented. This method is based on the sequential injection of two boluses of glucose tracer labeled with two different isotopes (short-lived /sup 18/F and long-lived /sup 3/H, respectively). An operational equation is derived which allows the determination of glucose utilization for the time period before the injection of the second tracer; this equation corrects for accumulation and loss of the first tracer from the metabolic pool occurring after the injection of the second tracer. An error analysis of this operational equation is performed. The double-label deoxyglucose method is validated in the primary somatosensory (''barrel'') cortex of the anesthetized rat. Two different rows of whiskers were stimulated sequentially in each rat; the two periods of stimulation were each preceded by an injection of glucose tracer. After decapitation, dried brain slices were first exposed, in direct contact, to standard X-ray film and then to uncoated, ''tritium-sensitive'' film. Results show that the double-label deoxyglucose method proposed in this paper allows the quantification and complete separation of glucose utilization patterns elicited by two different stimulations sequentially applied in the same animal.

  3. The maximum entropy determination of nuclear densities of calcium isotopes from elastic scattering of alpha particles

    International Nuclear Information System (INIS)

    Engel, Y.M.; Friedman, E.; Levine, R.D.

    1982-01-01

    Radial moments of the real part of the optical potential for elastic scattering of 104 MeV α particles are used as constraints, in determining the nuclear density of maximal entropy. The potential is related to the density by the folding model. (orig.)

  4. Determination of the isotope distribution in 14C-labelled hydrocarbons by thermal fragmentation

    International Nuclear Information System (INIS)

    Kopinke, F.D.; Dermietzel, J.; Jockisch, W.; Raeuber, G.

    1986-01-01

    The gas chromatographic analysis of pyrolysis products of properly labelled hydrocarbons allows a definite and quantitative determination of the 14 C-distribution in those compounds. For this purpose a simple, fast, and versatilely applicable method has been developed and described

  5. Measurement of zinc stable isotope ratios in biogeochemical matrices by double-spike MC-ICPMS and determination of the isotope ratio pool available for plants from soil.

    Science.gov (United States)

    Arnold, Tim; Schönbächler, Maria; Rehkämper, Mark; Dong, Schuofei; Zhao, Fang-Jie; Kirk, Guy J D; Coles, Barry J; Weiss, Dominik J

    2010-12-01

    Analysis of naturally occurring isotopic variations is a promising tool for investigating Zn transport and cycling in geological and biological settings. Here, we present the recently installed double-spike (DS) technique at the MAGIC laboratories at Imperial College London. The procedure improves on previous published DS methods in terms of ease of measurement and precisions obtained. The analytical method involves addition of a (64)Zn-(67)Zn double-spike to the samples prior to digestion, separation of Zn from the sample matrix by ion exchange chromatography, and isotopic analysis by multiple-collector inductively coupled plasma mass spectrometry. The accuracy and reproducibility of the method were validated by analyses of several in-house and international elemental reference materials. Multiple analyses of pure Zn standard solutions consistently yielded a reproducibility of about ±0.05‰ (2 SD) for δ(66)Zn, and comparable precisions were obtained for analyses of geological and biological materials. Highly fractionated Zn standards analyzed by DS and standard sample bracketing yield slightly varying results, which probably originate from repetitive fractionation events during manufacture of the standards. However, the δ(66)Zn values (all reported relative to JMC Lyon Zn) for two less fractionated in-house Zn standard solutions, Imperial Zn (0.10 ± 0.08‰: 2 SD) and London Zn (0.08 ± 0.04‰), are within uncertainties to data reported with different mass spectrometric techniques and instruments. Two standard reference materials, blend ore BCR 027 and ryegrass BCR 281, were also measured, and the δ(66)Zn were found to be 0.25 ± 0.06‰ (2 SD) and 0.40 ± 0.09‰, respectively. Taken together, these standard measurements ascertain that the double-spike methodology is suitable for accurate and precise Zn isotope analyses of a wide range of natural samples. The newly installed technique was consequently applied to soil samples and soil leachates to

  6. Standard test method for radiochemical determination of uranium isotopes in urine by alpha spectrometry

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2011-01-01

    1.1 This test method is applicable to the determination of uranium in urine at levels of detection dependent on sample size, count time, detector background, and tracer yield. It is designed as a screening tool for detection of possible exposure of occupational workers. 1.2 This test method is designed for 50 mL of urine. This test method does not address the sampling protocol or sample preservation methods associated with its use. 1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard. 1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

  7. Determination of radioactive emission origins based on analyses of isotopic composition

    International Nuclear Information System (INIS)

    Devell, L.

    1987-01-01

    The nature of radioactivity emissions can be determined through gamma spectroscopy of air samples with good precision, which means that the type of source of the emission may be found, e.g. nuclear weapons test, of nuclear power plant accident. Combined with information on wind trajectories it is normally possible to recognize time and area for the emission. In this preliminary study, the knowledge of and preparedness for such measurements are described. (L.E.)

  8. Determination of some trace elements in biological materials using the short living isotopes

    International Nuclear Information System (INIS)

    Taskaev, E.

    1985-01-01

    A method for determination of V, Cu, Rb, Mo and K in breast cancer tumors is described. Samples were irradiated with ICIS pneumatic irradiation system of University of London Reactor Centre for 5 min. with mixed neutron flux: 1,7.10 1 2 thermal neutrons.cm -2 .s -1 and 9.10 11 fast neutrons.cm -2 .s -1 . Wet ashing procedure of Byrne and Kosta was used for the dissolution. Consecutive separation procedures of V and Mo, Cu, Mn, K and Rb, followed by counting and activity measuring were carried out. In order to study the chemical yields for all the elements both animal and plant matrixes were used. The error of 3% ( 0.05 confidence level) for single determination of chemical yield was chosen as the highest value acceptable. The possibility of using 137-Cs tracer for K and Rb chemical yield determination was also checked. To check the whole procedure the standard reference materials SRM-1577 Bovine Liver, SRM-1571 Orchard Leaves and Bowen's Kale were analysed

  9. USE OF GC-MS/COMBUSTION/IRMS TO IDENTIFY AND DETERMINE THE STABLE CARBON ISOTOPIC RATIO OF INDIVIDUAL LIPIDS

    Science.gov (United States)

    A system that couples a gas chromatograph (GC) via a split to a quadrapole mass spectrometer (MS) and, through a combustion interface, to an isotope ratio mass spectrometer (IRMS) allows the simultaneous detection of electron impact mass spectra and stable carbon isotope ratio an...

  10. A new method for the determination of NO2 traces using isotope dilution and mass spectrometry analysis

    International Nuclear Information System (INIS)

    Stevens, C.; Barat, F.; Nguyen Nghi, H.

    1975-01-01

    A new method for the determination of NO 2 traces, in the order of 1ppb (10 -9 ), in atmosphere and stratosphere is described. The method consists in an isotope dilution technique using 15 NO 2 , followed by the reduction of NO 2 to N 2 and a mass spectrometry analysis. A known amount of 15 NO 2 is added to the air samples. Then, NO 2 is separated from H 2 O, HNO 3 , CO 2 and N 2 O and transferred to a SiO 2 reactor by trapping at -196 deg C. In the reactor NO 2 is reduced to N 2 by reaction with electrolytic Cu heated at 580 deg C. The mass 29/mass 30 ratio corresponding to 15 N 14 N and 15 N 15 N is determined by mass spectrometry. The sensitivity of the method depends on the contamination introduced during the analysis of the sample (reagents, separation and measuring devices). The contamination is reproducible and in the order of 4.5+-0.5 10 -2 mm 3 N 2 [fr

  11. Liquid chromatography with isotope-dilution mass spectrometry for determination of water-soluble vitamins in foods.

    Science.gov (United States)

    Phillips, Melissa M

    2015-04-01

    Vitamins are essential for improving and maintaining human health, and the main source of vitamins is the diet. Measurement of the quantities of water-soluble vitamins in common food materials is important to understand the impact of vitamin intake on human health, and also to provide necessary information for regulators to determine adequate intakes. Liquid chromatography (LC) and mass spectrometry (MS) based methods for water-soluble vitamin analysis are abundant in the literature, but most focus on only fortified foods or dietary supplements or allow determination of only a single vitamin. In this work, a method based on LC/MS and LC/MS/MS has been developed to allow simultaneous quantitation of eight water-soluble vitamins, including multiple forms of vitamins B3 and B6, in a variety of fortified and unfortified food-matrix Standard Reference Materials (SRMs). Optimization of extraction of unbound vitamin forms and confirmation using data from external laboratories ensured accuracy in the assigned values, and addition of stable isotope labeled internal standards for each of the vitamins allowed for increased precision.

  12. Determination of δ13C, δ15N, or δ34S by isotope-ratio-monitoring mass spectrometry using an elemental analyzer

    Science.gov (United States)

    Johnson, Craig A.; Stricker, Craig A.; Gulbransen, Cayce A.; Emmons, Matthew P.

    2018-02-14

    This report describes procedures used in the Geology, Geophysics, and Geochemistry Science Center of the U.S. Geological Survey in Denver, Colorado, to determine the stable-isotope ratios 13C/12C, 15N/14N, and 34S/32S in solid materials. The procedures use elemental analyzers connected directly to gas-source isotope-ratio mass spectrometers. A different elemental–analyzer–mass-spectrometer system is used for 13C/12C and 15N/14N than is used for 34S/32S to accommodate differences in reagents, catalysts, and instrument settings.

  13. Determination of 241Am in sediments by isotope dilution high resolution inductively coupled plasma mass spectrometry (ID HR ICP-MS).

    Science.gov (United States)

    Agarande, M; Benzoubir, S; Bouisset, P; Calmet, D

    2001-08-01

    Trace levels (pg kg(-1)) of 241Am in sediments were determined by isotope dilution high resolution inductively coupled plasma mass spectrometry (ID HR ICP-MS) using a microconcentric nebulizer. 241Am was isolated from major elements like Ca and Fe by different selective precipitations. In further steps. Am was first separated from other transuranic elements and purified by anion exchange and extraction chromatography prior to the mass spectrometric measurements. The ID HR ICP-MS results are compared with isotope dilution alpha spectrometry.

  14. Determination of plutonium isotopic abundances by gamma-ray spectrometry. Interim report on the status of methods and techniques developed by the Lawrence Livermore Laboratory

    International Nuclear Information System (INIS)

    Gunnink, R.

    1980-03-01

    This report presents an overview of methods and techniques developed by the Lawrence Livermore Laboratory for determining plutonium isotopic abundances from gamma-ray spectra that have been measured with germanium detectors. The methodology of fitting the spectral features includes discussions of algorithms for gamma-ray and x-ray peak shape fitting and generation of response spectra profiles characteristic of specific isotopes. Applications of the techniques developed at government, commercial, and Japanese reprocessing plants are described. Current development of the methodology for the nondestructive analysis of samples containing nondescript solid materials is also presented

  15. Nondestructive determination of burnup and fissile isotope balance in spent fuel assemblies of water cooled reactors

    International Nuclear Information System (INIS)

    Pinel, J.

    1983-03-01

    Two non-destructive methods for measuring fuel assemblies in storage pools have been developed: a gamma fuel scanning method, using the 134 Cs - 137 Cs and 144 Ce gamma rays, and the measurement of the neutron flux emitted by the fuel assembly. For interpreting the measurement, we have used calculated correlations to establish a connection between the measured phenomena and the parameters to be determined. A measurement campaign involving 58 assemblies from the C.N.A. reactor was conducted in the reprocessing plant of LA HAGUE. The results obtained show that the objectives can be achevied within an industrial environment [fr

  16. Determination of Isotopes Types and Activities in Radioactive Waste of Kosovo A Power Plant

    OpenAIRE

    , B Cena; , K Dollani; , G Hodolli

    2013-01-01

    The second nnportant event after the 1nventory of rad10act1ve waste 1n Kosovo, their location and the number of radioactive sources, is the determination of the type of radioisotope and their activities. This activity was conducted entirely in difŞcult terrain and was taken due to the absence in most cases of resource certiŞcates or any other document with the necessary information that will enable the identiŞcation of radioactive sources and their activity. In this way the activity was under...

  17. Chemical preparation of biological materials for accurate chromium determination by isotope dilution mass spectrometry

    International Nuclear Information System (INIS)

    Dunstan, L.P.; Garner, E.L.

    1977-01-01

    The current interest in trace elements in biological materials has created a need for accurate methods of analysis. The source of discrepancies and variations in chromium concentration determinations is often traceable to inadequate methods of sample preparation. Any method of Cr analysis that requires acid digestion of a biological matrix must take into consideration the existence or formation of a volatile Cr component. In addition, because Cr is often present at concentrations less than 1 μg/g, the analytical blank becomes a potential source of error. Chemical procedures have been developed for the digestion of the biological matrix and the separation of Cr without either large analytical blanks or significant losses by volatilization. These procedures have been used for the analysis of NBS Standard Reference Material (SRM) 1569 Brewers Yeast; SRM 1577 Bovine Liver; SRM 1570 Spinach and other biological materials including human hair and nails. At this time, samples containing 1 μg of Cr can be determined with an estimated accuracy of 2 percent

  18. Determination of enzyme-substrate dissociation rates by dynamic isotope exchange enhancement experiments

    International Nuclear Information System (INIS)

    Kim, S.C.; Raushel, F.M.

    1986-01-01

    A new method for the determination of dissociation rates of enzyme-substrate complexes has been developed. The rate of exchange of a labeled product back into the substrate is measured during catalysis of the forward reaction when the forward reaction is kept far from equilibrium by the enzymatic removal of the nonexchanging product. The ratio of the exchange rate and the net rate for product formation is then determined at various concentrations of the exchanging product. A plot of this ratio is a diagnostic indication of the kinetic mechanism and the relative rates of product dissociation from the binary and ternary enzyme complexes. This technique has been applied to the reaction catalyzed by bovine liver argininosuccinate lyase. The ratio for the rate of exchange of fumarate into argininosuccinate and the net rate for product formation was found to increase with the concentration of fumarate but to reach a limit of 3.3. The ratio of rates was half-maximal at 36 mM fumarate. The data have been interpreted to indicate the argininosuccinate lyase has a random kinetic mechanism. The calculated lower limit for the rate of release of arginine from the enzyme-fumarate-arginine complex is 0.35 times as fast as the Vmax in the reverse direction. The rate of release of arginine from the enzyme-arginine binary complex is 210 times faster than Vmax in the reverse direction

  19. Development of a portable mass spectrometric system for determination of isotopic composition of solid uranium samples using fluorine volatilization. Final report

    International Nuclear Information System (INIS)

    Loge, G.

    1994-01-01

    Using hardware and materials supplied by LANL, a prototype quadrupole mass spectrometer system designed for portable field analysis of isotopic composition of solid uranium samples was assembled and tested. The system contained the capability for fluorine volatilization of solid uranium samples with gas introduction, which was successfully tested and demonstrated using 100 mg samples of U 3 O 8 . Determination of precision and accuracy for measuring isotopic composition was performed using isotopic standards. Use with soil samples containing uranium were also attempted. Silicates in the soil forming SiF 4 were found to be a kinetic bottleneck to the formation of UF 6 . This could be avoided by performing some sort of chemical separation as a pre-treatment step, which was demonstrated using nitric acid

  20. Establishing Ideal Conditions for Complete Denitrification by Pseudomonas Aureofaciens - An Update on Determining Isotopic Composition of Dissolved Nitrate Using Bacterial Denitrification and Laser Spectroscopy

    International Nuclear Information System (INIS)

    Yi, Amelia Lee Zhi; Heiling, Maria; Toloza, Arsenio; Heng, Lee K.

    2017-01-01

    This serves as update on research entitled “Determining isotopic composition of dissolved nitrate using bacterial denitrification and laser spectroscopy” first published in the Vol. 39, No. 1, July 2016 SWMCN Soils Newsletter. In this research, isotopic δ"1"5N and δ"1"8O composition of dissolved nitrates is measured by laser spectroscopy after reduction of nitrate to N_2O by Pseudomonas aureofaciens. Quantifying the isotopic composition of nitrates in aqueous samples allows for better identification of potential nitrate sources, which in turn assists in remediation of nitrate-contaminated water and design of future agricultural management practises. The overall objective of the project is to establish a technical guide in the form of a standard operating procedure outlining best practises for denitrification method.

  1. Application of laser ablation inductively coupled plasma multicollector mass spectometry in determination of lead isotope ratios in common glass for forensic purposes

    International Nuclear Information System (INIS)

    Sjåstad, Knut-Endre; Andersen, Tom; Simonsen, Siri Lene

    2013-01-01

    Samples of glass used as trace evidence in criminal cases are commonly small, with particle sizes below a millimeter. To perform chemical analysis suitable for forensic purposes, methods capable of analyzing such small samples are required. In this paper, analyses of lead isotope ratios by means of laser ablation inductively coupled multicollector mass spectrometry (LA-MC-ICP-MS) are presented. Sampling by use of laser ablation allows fragments down to 0.1 mg to be analyzed with sufficient precision to discriminate between glasses of different origin. In fact, the use of lead isotopes determined by LA-MC-ICP-MS approaches the discrimination attainable by multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) analysis of dissolved samples of 5 mg or more. Further, we have obtained a probability distribution by two dimensional kernel density estimates for the collected data set as an alternative presentation method to the well-established bivariate plot. The underlying information available from kernel density estimates is of importance for forensic scientists involved in probabilistic interpretation of physical evidence. - Highlights: • Lead isotope ratios prove suitable to discriminate glass for forensic purposes. • 96% of glass samples from different sources were separated by lead isotopic ratios. • Laser ablation allows fragments of glass with extension of 0.5 mm to be analyzed. • Isotopic ratios of lead are well suited for statistical analysis of evidence

  2. [Determination of deuterium concentration in foods and influence of water with modified isotopic composition on oxidation parameters and heavy hydrogen isotopes content in experimental animals].

    Science.gov (United States)

    Basov, A A; Bykov, I M; Baryshev, M G; Dzhimak, S S; Bykov, M I

    2014-01-01

    The article presents the results of the study of the deuterium (D) content in food products as well as the influence of deuterium depleted water (DDW) on the concentration of heavy hydrogen isotopes in the blood and lyophilized tissues of rats. The most significant difference in the content of D was found between potato and pork fat, which indexes the standard delta notation (δ) D in promille, related to the international standard SMOW (Standard Mean Ocean of Water) amounted to -83,2 per thousand and -250,7 per thousand, respectively (phydrogen atoms in the body. The data obtained in the experimental modeling of the diet of male Wistar rats in the age of 5-6 mo (weight 235 ± 16 g) using DDW (δD = -743,2 per thousand) instead of drinking water (δD = -37,0 per thousand) with identical mineral composition showed that after 2 weeks significant (p tissue") is due to different rates ofisotopic exchange reactions in plasma and tissues (liver, kidney, heart), which can be explained by entering into the composition of a modified diet of organic substrates with more than DDW concentration D, which are involved in the construction of cellular structures and eventually lead to a redistribution of D and change direction of D/H gradient "plasmaisotopic composition, aimed at reducing the level of heavy non-radioactive atoms will allow the targeted nutritional correction of prooxidant-antioxidant status of the population in areas with adverse environmental conditions, stimulating by created isotopic D/H gradient cytoprotective mechanisms influencing the various components of nonspecific protection, including free radical oxidation processes. And then again, periodic assessment of the isotopic composition of nutrients will monitor the quality of food consumed by the population, and if

  3. Improved Technique for the Determination of Uranium Minor Isotopes Concentrations in Microparticles by Using Secondary Ion Mass-Spectrometer in Multicollection Mode

    International Nuclear Information System (INIS)

    Aleshin, M.; Elantyev, I.; Stebelkov, Y.

    2015-01-01

    Traditional method of the analysis implies simultaneous measuring of secondary ion currents of isotopes 234U + , 235U + , 238U + , ions with mass 236 amu (236U + and 235UH + ) and hydride ions 238UH + by using mass-spectrometer Cameca IMS1280 in multicollection mode. Calculating of uranium isotopic composition is performed using the results of 40 successive measurements of those currents (cycles). Duration of each measurement is 8 s. Small amounts of uranium minor isotopes are limitation for precise determination of their concentrations. To prevent the damage of the secondary ions detector the intensity of ion current should be no more than 5 x 10 5 s -1 . This limitation does not allow setting a higher primary ion current for the increasing of minor uranium isotopes ions emission because of the signal of ions 238U + gets too high. New technique is developed to improve the accuracy of determination of uranium minor isotopes concentrations. Process of measurement is divided on two steps. First step is a measurement of ion currents during 20 cycles by five detectors. The second step implies the elimination of ions 238U + hitting to the detector and 10 times increasing of primary ion current. The ratio 235U/238U is calculated from the first step results, so uncertainty of determination of this value is 1.4 times bigger than with duration of 40 cycles of the measurement. The ratios 234U/235U and 236U/235U are calculated during the second step. This technique allows to determine content of 234U and 236U with 3 and 5 times less uncertainties respectively, but with different degree of the sputtering particles. Moreover the duration of each cycle was set less (1 second) to use data more efficient. The technique accordingly with every second counting provides uncertainty of determination 236U concentration 4 times less than traditional method at the same degree of sputtering particles. (author)

  4. Fractionation of plutonium in environmental and bio-shielding concrete samples using dynamic sequential extraction

    DEFF Research Database (Denmark)

    Qiao, Jixin; Hou, Xiaolin

    2010-01-01

    Fractionation of plutonium isotopes (238Pu, 239,240Pu) in environmental samples (i.e. soil and sediment) and bio-shielding concrete from decommissioning of nuclear reactor were carried out by dynamic sequential extraction using an on-line sequential injection (SI) system combined with a specially...

  5. NGSI FY15 Final Report. Innovative Sample Preparation for in-Field Uranium Isotopic Determinations

    Energy Technology Data Exchange (ETDEWEB)

    Yoshida, Thomas M. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Meyers, Lisa [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

    2015-11-10

    Our FY14 Final Report included an introduction to the project, background, literature search of uranium dissolution methods, assessment of commercial off the shelf (COTS) automated sample preparation systems, as well as data and results for dissolution of bulk quantities of uranium oxides, and dissolution of uranium oxides from swipe filter materials using ammonium bifluoride (ABF). Also, discussed were reaction studies of solid ABF with uranium oxide that provided a basis for determining the ABF/uranium oxide dissolution mechanism. This report details the final experiments for optimizing dissolution of U3O8 and UO2 using ABF and steps leading to development of a Standard Operating Procedure (SOP) for dissolution of uranium oxides on swipe filters.

  6. Isotopes in heterogeneous catalysis

    CERN Document Server

    Hargreaves, Justin SJ

    2006-01-01

    The purpose of this book is to review the current, state-of-the-art application of isotopic methods to the field of heterogeneous catalysis. Isotopic studies are arguably the ultimate technique in in situ methods for heterogeneous catalysis. In this review volume, chapters have been contributed by experts in the field and the coverage includes both the application of specific isotopes - Deuterium, Tritium, Carbon-14, Sulfur-35 and Oxygen-18 - as well as isotopic techniques - determination of surface mobility, steady state transient isotope kinetic analysis, and positron emission profiling.

  7. Sequential stochastic optimization

    CERN Document Server

    Cairoli, Renzo

    1996-01-01

    Sequential Stochastic Optimization provides mathematicians and applied researchers with a well-developed framework in which stochastic optimization problems can be formulated and solved. Offering much material that is either new or has never before appeared in book form, it lucidly presents a unified theory of optimal stopping and optimal sequential control of stochastic processes. This book has been carefully organized so that little prior knowledge of the subject is assumed; its only prerequisites are a standard graduate course in probability theory and some familiarity with discrete-paramet

  8. High-precision quadruple isotope dilution method for simultaneous determination of nitrite and nitrate in seawater by GCMS after derivatization with triethyloxonium tetrafluoroborate

    Energy Technology Data Exchange (ETDEWEB)

    Pagliano, Enea, E-mail: enea.pagliano@nrc-cnrc.gc.ca; Meija, Juris; Mester, Zoltán

    2014-05-01

    Highlights: • High-precision determination of nitrite and nitrate in seawater. • Use of quadruple isotope dilution. • Aqueous Et₃O⁺BF₄]⁻ derivatization chemistry for GCMS analysis of nitrite and nitrate. Abstract: Quadruple isotope dilution mass spectrometry (ID⁴MS) has been applied for simultaneous determination of nitrite and nitrate in seawater. ID⁴MS allows high-precision measurements and entails the use of isotopic internal standards (¹⁸O-nitrite and ¹⁵N-nitrate). We include a tutorial on ID⁴MS outlining optimal experimental design which generates results with low uncertainties and obviates the need for direct (separate) evaluation of the procedural blank. Nitrite and nitrate detection was achieved using a headspace GCMS procedure based on single-step aqueous derivatization with triethyloxonium tetrafluoroborate at room temperature. In this paper the sample preparation was revised and fundamental aspects of this chemistry are presented. The proposed method has detection limits in the low parts-per-billion for both analytes, is reliable, precise, and has been validated using a seawater certified reference material (MOOS-2). Simplicity of the experimental design, low detection limits, and the use of quadruple isotope dilution makes the present method superior to the state-of-the-art for determination of nitrite and nitrate, and an ideal candidate for reference measurements of these analytes in seawater.

  9. Determination of radium isotopes in environmental samples by gamma spectrometry, liquid scintillation counting and alpha spectrometry: a review of analytical methodology

    International Nuclear Information System (INIS)

    Jia, Guogang; Jia, Jing

    2012-01-01

    Radium (Ra) isotopes are important from the viewpoints of radiation protection and environmental protection. Their high toxicity has stimulated the continuing interest in methodology research for determination of Ra isotopes in various media. In this paper, the three most routinely used analytical techniques for Ra isotope determination in biological and environmental samples, i.e. low-background γ-spectrometry, liquid scintillation counting and α-spectrometry, were reviewed, with emphasis on new methodological developments in sample preparation, preconcentration, separation, purification, source preparation and measurement techniques. The accuracy, selectivity, traceability, applicability and minimum detectable activity (MDA) of the three techniques were discussed. It was concluded that the MDA (0.1 mBq L −1 ) of the α-spectrometry technique coupled with chemical separation is about two orders of magnitude lower than that of low-background HPGe γ-spectrometry and LSC techniques. Therefore, when maximum sensitivity is required, the α-spectrometry technique remains the first choice. - Highlights: ► A review is made for determination of Ra isotopes in environmental samples. ► Gamma spectrometry, LSC and a-spectrometry are the main concerned radiometric approach. ► Sample preparation, preconcentration, separation and source preparation are discussed. ► The methods can analyse air, water, seawater, soil, sediment and foodstuffs samples. ► Some new data obtained recently from our laboratory for Ra method study are included.

  10. Improvements in Precise and Accurate Isotope Ratio Determination via LA-MC-ICP-MS by Application of an Alternative Data Reduction Protocol

    Science.gov (United States)

    Fietzke, J.; Liebetrau, V.; Guenther, D.; Frische, M.; Zumholz, K.; Hansteen, T. H.; Eisenhauer, A.

    2008-12-01

    An alternative approach for the evaluation of isotope ratio data using LA-MC-ICP-MS will be presented. In contrast to previously applied methods it is based on the simultaneous responses of all analyte isotopes of interest and the relevant interferences without performing a conventional background correction. Significant improvements in precision and accuracy can be achieved when applying this new method and will be discussed based on the results of two first methodical applications: a) radiogenic and stable Sr isotopes in carbonates b) stable chlorine isotopes of pyrohydrolytic extracts. In carbonates an external reproducibility of the 87Sr/86Sr ratios of about 19 ppm (RSD) was achieved, an improvement of about a factor of 5. For recent and sub-recent marine carbonates a mean radiogenic strontium isotope ratio 87Sr/86Sr of 0.709170±0.000007 (2SE) was determined, which agrees well with the value of 0.7091741±0.0000024 (2SE) reported for modern sea water [1,2]. Stable chlorine isotope ratios were determined ablating pyrohydrolytic extracts with a reproducibility of about 0.05‰ (RSD). For basaltic reference material JB1a and JB2 chlorine isotope ratios were determined relative to SMOC (standard mean ocean chlorinity) δ37ClJB-1a = (-0.99±0.06) ‰ and δ37ClJB-1a = (-0.60±0.03) ‰ (SD), respectively, in accordance with published data [3]. The described strategies for data reduction are considered to be generally applicable for all isotope ratio measurements using LA-MC-ICP-MS. [1] J.M. McArthur, D. Rio, F. Massari, D. Castradori, T.R. Bailey, M. Thirlwall, S. Houghton, Palaeogeo. Palaeoclim. Palaeoeco., 2006, 242 (126), doi: 10.1016/j.palaeo.2006.06.004 [2] J. Fietzke, V. Liebetrau, D. Guenther, K. Guers, K. Hametner, K. Zumholz, T.H. Hansteen and A. Eisenhauer, J. Anal. At. Spectrom., 2008, 23, 955-961, doi:10.1039/B717706B [3] J. Fietzke, M. Frische, T.H. Hansteen and A. Eisenhauer, J. Anal. At. Spectrom., 2008, 23, 769-772, doi:10.1039/B718597A

  11. Determination of the Geographical and Botanical Origin of Hops (Humulus lupulus L.) Using Stable Isotopes of C, N, and S.

    Science.gov (United States)

    Ocvirk, Miha; Ogrinc, Nives; Košir, Iztok Jože

    2018-02-28

    A need exists for a reliable method to determine the geographical and botanical origin of hops. For this study, three sets of samples were collected: the first set comprised 5 German samples; the second set comprised samples of hops from 10 of the world's major hop-growing regions; and the third comprised the 4 main Slovenian regions. The samples were analyzed using isotope ratio mass spectrometry (IRMS) to obtain δ 13 C, δ 15 N, and δ 34 S values. The δ 15 N (2.2 ‰ to 8.4 ‰) and δ 34 S (0.7 ‰ to 12.3 ‰) values were the most discriminating parameters for classifying hop according to geographical origin. ANOVA showed distinct groupings for 8 out of the 10 hop-growing regions. Although it was not possible to distinguish the geographical origin of hops based on δ 13 C (-28.9 ‰ to -24.7 ‰), in the case of botanical origin, δ 13 C values proved to be the most discriminative albeit with limited success.

  12. A state-of-the-art mass spectrometer system for determination of uranium and plutonium isotopic distributions in process samples

    International Nuclear Information System (INIS)

    Polson, C.A.

    1984-01-01

    A Finnigan MAT 261 automated thermal ionization mass spectrometer system was purchased by the Savannah River Plant and recently installed by Finnigan factory representatives. This instrument is a refinement of the MAT 260 which has been used routinely for three years in the laboratory at SRP. The MAT 261 is a highly precise, fully automated instrument. Many features make this instrument the state-of-the-art technology in precision isotopic composition measurements. A unique feature of the MAT 261 is the ion detection system which permits measurement of the three uranium or plutonium masses simultaneously. All Faraday cup measuring channels are of the same design and each is equipped with a dedicated amplifier. Each amplifier is connected to a linear voltage/frequency measuring system for ion current integration. These outputs are fed into a Hewlett-Packard 9845T desktop computer. The computer, and the Finnigan developed software package, control filament heating cycles, sample reconditioning, ion beam focusing, carrousel rotation, mass selection, and data collection and reduction. Precision, accuracy, and linearity were determined under normal laboratory conditions using a NBS uranium suite of standards. These results along with other developments in setting up the instrument are presented

  13. State-of-the-art mass spectrometer system for determination of uranium and plutonium isotopic distributions in process samples

    International Nuclear Information System (INIS)

    Polson, C.A.

    1983-01-01

    A Finnigan MAT 261 automated thermal ionization mass spectrometer system was purchased by the Savannah River Plant. The MAT 261 is a highly precise, fully automated instrument. Many features make this instrument the state-of-the-art technology in precision isotopic composition measurements. A unique feature of the MAT 261 is the ion detection system which permits measurement of the three uranium or plutonium masses simultaneously. All Faraday cup measuring channels are of the same design and each is equipped with a dedicated amplifier. Each amplifier is connected to a linear voltage/frequency measuring system for ion current integration. These outputs are fed into a Hewlett-Packard 9845T desk-top computer. The computer, and the Finnigan developed software package, control filament heating cycles, sample preconditioning, ion beam focusing, carrousel rotation, mass selection, and data collection and reduction. Precision, accuracy, and linearity were determined under normal laboratory conditions using a NBS uranium suite of standards. These results along with other development in setting up the instrument are presented

  14. The use of stable isotope dilution technique to determine the amount of breast milk consumed by infants

    International Nuclear Information System (INIS)

    Sajet, A. S.

    2011-01-01

    Exclusive breast feeding for six months to an infant, followed by the introduction of complementary food and continued with breast feeding is believed to be an optimal way of infants nutrition. There is a shortage in information about the amount of milk obtained from the infant's mother at least partially due to the difficulties associated with quantification of breast milk intake. The old technique, which depends on how the weight of the baby before and after breast feeding from mother, takes time and may be disturbing to the natural feeding pattern. It was possible to overcome these difficulties by using stable isotopes consumed by mother as D ose of deuterium oxide to mother i n particular dilution dose to mother and then move the dose from mother to baby through breast milk and this can calculate the total volume of breast milk consumed by the infant within 14 days since the dose oxide of deuterium consumed at first day. Dose of deuterium oxide to mother can also help to find out if there were any further quantity of water entering the child's body except breast milk, determine body composition for mother and infant, monitor the effects of programs strengthening food for pregnant mothers and lactating women in terms of quantity and quality of milk overnight, in addition to evaluating the effectiveness of programs to strengthen children's food. (author)

  15. Radium isotopes, alkaline earth diagenesis, and age determination of travertine from Mammoth Hot Springs, Wyoming, U.S.A

    International Nuclear Information System (INIS)

    Sturchio, N.C.

    1990-01-01

    Travertine from active springs, former vents, and drill core was analyzed for Ra isotopes, other alkaline earth elements, and mineralogical composition. Thermal water also was analyzed. Travertine, presently being deposited, contains 3.0-15.3 pCi/g 226 Ra, and has a 228 Ra/ 226 Ra ratio identical to that in thermal water. Travertine precipitates mostly as aragonite and experiences a complete diagenetic transformation to calcite within 9 a. Systematic compositional changes associated with this diagenetic transformation are enrichment of Mg and depletion of Sr, Ba and Ra. Apparent mineral-water distribution coefficients for Mg, Sr and Ba in aragonite and calcite are within the range of those determined experimentally, implying near-equilibrium conditions and high water-rock ratios during diagenesis. Impure travertine from near the base of a section in the Y-10 drill hole (at 72.9 m depth) has a 230 Th/ 234 U isochron age of 7700±440 a. The content of 226 Ra in the normal, subhorizontally layered, porous travertine decreases with depth. The observed 226 Ra vs depth relation is consistent with continuous deposition of travertine at the site from 7700 a BP to near present at a mean rate of ∼1.0 cm/a, and indicates minimal exchange of Ra between travertine and pore water after the early diagenetic transformation of aragonite to calcite. (author)

  16. Using stable isotopes to determine seasonal variations in water uptake of summer maize under different fertilization treatments

    Energy Technology Data Exchange (ETDEWEB)

    Ma, Ying, E-mail: maying@igsnrr.ac.cn [Key Laboratory of Water Cycle and Related Land Surface Processes, Institute of Geographic Sciences and Natural Resources Research, Chinese Academy of Sciences, 100101 Beijing (China); State Key Laboratory of Soil and Sustainable Agriculture, Institute of Soil Science, Chinese Academy of Sciences, 210008 Nanjing (China); Song, Xianfang [Key Laboratory of Water Cycle and Related Land Surface Processes, Institute of Geographic Sciences and Natural Resources Research, Chinese Academy of Sciences, 100101 Beijing (China)

    2016-04-15

    Fertilization and water both affect root water uptake in the nutrient and water cycle of the Soil-Plant-Atmosphere-Continuum (SPAC). In this study, dual stable isotopes (D and {sup 18}O) were used to determine seasonal variations in water uptake patterns of summer maize under different fertilization treatments in Beijing, China during 2013–2014. The contributions of soil water at different depths to water uptake were quantified by the MixSIAR Bayesian mixing model. Water uptake was mainly sourced from soil water in the 0–20 cm depth at the seeding (67.7%), jointing (60.5%), tasseling (47.5%), dough (41.4%), and harvest (43.9%) stages, and the 20–50 cm depth at the milk stage (32.8%). Different levels of fertilization application led to considerable differences in the proportional contribution of soil water at 0–20 cm (6.0–58.5%) and 20–50 cm (6.1–26.3%). There was little difference of contributions in the deep layers (50–200 cm) among treatments in 2013, whereas differences were observed in 50–90 cm at the milk stage and 50–200 cm at the dough stage during 2014. The main water uptake depth was concentrated in the upper soil layers (0–50 cm) during the wet season (2013), whereas a seasonal drought in 2014 promoted the contribution of soil water in deep layers. The contribution of soil water was significantly and positively correlated with the proportions of root length (r = 0.753, p < 0.01). The changes of soil water distribution were consistent with the seasonal variation in water uptake patterns. The present study identified water sources for summer maize under varying fertilization treatments and provided scientific implications for fertilization and irrigation management. - Highlights: • Dual stable isotopes and MixSIAR were coupled to quantify water uptake of maize. • Maize mainly used soil water in 20–50 cm at milk stage and 0–20 cm at other stages. • Fertilization treatments led to distinct water uptake pattern at 0–50 cm

  17. Using stable isotopes to determine seasonal variations in water uptake of summer maize under different fertilization treatments

    International Nuclear Information System (INIS)

    Ma, Ying; Song, Xianfang

    2016-01-01

    Fertilization and water both affect root water uptake in the nutrient and water cycle of the Soil-Plant-Atmosphere-Continuum (SPAC). In this study, dual stable isotopes (D and "1"8O) were used to determine seasonal variations in water uptake patterns of summer maize under different fertilization treatments in Beijing, China during 2013–2014. The contributions of soil water at different depths to water uptake were quantified by the MixSIAR Bayesian mixing model. Water uptake was mainly sourced from soil water in the 0–20 cm depth at the seeding (67.7%), jointing (60.5%), tasseling (47.5%), dough (41.4%), and harvest (43.9%) stages, and the 20–50 cm depth at the milk stage (32.8%). Different levels of fertilization application led to considerable differences in the proportional contribution of soil water at 0–20 cm (6.0–58.5%) and 20–50 cm (6.1–26.3%). There was little difference of contributions in the deep layers (50–200 cm) among treatments in 2013, whereas differences were observed in 50–90 cm at the milk stage and 50–200 cm at the dough stage during 2014. The main water uptake depth was concentrated in the upper soil layers (0–50 cm) during the wet season (2013), whereas a seasonal drought in 2014 promoted the contribution of soil water in deep layers. The contribution of soil water was significantly and positively correlated with the proportions of root length (r = 0.753, p < 0.01). The changes of soil water distribution were consistent with the seasonal variation in water uptake patterns. The present study identified water sources for summer maize under varying fertilization treatments and provided scientific implications for fertilization and irrigation management. - Highlights: • Dual stable isotopes and MixSIAR were coupled to quantify water uptake of maize. • Maize mainly used soil water in 20–50 cm at milk stage and 0–20 cm at other stages. • Fertilization treatments led to distinct water uptake pattern at 0–50 cm depth

  18. Determining CO2 storage potential during miscible CO2 enhanced oil recovery: Noble gas and stable isotope tracers

    Science.gov (United States)

    Shelton, Jenna L.; McIntosh, Jennifer C.; Hunt, Andrew; Beebe, Thomas L; Parker, Andrew D; Warwick, Peter D.; Drake, Ronald; McCray, John E.

    2016-01-01

    Rising atmospheric carbon dioxide (CO2) concentrations are fueling anthropogenic climate change. Geologic sequestration of anthropogenic CO2 in depleted oil reservoirs is one option for reducing CO2 emissions to the atmosphere while enhancing oil recovery. In order to evaluate the feasibility of using enhanced oil recovery (EOR) sites in the United States for permanent CO2 storage, an active multi-stage miscible CO2flooding project in the Permian Basin (North Ward Estes Field, near Wickett, Texas) was investigated. In addition, two major natural CO2 reservoirs in the southeastern Paradox Basin (McElmo Dome and Doe Canyon) were also investigated as they provide CO2 for EOR operations in the Permian Basin. Produced gas and water were collected from three different CO2 flooding phases (with different start dates) within the North Ward Estes Field to evaluate possible CO2 storage mechanisms and amounts of total CO2retention. McElmo Dome and Doe Canyon were sampled for produced gas to determine the noble gas and stable isotope signature of the original injected EOR gas and to confirm the source of this naturally-occurring CO2. As expected, the natural CO2produced from McElmo Dome and Doe Canyon is a mix of mantle and crustal sources. When comparing CO2 injection and production rates for the CO2 floods in the North Ward Estes Field, it appears that CO2 retention in the reservoir decreased over the course of the three injections, retaining 39%, 49% and 61% of the injected CO2 for the 2008, 2010, and 2013 projects, respectively, characteristic of maturing CO2 miscible flood projects. Noble gas isotopic composition of the injected and produced gas for the flood projects suggest no active fractionation, while δ13CCO2 values suggest no active CO2dissolution into formation water, or mineralization. CO2 volumes capable of dissolving in residual formation fluids were also estimated along with the potential to store pure-phase supercritical CO2. Using a combination

  19. Sequential memory: Binding dynamics

    Science.gov (United States)

    Afraimovich, Valentin; Gong, Xue; Rabinovich, Mikhail

    2015-10-01

    Temporal order memories are critical for everyday animal and human functioning. Experiments and our own experience show that the binding or association of various features of an event together and the maintaining of multimodality events in sequential order are the key components of any sequential memories—episodic, semantic, working, etc. We study a robustness of binding sequential dynamics based on our previously introduced model in the form of generalized Lotka-Volterra equations. In the phase space of the model, there exists a multi-dimensional binding heteroclinic network consisting of saddle equilibrium points and heteroclinic trajectories joining them. We prove here the robustness of the binding sequential dynamics, i.e., the feasibility phenomenon for coupled heteroclinic networks: for each collection of successive heteroclinic trajectories inside the unified networks, there is an open set of initial points such that the trajectory going through each of them follows the prescribed collection staying in a small neighborhood of it. We show also that the symbolic complexity function of the system restricted to this neighborhood is a polynomial of degree L - 1, where L is the number of modalities.

  20. Sequential Dependencies in Driving

    Science.gov (United States)

    Doshi, Anup; Tran, Cuong; Wilder, Matthew H.; Mozer, Michael C.; Trivedi, Mohan M.

    2012-01-01

    The effect of recent experience on current behavior has been studied extensively in simple laboratory tasks. We explore the nature of sequential effects in the more naturalistic setting of automobile driving. Driving is a safety-critical task in which delayed response times may have severe consequences. Using a realistic driving simulator, we find…