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....

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

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.

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.

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.

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

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)

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

Online stable carbon isotope ratio measurement in formic acid, acetic acid, methanol and ethanol in water by high performance liquid chromatography-isotope ratio mass spectrometry

International Nuclear Information System (INIS)

Tagami, Keiko; Uchida, Shigeo

2008-01-01

A suitable analysis condition was determined for high performance liquid chromatography-isotope ratio mass spectrometry (HPLC-IRMS) while making sequential measurements of stable carbon isotope ratios of δ 13 C in formic acid, acetic acid, methanol and ethanol dissolved in water. For this online column separation method, organic reagents are not applicable due to carbon contamination; thus, water and KH 2 PO 4 at low concentrations were tested as mobile phase in combination with a HyPURITY AQUASTAR TM column. Formic acid, acetic acid, methanol and ethanol were separated when 2 mM KH 2 PO 4 aqueous solution was used. Under the determined analysis condition for HPLC-IRMS, carbon concentrations could be measured quantitatively as well as carbon isotope ratio when carbon concentration was higher than 0.4 mM L for each chemical

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)

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

Mobility of radionuclides based on sequential extraction of soils

International Nuclear Information System (INIS)

Salbu, B.; Oughton, D.H.; Lien, H.N.; Oestby, G.; Strand, P.

1992-01-01

Since 1989, core samples of soil and vegetation from semi-natural pastures have been collected at selected sites in Norway during the growing season. The activity concentrations in soil and vegetation as well as transfer coefficients vary significantly between regions, within regions and even within sampling plot areas. In order to differentiate between mobil and inert fractions of radioactive and stable isotopes of Cs and Sr in soils, samples were extracted sequentially using agents with increasing dissolution power. The reproducibility of the sequential extraction technique is good and the data obtained seems most informative. As the distribution pattern for radioactive and stable isotopes of Cs and Sr are similar, a high degree of isotopic exchange is indicated. Based on easily leachable fractions, mobility factors are calculated. In general the mobility of 90 Sr is higher than for 137 Cs. Mobility factors are not significantly influenced by seasonal variations, but a decrease in the mobile fraction in soil with time is indicated. Mobility factors should be considered useful for modelling purposes. (au)

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

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...

Trace elements and Pb isotopes in soils and sediments impacted by uranium mining

Energy Technology Data Exchange (ETDEWEB)

Cuvier, A., E-mail: alicia.cuvier@hotmail.fr [ECOLAB, Université de Toulouse, CNRS, INPT, UPS, Toulouse (France); IRSN/PRP-ENV/SESURE/Laboratoire d' études radioécologiques en milieu continental et marin, BP 1, 13108 Saint Paul Lez Durance Cedex (France); Pourcelot, L. [IRSN/PRP-ENV/SESURE/Laboratoire d' études radioécologiques en milieu continental et marin, BP 1, 13108 Saint Paul Lez Durance Cedex (France); Probst, A. [ECOLAB, Université de Toulouse, CNRS, INPT, UPS, Toulouse (France); Prunier, J. [Observatoire Midi-Pyrénées, laboratoire Géosciences Environnement Toulouse, CNRS/IRD/Université Paul Sabatier, 14 avenue Edouard Belin, 31400 Toulouse (France); Le Roux, G., E-mail: gael.leroux@ensat.fr [ECOLAB, Université de Toulouse, CNRS, INPT, UPS, Toulouse (France)

2016-10-01

The purpose of this study is to evaluate the contamination in As, Ba, Co, Cu, Mn, Ni, Sr, V, Zn and REE, in a high uranium activity (up to 21,000 Bq ∙ kg{sup −1}) area, downstream of a former uranium mine. Different geochemical proxies like enrichment factor and fractions from a sequential extraction procedure are used to evaluate the level of contamination, the mobility and the availability of the potential contaminants. Pb isotope ratios are determined in the total samples and in the sequential leachates to identify the sources of the contaminants and to determine the mobility of radiogenic Pb in the context of uranium mining. In spite of the large uranium contamination measured in the soils and the sediments (EF ≫ 40), trace element contamination is low to moderate (2 < EF < 5), except for Ba (5 < EF < 15), due to the precipitation of barium sulfate resulting from mining activities. Most of the trace elements are associated with the most mobile fractions of the sediments/soils, implying an enhanced potential availability. Even if no Pb enrichment is highlighted, the Pb isotopic signature of the contaminated soils is strongly radiogenic. Measurements performed on the sequential leachates reveal inputs of radiogenic Pb in the most mobile fractions of the contaminated soil. Inputs of low-mobile radiogenic Pb from mining activities may also contribute to the Pb signature recorded in the residual phase of the contaminated samples. We demonstrate that Pb isotopes are efficient tools to trace the origin and the mobility of the contaminants in environments affected by uranium mining. - Highlights: • Contamination of soils is evidenced by a multiproxy approach. • Enrichment factors highlight a low contamination except for U, S and Ba. • Pb isotope ratios point out inputs of radiogenic Pb from the mine. • Radiogenic Pb is mainly in the acid-soluble and the reducible fractions.

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.

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

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

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

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

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

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)

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.

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.

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)

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.

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).

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

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

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)

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)

Broadband non-selective excitation of plutonium isotopes for isotope ratio measurements in resonance ionization mass spectrometry: a theoretical study.

Science.gov (United States)

Sankari, M

2012-10-15

simultaneous and much more accurate isotope ratios than those in the sequential and less accurate determination reported earlier. Application of these theoretical calculations to minimize the isotopic biases under these conditions for the rapid, efficient and accurate isotope ratio measurements using RIMS has been outlined. Copyright © 2012 John Wiley & Sons, Ltd.

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)

Isotopic scintigraphy in kidney grafting

International Nuclear Information System (INIS)

Renfro, Richard.

1976-01-01

Isotopic explorations of kidney transplants were performed on sixty-six patients. Three scintigraphic techniques were used: labelled ferrous ascorbate scintigraphy, sequential 99m technetium DTPA scintigraphy and the 131 I hippuran nephrogram. The aim of this study is to analyse the results obtained under different pathological circumstances affecting the transplant, to discuss the advantages of the techniques and to propose a working procedure. The most reliable and accurate technique is the 131 I hippuran nephrogram combined with sequential 99mTc DTPA, by which renal vascularisation may be judged labelled ferrous ascorbate on the other hand is too insensitive. Although the information supplied is mostly contained in the scintigraphic images, the nephrographic curves and the blood radioactivity decay time and rad V/rad R ratio measurements are very helpful in the early diagnosis and differential diagnosis of complications affecting the transplant. The proper use of isotopic scintigraphy in kidney grafting should provide optimum conditions for better survival of the transplant at minimum risk to the patient [fr

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)

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)

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)

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)

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)

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)

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.

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)

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

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

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)

Seasonal variation in kangaroo tooth enamel oxygen and carbon isotopes in southern Australia

Science.gov (United States)

Brookman, Tom H.; Ambrose, Stanley H.

2012-09-01

Serial sampling of tooth enamel growth increments for carbon and oxygen isotopic analyses of Macropus (kangaroo) teeth was performed to assess the potential for reconstructing paleoseasonality. The carbon isotope composition of tooth enamel apatite carbonate reflects the proportional intake of C3 and C4 vegetation. The oxygen isotopic composition of enamel reflects that of ingested and metabolic water. Tooth enamel forms sequentially from the tip of the crown to the base, so dietary and environmental changes during the tooth's formation can be detected. δ13C and δ18O values were determined for a series of enamel samples drilled from the 3rd and 4th molars of kangaroos that were collected along a 900 km north-south transect in southern Australia. The serial sampling method did not yield pronounced seasonal isotopic variation patterns in Macropus enamel. The full extent of dietary isotopic variation may be obscured by attenuation of the isotopic signal during enamel mineralisation. Brachydont (low-crowned) Macropus teeth may be less sensitive to seasonal variation in isotopic composition due to time-averaging during mineralisation. However, geographic variations observed suggest that there may be potential for tracking latitudinal shifts in vegetation zones and seasonal environmental patterns in response to climate change.

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.

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.

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.

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

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)

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)

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

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

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

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

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

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...

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.)

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

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

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

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

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.

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

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)

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

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.

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.

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.

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.)

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.)

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

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

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)

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...

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)

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)

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

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

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)

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

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....

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.

Lead isotope measurements on aerosol samples with ICP-MS

International Nuclear Information System (INIS)

Widmer, C.R.; Kraehenbuehl, U.; Kramers, J.; Tobler, L.

2000-01-01

Size fractionated aerosols were collected with low pressure Berner impactors on a radio/TV tower 110 m above ground on a hill 10 km east of Bern at a total elevation of 1060 m asl. Two different wind sectors were chosen with the goal of assessing any differences in lead concentration and the 3 radiogenic lead isotopes (206,207,208) for east and west wind, respectively. A leaching technique was used to extract the lead quantitatively from the surface of the impaction foils. This method has been proven to be better suited for airborne particles than complete microwave digestion because it is less time consuming and contamination risk is smaller. Blank considerations played a major role in choosing all the chemicals, tubes, beakers and selecting the analytical method. Lead concentrations were determined with GF-AAS and lead isotopes with two different ICP-MS systems, one being a multicollector system. Precision of the simultaneous multicollector system was found to be at least a factor of 3 better than that of the sequentially operating ICP-MS. The small variations in isotope ratios from the two wind sectors can be distinctly seen with this enhanced precision. The observed relative difference in isotope ratios between east- and westwind was ∝0.6% for 207 Pb/ 206 Pb and ∝0.5% for 208 Pb/ 206 Pb. (orig.)

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

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

Strontium isotope study of coal utilization by-products interacting with environmental waters.

Science.gov (United States)

Spivak-Birndorf, Lev J; Stewart, Brian W; Capo, Rosemary C; Chapman, Elizabeth C; Schroeder, Karl T; Brubaker, Tonya M

2012-01-01

Sequential leaching experiments on coal utilization by-products (CUB) were coupled with chemical and strontium (Sr) isotopic analyses to better understand the influence of coal type and combustion processes on CUB properties and the release of elements during interaction with environmental waters during disposal. Class C fly ash tended to release the highest quantity of minor and trace elements-including alkaline earth elements, sodium, chromium, copper, manganese, lead, titanium, and zinc-during sequential extraction, with bottom ash yielding the lowest. Strontium isotope ratios ((87)Sr/(86)Sr) in bulk-CUB samples (total dissolution of CUB) are generally higher in class F ash than in class C ash. Bulk-CUB ratios appear to be controlled by the geologic source of the mineral matter in the feed coal, and by Sr added during desulfurization treatments. Leachates of the CUB generally have Sr isotope ratios that are different than the bulk value, demonstrating that Sr was not isotopically homogenized during combustion. Variations in the Sr isotopic composition of CUB leachates were correlated with mobility of several major and trace elements; the data suggest that arsenic and lead are held in phases that contain the more radiogenic (high-(87)Sr/(86)Sr) component. A changing Sr isotope ratio of CUB-interacting waters in a disposal environment could forecast the release of certain strongly bound elements of environmental concern. This study lays the groundwork for the application of Sr isotopes as an environmental tracer for CUB-water interaction. Copyright © by the American Society of Agronomy, Crop Science Society of America, and Soil Science Society of America, Inc.

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)

Eyewitness confidence in simultaneous and sequential lineups: a criterion shift account for sequential mistaken identification overconfidence.

Science.gov (United States)

Dobolyi, David G; Dodson, Chad S

2013-12-01

Confidence judgments for eyewitness identifications play an integral role in determining guilt during legal proceedings. Past research has shown that confidence in positive identifications is strongly associated with accuracy. Using a standard lineup recognition paradigm, we investigated accuracy using signal detection and ROC analyses, along with the tendency to choose a face with both simultaneous and sequential lineups. We replicated past findings of reduced rates of choosing with sequential as compared to simultaneous lineups, but notably found an accuracy advantage in favor of simultaneous lineups. Moreover, our analysis of the confidence-accuracy relationship revealed two key findings. First, we observed a sequential mistaken identification overconfidence effect: despite an overall reduction in false alarms, confidence for false alarms that did occur was higher with sequential lineups than with simultaneous lineups, with no differences in confidence for correct identifications. This sequential mistaken identification overconfidence effect is an expected byproduct of the use of a more conservative identification criterion with sequential than with simultaneous lineups. Second, we found a steady drop in confidence for mistaken identifications (i.e., foil identifications and false alarms) from the first to the last face in sequential lineups, whereas confidence in and accuracy of correct identifications remained relatively stable. Overall, we observed that sequential lineups are both less accurate and produce higher confidence false identifications than do simultaneous lineups. Given the increasing prominence of sequential lineups in our legal system, our data argue for increased scrutiny and possibly a wholesale reevaluation of this lineup format. PsycINFO Database Record (c) 2013 APA, all rights reserved.

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)

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

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

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.)

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

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.)

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.

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

Intracrystalline site preference of hydrogen isotopes in the water of crystallization of copper sulfate pentahydrate

International Nuclear Information System (INIS)

Kita, I.; Matsuo, S.

1981-01-01

Difference in the isotopic partition at different sites of the water of crystallization of CuSO 4 .5H 2 O (the site preference) was estimated for the hydrogen isotopes. Fractional dehydration of CuSO 4 .5H 2 O under vacuum at 0 and 25 0 C was used to determine the isotopic ratio, the amount of dehydrated water, and the rate process of dehydration. The following results were obtained. (1) Two maxima occur in the isotopic ratio in the dehydration range, F < 0.8. (2) The dehydration occurs by the three sequential zeroth-order rate processes which have different rate constants for dehydration. The three different rate constants may be explained by the combination of the rate constants of dehydration of the water molecules dehydrated. The estimation of the difference in hydrogen isotope distribution for different sites, i.e., four of the five water molecules in the coordination sphere of copper ion (site A) and one bonded to the sulfate ion through hydrogen bonding (site B) was made. The site preference of hydrogen isotopes (delta D,%) was concluded to be -3.20 +- 0.52 for site A and +2.26 +- 2.09 for site B, where the delta D value was referred to the isotopic ratio of the mother liquor from which the crystal was formed

Intracrystalline site preference of hydrogen isotopes in the water of crystallization of copper sulfate pentahydrate

Energy Technology Data Exchange (ETDEWEB)

Kita, I.; Matsuo, S.

1981-04-02

Difference in the isotopic partition at different sites of the water of crystallization of CuSO/sub 4/.5H/sub 2/O (the site preference) was estimated for the hydrogen isotopes. Fractional dehydration of CuSO/sub 4/.5H/sub 2/O under vacuum at 0 and 25/sup 0/C was used to determine the isotopic ratio, the amount of dehydrated water, and the rate process of dehydration. The following results were obtained. (1) Two maxima occur in the isotopic ratio in the dehydration range, F < 0.8. (2) The dehydration occurs by the three sequential zeroth-order rate processes which have different rate constants for dehydration. The three different rate constants may be explained by the combination of the rate constants of dehydration of the water molecules dehydrated. The estimation of the difference in hydrogen isotope distribution for different sites, i.e., four of the five water molecules in the coordination sphere of copper ion (site A) and one bonded to the sulfate ion through hydrogen bonding (site B) was made. The site preference of hydrogen isotopes (delta D,%) was concluded to be -3.20 +- 0.52 for site A and +2.26 +- 2.09 for site B, where the delta D value was referred to the isotopic ratio of the mother liquor from which the crystal was formed.

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.

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

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

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

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

Isotope exchange investigation of nitrogen redistribution in expanded austenite

International Nuclear Information System (INIS)

Christiansen, T.L.; Drouet, M.; Martinavičius, A.; Somers, M.A.J.

2013-01-01

Sequential plasma and gaseous nitriding of Fe–18Cr–10Ni–3Mo stainless steel at 390 °C with 14 N and 15 N isotopes followed by denitriding in flowing hydrogen was investigated. Redistribution of plasma-inserted nitrogen atoms ( 15 N) by subsequent gaseous nitriding ( 14 N) was observed. Denitriding after plasma- and gaseous nitriding resulted in predominant retraction of 14 N, and only a minor amount of 15 N. The nitrogen isotope diffusion behaviour is explained by two different states of nitrogen bonding and short-range ordering between nitrogen and chromium

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.)

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.

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

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...

Cu-Zn-Pb multi isotopic characterization of a small watershed (Loire river basin, France)

Science.gov (United States)

Desaulty, A. M.; Millot, R.; Perret, S.; Bourrain, X.

2015-12-01

Combating metal pollution in surface water is a major environmental, public health and economic issue. Knowledge of the behavior of metals, such as copper (Cu), zinc (Zn) and lead (Pb) in sediments and dissolved load, is a key factor to improve the management of rivers. Recent advances in mass spectrometry related to the development of MC-ICPMS allow to analyze the isotopic composition of these elements, and previous studies show the effectiveness of isotopic analyses to determine the anthropogenic sources of pollution in environment. The goal of this study is to use the Cu-Zn-Pb multi-isotopic signature to track the pollutions in surface water, and to understand the complex processes causing the metals mobilization and transport in environment. More particularly we investigate the mechanisms of distribution between the dissolved load and particulate load, known to play an important role in the transport of metals through river systems. As case study, we chose a small watershed, poorly urbanized in the Loire river basin. Its spring is in a pristine area, while it is only impacted some kilometers further by the releases rich in metals coming from a hospital water treatment plant. First a sampling of these liquid effluents as well as dissolved load and sediment from upstream to downstream was realized and their concentrations and isotopic data were determined. Then to simulate a lot of potential natural and anthropogenic modifications of environmental conditions, we made sequential extraction protocol using various reagents on the sediments. Isotopic analyzes were performed also on the various extracting solutions. Isotopic ratios were measured using a Neptune MC-ICPMS at the BRGM, after a protocol of purification for Zn and Cu. The results showed that, these isotopic systematics reveal important informations about the mechanists of mobilization and transport of metals through river systems. However experiments performed under laboratory conditions will be necessary

Isotope exchange investigation of nitrogen redistribution in expanded austenite

DEFF Research Database (Denmark)

Christiansen, Thomas Lundin; Drouet, M.; Martinavičius, A.

2013-01-01

Sequential plasma and gaseous nitriding of Fe–18Cr–10Ni–3Mo stainless steel at 390°C with 14N and 15N isotopes followed by denitriding in flowing hydrogen was investigated. Redistribution of plasma-inserted nitrogen atoms (15N) by subsequent gaseous nitriding (14N) was observed. Denitriding after...

Uranium Age Determination by Measuring the 230Th / 234U Ratio

International Nuclear Information System (INIS)

LAMONT, STEPHEN P.

2004-01-01

A radiochemical isotope dilution mass spectrometry method has been developed to determine the age of uranium materials. The amount of 230Th activity, the first progeny of 234U, that had grown into a small uranium metal sample was used to determine the elapsed time since the material was last radiochemically purified. To preserve the sample, only a small amount of oxidized uranium was removed from the surface of the sample and dissolved. Aliquots of the dissolved sample were spiked with 233U tracer and radiochemically purified by anion-exchange chromatography. The 234U isotopic concentration was then determined by thermal ionization mass spectrometry. Additional aliquots of the sample were spiked with 229Th tracer, and the thorium was purified using two sequential anion-exchange chromatography separations. The isotopic concentrations of 230Th and 232Th were determined by TIMS. The lack of any 232Th confirmed the assumption that all thorium was removed from the uranium sample at the time of purification. The 230Th and 234U mass concentrations were converted to activities and the 230Th/234U ratio for the sample was calculated. The experimental 230Th/234U ratio showed the uranium in this sample was radiochemically purified in about 1945. Isotope dilution thermal ionization mass spectrometry has sufficient sensitivity to determine the age of 100 samples of uranium. This method could certainly be employed as a nuclear forensic method to determine the age of small quantities of uranium metal or salts. Accurate determination of the ultra-trace 230Th radiochemically separated from the uranium is possible due to the use of 229Th as an isotope dilution tracer. The precision in the experimental age of the uranium could be improved by making additional replicate measurements of the 230Th/234U isotopic ratio or using a larger initial sample

Chemical and isotopic composition of secondary organic aerosol generated by α-pinene ozonolysis

DEFF Research Database (Denmark)

Meusinger, Carl; Dusek, Ulrike; King, Stephanie M.

2017-01-01

-NOx conditions, with OH scavengers and in the absence of seed particles. The excess of ozone and long residence time in the flow chamber ensured that virtually all α-pinene had reacted. Product SOA was collected on two sequential quartz filters. The filters were analysed offline by heating them stepwise from 100...... it is difficult to apply because neither the isotopic composition of aerosol precursors nor the fractionation of aerosol forming processes is well characterised. In this paper, SOA formation from ozonolysis of α-pinene - an important precursor and perhaps the best-known model system used in laboratory studies...... - was investigated using position-dependent and average determinations of 13C in α-pinene and advanced analysis of reaction products using thermal-desorption proton-transfer-reaction mass spectrometry (PTR-MS). The total carbon (TC) isotopic composition δ13C of the initial α-pinene was measured, and the δ13C...

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

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.

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...

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

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

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)

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)

Isotope migration and barrier in a VLLW site

International Nuclear Information System (INIS)

Kang Houjun; Zhang Dong; Yang Yong; Shi Zhengkun; Li Kuanliang; Zhang Peicong

2010-01-01

In this work, adsorption and migration of 238 U and 90 Sr in unsaturated soil at a VLLW (very low level waste) site was investigated, in an attempt to find geochemical features of the site. Migration of the isotopes in heterosphere was studied under instantaneous and sequential conditions of the sources. The migration barrier experiment was carried out in two steps on wall rock absorption of the isotopes and addictives to improve the barrier of the wall rock to 90 Sr. The results show that the migration speed of 238 U and 90 Sr in the soil is 0.365 and 0.385 mm/a, respectively. The heterosphere effects on the isotope migration not only alleviated the mainstream contamination, but also prolonged the time of contaminated affection. And false zeolite should be used as barrier additive material for 90 Sr migration. (authors)

Factors controlling Li concentration and isotopic composition in formation waters and host rocks of Marcellus Shale, Appalachian Basin

Science.gov (United States)

Phan, Thai T.; Capo, Rosemary C; Stewart, Brian W.; Macpherson, Gwen; Rowan, Elisabeth L.; Hammack, Richard W.

2015-01-01

In this study, water and whole rock samples from hydraulically fractured wells in the Marcellus Shale (Middle Devonian), and water from conventional wells producing from Upper Devonian sandstones were analyzed for lithium concentrations and isotope ratios (δ7Li). The distribution of lithium concentrations in different mineral groups was determined using sequential extraction. Structurally bound Li, predominantly in clays, accounted for 75-91 wt. % of total Li, whereas exchangeable sites and carbonate cement contain negligible Li (shale in Greene Co., Pennsylvania, and Tioga Co., New York, ranged from -2.3 to + 4.3‰, similar to values reported for other shales in the literature. The δ7Li values in shale rocks with stratigraphic depth record progressive weathering of the source region; the most weathered and clay-rich strata with isotopically light Li are found closest to the top of the stratigraphic section. Diagenetic illite-smectite transition could also have partially affected the bulk Li content and isotope ratios of the Marcellus Shale.

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.

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

Application of heavy stable isotopes in forensic isotope geochemistry: A review

International Nuclear Information System (INIS)

Aggarwal, Jugdeep; Habicht-Mauche, Judith; Juarez, Chelsey

2008-01-01

Light stable isotopes have been used for many years to characterize the source and transport of materials. More recently heavy isotope systems such as Sr, Nd and Pb have been added to this list in order to aid source identification. With the advent of multiple collector ICP-MS, the range of isotopic tools now available has increased considerably, however, until the isotope systematics of these new non-traditional isotope systems have become better understood, they will not be as useful in characterizing material source and transportation. Applications using heavy metal stable isotopes (mostly traditional heavy isotopes) have reached most avenues in science, including earth sciences, archaeology, anthropology, animal physiology, ecology and toxicology. This field will continue to grow as new applications are developed and techniques become simpler and quicker. This paper provides a review of how this field has grown and presents two new applications using Pb and Sr isotopes in glazes to determine the source of ore used in glazes, and using Sr isotopes to determine the origin of undocumented deceased Mexican border crossers

Application of heavy stable isotopes in forensic isotope geochemistry: A review

Energy Technology Data Exchange (ETDEWEB)

Aggarwal, Jugdeep [W.M. Keck Isotope Laboratory, Department of Earth Sciences, University of California, Santa Cruz, CA 95064 (United States)], E-mail: jaggarwal@pmc.ucsc.edu; Habicht-Mauche, Judith; Juarez, Chelsey [Department of Anthropology, University of California, Santa Cruz, CA 95064 (United States)

2008-09-15

Light stable isotopes have been used for many years to characterize the source and transport of materials. More recently heavy isotope systems such as Sr, Nd and Pb have been added to this list in order to aid source identification. With the advent of multiple collector ICP-MS, the range of isotopic tools now available has increased considerably, however, until the isotope systematics of these new non-traditional isotope systems have become better understood, they will not be as useful in characterizing material source and transportation. Applications using heavy metal stable isotopes (mostly traditional heavy isotopes) have reached most avenues in science, including earth sciences, archaeology, anthropology, animal physiology, ecology and toxicology. This field will continue to grow as new applications are developed and techniques become simpler and quicker. This paper provides a review of how this field has grown and presents two new applications using Pb and Sr isotopes in glazes to determine the source of ore used in glazes, and using Sr isotopes to determine the origin of undocumented deceased Mexican border crossers.

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.

Simultaneous determination of left ventricular perfusion and function

International Nuclear Information System (INIS)

Gremillet, E.; Champailler, A.; Esquerre, J.P.; Ouhayoun, E.; Coca, F.; Furber, A.; Le Jeune, J.J.

1997-01-01

Myocardial perfusion scintigraphy is a very useful tool for the diagnosis and prognosis of coronary artery disease. The evaluation of left ventricular function during stress testing in also very useful to determine the prognosis of coronary artery disease. This chapter highlights three different imaging methods to assess left ventricular function and myocardial perfusion/ The first one consists of sequential dual isotope myocardial SPECT with ECG-gating. The second concerns magnetic resonance imaging and the third explores first pass exercise ventriculography and myocardial perfusion scintigraphy simultaneously evaluated by means of 99m Tc-sestamibi. (authors)

Plutonium speciation and isotope ratios in Yenisey and Ob river and Yenisey estuary

International Nuclear Information System (INIS)

Skipperud, L.; Oughton, DH.; Fifield, K.; Lind, O.C.; Salbu, B.; Brown, J.

2004-01-01

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 240 Pu isotope, with 240 Pu/ 239 Pu isotope ratio less than 0.05. In contrast, both global weapons fallout and spent nuclear fuel from civil reactors have higher 240 Pu/ 239 Pu isotope ratios (civil nuclear power reactors have 240 Pu/ 239 Pu 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. Together with activity measurements and isotope ratios, knowledge of plutonium speciation in the Ob and Yenisey rivers and processes controlling its behaviour in estuarine systems is a prerequisite for predicting the transfer and subsequent environmental impact to Arctic Seas. With this in mind, the study had two objectives: first to determine whether discharges from nuclear installations in the river catchment areas are having any influence on Pu levels in the estuaries; and, second, to investigate the transfer and mobility of plutonium in the Yenisey river and estuary. Plutonium 240/239 ratios were determined using accelerator mass spectrometry (AMS). The data indicated a clear influence from a low 240 Pu: 239 Pu source in surface sediments collected from the Yenisey Estuary, whereas plutonium in the Ob Estuary sediments are dominated by global fallout. The results also show an increase in plutonium concentration and a decrease in isotope ratio going upstream from the estuary. Sequential extractions of sediments indicate that up 70% of the Pu in the Yenisey river is easily mobilized with weak oxidizing agents, which indicates that the Pu is organically bound, while the Pu is more strongly irreversible bound further out

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.)

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)

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)

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.

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)

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.

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.

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.)

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.

The isotope record of short- and long-term dietary changes in sheep tooth enamel: Implications for quantitative reconstruction of paleodiets

Science.gov (United States)

Zazzo, A.; Balasse, M.; Passey, B. H.; Moloney, A. P.; Monahan, F. J.; Schmidt, O.

2010-06-01

Quantitative reconstruction of paleodiet by means of sequential sampling and carbon isotope analysis in hypsodont tooth enamel requires a precise knowledge of the isotopic enrichment between dietary carbon and carbon from enamel apatite ( ɛD-E), as well as of the timing and duration of the enamel mineralization process (amelogenesis). To better constrain these parameters, we performed a series of controlled feeding experiments on sheep ranging in age from 6 to 24 months-old. Twenty-eight lambs and 14 ewes were fed isotopically distinct diets for different periods of time, and then slaughtered, allowing the timing and rate of molar growth to be determined. High resolution sampling and stable carbon isotope analysis of breath CO 2 performed on six individuals following a diet-switch showed that 70-90% of dietary carbon had turned over in less than 24 h. Sequential sampling and carbon isotopic analysis was performed on the first (M 1) and second (M 2) lower molars of four lambs as well as on the third lower molar (M 3) of 11 ewes. The changes in diet were recorded in all molars. We found that the length of enamel matrix apposition is approximately one-quarter of the final tooth length during crown extension, and that enamel maturation spans slightly less than 3 months in M 1, and 4 months in M 2 and M 3. Portions of enamel in equilibrium with dietary carbon were used to calculate ɛD-E values. Animals on grass silage diets had values similar to previous observations, whereas animal switched to pelleted corn diets had values ca. 4‰ lower, a pattern consistent with lower methane production observed for animals fed concentrate diets. The tooth enamel forward model of Passey and Cerling (2002) closely predicted the amplitude of isotope changes recorded in tooth enamel, but slightly underestimated the rate of isotope change, suggesting that the rate of accumulation of carbonate during maturation may not be constant over time. Although stable isotope profiles in tooth

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)

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

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)

Uranium Isotopic Analysis with the FRAM Isotopic Analysis Code

International Nuclear Information System (INIS)

Vo, D.T.; Sampson, T.E.

1999-01-01

FRAM is the acronym for Fixed-Energy Response-Function Analysis with Multiple efficiency. This software was developed at Los Alamos National Laboratory originally for plutonium isotopic analysis. Later, it was adapted for uranium isotopic analysis in addition to plutonium. It is a code based on a self-calibration using several gamma-ray peaks for determining the isotopic ratios. The versatile-parameter database structure governs all facets of the data analysis. User editing of the parameter sets allows great flexibility in handling data with different isotopic distributions, interfering isotopes, and different acquisition parameters such as energy calibration and detector type

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)

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.

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)

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

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)

Simultaneous versus sequential penetrating keratoplasty and cataract surgery.

Science.gov (United States)

Hayashi, Ken; Hayashi, Hideyuki

2006-10-01

To compare the surgical outcomes of simultaneous penetrating keratoplasty and cataract surgery with those of sequential surgery. Thirty-nine eyes of 39 patients scheduled for simultaneous keratoplasty and cataract surgery and 23 eyes of 23 patients scheduled for sequential keratoplasty and secondary phacoemulsification surgery were recruited. Refractive error, regular and irregular corneal astigmatism determined by Fourier analysis, and endothelial cell loss were studied at 1 week and 3, 6, and 12 months after combined surgery in the simultaneous surgery group or after subsequent phacoemulsification surgery in the sequential surgery group. At 3 and more months after surgery, mean refractive error was significantly greater in the simultaneous surgery group than in the sequential surgery group, although no difference was seen at 1 week. The refractive error at 12 months was within 2 D of that targeted in 15 eyes (39%) in the simultaneous surgery group and within 2 D in 16 eyes (70%) in the sequential surgery group; the incidence was significantly greater in the sequential group (P = 0.0344). The regular and irregular astigmatism was not significantly different between the groups at 3 and more months after surgery. No significant difference was also found in the percentage of endothelial cell loss between the groups. Although corneal astigmatism and endothelial cell loss were not different, refractive error from target refraction was greater after simultaneous keratoplasty and cataract surgery than after sequential surgery, indicating a better outcome after sequential surgery than after simultaneous surgery.

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.

On-line double isotope dilution laser ablation inductively coupled plasma mass spectrometry for the quantitative analysis of solid materials.

Science.gov (United States)

Fernández, Beatriz; Rodríguez-González, Pablo; García Alonso, J Ignacio; Malherbe, Julien; García-Fonseca, Sergio; Pereiro, Rosario; Sanz-Medel, Alfredo

2014-12-03

We report on the determination of trace elements in solid samples by the combination of on-line double isotope dilution and laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). The proposed method requires the sequential analysis of the sample and a certified natural abundance standard by on-line IDMS using the same isotopically-enriched spike solution. In this way, the mass fraction of the analyte in the sample can be directly referred to the certified standard so the previous characterization of the spike solution is not required. To validate the procedure, Sr, Rb and Pb were determined in certified reference materials with different matrices, including silicate glasses (SRM 610, 612 and 614) and powdered samples (PACS-2, SRM 2710a, SRM 1944, SRM 2702 and SRM 2780). The analysis of powdered samples was carried out both by the preparation of pressed pellets and by lithium borate fusion. Experimental results for the analysis of powdered samples were in agreement with the certified values for all materials. Relative standard deviations in the range of 6-21% for pressed pellets and 3-21% for fused solids were obtained from n=3 independent measurements. Minimal sample preparation, data treatment and consumption of the isotopically-enriched isotopes are the main advantages of the method over previously reported approaches. Copyright © 2014 Elsevier B.V. All rights reserved.

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%

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

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

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

Great isotope effects in compounding of sodium isotopes by macrocyclic polyether

International Nuclear Information System (INIS)

Knoechel, A.; Wilken, R.D.

1978-01-01

Isotope effects appear in the compounding of the two sodium isotopes 24 Na + and 22 Na + with macrocyclic polyethers, whose value was determined for the 13 best known polyethers. A radiometric process was used for determining the different half life periods of the nuclides used. To separate the compound and non-compound types, these were distributed between water and chloroform. The isotope ratio in the chloroform phase was compared with the output isotope ratio and the separation facfor determined from this. When using crown ethers, there was enrichment of 24 Na + by a significant amount (large crown ether) up to 3.1 +- 0.4% for 18 crown 6. The remarkably high results can be correlated by Biegeleisen's theory with other chemical conditions. There is a report on the first results of transferring these conditions to the H + /T + system. (orig.) [de

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

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.)

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.)

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

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

Sequential mass spectrometric analysis of uranium and plutonium employing resin bead technique

International Nuclear Information System (INIS)

Ramakumar, K.L.; Aggarwal, S.K.; Chitambar, S.A.; Jain, H.C.

1985-01-01

Sequential mass spectrometric analysis of uranium and plutonium employing anion exchange resin bead technique is reported using a high sensitive single stage magnetic analyser instrument, the routinely employed rhenium double filament assembly and 0.5M HNO 3 as a wetting agent for loading the resin beads. A precision of bettter than 0.3per cent (2sigma) is obtained on the isotopic ratio measurements. However, extreme care has to be exercised to carry the resin bead experiments under ultra clean conditions so as to avoid pick up of contamination. (author)

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.

Geochemical and Pb isotopic evidence for sources and dispersal of metal contamination in stream sediments from the mining and smelting district of Pribram, Czech Republic

International Nuclear Information System (INIS)

Ettler, Vojtech; Mihaljevic, Martin; Sebek, Ondrej; Molek, Michael; Grygar, Tomas; Zeman, Josef

2006-01-01

Stream sediments from the mining and smelting district of Pribram, Czech Republic, were studied to determine the degree, sources and dispersal of metal contamination using a combination of bulk metal and mineralogical determinations, sequential extractions and Pb isotopic analyses. The highest metal concentrations were found 3-4 km downstream from the main polymetallic mining site (9800 mg Pb kg -1 , 26 039 mg Zn kg -1 , 316.4 mg Cd kg -1 , 256.9 mg Cu kg -1 ). The calculated enrichment factors (EFs) confirmed the extreme degree of contamination by Pb, Zn and Cd (EF > 40). Lead, Zn and Cd are bound mainly to Fe oxides and hydroxides. In the most contaminated samples Pb is also present as Pb carbonates and litharge (PbO). Lead isotopic analysis indicates that the predominant source of stream sediment contamination is historic Pb-Ag mining and primary Pb smelting ( 206 Pb/ 207 Pb = 1.16), while the role of secondary smelting (car battery processing) is negligible. - Pb isotopes properly complete traditional investigations of metal sources and dispersal in contaminated stream sediments

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

Advances in stable isotope assisted labeling strategies with information science.

Science.gov (United States)

Kigawa, Takanori

2017-08-15

Stable-isotope (SI) labeling of proteins is an essential technique to investigate their structures, interactions or dynamics by nuclear magnetic resonance (NMR) spectroscopy. The assignment of the main-chain signals, which is the fundamental first step in these analyses, is usually achieved by a sequential assignment method based on triple resonance experiments. Independently of the triple resonance experiment-based sequential assignment, amino acid-selective SI labeling is beneficial for discriminating the amino acid type of each signal; therefore, it is especially useful for the signal assignment of difficult targets. Various combinatorial selective labeling schemes have been developed as more sophisticated labeling strategies. In these strategies, amino acids are represented by combinations of SI labeled samples, rather than simply assigning one amino acid to one SI labeled sample as in the case of conventional amino acid-selective labeling. These strategies have proven to be useful for NMR analyses of difficult proteins, such as those in large complex systems, in living cells, attached or integrated into membranes, or with poor solubility. In this review, recent advances in stable isotope assisted labeling strategies will be discussed. Copyright © 2017 Elsevier Inc. All rights reserved.

Sequential Extraction Versus Comprehensive Characterization of Heavy Metal Species in Brownfield Soils

Energy Technology Data Exchange (ETDEWEB)

Dahlin, Cheryl L.; Williamson, Connie A.; Collins, W. Keith; Dahlin, David C.

2002-06-01

The applicability of sequential extraction as a means to determine species of heavy-metals was examined by a study on soil samples from two Superfund sites: the National Lead Company site in Pedricktown, NJ, and the Roebling Steel, Inc., site in Florence, NJ. Data from a standard sequential extraction procedure were compared to those from a comprehensive study that combined optical- and scanning-electron microscopy, X-ray diffraction, and chemical analyses. The study shows that larger particles of contaminants, encapsulated contaminants, and/or man-made materials such as slags, coke, metals, and plastics are subject to incasement, non-selectivity, and redistribution in the sequential extraction process. The results indicate that standard sequential extraction procedures that were developed for characterizing species of contaminants in river sediments may be unsuitable for stand-alone determinative evaluations of contaminant species in industrial-site materials. However, if employed as part of a comprehensive, site-specific characterization study, sequential extraction could be a very useful tool.

Studies of the utilization of phosphorus and nitrogen fertilizers by 32P and 15N isotopes

International Nuclear Information System (INIS)

Dombovari, Janos; Kiss, A.S.

1983-01-01

The utilization of phosphorus and nitrogen fertilizers in crop enhancement was studied with different plants and soils, using 15 N nad 32 P labelling. 15 N was determined by mass spectrometry, 32 P by radiometry. For nitrogen fertilizers better results were achieved by sequential small doses than by single higher doses. The utilization of phosphorus fertilizer strongly depends, in addition to the plant species, on the quality of the soil, especially on its Ca and N contents. Low and high soil liming increased and decreased the utilization of phosphorus, respectively, while nitrogen fertilizers increased it in each case. Measurement of the isotopically exchangable phosphorus content of soils represents a new technique for the determination of the phosphorus uptake. (A.L.)

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.

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

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.

High-precision isotopic characterization of USGS reference materials by TIMS and MC-ICP-MS

Science.gov (United States)

Weis, Dominique; Kieffer, Bruno; Maerschalk, Claude; Barling, Jane; de Jong, Jeroen; Williams, Gwen A.; Hanano, Diane; Pretorius, Wilma; Mattielli, Nadine; Scoates, James S.; Goolaerts, Arnaud; Friedman, Richard M.; Mahoney, J. Brian

2006-08-01

The Pacific Centre for Isotopic and Geochemical Research (PCIGR) at the University of British Columbia has undertaken a systematic analysis of the isotopic (Sr, Nd, and Pb) compositions and concentrations of a broad compositional range of U.S. Geological Survey (USGS) reference materials, including basalt (BCR-1, 2; BHVO-1, 2), andesite (AGV-1, 2), rhyolite (RGM-1, 2), syenite (STM-1, 2), granodiorite (GSP-2), and granite (G-2, 3). USGS rock reference materials are geochemically well characterized, but there is neither a systematic methodology nor a database for radiogenic isotopic compositions, even for the widely used BCR-1. This investigation represents the first comprehensive, systematic analysis of the isotopic composition and concentration of USGS reference materials and provides an important database for the isotopic community. In addition, the range of equipment at the PCIGR, including a Nu Instruments Plasma MC-ICP-MS, a Thermo Finnigan Triton TIMS, and a Thermo Finnigan Element2 HR-ICP-MS, permits an assessment and comparison of the precision and accuracy of isotopic analyses determined by both the TIMS and MC-ICP-MS methods (e.g., Nd isotopic compositions). For each of the reference materials, 5 to 10 complete replicate analyses provide coherent isotopic results, all with external precision below 30 ppm (2 SD) for Sr and Nd isotopic compositions (27 and 24 ppm for TIMS and MC-ICP-MS, respectively). Our results also show that the first- and second-generation USGS reference materials have homogeneous Sr and Nd isotopic compositions. Nd isotopic compositions by MC-ICP-MS and TIMS agree to within 15 ppm for all reference materials. Interlaboratory MC-ICP-MS comparisons show excellent agreement for Pb isotopic compositions; however, the reproducibility is not as good as for Sr and Nd. A careful, sequential leaching experiment of three first- and second-generation reference materials (BCR, BHVO, AGV) indicates that the heterogeneity in Pb isotopic compositions

Isotope analysis of closely adjacent minerals

International Nuclear Information System (INIS)

Smith, M.P.

1990-01-01

This patent describes a method of determining an indicator of at least one of hydrocarbon formation, migration, and accumulation during mineral development. It comprises: searching for a class of minerals in a mineral specimen comprising more than one class of minerals; identifying in the mineral specimen a target sample of the thus searched for class; directing thermally pyrolyzing laser beam radiation onto surface mineral substance of the target sample in the mineral specimen releasing surface mineral substance pyrolysate gases therefrom; and determining isotope composition essentially of the surface mineral substance from analyzing the pyrolysate gases released from the thus pyrolyzed target sample, the isotope composition including isotope(s) selected from the group consisting of carbon, hydrogen, and oxygen isotopes; determining an indicator of at least one of hydrocarbon formation, migration, and accumulation during mineral development of the target mineral from thus determined isotope composition of surface mineral substance pyrolysate

Sequential Power-Dependence Theory

NARCIS (Netherlands)

Buskens, Vincent; Rijt, Arnout van de

2008-01-01

Existing methods for predicting resource divisions in laboratory exchange networks do not take into account the sequential nature of the experimental setting. We extend network exchange theory by considering sequential exchange. We prove that Sequential Power-Dependence Theory—unlike

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)

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.

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)

A novel procedure for Rubidium separation and its isotope measurements on geological samples by MC-ICP-MS

Science.gov (United States)

Ma, J.; Zhang, Z.; Wei, G.; Zhang, L.

2017-12-01

A method including a novel column Rb separation procedure and high-precision Rb isotope measurement in geological materials by using multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS) in standard-sample-bracketing (SSB) mode has been developed. Sr-Spec resin was employed, in which the distribution coefficients for Rb, K, Ba and Sr are different in nitric acid, to sequentially separate them from the matrix. The dissolved samples were loaded on the column in 3 M HNO3, the main matrix such as Al, Ca, Fe, Mg, Mn and Na were removed by rinsing with 4.5 mL HNO3, Rb and K were then sequentially eluted by 3 M HNO3 in different volumes. After that, Ba was eluted by 8 M HNO3, and Sr was finally eluted by Milli-Q water. This enable us to collect the pure Rb, K, Ba and Sr one by one with recovery close to 100% for their isotopic compositions measurement on MC-ICP-MS. We here focus on Rb isotope measurement. The measurement using MC-ICP-MS yielded an internal precision for δ87Rb of external precision was generally better than ± 0.06‰ (2SD) based on the long-term results of the Rb standard solutions NIST SRM 984. A series of geological rock standards, were analyzed using this method, and the results indicate significant Rb isotope differences in different geologic materials. This will provide a powerful tool to investigate Rb isotope fractionation during geological processes.Based on this method, Rb isotope compositions from a basaltic weathering profile were carried out. The data show the lighter Rb (85Rb) isotope is preferentially leached from the weathering profile and remains heavy Rb isotope (87Rb) in the weathered residues during the incipient weathering stage. From the moderate to advanced weathering stage, the significant variations of Rb isotope were observed and multiple factors, such as leaching, adsorption, desorption, and precipitation, should play important role in fractionating Rb isotope.

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)

Uses of stable isotopes

International Nuclear Information System (INIS)

Axente, Damian

1998-01-01

The most important fields of stable isotope use with examples are presented. These are: 1. Isotope dilution analysis: trace analysis, measurements of volumes and masses; 2. Stable isotopes as tracers: transport phenomena, environmental studies, agricultural research, authentication of products and objects, archaeometry, studies of reaction mechanisms, structure and function determination of complex biological entities, studies of metabolism, breath test for diagnostic; 3. Isotope equilibrium effects: measurement of equilibrium effects, investigation of equilibrium conditions, mechanism of drug action, study of natural processes, water cycle, temperature measurements; 4. Stable isotope for advanced nuclear reactors: uranium nitride with 15 N as nuclear fuel, 157 Gd for reactor control. In spite of some difficulties of stable isotope use, particularly related to the analytical techniques, which are slow and expensive, the number of papers reporting on this subject is steadily growing as well as the number of scientific meetings organized by International Isotope Section and IAEA, Gordon Conferences, and regional meeting in Germany, France, etc. Stable isotope application development on large scale is determined by improving their production technologies as well as those of labeled compound and the analytical techniques. (author)

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)

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

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.

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

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

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

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

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)

Sequential contrast-enhanced MR imaging of the penis.

Science.gov (United States)

Kaneko, K; De Mouy, E H; Lee, B E

1994-04-01

To determine the enhancement patterns of the penis at magnetic resonance (MR) imaging. Sequential contrast material-enhanced MR images of the penis in a flaccid state were obtained in 16 volunteers (12 with normal penile function and four with erectile dysfunction). Subjects with normal erectile function showed gradual and centrifugal enhancement of the corpora cavernosa, while those with erectile dysfunction showed poor enhancement with abnormal progression. Sequential contrast-enhanced MR imaging provides additional morphologic information for the evaluation of erectile dysfunction.

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)

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)

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.

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

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)

AMS of actinides in ground- and seawater: a new procedure for simultaneous analysis of U, Np, Pu, Am and Cm isotopes below ppq levels

Energy Technology Data Exchange (ETDEWEB)

Quinto, Francesca; Lagos, Markus; Plaschke, Markus; Schaefer, Thorsten; Geckeis, Horst [Institut fuer Nukleare Entsorgung, KIT, Eggenstein-Leopoldshafen (Germany); Steier, Peter [VERA Laboratory, University of Vienna, Vienna (Austria)

2015-07-01

U-236, Np-237, Pu isotopes and Am-243 were determined in ground- and seawater samples at levels below ppq with a maximum sample size of 0.250 l. Such high sensitivity measurement was possible by using accelerator mass spectrometry (AMS) with an improved gas stripping and an additional high resolving magnet. The use of non-isotopic tracers was investigated in order to allow the determination of those nuclides, namely Np-237 and Am-243, for which isotopic tracers for mass spectrometry are rarely available. The actinides were concentrated from the sample matrix via iron hydroxide co-precipitation and measured sequentially without previous chemical separation from each other. The analytical method was validated with the analysis of IAEA 443 seawater Reference Material and applied to background samples from the Colloid Formation and Migration project at the Grimsel Test Site and to sea- and freshwater samples affected solely by global fallout. The sensitivity of the presented analytical method provides the capability to study the long-term release of actinide tracers in field experiments as well as the transport of actinides in a variety of environmental systems.

Sequential and simultaneous SLAR block adjustment. [spline function analysis for mapping

Science.gov (United States)

Leberl, F.

1975-01-01

Two sequential methods of planimetric SLAR (Side Looking Airborne Radar) block adjustment, with and without splines, and three simultaneous methods based on the principles of least squares are evaluated. A limited experiment with simulated SLAR images indicates that sequential block formation with splines followed by external interpolative adjustment is superior to the simultaneous methods such as planimetric block adjustment with similarity transformations. The use of the sequential block formation is recommended, since it represents an inexpensive tool for satisfactory point determination from SLAR images.

Strontium distribution and origins in a natural clayey formation (Callovian-Oxfordian, Paris Basin, France): a new sequential extraction procedure

International Nuclear Information System (INIS)

Lerouge, C.; Gaucher, E.C.; Tournassat, C.; Negrel, P.; Crouzet, C.; Guerrot, C.; Gautier, A.; Michel, P.; Vinsot, A.; Buschaert, S.

2010-01-01

Document available in extended abstract form only. Strontium is a minor element in the Callovian-Oxfordian clayey formation of Bure (ANDRA Underground Research laboratory, France) and may be interesting as a natural analogue of cationic radionuclides. The objective of our study was to better understand the chemical behaviour of this element since the sediment deposition. Previous mineralogical work showed that main strontium-bearing minerals in the clay-stones, in addition to clay minerals, are celestite, carbonates and accessory micas and K-feldspars. In order to establish the strontium distribution and determine its origins across the clayey formation and establish a strontium diffusion profile, a four step sequential extraction procedure combined with strontium isotopes was developed and adapted to the mineralogy of the Bure clay-stones. The four-steps sequential extraction developed and applied to sixteen samples of Callovian-Oxfordian clay-stones showed that the exchangeable fraction (27 to 48% of the total strontium) and the carbonate fraction (38-47% of the total strontium) are the two main fractions carrying the strontium, the detrital fraction being secondary (< 15%). Celestite is the major strontium-carrier mineral that can perturb the results of the sequential extraction but not significantly modify the distribution of strontium at the scale of the formation. The celestite was studied on micronic to centi-metric crystals, separated by hand-picking on core samples. The development of this sequential extraction procedure for the Callovian-Oxfordian formation shows the importance of the first cobalt hexamine trichloride step to extract the exchangeable strontium adsorbed on clay minerals and block the exchangeable sites with cobalt for the following steps, allowing a good separation of exchangeable fraction and carbonates. However the reagent/solid ratio of 20 seems to be less adapted to carbonate-rich samples. The good separation between exchangeable

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.

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.

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%

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.

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

A latitudinal study of oxygen isotopes within horsehair

Science.gov (United States)

Thompson, E.; Bronk Ramsey, C.; McConnell, J. R.

2016-12-01

This study aims to explore the hypothesis that 'if oxygen isotope ratios deplete with decreasing temperature then a study of oxygen isotope ratios within horsehair from Oxfordshire to Iceland will show a latitudinal depletion gradient'. By looking at oxygen isotope values at different geographical positions, we can track the relationship with latitude and with different regional climate features. This will provide a firmer understanding of how to compare climate records from different locations. Additionally, a comparison of the horse breeds from this study to those analysed within previous studies will create an even better understanding of the intra-species variation within the δ18O values of horsehair. A total of 24 horses were sampled on the 7th March from Thordale Stud in Shetland, the Icelandic Food And Veterinary Authority in Iceland, the Exmoor Pony Centre in Exmoor and the Pigeon House Equestrian Centre in Oxfordshire. By starting the sampling process from the most recent growth at the follicle, the sampling date becomes a chronological marker, temporally fixing the first sample within a sequential set of data points extending for one year or longer, depending on the length of each individual hair. The samples were analysed for oxygen isotope values using an IRMS coupled within a Sercon HTEA. Preliminary results show a latitudinal gradient is evident on comparison between the locations, consistent with the findings of Darling and Talbot's study of fresh water isotopes in the British Isles (2003). These results support the hypothesis, showing that a study of oxygen isotope ratios within horse hair from Oxfordshire to Iceland showing a latitudinal depletion gradient, consistent with a depletion of oxygen isotope ratios due to decreasing temperatures. Darling, W. and Talbot, J. (2003). The O and H stable isotope composition of freshwaters in the British Isles. 1. Rainfall. Hydrol. Earth System Science, 7(2), pp.163-181.

Electrochemical hydrogen isotope sensor based on solid electrolytes

International Nuclear Information System (INIS)

Matsumoto, Hiroshige; Hayashi, Hiroyuki; Iwahara, Hiroyasu

2002-01-01

An electrochemical sensor of hydrogen isotopes based on solid electrolytes for determining the hydrogen isotope ratios and/or total hydrogen pressures in gases has been developed. This paper describes the methodology of the hydrogen isotope sensing together with experimental results. When hydrogen isotope gases are introduced to an electrochemical cell using a proton-conducting electrolyte (hydrogen isotope cell), the electromotive force (EMF) of the cell agrees with that theoretically estimated. The EMF signals can be used for the determination of the hydrogen isotope ratio in gases if the total hydrogen pressure is predetermined. By supplementary use of an oxide ion conductor cell, both the ratio and total pressure of the hydrogen isotopes can be simultaneously determined. (author)

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

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...

Sequential chemical treatment of radium species in TENORM waste sludge produced from oil and natural gas production

International Nuclear Information System (INIS)

El Afifi, E.M.; Awwad, N.S.; Hilal, M.A.

2009-01-01

This paper is dedicated to the treatment of sludge occurring in frame of the Egyptian produced from oil and gas production. The activity levels of three radium isotopes: Ra-226 (of U-series), Ra-228 and Ra-224 (of Th-series) in the solid TENORM waste (sludge) were first evaluated and followed by a sequential treatment for all radium species (fractions) presented in TENORM. The sequential treatment was carried out based on two approaches 'A' and 'B' using different chemical solutions. The results obtained indicate that the activity levels of all radium isotopes (Ra-226, Ra-228 and Ra-224) of the environmental interest in the TENORM waste sludge were elevated with regard to exemption levels established by IAEA [International Atomic Energy Agency (IAEA), International basic safety standards for the protection against ionizing radiation and for the safety of radiation sources. GOV/2715/Vienna, 1994]. Each approach of the sequential treatment was performed through four steps using different chemical solutions to reduce the activity concentration of radium in a large extent. Most of the leached radium was found as an oxidizable Ra species. The actual removal % leached using approach B was relatively efficient compared to A. It is observed that the actual removal percentages (%) of Ra-226, Ra-228 and Ra-224 using approach A are 78 ± 2.8, 64.8 ± 4.1 and 76.4 ± 5.2%, respectively. Whereas in approach A, the overall removal % of Ra-226, Ra-228 and Ra-228 was increased to ∼91 ± 3.5, 87 ± 4.1 and 90 ± 6.2%, respectively

Factors controlling Li concentration and isotopic composition in formation waters and host rocks of Marcellus Shale, Appalachian Basin

Science.gov (United States)

Phan, Thai T.; Capo, Rosemary C; Stewart, Brian W.; Macpherson, Gwen; Rowan, Elisabeth L.; Hammack, Richard W.

2015-01-01

In this study, water and whole rock samples from hydraulically fractured wells in the Marcellus Shale (Middle Devonian), and water from conventional wells producing from Upper Devonian sandstones were analyzed for lithium concentrations and isotope ratios (δ7Li). The distribution of lithium concentrations in different mineral groups was determined using sequential extraction. Structurally bound Li, predominantly in clays, accounted for 75-91 wt. % of total Li, whereas exchangeable sites and carbonate cement contain negligible Li (< 3%). Up to 20% of the Li is present in the oxidizable fraction (organic matter and sulfides). The δ7Li values for whole rock shale in Greene Co., Pennsylvania, and Tioga Co., New York, ranged from -2.3 to + 4.3‰, similar to values reported for other shales in the literature. The δ7Li values in shale rocks with stratigraphic depth record progressive weathering of the source region; the most weathered and clay-rich strata with isotopically light Li are found closest to the top of the stratigraphic section. Diagenetic illite-smectite transition could also have partially affected the bulk Li content and isotope ratios of the Marcellus Shale.

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)

The isotopic contamination in electromagnetic isotope separators; La contagion isotopique dans les separateurs electromagnetiques d'isotopes

Energy Technology Data Exchange (ETDEWEB)

Cassignol, Ch [Commissariat a l' Energie Atomique, Saclay (France).Centre d' Etudes Nucleaires

1959-07-01

In the early years of isotope separation, and in particular electromagnetic isotope separation, needs for rapid results have conducted to empiric research. This paper describes fundamental research on the electromagnetic isotope separation to a better understanding of isotope separators as well as improving the performances. Focus has been made on the study of the principle of isotope contamination and the remedial action on the separator to improve the isotope separation ratio. In a first part, the author come back to the functioning of an electromagnetic separator and generalities on isotope contamination. Secondly, it describes the two stages separation method with two dispersive apparatus, an electromagnetic separation stage followed by an electrostatic separation stage, both separated by a diaphragm. The specifications of the electrostatic stage are given and its different settings and their consequences on isotope separation are investigated. In a third part, mechanisms and contamination factors in the isotope separation are discussed: natural isotope contamination, contamination by rebounding on the collector, contamination because of a low resolution, contamination by chromatism and diffusion effect, breakdown of condenser voltage. Analysis of experimental results shows the diffusion as the most important contamination factor in electromagnetic isotope separation. As contamination factors are dependent on geometric parameters, sector angle, radius of curvature in the magnetic field and clearance height are discussed in a fourth part. The better understanding of the mechanism of the different contamination factors and the study of influential parameters as pressure and geometric parameters lead to define a global scheme of isotope contamination and determinate optima separator design and experimental parameters. Finally, the global scheme of isotope contamination and hypothesis on optima specifications and experimental parameters has been checked during a

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

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...

Simulation of dual carbon-bromine stable isotope fractionation during 1,2-dibromoethane degradation.

Science.gov (United States)

Jin, Biao; Nijenhuis, Ivonne; Rolle, Massimo

2018-06-01

We performed a model-based investigation to simultaneously predict the evolution of concentration, as well as stable carbon and bromine isotope fractionation during 1,2-dibromoethane (EDB, ethylene dibromide) transformation in a closed system. The modelling approach considers bond-cleavage mechanisms during different reactions and allows evaluating dual carbon-bromine isotopic signals for chemical and biotic reactions, including aerobic and anaerobic biological transformation, dibromoelimination by Zn(0) and alkaline hydrolysis. The proposed model allowed us to accurately simulate the evolution of concentrations and isotope data observed in a previous laboratory study and to successfully identify different reaction pathways. Furthermore, we illustrated the model capabilities in degradation scenarios involving complex reaction systems. Specifically, we examined (i) the case of sequential multistep transformation of EDB and the isotopic evolution of the parent compound, the intermediate and the reaction product and (ii) the case of parallel competing abiotic pathways of EDB transformation in alkaline solution.

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)

Chromium isotope variations

DEFF Research Database (Denmark)

D'Arcy, Joan Mary

the δ53Cr value of continental runoff into the ocean. The major findings were that river water is characterised by heavy δ53Cr values (+0.1‰ to +1.6‰), while soils are characterised by light δ53Cr values (-0.3‰), relative to the catchment bedrock (-0.17‰ to -0.21‰), indicating that Cr isotopes......, and the quantification the Cr isotope composition of major Cr fluxes into and out of ocean. This thesis adds to the current knowledge of the Cr isotope system and is divided into two studies. The focus of the first study was to determine what processes control the Cr isotopic compositionof river water and to quantify......Chromium (Cr) stable isotopes are a useful tracer of changes in redox conditions because changes in its oxidation state are accompanied by an isotopic fractionation. For this reason the Cr isotope system is being developed as a potential tool for paleo-redox reconstruction. Dissolved Cr in seawater...

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.

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.

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.

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)

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)

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

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.)

Multi isotopic characterization (Li-Cu-Zn-Pb) of waste waters pollution in a small watershed (Loire River basin, France)

Science.gov (United States)

Millot, R.; Desaulty, A. M.; Perret, S.; Bourrain, X.

2016-12-01

The goal of this study is to use multi-isotopic signature to track the pollution in surface waters, and to understand the complex processes causing the metals mobilization and transport in the environment. In the present study, we investigate waste water releases from a hospital water treatment plant and its potential impact in a small river basin near Orléans in France (Egoutier watershed: 15 km²and 5 km long). We decided to monitor this small watershed which is poorly urbanized in the Loire river basin. Its spring is located in a pristine area (forested area), while it is only impacted some kilometers further by the releases rich in metals coming from a hospital water treatment plant. A sampling of these liquid effluents as well as dissolved load and sediment from upstream to downstream was realized and their concentrations and isotopic data were determined. Isotopic ratios were measured using a MC-ICP-MS at BRGM, after a specific protocol of purification for each isotopic systematics. Lithium isotopic compositions are rather homogeneous in river waters along the main course of the stream. The waste water signal is very different from the natural background with significant heavy lithium contribution (high δ7Li). Lead isotopic compositions are rather homogenous in river waters and sediments with values close to geologic background. For Zn, the sediments with high concentrations and depleted isotopic compositions (low δ66Zn), typical of an anthropic pollution, are strongly impacted. The analyses of Cu isotopes in sediments show the impact of waster waters, but also isotopic fractionations due to redox processes in the watershed. To better understand these processes controlling the release of metals in water, sequential extractions on sediments are in progress under laboratory conditions and will provide important constraints for metal distribution in this river basin.

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...

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.

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

Sequential analysis in neonatal research-systematic review.

Science.gov (United States)

Lava, Sebastiano A G; Elie, Valéry; Ha, Phuong Thi Viet; Jacqz-Aigrain, Evelyne

2018-05-01

As more new drugs are discovered, traditional designs come at their limits. Ten years after the adoption of the European Paediatric Regulation, we performed a systematic review on the US National Library of Medicine and Excerpta Medica database of sequential trials involving newborns. Out of 326 identified scientific reports, 21 trials were included. They enrolled 2832 patients, of whom 2099 were analyzed: the median number of neonates included per trial was 48 (IQR 22-87), median gestational age was 28.7 (IQR 27.9-30.9) weeks. Eighteen trials used sequential techniques to determine sample size, while 3 used continual reassessment methods for dose-finding. In 16 studies reporting sufficient data, the sequential design allowed to non-significantly reduce the number of enrolled neonates by a median of 24 (31%) patients (IQR - 4.75 to 136.5, p = 0.0674) with respect to a traditional trial. When the number of neonates finally included in the analysis was considered, the difference became significant: 35 (57%) patients (IQR 10 to 136.5, p = 0.0033). Sequential trial designs have not been frequently used in Neonatology. They might potentially be able to reduce the number of patients in drug trials, although this is not always the case. What is known: • In evaluating rare diseases in fragile populations, traditional designs come at their limits. About 20% of pediatric trials are discontinued, mainly because of recruitment problems. What is new: • Sequential trials involving newborns were infrequently used and only a few (n = 21) are available for analysis. • The sequential design allowed to non-significantly reduce the number of enrolled neonates by a median of 24 (31%) patients (IQR - 4.75 to 136.5, p = 0.0674).

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.

Use of isotope effects to elucidate enzyme mechanisms

International Nuclear Information System (INIS)

Cleland, W.W.

1982-01-01

The chemical bond breaking steps are normally not rate limiting for enzymatic reactions. However, comparison of deuterium and tritium isotope effects on the same reaction, especially when coupled with 13 C isotope effects for the same step measured with deuterated as well as unlabeled substrates, allows calculation of the intrinsic isotope effects on the bond breaking steps and thus a determination of the commitments to catalysis for the reactants. The variation in observed isotope effects as a function of reactant concentration can be used to determine kinetic mechanisms, while the pH variation of isotope effects can determine the stickiness of the reactants and which portions of the reactant mechanism are pH dependent. Finally the size of primary and secondary intrinsic isotope effects can be used to determine transition state structure

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

Climate and isotopic tracers

International Nuclear Information System (INIS)

Jean-Baptiste, Ph.

1997-01-01

The applications of natural radioactivity and isotopic measurements in the sciences concerning Earth and its atmosphere, are numerous: carbon 14 dating with the Tandetron apparatus at the Cea, measurement of oxygen 18 in coral or sediment limestone for the determination of ocean temperature and salinity, carbon 14 dating of corals for the determination of sea level variations, deuterium content in polar ice-cap leads to temperature variations determination; isotopic measurements also enable the determination of present climate features such as global warming, oceanic general circulation

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.

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)

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)

Monitoring sequential electron transfer with EPR

International Nuclear Information System (INIS)

Thurnauer, M.C.; Feezel, L.L.; Snyder, S.W.; Tang, J.; Norris, J.R.; Morris, A.L.; Rustandi, R.R.

1989-01-01

A completely general model which treats electron spin polarization (ESP) found in a system in which radical pairs with different magnetic interactions are formed sequentially has been described. This treatment has been applied specifically to the ESP found in the bacterial reaction center. Test cases show clearly how parameters such as structure, lifetime, and magnetic interactions within the successive radical pairs affect the ESP, and demonstrate that previous treatments of this problem have been incomplete. The photosynthetic bacterial reaction center protein is an ideal system for testing the general model of ESP. The radical pair which exhibits ESP, P 870 + Q - (P 870 + is the oxidized, primary electron donor, a bacteriochlorophyll special pair and Q - is the reduced, primary quinone acceptor) is formed via sequential electron transport through the intermediary radical pair P 870 + I - (I - is the reduced, intermediary electron acceptor, a bacteriopheophytin). In addition, it is possible to experimentally vary most of the important parameters, such as the lifetime of the intermediary radical pair and the magnetic interactions in each pair. It has been shown how selective isotopic substitution ( 1 H or 2 H) on P 870 , I and Q affects the ESP of the EPR spectrum of P 870 + Q - , observed at two different microwave frequencies, in Fe 2+ -depleted bacterial reaction centers of Rhodobacter sphaeroides R26. Thus, the relative magnitudes of the magnetic properties (nuclear hyperfine and g-factor differences) which influence ESP development were varied. The results support the general model of ESP in that they suggest that the P 870 + Q - radical pair interactions are the dominant source of ESP production in 2 H bacterial reaction centers

The isotopic contamination in electromagnetic isotope separators; La contagion isotopique dans les separateurs electromagnetiques d'isotopes

Energy Technology Data Exchange (ETDEWEB)

Cassignol, Ch. [Commissariat a l' Energie Atomique, Saclay (France).Centre d' Etudes Nucleaires

1959-07-01

In the early years of isotope separation, and in particular electromagnetic isotope separation, needs for rapid results have conducted to empiric research. This paper describes fundamental research on the electromagnetic isotope separation to a better understanding of isotope separators as well as improving the performances. Focus has been made on the study of the principle of isotope contamination and the remedial action on the separator to improve the isotope separation ratio. In a first part, the author come back to the functioning of an electromagnetic separator and generalities on isotope contamination. Secondly, it describes the two stages separation method with two dispersive apparatus, an electromagnetic separation stage followed by an electrostatic separation stage, both separated by a diaphragm. The specifications of the electrostatic stage are given and its different settings and their consequences on isotope separation are investigated. In a third part, mechanisms and contamination factors in the isotope separation are discussed: natural isotope contamination, contamination by rebounding on the collector, contamination because of a low resolution, contamination by chromatism and diffusion effect, breakdown of condenser voltage. Analysis of experimental results shows the diffusion as the most important contamination factor in electromagnetic isotope separation. As contamination factors are dependent on geometric parameters, sector angle, radius of curvature in the magnetic field and clearance height are discussed in a fourth part. The better understanding of the mechanism of the different contamination factors and the study of influential parameters as pressure and geometric parameters lead to define a global scheme of isotope contamination and determinate optima separator design and experimental parameters. Finally, the global scheme of isotope contamination and hypothesis on optima specifications and experimental parameters has been checked during a

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)

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.)

Sequential Analysis of Metals in Municipal Dumpsite Composts of ...

African Journals Online (AJOL)

... Ni) in Municipal dumpsite compost were determined by the sequential extraction method. Chemical parameters such as pH, conductivity, and organic carbon contents of the samples were also determined. Analysis of the extracts was carried out by atomic absorption spectrophotometer machine (Buck Scientific VPG 210).

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.

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.

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

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

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).

Multi-actinide analysis with AMS for ultra-trace determination and small sample sizes: advantages and drawbacks

Energy Technology Data Exchange (ETDEWEB)

Quinto, Francesca; Lagos, Markus; Plaschke, Markus; Schaefer, Thorsten; Geckeis, Horst [Institute for Nuclear Waste Disposal, Karlsruhe Institute of Technology (Germany); Steier, Peter; Golser, Robin [VERA Laboratory, Faculty of Physics, University of Vienna (Austria)

2016-07-01

With the abundance sensitivities of AMS for U-236, Np-237 and Pu-239 relative to U-238 at levels lower than 1E-15, a simultaneous determination of several actinides without previous chemical separation from each other is possible. The actinides are extracted from the matrix elements via an iron hydroxide co-precipitation and the nuclides sequentially measured from the same sputter target. This simplified method allows for the use of non-isotopic tracers and consequently the determination of Np-237 and Am-243 for which isotopic tracers with the degree of purity required by ultra-trace mass-spectrometric analysis are not available. With detection limits of circa 1E+4 atoms in a sample, 1E+8 atoms are determined with circa 1 % relative uncertainty due to counting statistics. This allows for an unprecedented reduction of the sample size down to 100 ml of natural water. However, the use of non-isotopic tracers introduces a dominating uncertainty of up to 30 % related to the reproducibility of the results. The advantages and drawbacks of the novel method will be presented with the aid of recent results from the CFM Project at the Grimsel Test Site and from the investigation of global fallout in environmental samples.

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)

Modelling sequentially scored item responses

NARCIS (Netherlands)

Akkermans, W.

2000-01-01

The sequential model can be used to describe the variable resulting from a sequential scoring process. In this paper two more item response models are investigated with respect to their suitability for sequential scoring: the partial credit model and the graded response model. The investigation is

Native Frames: Disentangling Sequential from Concerted Three-Body Fragmentation

Science.gov (United States)

Rajput, Jyoti; Severt, T.; Berry, Ben; Jochim, Bethany; Feizollah, Peyman; Kaderiya, Balram; Zohrabi, M.; Ablikim, U.; Ziaee, Farzaneh; Raju P., Kanaka; Rolles, D.; Rudenko, A.; Carnes, K. D.; Esry, B. D.; Ben-Itzhak, I.

2018-03-01

A key question concerning the three-body fragmentation of polyatomic molecules is the distinction of sequential and concerted mechanisms, i.e., the stepwise or simultaneous cleavage of bonds. Using laser-driven fragmentation of OCS into O++C++S+ and employing coincidence momentum imaging, we demonstrate a novel method that enables the clear separation of sequential and concerted breakup. The separation is accomplished by analyzing the three-body fragmentation in the native frame associated with each step and taking advantage of the rotation of the intermediate molecular fragment, CO2 + or CS2 + , before its unimolecular dissociation. This native-frame method works for any projectile (electrons, ions, or photons), provides details on each step of the sequential breakup, and enables the retrieval of the relevant spectra for sequential and concerted breakup separately. Specifically, this allows the determination of the branching ratio of all these processes in OCS3 + breakup. Moreover, we find that the first step of sequential breakup is tightly aligned along the laser polarization and identify the likely electronic states of the intermediate dication that undergo unimolecular dissociation in the second step. Finally, the separated concerted breakup spectra show clearly that the central carbon atom is preferentially ejected perpendicular to the laser field.

Oxygen isotopic fractionation of O₂ during adsorption and desorption processes using molecular sieve at low temperatures.

Science.gov (United States)

Ahn, Insu; Kusakabe, Minoru; Lee, Jong Ik

2014-06-15

Cryogenic trapping using molecular sieves is commonly used to collect O2 extracted from silicates for (17)O/(16)O and (18)O/(16)O analyses. However, gases which interfere with (17)O/(16)O analysis, notably NF3, are also trapped and their removal is essential for accurate direct measurement of the (17)O/(16)O ratio. It is also necessary to identify and quantify any isotopic fractionation associated with the use of cryogenic trapping using molecular sieves. The oxygen isotopic compositions of O2 before and after desorption from, and adsorption onto, 13X and 5A molecular sieves (MS13X and MS5A) at 0°C, -78°C, -114°C, and -130°C were measured in order to determine the oxygen isotopic fractionation at these temperatures. We also investigated whether isotopic fractionation occurred when O2 gas was transferred sequentially into a second cold finger, also containing molecular sieve. It was confirmed that significant oxygen isotopic fractionation occurs between the gaseous O2 and that adsorbed onto molecular sieve, if desorption and adsorption are incomplete. As the fraction of released or untrapped O2 becomes smaller with decreasing trapping temperature (from 0 to -130°C), the isotopic fractionation becomes larger. Approximately half of the total adsorbed O2 is released from the molecular sieve during desorption at -114°C, which is the temperature recommended for separation from NF3 (retained on the molecular sieve), and this will interfere with (17)O/(16)O measurements. The use of a single cold finger should be avoided, because partial desorption is accompanied by oxygen isotopic fractionation, thereby resulting in inaccurate isotopic data. The use of a dual cold finger arrangement is recommended because, as we have confirmed, the transfer of O2 from the first trap to the second is almost 100%. However, even under these conditions, a small isotopic fractionation (0.18 ± 0.05‰ in δ(17)O values and 0.26 ± 0.06‰ in δ(18)O values) occurred, with O2 in

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

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

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)

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.

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)

Determination of the isotopic abundance of 235U in rocks in search for an Oklo phenomenon in Brazil by activation analysis

International Nuclear Information System (INIS)

Vasconcellos, M.B.A.; Armelin, M.J.A.; Lima, F.W. de; Fulfaro, R.

1981-09-01

Isotopic analyses of uranium are generally carried out by mass spectrometry, with a precision better than 1%. In nuclear laboratories it is often necessary to perform rapid determinations of 235 U isotopic abundances. Thermal neutron activation analysis by delayed neutron counting or by high resolution gamma-ray spectrometry can be applied for this purpose, although with less precision than by mass spectrometry. In this work, delayed neutron counting and gamma-ray spectrometry are used for the determination of the isotopic abundance of 235 U in rocks from the Northeastern region of Brazil. In the case of the application of delayed neutron counting, the rocks are analyzed non-destructively. When high resolution gamma-ray spectrometry is applied, a pre-irradiation chemical separation had to be performed, by extraction of uranium with tributylphosphate. By both methods employed the results for the isotopic abundance of 235 U can be considered as equal to the natural value of 0.702%, for the rocks under study. The precision attained by gamma-ray spectrometry is better than that by delayed neutron couting. (Author) [pt

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

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)

Cost-effectiveness of simultaneous versus sequential surgery in head and neck reconstruction.

Science.gov (United States)

Wong, Kevin K; Enepekides, Danny J; Higgins, Kevin M

2011-02-01

To determine whether simultaneous (ablation and reconstruction overlaps by two teams) head and neck reconstruction is cost effective compared to sequentially (ablation followed by reconstruction) performed surgery. Case-controlled study. Tertiary care hospital. Oncology patients undergoing free flap reconstruction of the head and neck. A match paired comparison study was performed with a retrospective chart review examining the total time of surgery for sequential and simultaneous surgery. Nine patients were selected for both the sequential and simultaneous groups. Sequential head and neck reconstruction patients were pair matched with patients who had undergone similar oncologic ablative or reconstructive procedures performed in a simultaneous fashion. A detailed cost analysis using the microcosting method was then undertaken looking at the direct costs of the surgeons, anesthesiologist, operating room, and nursing. On average, simultaneous surgery required 3 hours 15 minutes less operating time, leading to a cost savings of approximately $1200/case when compared to sequential surgery. This represents approximately a 15% reduction in the cost of the entire operation. Simultaneous head and neck reconstruction is more cost effective when compared to sequential surgery.

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)

Multi-agent sequential hypothesis testing

KAUST Repository

Kim, Kwang-Ki K.

2014-12-15

This paper considers multi-agent sequential hypothesis testing and presents a framework for strategic learning in sequential games with explicit consideration of both temporal and spatial coordination. The associated Bayes risk functions explicitly incorporate costs of taking private/public measurements, costs of time-difference and disagreement in actions of agents, and costs of false declaration/choices in the sequential hypothesis testing. The corresponding sequential decision processes have well-defined value functions with respect to (a) the belief states for the case of conditional independent private noisy measurements that are also assumed to be independent identically distributed over time, and (b) the information states for the case of correlated private noisy measurements. A sequential investment game of strategic coordination and delay is also discussed as an application of the proposed strategic learning rules.

Isotope-dilution mass spectrometry in the measurement of plutonium isotope half-lives

International Nuclear Information System (INIS)

Abernathey, R.M.; Marsh, S.F.

1981-01-01

Isotope-dilution mass spectrometry has been used at Los Alamos to measure the half-lives of 239 Pu, 240 Pu, and 241 Pu. The latter was determined by measuring the rate of decrease of the 241 Pu/ 242 Pu ratio in an appropriate isotopic mixture over a period of several years. The half-lives of the two lighter isotopes are too long to be determined in this manner. They were determined by measuring the rate of production of the uranium daughter relative to a known added 233 U spike. Experimental procedures were designed to control sources of error and to permit a detailed statistical treatment which included all known sources of error and accounted for all covariances. The uncertainties, at the 95% confidence level, associated with the measured half-lives were less than 0.4% for 241 Pu and less than 0.2% for 239 Pu and 240 Pu

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

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.

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.

Heterogeneity of the Caribbean plateau mantle source: Sr, O and He isotopic compositions of olivine and clinopyroxene from Gorgona Island

Science.gov (United States)

Révillon, S.; Chauvel, C.; Arndt, N. T.; Pik, R.; Martineau, F.; Fourcade, S.; Marty, B.

2002-12-01

The composition of the mantle plumes that created large oceanic plateaus such as Ontong Java or the Caribbean is still poorly known. Geochemical and isotopic studies on accreted portions of the Caribbean plateau have shown that the plume source was heterogeneous and contained isotopically depleted and relatively enriched portions. A distinctive feature of samples from the Caribbean plateau is their unusual Sr isotopic compositions, which, at a given Nd isotopic ratio, are far higher than in samples from other oceanic plateaus. Sr, O and He isotopic compositions of whole rocks and magmatic minerals (clinopyroxene or olivine) separated from komatiites, gabbros and peridotites from Gorgona Island in Colombia were determined to investigate the origin of these anomalously radiogenic compositions. Sequentially leached clinopyroxenes have Sr isotopic compositions in the range 87Sr/ 86Sr=0.70271-0.70352, systematically lower than those of leached and unleached whole rocks. Oxygen isotopic ratios of clinopyroxene vary within the range δ 18O=5.18-5.35‰, similar to that recorded in oceanic island basalts. He isotopic ratios are high ( R/ Ra=8-19). The lower 87Sr/ 86Sr ratios of most of the clinopyroxenes shift the field of the Caribbean plateau in Nd-Sr isotope diagrams toward more 'normal' values, i.e. a position closer to the field defined by mid-ocean ridge basalts and oceanic-island basalts. Three clinopyroxenes have slightly higher 87Sr/ 86Sr ratios that cannot be explained by an assimilation model. The high 87Sr/ 86Sr and variations of 143Nd/ 144Nd are interpreted as a source characteristic. Trace-element ratios, however, are controlled mainly by fractionation during partial melting. We combine these isotopic data in a heterogeneous plume source model that accounts for the diversity of isotopic signatures recorded on Gorgona Island and throughout the Caribbean plateau. The heterogeneities are related to old recycled oceanic lithosphere in the plume source; the high 3

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)

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.

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)

Physics-based, Bayesian sequential detection method and system for radioactive contraband

Science.gov (United States)

Candy, James V; Axelrod, Michael C; Breitfeller, Eric F; Chambers, David H; Guidry, Brian L; Manatt, Douglas R; Meyer, Alan W; Sale, Kenneth E

2014-03-18

A distributed sequential method and system for detecting and identifying radioactive contraband from highly uncertain (noisy) low-count, radionuclide measurements, i.e. an event mode sequence (EMS), using a statistical approach based on Bayesian inference and physics-model-based signal processing based on the representation of a radionuclide as a monoenergetic decomposition of monoenergetic sources. For a given photon event of the EMS, the appropriate monoenergy processing channel is determined using a confidence interval condition-based discriminator for the energy amplitude and interarrival time and parameter estimates are used to update a measured probability density function estimate for a target radionuclide. A sequential likelihood ratio test is then used to determine one of two threshold conditions signifying that the EMS is either identified as the target radionuclide or not, and if not, then repeating the process for the next sequential photon event of the EMS until one of the two threshold conditions is satisfied.

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

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.

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.

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

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....

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.

Isotopic study of water evaporation in a clayey soil, experimentation and modelling

International Nuclear Information System (INIS)

Mathieu, R.; Bariac, T.

1995-01-01

The isotopic theory of soil water evaporation in steady-state was applied to the quantification of shallow water table discharge rates in arid and semi-arid climates. This approach is limited by the time needed by the soil to reach the steady state after the last significant rain event. The 1D numerical model ''Moise'', proposed here, was developed for the simulation of the vertical profiles of water and stable isotope contents in a drying soil for any initial profile and atmospheric condition. Six non-perturbed soil columns of 1.1 m length were taken from Barogo, Burkina Faso and were saturated in the laboratory by infiltration and free drainage of pounding water and then allowed to evaporate freely. The columns were then sequentially sampled after 11, 42, 92, 162 and 253 days of drying for 18 O and 2 H isotopic analyses. 18 O profiles show an exponential shape during the first drying stage with a maximum isotopic enrichment at the surface. During the second drying stage, the penetration of very depleted atmospheric vapor tends to lower the isotopic content at the surface. The water and isotopic content were simulated with the Moise model. The model satisfactory reproduces the hydrodynamic evolution and the qualitative evolution of soil water isotopic content, but it largely overestimates the overall enrichment. It is thus plausible that a fraction of the soil water may keep its own isotopic composition with restricted exchanges with the surrounding mobile water and vapor, while a mobile phase can be affected by the isotopic enrichment. (J.S.). 27 refs., 6 figs., 3 tabs

Comparative analysis of monoclonal antibody N-glycosylation using stable isotope labelling and UPLC-fluorescence-MS.

Science.gov (United States)

Millán Martín, Silvia; Delporte, Cédric; Farrell, Amy; Navas Iglesias, Natalia; McLoughlin, Niaobh; Bones, Jonathan

2015-03-07

A twoplex method using (12)C6 and (13)C6 stable isotope analogues (Δmass = 6 Da) of 2-aminobenzoic acid (2-AA) is described for quantitative analysis of N-glycans present on monoclonal antibodies and other glycoproteins using ultra performance liquid chromatography with sequential fluorescence and accurate mass tandem quadrupole time of flight (QToF) mass spectrometric detection.

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.

Basal ganglia and cortical networks for sequential ordering and rhythm of complex movements

Directory of Open Access Journals (Sweden)

Jeffery G. Bednark

2015-07-01

Full Text Available Voluntary actions require the concurrent engagement and coordinated control of complex temporal (e.g. rhythm and ordinal motor processes. Using high-resolution functional magnetic resonance imaging (fMRI and multi-voxel pattern analysis (MVPA, we sought to determine the degree to which these complex motor processes are dissociable in basal ganglia and cortical networks. We employed three different finger-tapping tasks that differed in the demand on the sequential temporal rhythm or sequential ordering of submovements. Our results demonstrate that sequential rhythm and sequential order tasks were partially dissociable based on activation differences. The sequential rhythm task activated a widespread network centered around the SMA and basal-ganglia regions including the dorsomedial putamen and caudate nucleus, while the sequential order task preferentially activated a fronto-parietal network. There was also extensive overlap between sequential rhythm and sequential order tasks, with both tasks commonly activating bilateral premotor, supplementary motor, and superior/inferior parietal cortical regions, as well as regions of the caudate/putamen of the basal ganglia and the ventro-lateral thalamus. Importantly, within the cortical regions that were active for both complex movements, MVPA could accurately classify different patterns of activation for the sequential rhythm and sequential order tasks. In the basal ganglia, however, overlapping activation for the sequential rhythm and sequential order tasks, which was found in classic motor circuits of the putamen and ventro-lateral thalamus, could not be accurately differentiated by MVPA. Overall, our results highlight the convergent architecture of the motor system, where complex motor information that is spatially distributed in the cortex converges into a more compact representation in the basal ganglia.

Accurate isotope ratio mass spectrometry. Some problems and possibilities

International Nuclear Information System (INIS)

Bievre, P. de

1978-01-01

The review includes reference to 190 papers, mainly published during the last 10 years. It covers the following: important factors in accurate isotope ratio measurements (precision and accuracy of isotope ratio measurements -exemplified by determinations of 235 U/ 238 U and of other elements including 239 Pu/ 240 Pu; isotope fractionation -exemplified by curves for Rb, U); applications (atomic weights); the Oklo natural nuclear reactor (discovered by UF 6 mass spectrometry at Pierrelatte); nuclear and other constants; isotope ratio measurements in nuclear geology and isotope cosmology - accurate age determination; isotope ratio measurements on very small samples - archaeometry; isotope dilution; miscellaneous applications; and future prospects. (U.K.)

Lead isotopes in tap water: implications for Pb sources within a municipal water supply system

International Nuclear Information System (INIS)

Cheng Zhongqi; Foland, Kenneth A.

2005-01-01

Residential tap waters were investigated to examine the feasibility of using isotopic ratios to identify dominant sources of water Pb in the Columbus (Ohio, USA) municipal supply system. Overall, both the concentrations, which are generally low (0.1-28 μg/L), and isotopic compositions of tap water Pb show wide variations. This contrasts with the situation for a limited number of available service lines, which exhibit only a limited Pb-isotope variation but contain Pb of two very different types with one significantly more radiogenic than the other. Most tap water samples in contact with Pb service lines have Pb-isotope ratios that are different from the pipe Pb. Furthermore, the Pb isotope compositions of sequentially drawn samples in the same residence generally are similar, but those from separate residences are different, implying dominant Pb sources from domestic plumbing. A separate pilot study at two residences without Pb service lines shows isotopic similarity between water and solders in each house, further suggesting that the major Pb sources are domestic in these cases and dominated by Pb from solder joints. Although complicated by the broad range of overall Pb-isotope variations observed and limited by sample availability, the results suggest that Pb isotopes can be used effectively to constrain the sources of Pb in tap waters, especially for individual houses where multiple source candidates can be identified

Comparison between IRMS and CRDS methods in the determination of isotopic ratios 2H/1H and 18O/16O in water

International Nuclear Information System (INIS)

Santos, T. H. R.; Zucchi, M. R.; Lemaire, T.; Azevedo, A. E. G.

2013-01-01

Traditionally, the method used for measuring the isotope ratios is the Isotope Ratio Mass Spectrometers (IRMS). A new method has been used to determine the isotopic abundances, the Cavity Ring-Down Spectroscopy (CRDS). It consists of a technique of direct absorption, of high sensitivity, which is based on measuring the absorption ratio, as a function of time, of the light confined in a high finesse optical cavity, instead of the magnitude of light beam absorption. The values of 18 O/ 16 O and D/H ratios are determined with respect to international standards VSMOW, GISP and SLAP from the International Atomic Energy Agency (IAEA). In this work, the IRMS and CRDS techniques are compared, verifying that the CRDS technique is promising and has some advantages compared to IRMS. It uses a smaller amount of sample, the isotope measurements are made simultaneously from the steam, reducing the analysis time. It also shows good reproducibility and accuracy, and it does not require a preliminary sample preparation.

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)

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

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

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.

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

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.

Separation of uranium and plutonium isotopes for measurement by multi collector inductively coupled plasma mass spectroscopy

International Nuclear Information System (INIS)

Martinelli, R.E.; Hamilton, T.F.; Kehl, S.R.; Williams, R.W.

2009-01-01

Uranium (U) and plutonium (Pu) isotopes in coral soils, contaminated by nuclear weapons testing in the northern Marshall Islands, were isolated by ion-exchange chromatography and analyzed by mass spectrometry. The soil samples were spiked with 233 U and 242 Pu tracers, dissolved in minerals acids, and U and Pu isotopes isolated and purified on commercially available ion-exchange columns. The ion-exchange technique employed a TEVA R column coupled to a UTEVA R column. U and Pu isotope fractions were then further isolated using separate elution schemes, and the purified fractions containing U and Pu isotopes analyzed sequentially using multi-collector inductively coupled plasma mass spectrometer (MCICP-MS). High precision measurements of 234 U/ 235 U, 238 U/ 235 U, 236 U/ 235 U, and 240 Pu/ 239 Pu in soil samples were attained using the described methodology and instrumentation, and provide a basis for conducting more detailed assessments of the behavior and transfer of uranium and plutonium in the environment. (author)

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

2. Workshop 'Isotopes in Nature'. 1

International Nuclear Information System (INIS)

1979-11-01

The workshop was aimed at discussing in detail the following problems: (1) distribution of stable and radioactive isotopes in nature, (2) theoretical and experimental studies of isotopic effects in natural processes, (3) problems of sample preparation and sample measurement in determining the relative abundance of stable isotopes or radioactive isotopes in nature, (4) age estimations of samples from different areas of the geosphere, (5) contributions to the specification of global and regional substance cycles in nature with the aid of isotopic and geochemical studies. 75 summaries are included

Isotope mixtures of hydrogen in vanadium

International Nuclear Information System (INIS)

Mecking-Schloetensack, P.

1982-03-01

The properties of isotope-mixtures of Protium and Deuterium stored in Vanadium have been studied. Protium and Deuterium are existing as interstitial-atoms on tetrahedral sites as well as on octahedral sites in this system. This feature leads to large isotopic-effects between the two isotopes. The dependence of the thermodynamic functions like heat of solution, nonconfigurational entropy, specific heat and ordering temperatures from the composition of the isotope-mixture has been determined. (orig.)

Triple oxygen isotopes in biogenic and sedimentary carbonates

Science.gov (United States)

Passey, Benjamin H.; Hu, Huanting; Ji, Haoyuan; Montanari, Shaena; Li, Shuning; Henkes, Gregory A.; Levin, Naomi E.

2014-09-01

The 17O anomaly (Δ17O) of natural waters has been shown to be sensitive to evaporation in a way analogous to deuterium excess, with evaporated bodies of water (e.g., leaf waters, lake waters, animal body waters) tending to have lower Δ17O than primary meteoric waters. In animal body water, Δ17O relates to the intake of evaporated waters, evaporative effluxes of water, and the Δ17O value of atmospheric O2, which itself carries signatures of global carbon cycling and photochemical reactions in the stratosphere. Carbonates have the potential to record the triple oxygen isotope compositions of parent waters, allowing reconstruction of past water compositions, but such investigations have awaited development of methods for high-precision measurement of Δ17O of carbonate. We describe optimized methods based on a sequential acid digestion/reduction/fluorination approach that yield Δ17O data with the high precision (∼0.010‰, 1σ) needed to resolve subtle environmental signals. We report the first high-precision Δ17O dataset for terrestrial carbonates, focusing on vertebrate biogenic carbonates and soil carbonates, but also including marine invertebrates and high-temperature carbonates. We determine apparent three-isotope fractionation factors between the O2 analyte derived from carbonate and the parent waters of the carbonate. These in combination with appropriate temperature estimates (from clumped isotope thermometry, or known or estimated body temperatures) are used to calculate the δ18O and Δ17O of parent waters. The clearest pattern to emerge is the strong 17O-depletion in avian, dinosaurian, and mammalian body water (from analyses of eggshell and tooth enamel) relative to meteoric waters, following expected influences of evaporated water (e.g., leaf water) and atmospheric O2 on vertebrate body water. Parent waters of the soil carbonates studied here have Δ17O values that are similar to or slightly lower than global precipitation. Our results suggest

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

Remarks on sequential designs in risk assessment

International Nuclear Information System (INIS)

Seidenfeld, T.

1982-01-01

The special merits of sequential designs are reviewed in light of particular challenges that attend risk assessment for human population. The kinds of ''statistical inference'' are distinguished and the problem of design which is pursued is the clash between Neyman-Pearson and Bayesian programs of sequential design. The value of sequential designs is discussed and the Neyman-Pearson vs. Bayesian sequential designs are probed in particular. Finally, warnings with sequential designs are considered, especially in relation to utilitarianism

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)

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...

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.

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...

Simultaneous determination of picogram per gram concentrations of Ba, Pb and Pb isotopes in Greenland ice by thermal ionisation mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Jimi, Salah I.; Rosman, Kevin J.R.; Candelone, Jean-Pierre; Burn, Laurie J. [Curtin University of Technology, Department of Imaging and Applied Physics, Perth (Australia); Hong, Sungmin [Polar Research Centre, Korean Ocean Research and Development Institute, Ansan, P.O. Box 29, Seoul (Korea); Boutron, Claude F. [Domaine Universitaire, Laboratoire de Glaciologie et Geophysique du l' Environnement, 54 rue Moliere, Saint Martin d' Heres (France); UFR de Mecanique, Universite Joseph Fourier de Grenoble (Institut Universitaire de France), Domaine Universitaire, Grenoble (France)

2008-01-15

A technique has been developed to simultaneously measure picogram per gram concentrations of Ba and Pb by isotope dilution mass spectrometry, as well as Pb isotopic ratios in polar ice by thermal ionisation mass spectrometry. BaPO{sup +}{sub 2} and Pb{sup +} ions were employed for these determinations. A calibrated mixture of enriched {sup 205}Pb and {sup 137}Ba was added to the samples providing an accuracy of better than approximately 2% for Pb/Ba element ratio determinations. Interference by molecular ions in the Pb mass spectrum occurred only at {sup 204}Pb and {sup 205}Pb, but these contributions were negligible in terms of precisions expected on picogram-sized Pb samples. The technique is illustrated with measurements on Greenland firn, using a drill-core section that includes the Laki volcanic eruption of 1783-1784. The data show deviations from the element concentrations indicating volatile metal enrichments, but the Pb isotopic signature of the Laki lava could not be identified. (orig.)

ISOTOPE METHODS IN HOMOGENEOUS CATALYSIS.

Energy Technology Data Exchange (ETDEWEB)

BULLOCK,R.M.; BENDER,B.R.

2000-12-01

The use of isotope labels has had a fundamentally important role in the determination of mechanisms of homogeneously catalyzed reactions. Mechanistic data is valuable since it can assist in the design and rational improvement of homogeneous catalysts. There are several ways to use isotopes in mechanistic chemistry. Isotopes can be introduced into controlled experiments and followed where they go or don't go; in this way, Libby, Calvin, Taube and others used isotopes to elucidate mechanistic pathways for very different, yet important chemistries. Another important isotope method is the study of kinetic isotope effects (KIEs) and equilibrium isotope effect (EIEs). Here the mere observation of where a label winds up is no longer enough - what matters is how much slower (or faster) a labeled molecule reacts than the unlabeled material. The most careti studies essentially involve the measurement of isotope fractionation between a reference ground state and the transition state. Thus kinetic isotope effects provide unique data unavailable from other methods, since information about the transition state of a reaction is obtained. Because getting an experimental glimpse of transition states is really tantamount to understanding catalysis, kinetic isotope effects are very powerful.

Sequential lineup laps and eyewitness accuracy.

Science.gov (United States)

Steblay, Nancy K; Dietrich, Hannah L; Ryan, Shannon L; Raczynski, Jeanette L; James, Kali A

2011-08-01

Police practice of double-blind sequential lineups prompts a question about the efficacy of repeated viewings (laps) of the sequential lineup. Two laboratory experiments confirmed the presence of a sequential lap effect: an increase in witness lineup picks from first to second lap, when the culprit was a stranger. The second lap produced more errors than correct identifications. In Experiment 2, lineup diagnosticity was significantly higher for sequential lineup procedures that employed a single versus double laps. Witnesses who elected to view a second lap made significantly more errors than witnesses who chose to stop after one lap or those who were required to view two laps. Witnesses with prior exposure to the culprit did not exhibit a sequential lap effect.

Isotopic composition of rainfall and runoff in a small arid basin with implications for deep percolation

International Nuclear Information System (INIS)

Dody, A.

1995-08-01

The aim of this work was to characterize the isotopic composition of potential recharge in an arid rocky watershed. Unique field observations were obtained from an arid watershed in the Negev Highlands, Israel, through utilization of the dynamic variations in the isotopic composition of rainfall and runoff. The hydrological system's inputs are rainfall and its isotopic composition. Rainfall and runoff were sampled in eight storms. High variability in the isotopic composition of rainfall was observed during any single rainstorm. The isotopic distribution in the runoff at the outlet of the basin appeared often not to be correlated to the isotopic patterns of the associated rain storm. A new mathematical model was developed to describe these physical processes. The model called A Double-Component Kinematic Wave Flow and Transport Approach, was designated to assess the dynamic isotopic distribution in arid rain storms and runoff. This model simulates the transport of rainfall into overland flow and runoff in an arid rocky watershed with uniformly distributed shallow depression storage. A numerical solution for the problem was developed, to estimate the depression storage parameters. The model also reflects the isotopic memory effect due to the depression storage between sequential rain showers. A good agreement between the observed and computed hydrograph and the change of the δ 18O values in runoff in time confirms the validity of the model. (author) 138 figs., 125 refs

Impacts of Dust on Tropical Volcanic Soil Formation: Insights from Strontium and Uranium-Series Isotopes in Soils from Basse-Terre Island, French Guadeloupe

Science.gov (United States)

Pereyra, Y.; Ma, L.; Sak, P. B.; Gaillardet, J.; Buss, H. L.; Brantley, S. L.

2015-12-01

Dust inputs play an important role in soil formation, especially for thick soils developed on tropical volcanic islands. In these regions, soils are highly depleted due to intensive chemical weathering, and mineral nutrients from dusts have been known to be important in sustaining soil fertility and productivity. Tropical volcanic soils are an ideal system to study the impacts of dust inputs on the ecosystem. Sr and U-series isotopes are excellent tracers to identify sources of materials in an open system if the end-members have distinctive isotope signatures. These two isotope systems are particularly useful to trace the origin of atmospheric inputs into soils and to determine rates and timescales of soil formation. This study analyzes major elemental concentrations, Sr and U-series isotope ratios in highly depleted soils in the tropical volcanic island of Basse-Terre in French Guadeloupe to determine atmospheric input sources and identify key soil formation processes. We focus on three soil profiles (8 to 12 m thick) from the Bras-David, Moustique Petit-Bourg, and Deshaies watersheds; and on the adjacent rivers to these sites. Results have shown a significant depletion of U, Sr, and major elements in the deep profile (12 to 4 m) attributed to rapid chemical weathering. The top soil profiles (4 m to the surface) all show addition of elements such as Ca, Mg, U, and Sr due to atmospheric dust. More importantly, the topsoil profiles have distinct Sr and U-series isotope compositions from the deep soils. Sr and U-series isotope ratios of the top soils and sequential extraction fractions confirm that the sources of the dust are from the Saharan dessert, through long distance transport from Africa to the Caribbean region across the Atlantic Ocean. During the transport, some dust isotope signatures may also have been modified by local volcanic ashes and marine aerosols. Our study highlights that dusts and marine aerosols play important roles in element cycles and

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.

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.

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.

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)

Robustness of the Sequential Lineup Advantage

Science.gov (United States)

Gronlund, Scott D.; Carlson, Curt A.; Dailey, Sarah B.; Goodsell, Charles A.

2009-01-01

A growing movement in the United States and around the world involves promoting the advantages of conducting an eyewitness lineup in a sequential manner. We conducted a large study (N = 2,529) that included 24 comparisons of sequential versus simultaneous lineups. A liberal statistical criterion revealed only 2 significant sequential lineup…

Isotopic characterization of targets for nuclear measurements at CBNM

International Nuclear Information System (INIS)

Bievre, P. de

1985-01-01

Nuclear measurements for which ''nuclear'' targets are prepared are almost always isotope-specific i.e. they are normally related to a particular nuclide in the target. The amount of this nuclide must be accurately assessed. There are essentially two ways to determine the number of atoms of this particular nuclide. (1) By determination of the amount of element, to which the nuclide belongs, on the target via classsical means; weighing substraction of impurities, calculation of element amount using known of the chemical compound in which the element is incorporated and, finally, measurement of the isotopic composition in order to determine the fraction of the nuclide concerned in the element. An alternative way may be to perform an elemental assay on the target followed by determination of the isotopic composition. (2) Another approach is isotope dilution mass spectrometry where a change in the isotopic composition of the ''target'' is induced by adding a known number of atoms (called ''spike'') of the element with a quite different composition. Measurement of the resulting change in isotopic composition yields directly the number of atoms of the nuclide under investigation. The method is highly selective, accurate and isotope-specific. (orig.)

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.

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

Isotopic research in Antarctica

International Nuclear Information System (INIS)

Schuetze, H.

1983-01-01

Since 1978 scientists of the Central Institute of Isotope- and Radiation Research of the Academy of Sciences of the GDR have participated in antarctic research. Substantial results have been achieved in research on isotope ratios, on the dynamics of water resources, on concentration of deuterium in lichens, and on age determination of a mummified seal and a penguin colony

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)

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

Isotope applications in the environmental field

International Nuclear Information System (INIS)

DeWitt, R.

1978-01-01

Established uses of enriched isotopes in the environmental field were surveyed to determine future trends in isotope needs. Based on established isotope uses, on the projected increase in the pollution problem, and on the apparent social and economic pressure for pollution abatement, a significant demand for enriched isotopes appears to be developing for the assessment and control of air, water, and soil pollutants. Isotopic techniques will be used in combination with conventional methods of detection and measurement, such as gas chromatography, x-ray fluorescence, and atomic absorption. Recent advances in economical isotope separation methods, instrumentation, and methodology promise to place isotopic technology within the reach of most research and industrial institutions. Increased application of isotope techniques appears most likely to occur in areas where data are needed to characterize the movement, behavior, and fate of pollutants in the environment

Chemical separation of boron isotopes

Energy Technology Data Exchange (ETDEWEB)

Palko, A.A.

1978-06-01

This is the final report of the research performed at ORNL on the chemical fractionation of boron isotopes between BF/sub 3/ gas and the liquid molecular addition compounds of BF/sub 3/. Thirty compounds were studied, ten of them in detail. Graphs and equations are given for variation of isotopic equilibrium constant, vapor pressure, and BF/sub 3/ solubility as a function of temperature. Rate of isotopic exchange and melting points were determined. Several of the compounds are likely candidates for use in a gas-liquid countercurrent exchange system for large-scale separation of boron isotopes. 23 figs, 53 tables, 39 references.

Chemical separation of boron isotopes

International Nuclear Information System (INIS)

Palko, A.A.

1978-06-01

This is the final report of the research performed at ORNL on the chemical fractionation of boron isotopes between BF 3 gas and the liquid molecular addition compounds of BF 3 . Thirty compounds were studied, ten of them in detail. Graphs and equations are given for variation of isotopic equilibrium constant, vapor pressure, and BF 3 solubility as a function of temperature. Rate of isotopic exchange and melting points were determined. Several of the compounds are likely candidates for use in a gas-liquid countercurrent exchange system for large-scale separation of boron isotopes. 23 figs, 53 tables, 39 references

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.

Inter- and intra-storm variability of the isotope composition of precipitation in Southern Israel: Are local or large-scale factors responsible?

International Nuclear Information System (INIS)

Gat, J.R.; Adar, E.; Alpert, P.

2002-01-01

A detailed sequential rain sampling of rainstorms was carried out during the 1989/90 and 1990/91 rainy season in the coastal plain of Israel with an annual average of 530 mm of rain and in the western Negev where the average annual rainfall is 93 mm. On four occasions, rain was concurrently available at both stations. The variability of the isotope composition within a rainy spell is quite considerable but falls short of the range of isotopic values encountered during the total season. Different rainy episodes show distinguishable isotope compositions, which evidently are characteristic of a larger time/space niche than that of the momentary, local, rain event. This is confirmed by the good correlation between the mean isotope composition of concurrently sampled events at both stations. A 'rain amount effect' is not apparent when the amount-weighted data for each complete rain episode are compared, because any possible effect is masked by the inter-storm variability. However by singling out the data within each storm sequence separately, a moderate effect is seen. On the whole, the results seem to support the notion that the isotope data are determined by the large, synoptic scale, situation. However within the range of values characteristic of the origin of the air masses there is a pronounced dependence of the isotope composition on the extent of the cloud field associated with each event, which is interpreted as a measure of the degree of rainout from the air mass, i.e. a typical Rayleigh effect. Local effects related to momentary rain intensity contribute only to a residual modulation of the above-mentioned effects. (author)

Sequential extraction applied to Peruibe black mud, SP, Brazil

International Nuclear Information System (INIS)

Torrecilha, Jefferson Koyaishi

2014-01-01

The Peruibe Black mud is used in therapeutic treatments such as psoriasis, peripheral dermatitis, acne and seborrhoea, as well as in the treatment of myalgia, arthritis, rheumatism and non-articular processes. Likewise other medicinal clays, it may not be free from possible adverse health effects due to possible hazardous minerals leading to respiratory system occurrences and other effects, caused by the presence of toxic elements. Once used for therapeutic purposes, any given material should be fully characterized and thus samples of Peruibe black mud were analyzed to determine physical and chemical properties: moisture content, organic matter and loss on ignition; pH, particle size, cation exchange capacity and swelling index. The elemental composition was determined by Neutron Activation Analysis, Atomic Absorption Graphite Furnace and X-ray fluorescence; the mineralogical composition was determined by X-ray diffraction. Another tool widely used to evaluate the behavior of trace elements, in various environmental matrices, is the sequential extraction. Thus, a sequential extraction procedure was applied to fractionate the mud in specific geochemical forms and verify how and how much of the elements may be contained in it. Considering the several sequential extraction procedures, BCR-701 method (Community Bureau of Reference) was used since it is considered the most reproducible among them. A simple extraction with an artificial sweat was, also, applied in order to verify which components are potentially available for absorption by the patient skin during the topical treatment. The results indicated that the mud is basically composed by a silty-clay material, rich in organic matter and with good cation exchange capacity. There were no significant variations in mineralogy and elemental composition of both, in natura and mature mud forms. The analysis by sequential extraction and by simple extraction indicated that the elements possibly available in larger

A sequential/parallel track selector

CERN Document Server

Bertolino, F; Bressani, Tullio; Chiavassa, E; Costa, S; Dellacasa, G; Gallio, M; Musso, A

1980-01-01

A medium speed ( approximately 1 mu s) hardware pre-analyzer for the selection of events detected in four planes of drift chambers in the magnetic field of the Omicron Spectrometer at the CERN SC is described. Specific geometrical criteria determine patterns of hits in the four planes of vertical wires that have to be recognized and that are stored as patterns of '1's in random access memories. Pairs of good hits are found sequentially, then the RAMs are used as look-up tables. (6 refs).

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

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)

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.

[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.

Isotope analytics for the evaluation of the feeding influence on the isotope ratio in beef samples

International Nuclear Information System (INIS)

Herwig, Nadine

2010-01-01

Information about the origin of food and associated production systems has a high significance for food control. An extremely promising approach to obtain such information is the determination of isotope ratios of different elements. In this study the correlation of the isotope ratios C-13/C-12, N-15/N-14, Mg-25/Mg-24, and Sr-87/Sr-86 in bovine samples (milk and urine) and the corresponding isotope ratios in feed was investigated. It was shown that in the bovine samples all four isotope ratios correlate with the isotope composition of the feed. The isotope ratios of strontium and magnesium have the advantage that they directly reflect the isotope ratios of the ingested feed since there is no isotope fractionation in the bovine organism which is in contrast to the case of carbon and nitrogen isotope ratios. From the present feeding study it is evident, that a feed change leads to a significant change in the delta C-13 values in milk and urine within 10 days already. For the deltaN-15 values the feed change was only visible in the bovine urine after 49 days. Investigations of cows from two different regions (Berlin/Germany and Goestling/Austria) kept at different feeding regimes revealed no differences in the N-15/N-14 and Mg-26/Mg-24 isotope ratios. The strongest correlation between the isotope ratio of the bovine samples and the kind of ingested feed was observed for the carbon isotope ratio. With this ratio even smallest differences in the feed composition were traceable in the bovine samples. Since different regions usually coincide with different feeding regimes, carbon isotope ratios can be used to distinguish bovine samples from different regions if the delta C-13 values of the ingested feed are different. Furthermore, the determination of strontium isotope ratios revealed significant differences between bovine and feed samples of Berlin and Goestling due to the different geologic realities. Hence the carbon and strontium isotope ratios allow the best

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)

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)

Multi-agent sequential hypothesis testing

KAUST Repository

Kim, Kwang-Ki K.; Shamma, Jeff S.

2014-01-01

incorporate costs of taking private/public measurements, costs of time-difference and disagreement in actions of agents, and costs of false declaration/choices in the sequential hypothesis testing. The corresponding sequential decision processes have well

A new method for precise determination of iron, zinc and cadmium stable isotope ratios in seawater by double-spike mass spectrometry

International Nuclear Information System (INIS)

Conway, Tim M.; Rosenberg, Angela D.; Adkins, Jess F.; John, Seth G.

2013-01-01

Graphical abstract: ‘Metal-free’ seawater doped with varying concentrations of ‘zero’ isotope standards, processed through our simultaneous method, and then analyzed by double spike MC-ICPMS for Fe, Zn and Cd isotope ratios. All values were determined within 2 σ error (error bars shown) of zero. -- Highlights: •The first simultaneous method for isotopic analysis of Fe, Zn and Cd in seawater. •Designed for 1 L samples, a 1–20 fold improvement over previous methods. •Low blanks and high precision allow measurement of low concentration samples. •Small volume and fast processing are ideal for high-resolution large-scale studies. •Will facilitate investigation of marine trace-metal isotope cycling. -- Abstract: The study of Fe, Zn and Cd stable isotopes (δ 56 Fe, δ 66 Zn and δ 114 Cd) in seawater is a new field, which promises to elucidate the marine cycling of these bioactive trace metals. However, the analytical challenges posed by the low concentration of these metals in seawater has meant that previous studies have typically required large sample volumes, highly limiting data collection in the oceans. Here, we present the first simultaneous method for the determination of these three isotope systems in seawater, using Nobias PA-1 chelating resin to extract metals from seawater, purification by anion exchange chromatography, and analysis by double spike MC-ICPMS. This method is designed for use on only a single litre of seawater and has blanks of 0.3, 0.06 and <0.03 ng for Fe, Zn and Cd respectively, representing a 1–20 fold reduction in sample size and a 4–130 decrease in blank compared to previously reported methods. The procedure yields data with high precision for all three elements (typically 0.02–0.2‰; 1σ internal precision), allowing us to distinguish natural variability in the oceans, which spans 1–3‰ for all three isotope systems. Simultaneous extraction and purification of three metals makes this method ideal for high

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.

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.

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.

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

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.

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

Isotope ratio in stellar atmospheres and nucleosynthesis

International Nuclear Information System (INIS)

Barbuy, B.L.S.

1987-01-01

The determination of isotopic ratios in stellar atmospheres is studied. The isotopic shift of atomic and molecular lines of different species of a certain element is examined. CH and MgH lines are observed in order to obtain the 12 C: 13 C and 24 Mg: 25 Mg: 26 Mg isotpic ratios. The formation of lines in stellar atmospheres is computed and the resulting synthetic spectra are employed to determine the isotopic abundances. The results obtained for the isotopic ratios are compared to predictions of nucleosynthesis theories. Finally, the concept of primary and secondary element is discussed, and these definitions are applied to the observed variations in the abundance of elements as a function of metallicity. (author) [pt

Exploring the sequential lineup advantage using WITNESS.

Science.gov (United States)

Goodsell, Charles A; Gronlund, Scott D; Carlson, Curt A

2010-12-01

Advocates claim that the sequential lineup is an improvement over simultaneous lineup procedures, but no formal (quantitatively specified) explanation exists for why it is better. The computational model WITNESS (Clark, Appl Cogn Psychol 17:629-654, 2003) was used to develop theoretical explanations for the sequential lineup advantage. In its current form, WITNESS produced a sequential advantage only by pairing conservative sequential choosing with liberal simultaneous choosing. However, this combination failed to approximate four extant experiments that exhibited large sequential advantages. Two of these experiments became the focus of our efforts because the data were uncontaminated by likely suspect position effects. Decision-based and memory-based modifications to WITNESS approximated the data and produced a sequential advantage. The next step is to evaluate the proposed explanations and modify public policy recommendations accordingly.

The determination of specific surface of sodium polyuranates

International Nuclear Information System (INIS)

Bilgin, B.; Atun, G.

2002-01-01

Three different sodium polyuranates were prepared by titration of uranyl nitrate with a sodium hydroxide solution labeled with 22 Na as the radiotracer. Polyuranates whose composition was *Na 2 O.7,5UO 3 .11H 2 O (sample A), *Na 2 O.4,3 UO 3 .4,7H 2 O (sample B), and *Na 2 O.2UO 3 .4H 2 O (sample C) were precipitated at pH 5.6, 8.5 and 11.2, respectively. The specific surface areas of these samples were determined by the BET method using methylene blue (MB) as the adsorbate. The sodium polyuranate surfaces were saturated by sequential adsorption of MB. The adsorption data gave an S-shaped isotherm and were fitted to the BET equation. The specific surface areas calculated from the BET isotherm decreased in order A > B > C. The isotope and ion exchange reactions between the sodium polyuranates and Li + , Na + , K + , Rb + , Cs + , Ca 2+ , Sr 2+ , and Ba 2+ ions were compared before and after MB coverage. The results showed that the isotope and ion exchange fractions decrease on the covered surfaces indicating particle diffusion mechanism dominated exchange reactions

Sequential and simultaneous choices: testing the diet selection and sequential choice models.

Science.gov (United States)

Freidin, Esteban; Aw, Justine; Kacelnik, Alex

2009-03-01

We investigate simultaneous and sequential choices in starlings, using Charnov's Diet Choice Model (DCM) and Shapiro, Siller and Kacelnik's Sequential Choice Model (SCM) to integrate function and mechanism. During a training phase, starlings encountered one food-related option per trial (A, B or R) in random sequence and with equal probability. A and B delivered food rewards after programmed delays (shorter for A), while R ('rejection') moved directly to the next trial without reward. In this phase we measured latencies to respond. In a later, choice, phase, birds encountered the pairs A-B, A-R and B-R, the first implementing a simultaneous choice and the second and third sequential choices. The DCM predicts when R should be chosen to maximize intake rate, and SCM uses latencies of the training phase to predict choices between any pair of options in the choice phase. The predictions of both models coincided, and both successfully predicted the birds' preferences. The DCM does not deal with partial preferences, while the SCM does, and experimental results were strongly correlated to this model's predictions. We believe that the SCM may expose a very general mechanism of animal choice, and that its wider domain of success reflects the greater ecological significance of sequential over simultaneous choices.

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

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

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.

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.)

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.

Absolute isotopic abundances of Ti in meteorites

International Nuclear Information System (INIS)

Niederer, F.R.; Papanastassiou, D.A.; Wasserburg, G.J.

1985-01-01

The absolute isotope abundance of Ti has been determined in Ca-Al-rich inclusions from the Allende and Leoville meteorites and in samples of whole meteorites. The absolute Ti isotope abundances differ by a significant mass dependent isotope fractionation transformation from the previously reported abundances, which were normalized for fractionation using 46 Ti/ 48 Ti. Therefore, the absolute compositions define distinct nucleosynthetic components from those previously identified or reflect the existence of significant mass dependent isotope fractionation in nature. We provide a general formalism for determining the possible isotope compositions of the exotic Ti from the measured composition, for different values of isotope fractionation in nature and for different mixing ratios of the exotic and normal components. The absolute Ti and Ca isotopic compositions still support the correlation of 50 Ti and 48 Ca effects in the FUN inclusions and imply contributions from neutron-rich equilibrium or quasi-equilibrium nucleosynthesis. The present identification of endemic effects at 46 Ti, for the absolute composition, implies a shortfall of an explosive-oxygen component or reflects significant isotope fractionation. Additional nucleosynthetic components are required by 47 Ti and 49 Ti effects. Components are also defined in which 48 Ti is enhanced. Results are given and discussed. (author)

Rapid isolation of plutonium in environmental solid samples using sequential injection anion exchange chromatography followed by detection with inductively coupled plasma mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Qiao Jixin, E-mail: jixin.qiao@risoe.d [Radiation Research Division, Riso National Laboratory for Sustainable Energy, Technical University of Denmark, DK-4000 Roskilde (Denmark); Hou Xiaolin; Roos, Per [Radiation Research Division, Riso National Laboratory for Sustainable Energy, Technical University of Denmark, DK-4000 Roskilde (Denmark); Miro, Manuel [Department of Chemistry, Faculty of Sciences, University of the Balearic Islands, Carretera de Valldemossa km. 7.5, E-07122 Palma de Mallorca, Illes Balears (Spain)

2011-01-31

This paper reports an automated analytical method for rapid determination of plutonium isotopes ({sup 239}Pu and {sup 240}Pu) in environmental solid extracts. Anion exchange chromatographic columns were incorporated in a sequential injection (SI) system to undertake the automated separation of plutonium from matrix and interfering elements. The analytical results most distinctly demonstrated that the crosslinkage of the anion exchanger is a key parameter controlling the separation efficiency. AG 1-x4 type resin was selected as the most suitable sorbent material for analyte separation. Investigation of column size effect upon the separation efficiency revealed that small-sized (2 mL) columns sufficed to handle up to 50 g of environmental soil samples. Under the optimum conditions, chemical yields of plutonium exceeded 90% and the decontamination factors for uranium, thorium and lead ranged from 10{sup 3} to 10{sup 4}. The determination of plutonium isotopes in three standard/certified reference materials (IAEA-375 soil, IAEA-135 sediment and NIST-4359 seaweed) and two reference samples (Irish Sea sediment and Danish soil) revealed a good agreement with reference/certified values. The SI column-separation method is straightforward and less labor intensive as compared with batch-wise anion exchange chromatographic procedures. Besides, the automated method features low consumption of ion-exchanger and reagents for column washing and elution, with the consequent decrease in the generation of acidic waste, thus bearing green chemical credentials.

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

Mean-Variance-Validation Technique for Sequential Kriging Metamodels

International Nuclear Information System (INIS)

Lee, Tae Hee; Kim, Ho Sung

2010-01-01

The rigorous validation of the accuracy of metamodels is an important topic in research on metamodel techniques. Although a leave-k-out cross-validation technique involves a considerably high computational cost, it cannot be used to measure the fidelity of metamodels. Recently, the mean 0 validation technique has been proposed to quantitatively determine the accuracy of metamodels. However, the use of mean 0 validation criterion may lead to premature termination of a sampling process even if the kriging model is inaccurate. In this study, we propose a new validation technique based on the mean and variance of the response evaluated when sequential sampling method, such as maximum entropy sampling, is used. The proposed validation technique is more efficient and accurate than the leave-k-out cross-validation technique, because instead of performing numerical integration, the kriging model is explicitly integrated to accurately evaluate the mean and variance of the response evaluated. The error in the proposed validation technique resembles a root mean squared error, thus it can be used to determine a stop criterion for sequential sampling of metamodels

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.

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

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.

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...

Determination of the activity of the uranium isotopes U-234, U-235 and U-238 in environmental samples by alpha spectrometry

International Nuclear Information System (INIS)

Kromphorn, G.

1996-02-01

Different materials containing urandium are regularly investigated in the Laboratory for Environmental Radioactivity of the Physikalisch-Technische Bundesanstalt (PTB) with respect to the activity of the uranium isotopes ( 234 U, 235 U, and 238 U). Moreover for reasons of quality assurance, the PTB takes part in international comparisons where also uranium contents are to be determined in environmental samples and in the framework of which reference materials can be certified. Finally in national comparisons the PTB has the task to determine values of the specific activity for the different isotopes which can play the role of nominal (orientation) values. The single steps of uranium analyses are described after a compilation of the most important data of the uranium isotopes contained in natural uranium: The use of 232 U as tracer, the chemical separation analytics, the production of α-sources and the measuring methods. Analyses of a soil sample and a waste water sample with respect to their specific uranium activity have been chosen as examples of a practical application. (orig.) [de

Sequential Probability Ration Tests : Conservative and Robust

NARCIS (Netherlands)

Kleijnen, J.P.C.; Shi, Wen

2017-01-01

In practice, most computers generate simulation outputs sequentially, so it is attractive to analyze these outputs through sequential statistical methods such as sequential probability ratio tests (SPRTs). We investigate several SPRTs for choosing between two hypothesized values for the mean output

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

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

Isotopic composition of rainfall and runoff in a small arid basin with implications for deep percolation

Energy Technology Data Exchange (ETDEWEB)

Dody, A [Ben-Gurion Univ. of the Negev, Beersheba (Israel)

1995-08-01

The aim of this work was to characterize the isotopic composition of potential recharge in an arid rocky watershed. Unique field observations were obtained from an arid watershed in the Negev Highlands, Israel, through utilization of the dynamic variations in the isotopic composition of rainfall and runoff. The hydrological system`s inputs are rainfall and its isotopic composition. Rainfall and runoff were sampled in eight storms. High variability in the isotopic composition of rainfall was observed during any single rainstorm. The isotopic distribution in the runoff at the outlet of the basin appeared often not to be correlated to the isotopic patterns of the associated rain storm. A new mathematical model was developed to describe these physical processes. The model called A Double-Component Kinematic Wave Flow and Transport Approach, was designated to assess the dynamic isotopic distribution in arid rain storms and runoff. This model simulates the transport of rainfall into overland flow and runoff in an arid rocky watershed with uniformly distributed shallow depression storage. A numerical solution for the problem was developed, to estimate the depression storage parameters. The model also reflects the isotopic memory effect due to the depression storage between sequential rain showers. A good agreement between the observed and computed hydrograph and the change of the {delta}{sup 18O} values in runoff in time confirms the validity of the model. (author) 138 figs., 125 refs.

Use of Isotopes for Studying Reaction Mechanisms

Indian Academy of Sciences (India)

In the first part of this series, we discussed how isotopes can be used as markers to determine the nature of intermediates in chemical reactions. The second part covered the effect of isotopes on equilibria and reactions, in processes where the bond to the isotopic a tom is broken. We showed with specific examples how.

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)

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)

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

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.

Sequential lineup presentation: Patterns and policy

OpenAIRE

Lindsay, R C L; Mansour, Jamal K; Beaudry, J L; Leach, A-M; Bertrand, M I

2009-01-01

Sequential lineups were offered as an alternative to the traditional simultaneous lineup. Sequential lineups reduce incorrect lineup selections; however, the accompanying loss of correct identifications has resulted in controversy regarding adoption of the technique. We discuss the procedure and research relevant to (1) the pattern of results found using sequential versus simultaneous lineups; (2) reasons (theory) for differences in witness responses; (3) two methodological issues; and (4) im...

Sequential Product of Quantum Effects: An Overview

Science.gov (United States)

Gudder, Stan

2010-12-01

This article presents an overview for the theory of sequential products of quantum effects. We first summarize some of the highlights of this relatively recent field of investigation and then provide some new results. We begin by discussing sequential effect algebras which are effect algebras endowed with a sequential product satisfying certain basic conditions. We then consider sequential products of (discrete) quantum measurements. We next treat transition effect matrices (TEMs) and their associated sequential product. A TEM is a matrix whose entries are effects and whose rows form quantum measurements. We show that TEMs can be employed for the study of quantum Markov chains. Finally, we prove some new results concerning TEMs and vector densities.

Optimal Sequential Rules for Computer-Based Instruction.

Science.gov (United States)

Vos, Hans J.

1998-01-01

Formulates sequential rules for adapting the appropriate amount of instruction to learning needs in the context of computer-based instruction. Topics include Bayesian decision theory, threshold and linear-utility structure, psychometric model, optimal sequential number of test questions, and an empirical example of sequential instructional…

Separation and activity determination of 239+240Pu, 241Am and Curium (242and244Cm) in evaporator concentrate by Alpha Spectrometry

International Nuclear Information System (INIS)

Reis Junior, Aluisio S.; Temba, Eliane S.C.; Kastner, Geraldo F.; Monteiro, Roberto P.G.

2013-01-01

Alpha spectrometry analysis was used for activity determinations of Pu, Am and Cm isotopes in evaporator concentrate samples from nuclear power plants. Using a sequential procedure the first step was Pu isolation by an anion exchange column followed by an Am and Cm separation of U and Fe by a co-precipitation with oxalic acid. The precipitate was used for americium and curium separation of strontium by using a TRU resin extraction chromatography column. Due to their chemical similarities and energy difference it was seen that the simultaneous determination of 241 Am, 242 Cm and 24 3 ,244 Cm isotopes is possible using the 243 Am as tracer, once they have peaks in different region of interest (ROI) in the alpha spectrum. In this work it was used tracers, 238 Pu, 243 Am, 244 Cm and 232 U, for determination and quantification of theirs isotopes, respectively. The standard deviations for replicate analysis were calculated and for 241 Am it was (1,040 ± 160 mBqKg -1 ), relative standard deviation 15.38%, and for 239+240 Pu it was (551 +- 44 mBqKg -1 ), relative standard deviation 7.98%. In addition, for the 242 Cm isotope the standard deviation for determinations was(75 ± 23 mBqKg -1 ), with the relative standard deviation 30.67% higher than for 241 Am and 239+240 Pu. The radiometric yields ranged from 90% to 105% and the lower limit of detection was estimated as being 2.05 mBqKg -1 . (author)

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.)

The measurement of the isotope ratios and concentrations of zinc by thermal ionization mass spectrometry using double isotope dilution

International Nuclear Information System (INIS)

Deng Zhongguo

1994-01-01

The isotope ratios and concentrations of zinc are measured by silicagel-thermal ionization mass spectrometry using the double isotope spikers. The double isotope spikers ( 70 Zn and 67 Zn-enriched isotopes) are used to correct the isotope mass fractionation for the zinc isotope ratios, and to certify the zinc concentrations in the unknown samples. The zinc concentrations of these double isotope spikers are surveyed by a spiker made of pure (99.99%) natural zinc metal powder. The correcting factors (f a , f t and f n ) of the zinc isotope ratios in the spiked mixture, spike and unspiked samples for the isotope mass fractionation, and the spike-to-unspiked ratios (X r ) of the zinc isotope r in the spiked mixture samples can be obtained to solve the matrix equations by numerical approximation. The natural zinc isotope ratios are: 64 Zn/ 67 Zn = 11.8498, 66 Zn/ 67 Zn = 6.7977, 68 Zn/ 67 Zn = 4.5730 and 70 Zn/ 67 Zn = 0.1520. The uncertainties determined of the isotope ratios and concentrations of zinc are +- 0.16% and +-0.31%, respectively

Intracellular Cadmium Isotope Fractionation

Science.gov (United States)

Horner, T. J.; Lee, R. B.; Henderson, G. M.; Rickaby, R. E.

2011-12-01

Recent stable isotope studies into the biological utilization of transition metals (e.g. Cu, Fe, Zn, Cd) suggest several stepwise cellular processes can fractionate isotopes in both culture and nature. However, the determination of fractionation factors is often unsatisfactory, as significant variability can exist - even between different organisms with the same cellular functions. Thus, it has not been possible to adequately understand the source and mechanisms of metal isotopic fractionation. In order to address this problem, we investigated the biological fractionation of Cd isotopes within genetically-modified bacteria (E. coli). There is currently only one known biological use or requirement of Cd, a Cd/Zn carbonic anhydrase (CdCA, from the marine diatom T. weissfloggii), which we introduce into the E. coli genome. We have also developed a cleaning procedure that allows for the treating of bacteria so as to study the isotopic composition of different cellular components. We find that whole cells always exhibit a preference for uptake of the lighter isotopes of Cd. Notably, whole cells appear to have a similar Cd isotopic composition regardless of the expression of CdCA within the E. coli. However, isotopic fractionation can occur within the genetically modified E. coli during Cd use, such that Cd bound in CdCA can display a distinct isotopic composition compared to the cell as a whole. Thus, the externally observed fractionation is independent of the internal uses of Cd, with the largest Cd isotope fractionation occurring during cross-membrane transport. A general implication of these experiments is that trace metal isotopic fractionation most likely reflects metal transport into biological cells (either actively or passively), rather than relating to expression of specific physiological function and genetic expression of different metalloenzymes.

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,

The development of an automatic sample-changer and control instrumentation for isotope-source neutron-activation analysis

International Nuclear Information System (INIS)

Andeweg, A.H.; Watterson, J.I.W.

1983-01-01

An automatic sample-changer was developed at the Council for Mineral Technology for use in isotope-source neutron-activation analysis. Tests show that the sample-changer can transfer a sample of up to 3 kg in mass over a distance of 3 m within 5 s. In addition, instrumentation in the form of a three-stage sequential timer was developed to control the sequence of irradiation transfer and analysis

A fast and accurate online sequential learning algorithm for feedforward networks.

Science.gov (United States)

Liang, Nan-Ying; Huang, Guang-Bin; Saratchandran, P; Sundararajan, N

2006-11-01

In this paper, we develop an online sequential learning algorithm for single hidden layer feedforward networks (SLFNs) with additive or radial basis function (RBF) hidden nodes in a unified framework. The algorithm is referred to as online sequential extreme learning machine (OS-ELM) and can learn data one-by-one or chunk-by-chunk (a block of data) with fixed or varying chunk size. The activation functions for additive nodes in OS-ELM can be any bounded nonconstant piecewise continuous functions and the activation functions for RBF nodes can be any integrable piecewise continuous functions. In OS-ELM, the parameters of hidden nodes (the input weights and biases of additive nodes or the centers and impact factors of RBF nodes) are randomly selected and the output weights are analytically determined based on the sequentially arriving data. The algorithm uses the ideas of ELM of Huang et al. developed for batch learning which has been shown to be extremely fast with generalization performance better than other batch training methods. Apart from selecting the number of hidden nodes, no other control parameters have to be manually chosen. Detailed performance comparison of OS-ELM is done with other popular sequential learning algorithms on benchmark problems drawn from the regression, classification and time series prediction areas. The results show that the OS-ELM is faster than the other sequential algorithms and produces better generalization performance.

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...

A new method for precise determination of iron, zinc and cadmium stable isotope ratios in seawater by double-spike mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Conway, Tim M., E-mail: conway.tm@gmail.com [Department of Earth and Ocean Sciences, University of South Carolina, Columbia, SC 29208 (United States); Rosenberg, Angela D. [Department of Earth and Ocean Sciences, University of South Carolina, Columbia, SC 29208 (United States); Adkins, Jess F. [California Institute of Technology, Division of Geological and Planetary Sciences, Pasadena, CA 91125 (United States); John, Seth G. [Department of Earth and Ocean Sciences, University of South Carolina, Columbia, SC 29208 (United States)

2013-09-02

Graphical abstract: ‘Metal-free’ seawater doped with varying concentrations of ‘zero’ isotope standards, processed through our simultaneous method, and then analyzed by double spike MC-ICPMS for Fe, Zn and Cd isotope ratios. All values were determined within 2 σ error (error bars shown) of zero. -- Highlights: •The first simultaneous method for isotopic analysis of Fe, Zn and Cd in seawater. •Designed for 1 L samples, a 1–20 fold improvement over previous methods. •Low blanks and high precision allow measurement of low concentration samples. •Small volume and fast processing are ideal for high-resolution large-scale studies. •Will facilitate investigation of marine trace-metal isotope cycling. -- Abstract: The study of Fe, Zn and Cd stable isotopes (δ{sup 56}Fe, δ{sup 66}Zn and δ{sup 114}Cd) in seawater is a new field, which promises to elucidate the marine cycling of these bioactive trace metals. However, the analytical challenges posed by the low concentration of these metals in seawater has meant that previous studies have typically required large sample volumes, highly limiting data collection in the oceans. Here, we present the first simultaneous method for the determination of these three isotope systems in seawater, using Nobias PA-1 chelating resin to extract metals from seawater, purification by anion exchange chromatography, and analysis by double spike MC-ICPMS. This method is designed for use on only a single litre of seawater and has blanks of 0.3, 0.06 and <0.03 ng for Fe, Zn and Cd respectively, representing a 1–20 fold reduction in sample size and a 4–130 decrease in blank compared to previously reported methods. The procedure yields data with high precision for all three elements (typically 0.02–0.2‰; 1σ internal precision), allowing us to distinguish natural variability in the oceans, which spans 1–3‰ for all three isotope systems. Simultaneous extraction and purification of three metals makes this method ideal

Quantification of Labile Soil Mercury by Stable Isotope Dilution Techniques

Science.gov (United States)

Shetaya, Waleed; Huang, Jen-How; Osterwalder, Stefan; Alewell, Christine

2016-04-01

Mercury (Hg) is a toxic element that can cause severe health problems to humans. Mercury is emitted to the atmosphere from both natural and anthropogenic sources and can be transported over long distances before it is deposited to aquatic and terrestrial environments. Aside from accumulation in soil solid phases, Hg deposited in soils may migrate to surface- and ground-water or enter the food chain, depending on its lability. There are many operationally-defined extraction methods proposed to quantify soil labile metals. However, these methods are by definition prone to inaccuracies such as non-selectivity, underestimation or overestimation of the labile metal pool. The isotopic dilution technique (ID) is currently the most promising method for discrimination between labile and non-labile metal fractions in soil with a minimum disturbance to soil-solid phases. ID assesses the reactive metal pool in soil by defining the fraction of metal both in solid and solution phases that is isotopically-exchangeable known as the 'E-value'. The 'E-value' represents the metal fraction in a dynamic equilibrium with the solution phase and is potentially accessible to plants. This is carried out by addition of an enriched metal isotope to soil suspensions and quantifying the fraction of metal that is able to freely exchange with the added isotope by measuring the equilibrium isotopic ratio by ICP-MS. E-value (mg kg-1) is then calculated as follows: E-Value = (Msoil/ W) (CspikeVspike/ Mspike) (Iso1IAspike -Iso2IAspikeRss / Iso2IAsoil Rss - Iso1IAsoil) where M is the average atomic mass of the metal in the soil or the spike, W is the mass of soil (kg), Cspike is the concentration of the metal in the spike (mg L-1), Vspike is the volume of spike (L), IA is isotopic abundance, and Rss is the equilibrium ratio of isotopic abundances (Iso1:Iso2). Isotopic dilution has been successfully applied to determine E-values for several elements. However, to our knowledge, this method has not yet

Iodine isotopes and radiation safety

International Nuclear Information System (INIS)

Styro, B.; Nedvekajte, T.; Filistovich, V.

1992-01-01

Methods of concentration determination of stable and radioactive iodine isotopes in the Earth's different geospheres are described. Iodine isotopes concentration data, chemical forms and transformations as well as their exchange among separate geospheres of their global biochemical circulation (ocean, atmosphere, lithosphere and biosphere) are presented. Information on iodine isotopes as after-effects of nuclear installations accident (in particular, the Chernobyl accident) is generalized. The book is intended for scientists and practical workers in ecology and radioactivity protection and for a students of physics. 442 refs.; 82 figs.; 36 tabs

Quantum Inequalities and Sequential Measurements

International Nuclear Information System (INIS)

Candelpergher, B.; Grandouz, T.; Rubinx, J.L.

2011-01-01

In this article, the peculiar context of sequential measurements is chosen in order to analyze the quantum specificity in the two most famous examples of Heisenberg and Bell inequalities: Results are found at some interesting variance with customary textbook materials, where the context of initial state re-initialization is described. A key-point of the analysis is the possibility of defining Joint Probability Distributions for sequential random variables associated to quantum operators. Within the sequential context, it is shown that Joint Probability Distributions can be defined in situations where not all of the quantum operators (corresponding to random variables) do commute two by two. (authors)

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.

Validation of the method for determination of plutonium isotopes in urine samples and its application in a nuclear facility at Otwock

Directory of Open Access Journals (Sweden)

Rzemek Katarzyna

2015-03-01

Full Text Available The studies aimed at determining low activities of alpha radioactive elements are widely recognized as essential for the human health, because of their high radiotoxicity in case of internal contamination. Some groups of workers of nuclear facility at Otwock are potentially exposed to contamination with plutonium isotopes. For this reason, the method for determination of plutonium isotopes has been introduced and validated in Radiation Protection Measurements Laboratory (LPD of the National Centre for Nuclear Research (NCBJ. In this method the plutonium is isolated from a sample by coprecipitation with phosphates and separated on a AG 1-X2 Resin. After electrodeposition, the sample is measured by alpha spectrometry. Validation was performed in order to assess parameters such as: selectivity, accuracy (trueness and precision and linearity of the method. The results of plutonium determination in urine samples of persons potentially exposed to internal contamination are presented in this work.

A comparison of the interactions between sequential Ga-P and Ga-As diffusions in silicon

International Nuclear Information System (INIS)

Jones, C.L.; Willoughby, A.F.W.

1976-01-01

Investigation of the interactions between sequential gallium-phosphorus and gallium-arsenic diffusions have been made using radiotracer profiling techniques. Gallium diffusions were first carried out using isotope 67 Ga diffused from a solid gallium oxide source, and subsequently phosphorus or arsenic were diffused into the same surface. The effect of phosphorus diffusion of high surface concentration was found to be a large enhancement (up to a factor of 100)in the diffusion coefficient of the tail of the gallium profile, while similar arsenic diffusion produced either a small enhancement or a retardation, depending on the conditions used. In addition, the diffusion of both phosphorus and arsenic produced a pronounced dip in the gallium profiles, which is discussed in terms of the built-in electric field produced during the emitter diffusions. The differences between the positions of the dips produced by phosphorus and arsenic are explained by the differences in their profile shape and hence in the electric field distribution. In the case of arsenic, the dip is located at the steeply falling front of the arsenic profile which resolves discrepancies in previous studies of boron-arsenic sequential diffusions. (author)

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

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.

Effects of must concentration techniques on wine isotopic parameters.

Science.gov (United States)

Guyon, Francois; Douet, Christine; Colas, Sebastien; Salagoïty, Marie-Hélène; Medina, Bernard

2006-12-27

Despite the robustness of isotopic methods applied in the field of wine control, isotopic values can be slightly influenced by enological practices. For this reason, must concentration technique effects on wine isotopic parameters were studied. The two studied concentration techniques were reverse osmosis (RO) and high-vacuum evaporation (HVE). Samples (must and extracted water) have been collected in various French vineyards. Musts were microfermented at the laboratory, and isotope parameters were determined on the obtained wine. Deuterium and carbon-13 isotope ratios were studied on distilled ethanol by nuclear magnetic resonance (NMR) and isotope ratio mass spectrometry (IRMS), respectively. The oxygen-18 ratio was determined on extracted and wine water using IRMS apparatus. The study showed that the RO technique has a very low effect on isotopic parameters, indicating that this concentration technique does not create any isotopic fractionation, neither at sugar level nor at water level. The effect is notable for must submitted to HVE concentration: water evaporation leads to a modification of the oxygen-18 ratio of the must and, as a consequence, ethanol deuterium concentration is also modified.

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...

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

Performance of alpha spectrometry in the analysis of uranium isotopes in environmental and nuclear materials

International Nuclear Information System (INIS)

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

2009-01-01

The accuracy of alpha spectrometry in the determination of uranium isotopes at various concentrations levels and with various isotope ratios was tested in a round robin international intercomparison exercise. Results of isotope activity/mass and isotope mass ratios obtained by alpha spectrometry were accurate in a wide range of uranium masses and in isotopic ratios typical of depleted, natural, and low enriched uranium samples. Determinations by alpha spectrometry compared very satisfactorily in accuracy with those by mass spectrometry. For example, determination of U isotopes in natural uranium by alpha spectrometry agreed with mass spectrometry determinations at within ±1%. However, the 236 U isotope, particularly if present in activities much lower than 235 U, might not be determined accurately due to overlap in the alpha particle energies of these two uranium isotopes. (author)

Reactive transport modeling of chemical and isotope data to identify degradation processes of chlorinated ethenes in a diffusion-dominated media

DEFF Research Database (Denmark)

Chambon, Julie Claire Claudia; Damgaard, Ida; Jeannottat, Simon

. Degradation and transport processes of chlorinated ethenes are not well understood in such geological settings, therefore risk assessment and remediation at these sites are particularly challenging. In this work, a combined approach of chemical and isotope analysis on core samples, and reactive transport...... the source zone (between 6 and 12 mbs). Concentrations and stable isotope ratios of the mother compounds and their daughter products, as well as redox parameters, fatty acids and microbial data, were analyzed with discrete sub-sampling along the cores. More samples (each 5 mm) were collected around...... of dechlorination and degradation pathways (biotic reductive dechlorination or abiotic β-elimination with iron minerals) in three core profiles. The model includes diffusion in the matrix, sequential reductive dechlorination, abiotic degradation, isotope fractionation due to degradation and due to diffusion...

Determination of trace element concentrations and stable lead, uranium and thorium isotope ratios by quadrupole-ICP-MS in NORM and NORM-polluted sample leachates

International Nuclear Information System (INIS)

Mas, J.L.; Villa, M.; Hurtado, S.; García-Tenorio, R.

2012-01-01

Highlights: ► Polluted sediment and NORM samples. ► An efficient yet fast process allowing multi-parametric determinations in 206 Pb/ 207 Pb/ 208 Pb, 238 U/ 234 U and 232 Th/ 230 Th isotope ratios using a single sample aliquot and a single instrument (ICP-QMS). Eichrom UTEVA ® extraction chromatography minicolumns were used to separate uranium and thorium in sample leachates. Independent ICP-MS determinations of uranium and thorium isotope ratios were carried out afterwards. Previously a small aliquot of the leachate was used for the determination of trace element concentrations and lead isotope ratios. Several radiochemical arrangements were tested to get maximum performances and simplicity of the method. The performances of the method were studied in terms of chemical yields of uranium and thorium and removal of the potentially interfering elements. The established method was applied to samples from a chemical industry and sediments collected in a NORM-polluted scenario. The results obtained from our method allowed us to infer not only the extent, but also the sources of the contamination in the area.

Expeditious syntheses of stable and radioactive isotope-labeled anticonvulsant agent, JNJ-26990990, and its metabolites.

Science.gov (United States)

Lin, Ronghui; Weaner, Larry E; Hoerr, David C; Salter, Rhys; Gong, Yong

2013-01-01

Syntheses of stable and radioactive isotope-labeled anticonvulsant agent, JNJ-26990990, that is, N-(benzo[b]thien-3-ylmethyl)-sulfamide and its metabolites are described. [(13)C(15)N]Benzo[b]thiophene-3-carbonitrile was first prepared by coupling of 3-bromo-benzo[b]thiophene with [(13)C(15)N]-copper cyanide. The resultant [(13)C(15)N]benzo[b]thiophene-3-carbonitrile was reduced with lithium aluminum deuteride to give [(13)CD2(15)N]benzo[b]thiophen-3-yl-methylamine; which was then coupled with sulfamide to afford [(13)CD2(15)N]-N-(benzo[b]thien-3-ylmethyl)-sulfamide, the stable isotope-labeled compound with four stable isotope atoms. Direct oxidation of [(13)CD2(15)N]-N-(benzo[b]thien-3-ylmethyl)-sulfamide with hydrogen peroxide and peracetic acid gave the stable isotope-labeled sulfoxide and sulfone metabolites. On the other hand, radioactive (14)C-labeled N-(benzo[b]thien-3-ylmethyl)-sulfamide was prepared conveniently by sequential coupling of 3-bromo-benzo[b]thiophene with [(14)C]-copper cyanide, reduction of the carbonitrile to carboxaldehyde, and reductive amination with sulfamide. Copyright © 2013 John Wiley & Sons, Ltd.

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)

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

Enhanced forensic discrimination of pollutants by position-specific isotope analysis using isotope ratio monitoring by (13)C nuclear magnetic resonance spectrometry.

Science.gov (United States)

Julien, Maxime; Nun, Pierrick; Höhener, Patrick; Parinet, Julien; Robins, Richard J; Remaud, Gérald S

2016-01-15

In forensic environmental investigations the main issue concerns the inference of the original source of the pollutant for determining the liable party. Isotope measurements in geochemistry, combined with complimentary techniques for contaminant identification, have contributed significantly to source determination at polluted sites. In this work we have determined the intramolecular (13)C profiles of several molecules well-known as pollutants. By giving additional analytical parameters, position-specific isotope analysis performed by isotope ratio monitoring by (13)C nuclear magnetic resonance (irm-(13)C NMR) spectrometry gives new information to help in answering the major question: what is the origin of the detected contaminant? We have shown that isotope profiling of the core of a molecule reveals both the raw materials and the process used in its manufacture. It also can reveal processes occurring between the contamination site 'source' and the sampling site. Thus, irm-(13)C NMR is shown to be a very good complement to compound-specific isotope analysis currently performed by mass spectrometry for assessing polluted sites involving substantial spills of pollutant. Copyright © 2015 Elsevier B.V. All rights reserved.

On effeciency of isotopes application in industry

International Nuclear Information System (INIS)

Yankovskij, L.

1979-01-01

The final results of the long term work in the field of research, projecting and pilot production are: the technology; methods and instruments of the isotope technique and their applications in the peoples economy, especially in industry. Effectiveness of isotope technique and especially its economic effectiveness depends on the scale of application of these techniques (instrument, method, technology) in different branches of the peoples economy. Comparing expenses on istope and radiation researches with total economic effectiveness of the isotope techniques application in some countries, the total economic effectiveness of the isotope researches has been determined. The main content of the paper is the analysis of structure and dynamics of the efficiency factor for the isotope technique application in separate countries for long period of time. Determination of the total economic efficiency of the whole branch of researches, conducted according to the methodology developed by the author, on the example of isotope research in some countries, permits to make a conclusion about the state and development tendencies of these researches in the international scale and can be a good base for making decisions in the field of the scientific policy of countries [ru

Use of sequential extraction to assess metal partitioning in soils

International Nuclear Information System (INIS)

Kaasalainen, Marika; Yli-Halla, Markku

2003-01-01

The state of heavy metal pollution and the mobility of Cd, Cu, Ni, Cr, Pb and Zn were studied in three texturally different agricultural soil profiles near a Cu-Ni smelter in Harjavalta, Finland. The pseudo-total concentrations were determined by an aqua regia procedure. Metals were also determined after division into four fractions by sequential extraction with (1) acetic acid (exchangeable and specifically adsorbed metals), (2) a reducing agent (bound to Fe/Mn hydroxides), (3) an oxidizing agent (bound to soil organic matter) and (4) aqua regia (bound to mineral structures). Fallout from the smelter has increased the concentrations of Cd, Cu and Ni in the topsoil, where 75-90% of Cd, 49-72% of Cu and 22-52% of Ni occurred in the first two fractions. Slight Pb and Zn pollution was evident as well. High proportions of mobile Cd, Cu and Ni also deeper in the sandy soil, closest to the smelter, indicated some downward movement of metals. The hydroxide-bound fraction of Pb dominated in almost all soils and horizons, while Ni, Cr and Zn mostly occurred in mineral structures. Aqua regia extraction is usefully supplemented with sequential extraction, particularly in less polluted soils and in soils that exhibit substantial textural differences within the profiles. - Sequential extraction is most useful with soils with low metal pollutant levels

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)

Quantifying Uranium Isotope Ratios Using Resonance Ionization Mass Spectrometry: The Influence of Laser Parameters on Relative Ionization Probability

Energy Technology Data Exchange (ETDEWEB)

Isselhardt, Brett H. [Univ. of California, Berkeley, CA (United States)

2011-09-01

Resonance Ionization Mass Spectrometry (RIMS) has been developed as a method to measure relative uranium isotope abundances. In this approach, RIMS is used as an element-selective ionization process to provide a distinction between uranium atoms and potential isobars without the aid of chemical purification and separation. We explore the laser parameters critical to the ionization process and their effects on the measured isotope ratio. Specifically, the use of broad bandwidth lasers with automated feedback control of wavelength was applied to the measurement of ²³⁵U/²³⁸U ratios to decrease laser-induced isotopic fractionation. By broadening the bandwidth of the first laser in a 3-color, 3-photon ionization process from a bandwidth of 1.8 GHz to about 10 GHz, the variation in sequential relative isotope abundance measurements decreased from >10% to less than 0.5%. This procedure was demonstrated for the direct interrogation of uranium oxide targets with essentially no sample preparation. A rate equation model for predicting the relative ionization probability has been developed to study the effect of variation in laser parameters on the measured isotope ratio. This work demonstrates that RIMS can be used for the robust measurement of uranium isotope ratios.

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.

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...

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)

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

Kinetic mechanism and isotope effects of Pseudomonas cepacia 3-hydroxybenzoate-t-hydroxylase

International Nuclear Information System (INIS)

Wang, L.H.; Yu, Y.; Hamzah, R.Y.; Tu, S.C.

1986-01-01

The kinetic mechanism of Pseudomonas cepacia 3-hydroxybenzoate-6-hydroxylase has been delineated. Double reciprocal plots of initial rate versus m-hydroxybenzoate concentration at a constant level of oxygen and several fixed concentrations of NADH yielded a set of converging lines. Similar reciprocal plots of velocity versus NADH concentration at a constant oxygen level and several fixed m-hydroxybenzoate concentrations also showed converging lines. In contrast, double reciprocal plots of initial rate versus NADH concentration at a fixed m-hydroxybenzoate level and several oxygen concentrations showed a series of parallel lines. Parallel lines were also obtained from double reciprocal plots of initial rate versus m-hydroxybenzoate concentration at a fixed NADH level and varying oxygen concentrations. These results suggest a sequential binding of m-hydroxybenzoate and NADH by the hydroxylase. The enzyme-bound FAD is reduced and NAD is released. The reduced enzyme subsequently reacts with oxygen leading to the formation of other products. This hydroxylase exhibited a primary isotope effect of /sup D/V = 3.5 for (4R)-[4- 2 H] NADH but no isotope effect was observed with (4S)-[4- 2 H]NADH. An isotope effect of /sup T/V/K = 5.0 was also observed using (4R)-[4- 3 H]NADH. This tritium isotope effect was apparently independent of m-hydroxybenzoate concentration

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

Oxygen isotopic tracing study of the dry thermal oxidation of 6H SiC

International Nuclear Information System (INIS)

Vickridge, I.C.; Ganem, J.-J.; Battistig, G.; Szilagyi, E.

2000-01-01

The (0 0 0 1) and (0 0 0 1-bar) faces of 6H SiC have been oxidised sequentially at 1100 deg. C and 100 mbar in ultra-dry oxygen of natural isotopic concentration and in ultra-dry oxygen highly enriched in 18 O. Measurement of the 18 O isotopic concentration profiles by nuclear resonance profiling with the narrow resonance at 151 keV in 18 O(p,α) 15 N shows that on the carbon-terminated face (0 0 0 1-bar) the oxidation mechanism is rather similar to that observed on Si(1 0 0), but that on the silicon-terminated face (0 0 0 1) the surface isotopic exchange and oxide formation are superposed. The surface exchange observed during a third dry oxidation, in 16 O 2 , is very similar in magnitude and spatial extent on Si(1 0 0), and the two 6H SiC faces, suggesting that at least near the surface the nature and composition of the three oxides are very similar

Oxygen isotopic tracing study of the dry thermal oxidation of 6H SiC

Energy Technology Data Exchange (ETDEWEB)

Vickridge, I.C. E-mail: vickridge@gps.jussieu.fr; Ganem, J.-J.; Battistig, G.; Szilagyi, E

2000-03-01

The (0 0 0 1) and (0 0 0 1-bar) faces of 6H SiC have been oxidised sequentially at 1100 deg. C and 100 mbar in ultra-dry oxygen of natural isotopic concentration and in ultra-dry oxygen highly enriched in {sup 18}O. Measurement of the {sup 18}O isotopic concentration profiles by nuclear resonance profiling with the narrow resonance at 151 keV in {sup 18}O(p,{alpha}){sup 15}N shows that on the carbon-terminated face (0 0 0 1-bar) the oxidation mechanism is rather similar to that observed on Si(1 0 0), but that on the silicon-terminated face (0 0 0 1) the surface isotopic exchange and oxide formation are superposed. The surface exchange observed during a third dry oxidation, in {sup 16}O{sub 2}, is very similar in magnitude and spatial extent on Si(1 0 0), and the two 6H SiC faces, suggesting that at least near the surface the nature and composition of the three oxides are very similar.

Precise and accurate isotope ratio measurements by ICP-MS.

Science.gov (United States)

Becker, J S; Dietze, H J

2000-09-01

The precise and accurate determination of isotope ratios by inductively coupled plasma mass spectrometry (ICP-MS) and laser ablation ICP-MS (LA-ICP-MS) is important for quite different application fields (e.g. for isotope ratio measurements of stable isotopes in nature, especially for the investigation of isotope variation in nature or age dating, for determining isotope ratios of radiogenic elements in the nuclear industry, quality assurance of fuel material, for reprocessing plants, nuclear material accounting and radioactive waste control, for tracer experiments using stable isotopes or long-lived radionuclides in biological or medical studies). Thermal ionization mass spectrometry (TIMS), which used to be the dominant analytical technique for precise isotope ratio measurements, is being increasingly replaced for isotope ratio measurements by ICP-MS due to its excellent sensitivity, precision and good accuracy. Instrumental progress in ICP-MS was achieved by the introduction of the collision cell interface in order to dissociate many disturbing argon-based molecular ions, thermalize the ions and neutralize the disturbing argon ions of plasma gas (Ar+). The application of the collision cell in ICP-QMS results in a higher ion transmission, improved sensitivity and better precision of isotope ratio measurements compared to quadrupole ICP-MS without the collision cell [e.g., for 235U/238U approximately 1 (10 microg x L(-1) uranium) 0.07% relative standard deviation (RSD) vs. 0.2% RSD in short-term measurements (n = 5)]. A significant instrumental improvement for ICP-MS is the multicollector device (MC-ICP-MS) in order to obtain a better precision of isotope ratio measurements (with a precision of up to 0.002%, RSD). CE- and HPLC-ICP-MS are used for the separation of isobaric interferences of long-lived radionuclides and stable isotopes by determination of spallation nuclide abundances in an irradiated tantalum target.

Sequential Generalized Transforms on Function Space

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Jae Gil Choi

2013-01-01

Full Text Available We define two sequential transforms on a function space Ca,b[0,T] induced by generalized Brownian motion process. We then establish the existence of the sequential transforms for functionals in a Banach algebra of functionals on Ca,b[0,T]. We also establish that any one of these transforms acts like an inverse transform of the other transform. Finally, we give some remarks about certain relations between our sequential transforms and other well-known transforms on Ca,b[0,T].

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.

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.

Forced Sequence Sequential Decoding

DEFF Research Database (Denmark)