Table of specific activities of selected isotopes

International Nuclear Information System (INIS)

Shipley, G.

The bulk of this publication consists of a table of the half-lives, decay modes, and specific activities of isotopes selected for their particular interest to the Environmental Health and Safety Department, LBL. The specific activities were calculated with a PDP 9/15 computer. Also included in the report is a table of stable isotopes, the Th and U decay chains, a chart of the nuclides for elements 101 through 106, the heavy element region of the periodic table, and a specific activity monograph. 5 figures, 2 tables

Compound-specific nitrogen isotope analysis of D-alanine, L-alanine, and valine: application of diastereomer separation to delta15N and microbial peptidoglycan studies.

Science.gov (United States)

Takano, Yoshinori; Chikaraishi, Yoshito; Ogawa, Nanako O; Kitazato, Hiroshi; Ohkouchi, Naohiko

2009-01-01

We have developed an analytical method to determine the compound-specific nitrogen isotope compositions of individual amino acid enantiomers using gas chromatography/combustion/isotope ratio mass spectrometry. A novel derivatization of amino acid diastereomers by optically active (R)-(-)-2-butanol or (S)-(+)-2-butanol offers two advantages for nitrogen isotope analysis. First, chromatographic chiral separation can be achieved without the use of chiral stationary-phase columns. Second, the elution order of these compounds on the chromatogram can be switched by a designated esterification reaction. We applied the method to the compound-specific nitrogen isotope analysis of D- and L-alanine in a peptidoglycan derived from the cell walls of cultured bacteria (Firmicutes and Actinobacteria; Enterococcus faecalis, Staphylococcus aureus, Staphylococcus staphylolyticus, Lactobacillus acidophilus, Bacillus subtilis, Micrococcus luteus, and Streptomyces sp.), natural whole bacterial cells (Bacillus subtilis var. natto), (pseudo)-peptidoglycan from archaea (Methanobacterium sp.), and cell wall from eukaryota (Saccharomyces cerevisiae). We observed statistically significant differences in nitrogen isotopic compositions; e.g., delta15N ( per thousand vs air) in Staphylococcus staphylolyticus for d-alanine (19.2 +/- 0.5 per thousand, n = 4) and L-alanine (21.3 +/- 0.8 per thousand, n = 4) and in Bacillus subtilis for D-alanine (6.2 +/- 0.2 per thousand, n = 3) and L-alanine (8.2 +/- 0.4 per thousand, n = 3). These results suggest that enzymatic reaction pathways, including the alanine racemase reaction, produce a nitrogen isotopic difference in amino acid enantiomers, resulting in 15N-depleted D-alanine. This method is expected to facilitate compound-specific nitrogen isotope studies of amino acid stereoisomers.

Insights into Mechanistic Models for Evaporation of Organic Liquids in the Environment Obtained by Position-Specific Carbon Isotope Analysis.

Science.gov (United States)

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

2015-11-03

Position-specific isotope effects (PSIEs) have been measured by isotope ratio monitoring (13)C nuclear magnetic resonance spectrometry during the evaporation of 10 liquids of different polarities under 4 evaporation modes (passive evaporation, air-vented evaporation, low pressure evaporation, distillation). The observed effects are used to assess the validity of the Craig-Gordon isotope model for organic liquids. For seven liquids the overall isotope effect (IE) includes a vapor-liquid contribution that is strongly position-specific in polar compounds but less so in apolar compounds and a diffusive IE that is not position-specific, except in the alcohols, ethanol and propan-1-ol. The diffusive IE is diminished under forced evaporation. The position-specific isotope pattern created by liquid-vapor IEs is manifest in five liquids, which have an air-side limitation for volatilization. For the alcohols, undefined processes in the liquid phase create additional PSIEs. Three other liquids with limitations on the liquid side have a lower, highly position-specific, bulk diffusive IE. It is concluded that evaporation of organic pollutants creates unique position-specific isotope patterns that may be used to assess the progress of remediation or natural attenuation of pollution and that the Craig-Gordon isotope model is valid for the volatilization of nonpolar organic liquids with air-side limitation of the volatilization rate.

Compound-specific isotope analysis of light elements using gas chromatography/combustion/isotope ratio mass spectrometry (GC/C/IRMS) and its application to geochemistry

International Nuclear Information System (INIS)

Naraoka, Hiroshi; Yamada, Keita; Matsumoto, Kohei; Ishiwatari, Ryoshi

1997-01-01

Compound-specific isotope analysis has been developed recently using gas chromatography/combustion/mass spectrometry (GC/C/IRMS). This paper summarizes principles and progress of GC/C/IRMS, and reviews recent some important works using this new method. GC/C/IRMS is a novel tool for (1) biomarker analysis in sediments and living matter, (2) paleoenvironment analysis including reconstruction of ancient biogeochemical processes, (3) geochemical cycle study of organic compounds in a terrestrial-marine system, (4) evaluation of maturity and diagenesis of organic matter including petroleum formation, (5) ecological analysis, (6) evaluation of anthropologenic pollution in environment, (7) detection of extraterrestrial organic compounds and the formation mechanism study, (8) tracer studies in environment. (author)

Pico-CSIA: Picomolar Scale Compound-Specific Isotope Analyses

Science.gov (United States)

Baczynski, A. A.; Polissar, P. J.; Juchelka, D.; Schwieters, J. B.; Hilkert, A.; Freeman, K. H.

2016-12-01

The basic approach to analyzing molecular isotopes has remained largely unchanged since the late 1990s. Conventional compound-specific isotope analyses (CSIA) are conducted using capillary gas chromatography (GC), a combustion interface, and an isotope-ratio mass spectrometer (IRMS). Commercially available GC-IRMS systems are comprised of components with inner diameters ≥0.25 mm and employ helium flow rates of 1-4 mL/min. These flow rates are an order of magnitude larger than what the IRMS can accept. Consequently, ≥90% of the sample is lost through the open split, and 1-10s of nanomoles of carbon are required for analysis. These sample requirements are prohibitive for many biomarkers, which are often present in picomolar concentrations. We utilize the resolving power and low flows of narrow-bore capillary GC to improve the sensitivity of CSIA. Narrow bore capillary columns (<0.25 mm ID) allow low helium flow rates of ≤0.5mL/min for more efficient sample transfer to the ion source of the IRMS while maintaining the high linear flow rates necessary to preserve narrow peak widths ( 250 ms). The IRMS has been fitted with collector amplifiers configured to 25 ms response times for rapid data acquisition across narrow peaks. Previous authors (e.g., Sacks et al., 2007) successfully demonstrated improved sensitivity afforded by narrow-bore GC columns. They reported an accuracy and precision of 1.4‰ for peaks with an average width at half maximum of 720 ms for 100 picomoles of carbon on column. Our method builds on their advances and further reduces peak widths ( 600 ms) and the amount of sample lost prior to isotopic analysis. Preliminary experiments with 100 picomoles of carbon on column show an accuracy and standard deviation <1‰. With further improvement, we hope to demonstrate robust isotopic analysis of 10s of picomoles of carbon, more than 2 orders of magnitude lower than commercial systems. The pico-CSIA method affords high-precision isotopic analyses for

Development and validation of an universal interface for compound-specific stable isotope analysis of chlorine (37Cl/35Cl) by GC-high-temperature conversion (HTC)-MS/IRMS.

Science.gov (United States)

Renpenning, Julian; Hitzfeld, Kristina L; Gilevska, Tetyana; Nijenhuis, Ivonne; Gehre, Matthias; Richnow, Hans-Hermann

2015-03-03

A universal application of compound-specific isotope analysis of chlorine was thus far limited by the availability of suitable analysis techniques. In this study, gas chromatography in combination with a high-temperature conversion interface (GC-HTC), converting organic chlorine in the presence of H2 to gaseous HCl, was coupled to a dual-detection system, combining an ion trap mass spectrometer (MS) and isotope-ratio mass spectrometer (IRMS). The combination of the MS/IRMS detection enabled a detailed characterization, optimization, and online monitoring of the high-temperature conversion process via ion trap MS as well as a simultaneous chlorine isotope analysis by the IRMS. Using GC-HTC-MS/IRMS, chlorine isotope analysis at optimized conversion conditions resulted in very accurate isotope values (δ(37)Cl(SMOC)) for measured reference material with known isotope composition, including chlorinated ethylene, chloromethane, hexachlorocyclohexane, and trichloroacetic acids methyl ester. Respective detection limits were determined to be <15 nmol Cl on column with achieved precision of <0.3‰.

High Flux Isotope Reactor technical specifications

International Nuclear Information System (INIS)

1985-11-01

This report gives technical specifications for the High Flux Isotope Reactor (HFIR) on the following: safety limits and limiting safety system settings; limiting conditions for operation; surveillance requirements; design features; and administrative controls

Biometrics from the carbon isotope ratio analysis of amino acids in human hair.

Science.gov (United States)

Jackson, Glen P; An, Yan; Konstantynova, Kateryna I; Rashaid, Ayat H B

2015-01-01

This study compares and contrasts the ability to classify individuals into different grouping factors through either bulk isotope ratio analysis or amino-acid-specific isotope ratio analysis of human hair. Using LC-IRMS, we measured the isotope ratios of 14 amino acids in hair proteins independently, and leucine/isoleucine as a co-eluting pair, to provide 15 variables for classification. Multivariate analysis confirmed that the essential amino acids and non-essential amino acids were mostly independent variables in the classification rules, thereby enabling the separation of dietary factors of isotope intake from intrinsic or phenotypic factors of isotope fractionation. Multivariate analysis revealed at least two potential sources of non-dietary factors influencing the carbon isotope ratio values of the amino acids in human hair: body mass index (BMI) and age. These results provide evidence that compound-specific isotope ratio analysis has the potential to go beyond region-of-origin or geospatial movements of individuals-obtainable through bulk isotope measurements-to the provision of physical and characteristic traits about the individuals, such as age and BMI. Further development and refinement, for example to genetic, metabolic, disease and hormonal factors could ultimately be of great assistance in forensic and clinical casework. Copyright © 2014 Forensic Science Society. Published by Elsevier Ireland Ltd. All rights reserved.

Position-specific isotope modeling of organic micropollutants transformation through different reaction pathways

DEFF Research Database (Denmark)

Jin, Biao; Rolle, Massimo

2016-01-01

The degradation of organic micropollutants occurs via different reaction pathways. Compound specific isotope analysis is a valuable tool to identify such degradation pathways in different environmental systems. We propose a mechanism-based modeling approach that provides a quantitative framework ...

A protocol for pressurized liquid extraction and processing methods to isolate modern and ancient bone cholesterol for compound-specific stable isotope analysis.

Science.gov (United States)

Laffey, Ann O; Krigbaum, John; Zimmerman, Andrew R

2017-02-15

Bone lipid compound-specific isotope analysis (CSIA) and bone collagen and apatite stable isotope ratio analysis are important sources of ecological and paleodietary information. Pressurized liquid extraction (PLE) is quicker and utilizes less solvent than traditional methods of lipid extraction such as soxhlet and ultrasonication. This study facilitates dietary analysis by optimizing and testing a standardized methodology for PLE of bone cholesterol. Modern and archaeological bones were extracted by PLE using varied temperatures, solvent solutions, and sample weights. The efficiency of PLE was assessed via quantification of cholesterol yields. Stable isotopic ratio integrity was evaluated by comparing isotopic signatures (δ 13 C and δ 18 O values) of cholesterol derived from whole bone, bone collagen and bone apatite. Gas chromatography/mass spectrometry (GC/MS) and gas chromatography isotope ratio mass spectrometry (GC/IRMS) were conducted on purified collagen and lipid extracts to assess isotopic responses to PLE. Lipid yield was optimized at two PLE extraction cycles of 75 °C using dichloromethane/methanol (2:1 v/v) as a solvent with 0.25-0.75 g bone sample. Following lipid extraction, saponification combined with the derivatization of the neutral fraction using trimethylsilylation yielded nearly twice the cholesterol of non-saponified or non-derivatized samples. It was also found that lipids extracted from purified bone collagen and apatite could be used for cholesterol CSIA. There was no difference in the bulk δ 13 C values of collagen extracted from bone with or without lipid. However, there was a significant depletion in 18 O of bone apatite due to lipid presence or processing. These results should assist sample selection and provide an effective, alternative extraction method for bone cholesterol that may be used for isotopic and paleodietary analysis. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Metabolism of Seriola lalandi during Starvation as Revealed by Fatty Acid Analysis and Compound-Specific Analysis of Stable Isotopes within Amino Acids.

Directory of Open Access Journals (Sweden)

Fernando Barreto-Curiel

Full Text Available Fish starvation is defined as food deprivation for a long period of time, such that physiological processes become confined to basal metabolism. Starvation provides insights in physiological processes without interference from unknown factors in digestion and nutrient absorption occurring in fed state. Juveniles of amberjack Seriola lalandi were isotopically equilibrated to a formulated diet for 60 days. One treatment consisted of fish that continued to be fed and fish in the other treatment were not fed for 35 days. The isotopic signatures prior to the beginning of and after the starvation period, for fish in the starvation and control treatments, were analysed for lipid content, fatty acid composition and isotopic analysis of bulk (EA-IRMS and of amino acids (compound specific isotope analysis, CSIA. There were three replicates for the starvation group. Fatty acid content in muscle and liver tissue before and after starvation was determined to calculate percent change. Results showed that crude lipid was the most used source of energy in most cases; the PUFAs and LC-PUFAs were highly conserved. According to the protein signature in bulk (δ15N and per amino acid (δ13C and δ15N, in muscle tissue, protein synthesis did not appear to occur substantially during starvation, whereas in liver, increases in δ13C and δ15N indicate that protein turnover occurred, probably for metabolic routing to energy-yielding processes. As a result, isotopic values of δ15N in muscle tissue do not change, whereas CSIA net change occurred in the liver tissue. During the study period of 35 days, muscle protein was largely conserved, being neither replenished from amino acid pools in the plasma and liver nor catabolized.

Isotope specific arbitrary material flow meter

Science.gov (United States)

Barty, Christopher P. J.; Post, John C.; Jones, Edwin

2016-10-25

A laser-based mono-energetic gamma-ray source is used to provide non-destructive and non-intrusive, quantitative determination of the absolute amount of a specific isotope contained within pipe as part of a moving fluid or quasi-fluid material stream.

Isotope dilution analysis

Energy Technology Data Exchange (ETDEWEB)

Fudge, A.

1978-12-15

The following aspects of isotope dilution analysis are covered in this report: fundamental aspects of the technique; elements of interest in the nuclear field, choice and standardization of spike nuclide; pre-treatment to achieve isotopic exchange and chemical separation; sensitivity; selectivity; and accuracy.

Identification of chlorinated solvents degradation zones in clay till by high resolution chemical, microbial and compound specific isotope analysis

DEFF Research Database (Denmark)

Damgaard, Ida; Bjerg, Poul Løgstrup; Bælum, Jacob

2013-01-01

subsampling of the clay till cores. The study demonstrates that an integrated approach combining chemical analysis, molecular microbial tools and compound specific isotope analysis (CSIA) was required in order to document biotic and abiotic degradations in the clay till system. © 2013 Elsevier B.V.......The degradation of chlorinated ethenes and ethanes in clay till was investigated at a contaminated site (Vadsby, Denmark) by high resolution sampling of intact cores combined with groundwater sampling. Over decades of contamination, bioactive zones with degradation of trichloroethene (TCE) and 1...

Compound-specific radiocarbon analysis - Analytical challenges and applications

Science.gov (United States)

Mollenhauer, G.; Rethemeyer, J.

2009-01-01

Within the last decades, techniques have become available that allow measurement of isotopic compositions of individual organic compounds (compound-specific isotope measurements). Most often the carbon isotopic composition of these compounds is studied, including stable carbon (δ13C) and radiocarbon (Δ14C) measurements. While compound-specific stable carbon isotope measurements are fairly simple, and well-established techniques are widely available, radiocarbon analysis of specific organic compounds is a more challenging method. Analytical challenges include difficulty obtaining adequate quantities of sample, tedious and complicated laboratory separations, the lack of authentic standards for measuring realistic processing blanks, and large uncertainties in values of Δ14C at small sample sizes. The challenges associated with sample preparation for compound-specific Δ14C measurements will be discussed in this contribution. Several years of compound-specific radiocarbon analysis have revealed that in most natural samples, purified organic compounds consist of heterogeneous mixtures of the same compound. These mixtures could derive from multiple sources, each having a different initial reservoir age but mixed in the same terminal reservoir, from a single source but mixed after deposition, or from a prokaryotic organism using variable carbon sources including mobilization of ancient carbon. These processes not only represent challenges to the interpretation of compound-specific radiocarbon data, but provide unique tools for the understanding of biogeochemical and sedimentological processes influencing the preserved organic geochemical records in marine sediments. We will discuss some examples where compound-specific radiocarbon analysis has provided new insights for the understanding of carbon source utilization and carbon cycling.

Reconstructing hydroclimatic variations using compound-specific hydrogen isotope analysis of biomarkers from a maar lake in the Central Highlands, Vietnam

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Doiron, Kelsey; Stevens, Lora; Sauer, Peter

2017-04-01

Monsoonal variation in Southeast Asia affects a significant portion of the global population, but knowledge regarding response of the monsoon system to changing boundary conditions is limited. The paleoclimatic tool of compound-specific isotope analysis(CSIA) provides the ability to reconstruct past precipitation using a diverse set of biomarkers preserved in the sedimentary record. Limited proxies in tropical southeast Asia and difficult site access have led to a deficit in paleoclimate records. Ia M'He (14˚ 10'45" N, 107˚ 52' E) is a shallow volcanic crater (maar) lake, approximately 57 ha, located in the Central Highlands of Vietnam. Precipitation in the Central Highlands is sensitive to reorganizations of major climatic features, such as the migration of the ITCZ and the coupled Indo-Asian monsoon, ENSO and related shifts in the Pacific Walker Circulation and typhoon frequency. To examine this complex behavior, this pilot study aims to provide a 500-year record of effective moisture inferred from CSIA of hydrogen isotopes on biomarkers. Carbon/nitrogen ratios and carbon isotope ratios indicate that bulk organic matter is a combination of algae and C3 vegetation, offering the potential to use compound-specific hydrogen isotopes of aquatic and terrestrial organic matter in tandem. Preliminary analysis of the core shows dominant alkane chain lengths of C27 and C29, associated with terrestrial plant leaf waxes. The hydrogen isotope ratios of the plant wax components provide a proxy for paleo precipitation in a region where rainfall and droughts heavily influence population dynamics and create social discord. The CSIA record is expected to correlate with records from northern Vietnam, the South China Sea and Indonesia, with greater precipitation during the Little Ice Age. The degree to which evaporative modification of lake water (i.e., seasonal drying) occurs will be estimated by comparing the terrestrial CSIA values indicative of meteoric water with aquatic CSIA

Using compound-specific isotope analysis to assess the degradation of chloroacetanilide herbicides in lab-scale wetlands.

Science.gov (United States)

Elsayed, O F; Maillard, E; Vuilleumier, S; Nijenhuis, I; Richnow, H H; Imfeld, G

2014-03-01

Compound-specific isotope analysis (CSIA) is a promising tool to study the environmental fate of a wide range of contaminants including pesticides. In this study, a novel CSIA method was developed to analyse the stable carbon isotope signatures of widely used chloroacetanilide herbicides. The developed method was applied in combination with herbicide concentration and hydrochemical analyses to investigate in situ biodegradation of metolachlor, acetochlor and alachlor during their transport in lab-scale wetlands. Two distinct redox zones were identified in the wetlands. Oxic conditions prevailed close to the inlet of the four wetlands (oxygen concentration of 212±24μM), and anoxic conditions (oxygen concentrations of 28±41μM) prevailed towards the outlet, where dissipation of herbicides mainly occurred. Removal of acetochlor and alachlor from inlet to outlet of wetlands was 56% and 51%, whereas metolachlor was more persistent (23% of load dissipation). CSIA of chloroacetanilides at the inlet and outlet of the wetlands revealed carbon isotope fractionation of alachlor (εbulk=-2.0±0.3‰) and acetochlor (εbulk=-3.4±0.5‰), indicating that biodegradation contributes to the dissipation of both herbicides. This study is a first step towards the application of CSIA to evaluate the transport and degradation of chloroacetanilide herbicides in the environment. Copyright © 2013 Elsevier Ltd. All rights reserved.

Modeling of isotope fractionation at the catchment scale: How promising is compound specific isotope analysis (CSIA) as a tool for analyzing diffuse pollution by agrochemicals?

Science.gov (United States)

Lutz, S. R.; van Meerveld, H. J.; Waterloo, M. J.; Broers, H. P.; van Breukelen, B. M.

2012-04-01

Concentration measurements are indispensable for the assessment of subsurface and surface water pollution by agrochemicals such as pesticides. However, monitoring data is often ambiguous and easily misinterpreted as a decrease in concentration could be caused by transformation, dilution or changes in the application of the pesticide. In this context, compound specific isotope analysis (CSIA) has recently emerged as a complementary monitoring technique. It is based on the measurement of the isotopic composition (e.g. δ13C and δ2H) of the contaminant. Since transformation processes are likely accompanied by isotope fractionation, thus a change in this composition, CSIA offers the opportunity to gain additional knowledge about transport and degradation processes as well as to track pollutants back to their sources. Isotopic techniques have not yet been applied in a comprehensive way in the analysis of catchment-wide organic pollution. We therefore incorporated fractionation processes associated with the fate of pesticides into the numerical flow and solute transport model HydroGeoSphere in order to assess the feasibility of CSIA within the context of catchment monitoring. The model was set up for a hypothetical hillslope transect which drains into a river. Reactive solute transport was driven by two pesticides applications within one year and actual data for rainfall and potential evapotranspiration from a meteorological station in the Netherlands. Degradation of the pesticide was assumed to take place at a higher rate under the prevailing oxic conditions in the topsoil than in deeper, anoxic subsurface layers. In terms of CSIA, these two degradation pathways were associated with different strengths of isotope fractionation for both hydrogen and carbon atoms. By simulating changes in δ13C and δ2H, the share of the oxic and the anoxic reaction on the overall degradation could be assessed. Model results suggest that CSIA is suitable for assessing degradation of

Separation of polybrominated diphenyl ethers in fish for compound-specific stable carbon isotope analysis

Energy Technology Data Exchange (ETDEWEB)

Zeng, Yan-Hong [State Key Laboratory of Organic Geochemistry, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou 510640 (China); Graduate University of Chinese Academy of Sciences, Beijing, 100049 (China); Luo, Xiao-Jun, E-mail: luoxiaoj@gig.ac.cn [State Key Laboratory of Organic Geochemistry, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou 510640 (China); Chen, Hua-Shan; Wu, Jiang-Ping; Chen, She-Jun; Mai, Bi-Xian [State Key Laboratory of Organic Geochemistry, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou 510640 (China)

2012-05-15

A separation and isotopic analysis method was developed to accurately measure the stable carbon isotope ratios of polybrominated diphenyl ethers (PBDEs) with three to six substituted bromine atoms in fish samples. Sample extracts were treated with concentrated sulfuric acid to remove lipids, purified using complex silica gel column chromatography, and finally processed using alumina/silica (Al/Si) gel column chromatography. The purities of extracts were verified by gas chromatography and mass spectrometry (GC-MS) in the full-scan mode. The average recoveries of all compounds across the purification method were between 60% and 110%, with the exception of BDE-154. The stable carbon isotopic compositions of PBDEs can be measured with a standard deviation of less than 0.5 Per-Mille-Sign . No significant isotopic fraction was found during the purification of the main PBDE congeners. A significant change in the stable carbon isotope ratio of BDE-47 was observed in fish carcasses compared to the original isotopic signatures, implying that PBDE stable carbon isotopic compositions can be used to trace the biotransformation of PBDEs in biota. - Highlights: Black-Right-Pointing-Pointer A method for the purification of PBDEs for CSIA was developed. Black-Right-Pointing-Pointer The {delta}{sup 13}C of PBDE congeners can be measured with a standard deviation of less than 0.5 Per-Mille-Sign . Black-Right-Pointing-Pointer Common carp were exposed to a PBDE mixture to investigate debromination. Black-Right-Pointing-Pointer Ratios of the {delta}{sup 13}C values can be used to trace the debromination of PBDE in fish.

Compound-Specific Isotope Analyses to Assess TCE Biodegradation in a Fractured Dolomitic Aquifer.

Science.gov (United States)

Clark, Justin A; Stotler, Randy L; Frape, Shaun K; Illman, Walter A

2017-01-01

The potential for trichloroethene (TCE) biodegradation in a fractured dolomite aquifer at a former chemical disposal site in Smithville, Ontario, Canada, is assessed using chemical analysis and TCE and cis-DCE compound-specific isotope analysis of carbon and chlorine collected over a 16-month period. Groundwater redox conditions change from suboxic to much more reducing environments within and around the plume, indicating that oxidation of organic contaminants and degradation products is occurring at the study site. TCE and cis-DCE were observed in 13 of 14 wells sampled. VC, ethene, and/or ethane were also observed in ten wells, indicating that partial/full dechlorination has occurred. Chlorine isotopic values (δ 37 Cl) range between 1.39 to 4.69‰ SMOC for TCE, and 3.57 to 13.86‰ SMOC for cis-DCE. Carbon isotopic values range between -28.9 and -20.7‰ VPDB for TCE, and -26.5 and -11.8‰ VPDB for cis-DCE. In most wells, isotopic values remained steady over the 15-month study. Isotopic enrichment from TCE to cis-DCE varied between 0 and 13‰ for carbon and 1 and 4‰ for chlorine. Calculated chlorine-carbon isotopic enrichment ratios (ϵ Cl /ϵ C ) were 0.18 for TCE and 0.69 for cis-DCE. Combined, isotopic and chemical data indicate very little dechlorination is occurring near the source zone, but suggest bacterially mediated degradation is occurring closer to the edges of the plume. © 2016, National Ground Water Association.

Romanian wines characterization with CF-IRMS (Continuous Flow Isotope Ratio Mass Spectrometry) isotopic analysis

International Nuclear Information System (INIS)

Costinel, Diana; Ionete, Roxana Elena; Vremera, Raluca; Stanciu, Vasile

2007-01-01

Wine growing has been known for centuries long in Romania. The country has been favored by its geographical position in south-eastern Europe, by its proximity to the Black Sea, as well as by the specificity of the local soil and climate. Alongside France, Italy, Spain, Germany, countries in this area like Romania could also be called 'a vine homeland' in Europe. High quality wines produced in this region were object of trade ever since ancient times. Under current EU research projects, it is necessary to develop new methods of evidencing wine adulteration and safety. The use of mass spectrometry (MS) to determine the ratios of stable isotopes in bio-molecules now provides the means to prove the botanical and geographical origin of a wide variety of foodstuffs - and therefore, to authenticate and eliminate fraud. Isotope analysis has been officially adopted by the EU as a means of controlling adulteration of wine. Adulteration of wine can happen in many ways, e.g. addition of non-grape ethanol, addition of non-grape sugar, water or other unauthorized substances, undeclared mixing of wines from different wards, geographical areas or countries, mislabelling of variety and age. The present paper emphasize the isotopic analysis for D/H, 18 O/ 16 O, 13 C/ 12 C from wines, using a new generation Isotope Ratio MS, Finnigan Delta V Plus, coupling with a three flexible continuous flow preparation device (GasBench II, TC Elemental Analyser and GC-C/TC). Therefore authentication of wines is an important problem to which isotopic analysis has made a significant contribution. (authors)

Actinide isotopic analysis systems

International Nuclear Information System (INIS)

Koenig, Z.M.; Ruhter, W.D.; Gunnink, R.

1990-01-01

This manual provides instructions and procedures for using the Lawrence Livermore National Laboratory's two-detector actinide isotope analysis system to measure plutonium samples with other possible actinides (including uranium, americium, and neptunium) by gamma-ray spectrometry. The computer program that controls the system and analyzes the gamma-ray spectral data is driven by a menu of one-, two-, or three-letter options chosen by the operator. Provided in this manual are descriptions of these options and their functions, plus detailed instructions (operator dialog) for choosing among the options. Also provided are general instructions for calibrating the actinide isotropic analysis system and for monitoring its performance. The inventory measurement of a sample's total plutonium and other actinides content is determined by two nondestructive measurements. One is a calorimetry measurement of the sample's heat or power output, and the other is a gamma-ray spectrometry measurement of its relative isotopic abundances. The isotopic measurements needed to interpret the observed calorimetric power measurement are the relative abundances of various plutonium and uranium isotopes and americium-241. The actinide analysis system carries out these measurements. 8 figs

Basic methods of isotope analysis

International Nuclear Information System (INIS)

Ochkin, A.V.; Rozenkevich, M.B.

2000-01-01

The bases of the most applied methods of the isotope analysis are briefly presented. The possibilities and analytical characteristics of the mass-spectrometric, spectral, radiochemical and special methods of the isotope analysis, including application of the magnetic resonance, chromatography and refractometry, are considered [ru

Existing and emerging technologies for measuring stable isotope labelled retinol in biological samples: isotope dilution analysis of body retinol stores.

Science.gov (United States)

Preston, Tom

2014-01-01

This paper discusses some of the recent improvements in instrumentation used for stable isotope tracer measurements in the context of measuring retinol stores, in vivo. Tracer costs, together with concerns that larger tracer doses may perturb the parameter under study, demand that ever more sensitive mass spectrometric techniques are developed. GCMS is the most widely used technique. It has high sensitivity in terms of sample amount and uses high resolution GC, yet its ability to detect low isotope ratios is limited by background noise. LCMSMS may become more accessible for tracer studies. Its ability to measure low level stable isotope tracers may prove superior to GCMS, but it is isotope ratio MS (IRMS) that has been designed specifically for low level stable isotope analysis through accurate analysis of tracer:tracee ratios (the tracee being the unlabelled species). Compound-specific isotope analysis, where GC is interfaced to IRMS, is gaining popularity. Here, individual 13C-labelled compounds are separated by GC, combusted to CO2 and transferred on-line for ratiometric analysis by IRMS at the ppm level. However, commercially-available 13C-labelled retinol tracers are 2 - 4 times more expensive than deuterated tracers. For 2H-labelled compounds, GC-pyrolysis-IRMS has now become more generally available as an operating mode on the same IRMS instrument. Here, individual compounds are separated by GC and pyrolysed to H2 at high temperature for analysis by IRMS. It is predicted that GC-pyrolysis-IRMS will facilitate low level tracer procedures to measure body retinol stores, as has been accomplished in the case of fatty acids and amino acids. Sample size requirements for GC-P-IRMS may exceed those of GCMS, but this paper discusses sample preparation procedures and predicts improvements, particularly in the efficiency of sample introduction.

Development of an enantiomer-specific stable carbon isotope analysis (ESIA) method for assessing the fate of α-hexachlorocyclo-hexane in the environment.

Science.gov (United States)

Badea, Silviu-Laurentiu; Vogt, Carsten; Gehre, Matthias; Fischer, Anko; Danet, Andrei-Florin; Richnow, Hans-Hermann

2011-05-30

α-Hexachlorocyclohexane (α-HCH) is the only chiral isomer of the eight 1,2,3,4,5,6-HCHs and we have developed an enantiomer-specific stable carbon isotope analysis (ESIA) method for the evaluation of its fate in the environment. The carbon isotope ratios of the α-HCH enantiomers were determined for a commercially available α-HCH sample using a gas chromatography-combustion-isotope ratio mass spectrometry (GC-C-IRMS) system equipped with a chiral column. The GC-C-IRMS measurements revealed δ-values of -32.5 ± 0.8‰ and -32.3 ± 0.5‰ for (-) α-HCH and (+) α-HCH, respectively. The isotope ratio of bulk α-HCH was estimated to be -32.4 ± 0.6‰ which was in accordance with the δ-values obtained by GC-C-IRMS (-32.7 ± 0.2‰) and elemental analyzer-isotope ratio mass spectrometry (EA-IRMS) of the bulk α-HCH (-32.1 ± 0.1‰). The similarity of the isotope ratio measurements of bulk α-HCH by EA-IRMS and GC-C-IRMS indicates the accuracy of the chiral GC-C-IRMS method. The linearity of the α-HCH ESIA method shows that carbon isotope ratios can be obtained for a signal size above 100 mV. The ESIA measurements exhibited standard deviations (2σ) that were mostly IRMS method, the isotope compositions of individual enantiomers in biodegradation experiments of α-HCH with Clostridium pasteurianum and samples from a contaminated field site were determined. The isotopic compositions of the α-HCH enantiomers show a range of enantiomeric and isotope patterns, suggesting that enantiomeric and isotope fractionation can serve as an indicator for biodegradation and source characterization of α-HCH in the environment. Copyright © 2011 John Wiley & Sons, Ltd.

Compound-specific isotope analysis resolves the dietary origin of docosahexaenoic acid in the mouse brain.

Science.gov (United States)

Lacombe, R J Scott; Giuliano, Vanessa; Colombo, Stefanie M; Arts, Michael T; Bazinet, Richard P

2017-10-01

DHA (22:6n-3) may be derived from two dietary sources, preformed dietary DHA or through synthesis from α-linolenic acid (ALA; 18:3n-3). However, conventional methods cannot distinguish between DHA derived from either source without the use of costly labeled tracers. In the present study, we demonstrate the proof-of-concept that compound-specific isotope analysis (CSIA) by GC-isotope ratio mass spectrometry (IRMS) can differentiate between sources of brain DHA based on differences in natural 13 C enrichment. Mice were fed diets containing either purified ALA or DHA as the sole n-3 PUFA. Extracted lipids were analyzed by CSIA for natural abundance 13 C enrichment. Brain DHA from DHA-fed mice was significantly more enriched (-23.32‰ to -21.92‰) compared with mice on the ALA diet (-28.25‰ to -27.49‰). The measured 13 C enrichment of brain DHA closely resembled the dietary n-3 PUFA source, -21.86‰ and -28.22‰ for DHA and ALA, respectively. The dietary effect on DHA 13 C enrichment was similar in liver and blood fractions. Our results demonstrate the effectiveness of CSIA, at natural 13 C enrichment, to differentiate between the incorporation of preformed or synthesized DHA into the brain and other tissues without the need for tracers. Copyright © 2017 by the American Society for Biochemistry and Molecular Biology, Inc.

Evaluation of ethyl tert-butyl ether biodegradation in a contaminated aquifer by compound-specific isotope analysis and in situ microcosms

Energy Technology Data Exchange (ETDEWEB)

Bombach, Petra, E-mail: petra.bombach@ufz.de [UFZ – Helmholtz Centre for Environmental Research, Department of Isotope Biogeochemistry, Permoserstrasse 15, D-04318 Leipzig (Germany); Isodetect GmbH Leipzig, Deutscher Platz 5b, D-04103 Leipzig (Germany); Nägele, Norbert [Kuvier the Biotech Company S.L., Ctra. N-I, p.k. 234–P.E. INBISA 23" a, E-09001 Burgos (Spain); Rosell, Mònica [UFZ – Helmholtz Centre for Environmental Research, Department of Isotope Biogeochemistry, Permoserstrasse 15, D-04318 Leipzig (Germany); Grup de Mineralogia Aplicada i Medi Ambient, Departament de Cristallografia, Mineralogia i Dipòsits Minerals, Facultat de Geologia, Universitat de Barcelona (UB), C/Martí i Franquès s/n, 08028 Barcelona (Spain); Richnow, Hans H. [UFZ – Helmholtz Centre for Environmental Research, Department of Isotope Biogeochemistry, Permoserstrasse 15, D-04318 Leipzig (Germany); Fischer, Anko [Isodetect GmbH Leipzig, Deutscher Platz 5b, D-04103 Leipzig (Germany)

2015-04-09

Highlights: • In situ biodegradation of ETBE was investigated in a fuel contaminated aquifer. • Degradation was studied by CSIA and in situ microcosms in combination with TLFA-SIP. • ETBE was degraded when ETBE was the main groundwater contaminant. • ETBE was also degraded in the presence of BTEX and MTBE. • Hydrochemical analysis indicated aerobic and anaerobic ETBE biodegradation. - Abstract: Ethyl tert-butyl ether (ETBE) is an upcoming groundwater pollutant in Europe whose environmental fate has been less investigated, thus far. In the present study, we investigated the in situ biodegradation of ETBE in a fuel-contaminated aquifer using compound-specific stable isotope analysis (CSIA), and in situ microcosms in combination with total lipid fatty acid (TLFA)-stable isotope probing (SIP). In a first field investigation, CSIA revealed insignificant carbon isotope fractionation, but low hydrogen isotope fractionation of up to +14‰ along the prevailing anoxic ETBE plume suggesting biodegradation of ETBE. Ten months later, oxygen injection was conducted to enhance the biodegradation of petroleum hydrocarbons (PH) at the field site. Within the framework of this remediation measure, in situ microcosms loaded with [{sup 13}C{sub 6}]-ETBE (BACTRAP{sup ®}s) were exposed for 119 days in selected groundwater wells to assess the biodegradation of ETBE by TLFA-SIP under the following conditions: (i) ETBE as main contaminant; (ii) ETBE as main contaminant subjected to oxygen injection; (iii) ETBE plus other PH; (iv) ETBE plus other PH subjected to oxygen injection. Under all conditions investigated, significant {sup 13}C-incorporation into microbial total lipid fatty acids extracted from the in situ microcosms was found, providing clear evidence of ETBE biodegradation.

Evaluation of ethyl tert-butyl ether biodegradation in a contaminated aquifer by compound-specific isotope analysis and in situ microcosms

International Nuclear Information System (INIS)

Bombach, Petra; a, E-09001 Burgos (Spain))" data-affiliation=" (Kuvier the Biotech Company S.L., Ctra. N-I, p.k. 234–P.E. INBISA 23a, E-09001 Burgos (Spain))" >Nägele, Norbert; Rosell, Mònica; Richnow, Hans H.; Fischer, Anko

2015-01-01

Highlights: • In situ biodegradation of ETBE was investigated in a fuel contaminated aquifer. • Degradation was studied by CSIA and in situ microcosms in combination with TLFA-SIP. • ETBE was degraded when ETBE was the main groundwater contaminant. • ETBE was also degraded in the presence of BTEX and MTBE. • Hydrochemical analysis indicated aerobic and anaerobic ETBE biodegradation. - Abstract: Ethyl tert-butyl ether (ETBE) is an upcoming groundwater pollutant in Europe whose environmental fate has been less investigated, thus far. In the present study, we investigated the in situ biodegradation of ETBE in a fuel-contaminated aquifer using compound-specific stable isotope analysis (CSIA), and in situ microcosms in combination with total lipid fatty acid (TLFA)-stable isotope probing (SIP). In a first field investigation, CSIA revealed insignificant carbon isotope fractionation, but low hydrogen isotope fractionation of up to +14‰ along the prevailing anoxic ETBE plume suggesting biodegradation of ETBE. Ten months later, oxygen injection was conducted to enhance the biodegradation of petroleum hydrocarbons (PH) at the field site. Within the framework of this remediation measure, in situ microcosms loaded with [ 13 C 6 ]-ETBE (BACTRAP ® s) were exposed for 119 days in selected groundwater wells to assess the biodegradation of ETBE by TLFA-SIP under the following conditions: (i) ETBE as main contaminant; (ii) ETBE as main contaminant subjected to oxygen injection; (iii) ETBE plus other PH; (iv) ETBE plus other PH subjected to oxygen injection. Under all conditions investigated, significant 13 C-incorporation into microbial total lipid fatty acids extracted from the in situ microcosms was found, providing clear evidence of ETBE biodegradation

Degradation of sulfamethoxazole using ozone and chlorine dioxide - Compound-specific stable isotope analysis, transformation product analysis and mechanistic aspects.

Science.gov (United States)

Willach, Sarah; Lutze, Holger V; Eckey, Kevin; Löppenberg, Katja; Lüling, Michelle; Terhalle, Jens; Wolbert, Jens-Benjamin; Jochmann, Maik A; Karst, Uwe; Schmidt, Torsten C

2017-10-01

The sulfonamide antibiotic sulfamethoxazole (SMX) is a widely detected micropollutant in surface and groundwaters. Oxidative treatment with e.g. ozone or chlorine dioxide is regularly applied for disinfection purposes at the same time exhibiting a high potential for removal of micropollutants. Especially for nitrogen containing compounds such as SMX, the related reaction mechanisms are largely unknown. In this study, we systematically investigated reaction stoichiometry, product formation and reaction mechanisms in reactions of SMX with ozone and chlorine dioxide. To this end, the neutral and anionic SMX species, which may occur at typical pH-values of water treatment were studied. Two moles of chlorine dioxide and approximately three moles of ozone were consumed per mole SMX degraded. Oxidation of SMX with ozone and chlorine dioxide leads in both cases to six major transformation products (TPs) as revealed by high-resolution mass spectrometry (HRMS). Tentatively formulated TP structures from other studies could partly be confirmed by compound-specific stable isotope analysis (CSIA). However, for one TP, a hydroxylated SMX, it was not possible by HRMS alone to identify whether hydroxylation occurred at the aromatic ring, as suggested in literature before, or at the anilinic nitrogen. By means of CSIA and an analytical standard it was possible to identify sulfamethoxazole hydroxylamine unequivocally as one of the TPs of the reaction of SMX with ozone as well as with chlorine dioxide. H-abstraction and electron transfer at the anilinic nitrogen are suggested as likely initial reactions of ozone and chlorine dioxide, respectively, leading to its formation. Oxidation of anionic SMX with ozone did not show any significant isotopic fractionation whereas the other reactions studied resulted in a significant carbon isotope fractionation. Copyright © 2017 Elsevier Ltd. All rights reserved.

Complementing approaches to demonstrate chlorinated solvent biodegradation in a complex pollution plume: mass balance, PCR and compound-specific stable isotope analysis.

OpenAIRE

Courbet Christelle; Rivière Agnès; Jeannottat Simon; Rinaldi Sandro; Hunkeler Daniel; Bendjoudi Hocine; De Marsily Ghislain

2011-01-01

This work describes the use of different complementing methods (mass balance polymerase chain reaction assays and compound specific stable isotope analysis) to demonstrate the existence and effectiveness of biodegradation of chlorinated solvents in an alluvial aquifer. The solvent contaminated site is an old chemical factory located in an alluvial plain in France. As most of the chlorinated contaminants currently found in the groundwater at this site were produced by local industries at vario...

The application of compound-specific isotope analysis of fatty acids for traceability of sea cucumber (Apostichopus japonicus) in the coastal areas of China.

Science.gov (United States)

Liu, Yu; Zhang, Xufeng; Li, Ying; Wang, Haixia

2017-11-01

Geographical origin traceability is an important issue for controlling the quality of seafood and safeguarding the interest of consumers. In the present study, a new method of compound-specific isotope analysis (CSIA) of fatty acids was established to evaluate its applicability in establishing the origin traceability of Apostichopus japonicus in the coastal areas of China. Moreover, principal component analysis (PCA) and discriminant analysis (DA) were applied to distinguish between the origins of A. japonicus. The results show that the stable carbon isotope compositions of fatty acids of A. japonicus significantly differ in terms of both season and origin. They also indicate that the stable carbon isotope composition of fatty acids could effectively discriminate between the origins of A. japonicus, except for between Changhai Island and Zhangzi Island in the spring of 2016 because of geographical proximity or the similarity of food sources. The fatty acids that have the highest contribution to identifying the geographical origins of A. japonicus are C22:6n-3, C16:1n-7, C20:5n-3, C18:0 and C23:1n-9, when considering the fatty acid contents, the stable carbon isotope composition of fatty acids and the results of the PCA and DA. We conclude that CSIA of fatty acids, combined with multivariate statistical analysis such as PCA and DA, may be an effective tool for establishing the traceability of A. japonicus in the coastal areas of China. The relevant conclusions of the present study provide a new method for determining the traceability of seafood or other food products. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

Isotope specific resolution recovery image reconstruction in high resolution PET imaging

NARCIS (Netherlands)

Kotasidis, Fotis A.; Angelis, Georgios I.; Anton-Rodriguez, Jose; Matthews, Julian C.; Reader, Andrew J.; Zaidi, Habib

Purpose: Measuring and incorporating a scanner-specific point spread function (PSF) within image reconstruction has been shown to improve spatial resolution in PET. However, due to the short half-life of clinically used isotopes, other long-lived isotopes not used in clinical practice are used to

Brayton Isotope Power System (BIPS) facility specification

International Nuclear Information System (INIS)

1976-01-01

General requirements for the Brayton Isotope Power System (BIPS)/Ground Demonstration System (GDS) assembly and test facility are defined. The facility will include provisions for a complete test laboratory for GDS checkout, performance, and endurance testing, and a contamination-controlled area for assembly, fabrication, storage, and storage preparation of GDS components. Specifications, schedules, and drawings are included

Brayton Isotope Power System (BIPS) facility specification

Energy Technology Data Exchange (ETDEWEB)

1976-05-31

General requirements for the Brayton Isotope Power System (BIPS)/Ground Demonstration System (GDS) assembly and test facility are defined. The facility will include provisions for a complete test laboratory for GDS checkout, performance, and endurance testing, and a contamination-controlled area for assembly, fabrication, storage, and storage preparation of GDS components. Specifications, schedules, and drawings are included.

Triple-element compound-specific stable isotope analysis of 1,2-dichloroethane for characterization of the underlying dehalogenation reaction in two Dehalococcoides mccartyi strains.

Science.gov (United States)

Franke, Steffi; Lihl, Christina; Renpenning, Julian; Elsner, Martin; Nijenhuis, Ivonne

2017-12-01

Chlorinated ethanes belong to the most common groundwater and soil contaminants. Of these, 1,2-dichloroethane (1,2-DCA) is a man-made, persistent and toxic contaminant, released due to improper waste treatment at versatile production sites. This study investigated the anaerobic transformation of 1,2-DCA by Dehalococcoides mccartyi strain 195 and strain BTF08 using triple-element compound-specific stable isotope analysis of carbon, chlorine and hydrogen for the first time. Isotope fractionation patterns for carbon (εCBTF08 = -28.4 ± 3.7‰; εC195 = -30.9 ± 3.6‰) and chlorine (εClBTF08 = -4.6 ± 0.7‰; εCl195 = -4.2 ± 0.5‰) within both investigated D. mccartyi strains, as well as the dual-element analysis (ΛBTF08 = 6.9 ± 1.2; Λ195 = 7.1 ± 0.2), supported identical reaction mechanisms for dehalogenation of 1,2-DCA. Hydrogen isotope fractionation analysis revealed dihaloelimination as prevalent reaction mechanism. Vinyl chloride as major intermediate could be excluded by performing the experiment in deuterated aqueous media. Furthermore, evaluation of the derived apparent kinetic isotope effects (AKIECBTF08 = 1.029/AKIEC195 = 1.031; AKIEClBTF08 = 1.005/AKIECl195 = 1.004) pointed towards simultaneous abstraction of both involved chlorine-substituents in a concerted matter. It was shown that D. mccartyi strain BTF08 and strain 195 are capable of complete, direct dihaloelimination of 1,2-DCA to ethene. © FEMS 2017. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

Species-specific isotopic fractionation of mercury during methylation by bacteria

International Nuclear Information System (INIS)

Rodriguez-Gonzalez, P.; Epov, V.N.; Bridou, R.; Tessier, E.; Monperrus, M.; Guyoneaud, R.; Amouroux, D.

2009-01-01

Full text: The environmental reactivity of Hg is extremely dependent on its chemical form. In fact, Hg bioaccumulation is due to the greater trophic transfer efficiency of methylmercury which is formed as a result of biotic or abiotic transformations caused by specific redox gradients and bacterial activity. The study of stable isotope biogeochemistry of Hg may provide a powerful tool to track and understand its cycle and pathways in the environment. This work presents the measurement of species-specific Hg isotopic composition by GC-MCICPMS during Hg methylation experiments using cultures of pure bacterial strains incubated with Hg (II) standard NIST 3133. (author)

Stable-isotope analysis: a neglected tool for placing parasites in food webs.

Science.gov (United States)

Sabadel, A J M; Stumbo, A D; MacLeod, C D

2018-02-28

Parasites are often overlooked in the construction of food webs, despite their ubiquitous presence in almost every type of ecosystem. Researchers who do recognize their importance often struggle to include parasites using classical food-web theory, mainly due to the parasites' multiple hosts and life stages. A novel approach using compound-specific stable-isotope analysis promises to provide considerable insight into the energetic exchanges of parasite and host, which may solve some of the issues inherent in incorporating parasites using a classical approach. Understanding the role of parasites within food webs, and tracing the associated biomass transfers, are crucial to constructing new models that will expand our knowledge of food webs. This mini-review focuses on stable-isotope studies published in the past decade, and introduces compound-specific stable-isotope analysis as a powerful, but underutilized, newly developed tool that may answer many unresolved questions regarding the role of parasites in food webs.

Isotope Specific Remediation Media and Systems - 13614

Energy Technology Data Exchange (ETDEWEB)

Denton, Mark S.; Mertz, Joshua L. [Kurion, Inc. Oak Ridge, Tennessee 37831 (United States); Morita, Keisuke [Japan Atomic Energy Agency, Tokai Research and Development Center, Fukushima Project Team, Tokai-mura, Ibaraki-ken, 319-1195 (Japan)

2013-07-01

On March 11, 2011, now two years ago, the magnitude 9.0 Great East Japan earthquake, Tohoku, hit off the Fukushima coast of Japan. While, of course, most of the outcome of this unprecedented natural and manmade disaster was a negative, both in Japan and worldwide, there have been some extremely invaluable lessons learned and new emergency recovery technologies and systems developed. As always, the mother of invention is necessity. Among these developments has been the development and full-scale implementation of proven isotope specific media (ISMs) with the intent of surgically removing specific hazardous isotopes for the purpose of minimizing dose to workers and the environment. The first such ISMs to be deployed at the Fukushima site were those removing cesium (Cs-137) and iodine (I-129). Since deployment on June 17, 2011, along with treated cooling water recycle, some 70% of the curies in the building liquid wastes have been removed by the Kurion system alone. The current levels of cesium are now only 2% of the original levels. Such an unprecedented, 'external cooling system' not only allowed the eventual cold shut down of the reactors in mid-December, 2011, but has allowed workers to concentrate on the cleanup of other areas of the site. Water treatment will continue for quite some time due to continued leakage into the buildings and the eventual goal of cleaning up the reactors and fuel pools themselves. With the cesium removal now in routine operation, other isotopes of concern are likely to become priorities. One such isotope is that of strontium, and yttrium (Sr-90 and Y-90), which is still at original levels causing further dose issues as well as impediments to discharge of the treated waste waters. For over a year now, a new synthetic strontium specific media has been under development and testing both in our licensed facility in Oak Ridge, Tennessee, but also in confirmatory tests by the Japan Atomic Energy Agency (JAEA) in Japan for Tokyo

Compound-specific chlorine isotope ratios of TCE, PCE and DCE isomers by direct injection using CF-IRMS

International Nuclear Information System (INIS)

Shouakar-Stash, Orfan; Drimmie, Robert J.; Zhang Min; Frape, Shaun K.

2006-01-01

A method for determining compound-specific Cl isotopic compositions (δ 37 Cl) was developed for tetrachloroethene (PCE), trichloroethene (TCE), cis-dichloroethene (cis-DCE), trans-dichloroethene (trans-DCE) and 1,1-dichloroethene (1,1-DCE). The isotope ratio mass spectrometry (IRMS) used in this study has nine collectors, including two for m/z 50 and 52 (CH 3 Cl) and two for m/z 94 and 96 (CH 3 Br). The development of this method is based on the fact that fragments with mass ratios of 94/96, 95/97 and 96/98 are produced from PCE, TCE and DCE isomers during ion bombardment in the source of a mass spectrometer. Using continuous flow isotope ratio mass spectrometry coupled with gas chromatography (GC-CF-IRMS), it is possible to separate these compounds on-line and directly measure the Cl isotopic ratios of the fragments with the specific mass ratios. Both pure phase and aqueous samples were used for Cl isotopic analysis. For pure phase samples, a vapour phase of the chlorinated ethenes was injected directly into the GC, whereas the solid phase micro extraction (SPME) method was used to extract these compounds from aqueous solutions. The precisions of this analytical technique were ±0.12 per mille (1σ, n = 30), ±0.06 per mille (1σ, n = 30), and ±0.08 per mille (1σ, n = 15) for PCE, TCE and DCE isomers, respectively. The limits of quantification (LOQ) for analyzing Cl isotopic composition in aqueous solutions were 20, 5, and 5 μg/L for PCE, TCE and DCE isomers, respectively. This corresponds to 6-9 nano-mole of Cl, which is approximately 80 times lower than the most sensitive existing method. Compared to methods previously available, this new development offers the following advantages: (1) The much lower LOQ make it possible to extract these compounds directly from aqueous solutions using SPME without pre-concentration; (2) The linking of a GC with an IRMS eliminates off-line separation; and (3) Because the fragments used for isotopic ratio measurement are

Isotope specific resolution recovery image reconstruction in high resolution PET imaging

Energy Technology Data Exchange (ETDEWEB)

Kotasidis, Fotis A. [Division of Nuclear Medicine and Molecular Imaging, Geneva University Hospital, CH-1211 Geneva, Switzerland and Wolfson Molecular Imaging Centre, MAHSC, University of Manchester, M20 3LJ, Manchester (United Kingdom); Angelis, Georgios I. [Faculty of Health Sciences, Brain and Mind Research Institute, University of Sydney, NSW 2006, Sydney (Australia); Anton-Rodriguez, Jose; Matthews, Julian C. [Wolfson Molecular Imaging Centre, MAHSC, University of Manchester, Manchester M20 3LJ (United Kingdom); Reader, Andrew J. [Montreal Neurological Institute, McGill University, Montreal QC H3A 2B4, Canada and Department of Biomedical Engineering, Division of Imaging Sciences and Biomedical Engineering, King' s College London, St. Thomas’ Hospital, London SE1 7EH (United Kingdom); Zaidi, Habib [Division of Nuclear Medicine and Molecular Imaging, Geneva University Hospital, CH-1211 Geneva (Switzerland); Geneva Neuroscience Centre, Geneva University, CH-1205 Geneva (Switzerland); Department of Nuclear Medicine and Molecular Imaging, University of Groningen, University Medical Center Groningen, PO Box 30 001, Groningen 9700 RB (Netherlands)

2014-05-15

Purpose: Measuring and incorporating a scanner-specific point spread function (PSF) within image reconstruction has been shown to improve spatial resolution in PET. However, due to the short half-life of clinically used isotopes, other long-lived isotopes not used in clinical practice are used to perform the PSF measurements. As such, non-optimal PSF models that do not correspond to those needed for the data to be reconstructed are used within resolution modeling (RM) image reconstruction, usually underestimating the true PSF owing to the difference in positron range. In high resolution brain and preclinical imaging, this effect is of particular importance since the PSFs become more positron range limited and isotope-specific PSFs can help maximize the performance benefit from using resolution recovery image reconstruction algorithms. Methods: In this work, the authors used a printing technique to simultaneously measure multiple point sources on the High Resolution Research Tomograph (HRRT), and the authors demonstrated the feasibility of deriving isotope-dependent system matrices from fluorine-18 and carbon-11 point sources. Furthermore, the authors evaluated the impact of incorporating them within RM image reconstruction, using carbon-11 phantom and clinical datasets on the HRRT. Results: The results obtained using these two isotopes illustrate that even small differences in positron range can result in different PSF maps, leading to further improvements in contrast recovery when used in image reconstruction. The difference is more pronounced in the centre of the field-of-view where the full width at half maximum (FWHM) from the positron range has a larger contribution to the overall FWHM compared to the edge where the parallax error dominates the overall FWHM. Conclusions: Based on the proposed methodology, measured isotope-specific and spatially variant PSFs can be reliably derived and used for improved spatial resolution and variance performance in resolution

Isotope specific resolution recovery image reconstruction in high resolution PET imaging

International Nuclear Information System (INIS)

Kotasidis, Fotis A.; Angelis, Georgios I.; Anton-Rodriguez, Jose; Matthews, Julian C.; Reader, Andrew J.; Zaidi, Habib

2014-01-01

Purpose: Measuring and incorporating a scanner-specific point spread function (PSF) within image reconstruction has been shown to improve spatial resolution in PET. However, due to the short half-life of clinically used isotopes, other long-lived isotopes not used in clinical practice are used to perform the PSF measurements. As such, non-optimal PSF models that do not correspond to those needed for the data to be reconstructed are used within resolution modeling (RM) image reconstruction, usually underestimating the true PSF owing to the difference in positron range. In high resolution brain and preclinical imaging, this effect is of particular importance since the PSFs become more positron range limited and isotope-specific PSFs can help maximize the performance benefit from using resolution recovery image reconstruction algorithms. Methods: In this work, the authors used a printing technique to simultaneously measure multiple point sources on the High Resolution Research Tomograph (HRRT), and the authors demonstrated the feasibility of deriving isotope-dependent system matrices from fluorine-18 and carbon-11 point sources. Furthermore, the authors evaluated the impact of incorporating them within RM image reconstruction, using carbon-11 phantom and clinical datasets on the HRRT. Results: The results obtained using these two isotopes illustrate that even small differences in positron range can result in different PSF maps, leading to further improvements in contrast recovery when used in image reconstruction. The difference is more pronounced in the centre of the field-of-view where the full width at half maximum (FWHM) from the positron range has a larger contribution to the overall FWHM compared to the edge where the parallax error dominates the overall FWHM. Conclusions: Based on the proposed methodology, measured isotope-specific and spatially variant PSFs can be reliably derived and used for improved spatial resolution and variance performance in resolution

Isotope specific resolution recovery image reconstruction in high resolution PET imaging.

Science.gov (United States)

Kotasidis, Fotis A; Angelis, Georgios I; Anton-Rodriguez, Jose; Matthews, Julian C; Reader, Andrew J; Zaidi, Habib

2014-05-01

Measuring and incorporating a scanner-specific point spread function (PSF) within image reconstruction has been shown to improve spatial resolution in PET. However, due to the short half-life of clinically used isotopes, other long-lived isotopes not used in clinical practice are used to perform the PSF measurements. As such, non-optimal PSF models that do not correspond to those needed for the data to be reconstructed are used within resolution modeling (RM) image reconstruction, usually underestimating the true PSF owing to the difference in positron range. In high resolution brain and preclinical imaging, this effect is of particular importance since the PSFs become more positron range limited and isotope-specific PSFs can help maximize the performance benefit from using resolution recovery image reconstruction algorithms. In this work, the authors used a printing technique to simultaneously measure multiple point sources on the High Resolution Research Tomograph (HRRT), and the authors demonstrated the feasibility of deriving isotope-dependent system matrices from fluorine-18 and carbon-11 point sources. Furthermore, the authors evaluated the impact of incorporating them within RM image reconstruction, using carbon-11 phantom and clinical datasets on the HRRT. The results obtained using these two isotopes illustrate that even small differences in positron range can result in different PSF maps, leading to further improvements in contrast recovery when used in image reconstruction. The difference is more pronounced in the centre of the field-of-view where the full width at half maximum (FWHM) from the positron range has a larger contribution to the overall FWHM compared to the edge where the parallax error dominates the overall FWHM. Based on the proposed methodology, measured isotope-specific and spatially variant PSFs can be reliably derived and used for improved spatial resolution and variance performance in resolution recovery image reconstruction. The

C, Cl and H compound-specific isotope analysis to assess natural versus Fe(0) barrier-induced degradation of chlorinated ethenes at a contaminated site

Energy Technology Data Exchange (ETDEWEB)

Audí-Miró, Carme, E-mail: carmeaudi@ub.edu [Grup de Mineralogia Aplicada i Medi Ambient, Departament de Cristal.lografia, Mineralogia i Dipòsits Minerals, Facultat de Geologia, Universitat de Barcelona (UB), Martí Franquès s/n, 08028, Barcelona (Spain); Cretnik, Stefan [Institute of Groundwater Ecology, Helmholtz Zentrum München-National Research Center for Environmental Health, Ingolstädter Landstrasse 1, D-85764 Neuherberg (Germany); Torrentó, Clara; Rosell, Mònica [Grup de Mineralogia Aplicada i Medi Ambient, Departament de Cristal.lografia, Mineralogia i Dipòsits Minerals, Facultat de Geologia, Universitat de Barcelona (UB), Martí Franquès s/n, 08028, Barcelona (Spain); Shouakar-Stash, Orfan [Department of Earth & Environmental Sciences, 200 University Ave. W, N2L 3G1 Waterloo, Ontario (Canada); Otero, Neus [Grup de Mineralogia Aplicada i Medi Ambient, Departament de Cristal.lografia, Mineralogia i Dipòsits Minerals, Facultat de Geologia, Universitat de Barcelona (UB), Martí Franquès s/n, 08028, Barcelona (Spain); Palau, Jordi [Université de Neuchâtel, CHYN - Centre d' Hydrogéologie, Rue Emile-Argand 11, CH-2000 Neuchâtel (Switzerland); and others

2015-12-15

Highlights: • {sup 13}C to evaluate natural chlorinated ethenes biodegradation. • {sup 13}C to evaluate the efficiency of a zero-valent iron-permeable reactive barrier. • {sup 13}C-{sup 37}Cl to discriminate biotic from abiotic degradation of cis-dichloroethene. • {sup 13}C-{sup 37}Cl-{sup 2}H of cis-DCE and TCE to elucidate different contaminant sources. - Abstract: Compound-specific isotopic analysis of multiple elements (C, Cl, H) was tested to better assess the effect of a zero-valent iron-permeable reactive barrier (ZVI-PRB) installation at a site contaminated with tetrachloroethene (PCE) and trichloroethene (TCE). The focus was on (1) using {sup 13}C to evaluate natural chlorinated ethene biodegradation and the ZVI-PRB efficiency; (2) using dual element {sup 13}C-{sup 37}Cl isotopic analysis to distinguish biotic from abiotic degradation of cis-dichloroethene (cis-DCE); and (3) using {sup 13}C-{sup 37}Cl-{sup 2}H isotopic analysis of cis-DCE and TCE to elucidate different contaminant sources. Both biodegradation and degradation by ZVI-PRB were indicated by the metabolites that were detected and the {sup 13}C data, with a quantitative estimate of the ZVI-PRB efficiency of less than 10% for PCE. Dual element {sup 13}C-{sup 37}Cl isotopic plots confirmed that biodegradation was the main process at the site including the ZVI-PRB area. Based on the carbon isotope data, approximately 45% and 71% of PCE and TCE, respectively, were estimated to be removed by biodegradation. {sup 2}H combined with {sup 13}C and {sup 37}Cl seems to have identified two discrete sources contributing to the contaminant plume, indicating the potential of δ{sup 2}H to discriminate whether a compound is of industrial origin, or whether a compound is formed as a daughter product during degradation.

C, Cl and H compound-specific isotope analysis to assess natural versus Fe(0) barrier-induced degradation of chlorinated ethenes at a contaminated site

International Nuclear Information System (INIS)

Audí-Miró, Carme; Cretnik, Stefan; Torrentó, Clara; Rosell, Mònica; Shouakar-Stash, Orfan; Otero, Neus; Palau, Jordi

2015-01-01

Highlights: • 13 C to evaluate natural chlorinated ethenes biodegradation. • 13 C to evaluate the efficiency of a zero-valent iron-permeable reactive barrier. • 13 C- 37 Cl to discriminate biotic from abiotic degradation of cis-dichloroethene. • 13 C- 37 Cl- 2 H of cis-DCE and TCE to elucidate different contaminant sources. - Abstract: Compound-specific isotopic analysis of multiple elements (C, Cl, H) was tested to better assess the effect of a zero-valent iron-permeable reactive barrier (ZVI-PRB) installation at a site contaminated with tetrachloroethene (PCE) and trichloroethene (TCE). The focus was on (1) using 13 C to evaluate natural chlorinated ethene biodegradation and the ZVI-PRB efficiency; (2) using dual element 13 C- 37 Cl isotopic analysis to distinguish biotic from abiotic degradation of cis-dichloroethene (cis-DCE); and (3) using 13 C- 37 Cl- 2 H isotopic analysis of cis-DCE and TCE to elucidate different contaminant sources. Both biodegradation and degradation by ZVI-PRB were indicated by the metabolites that were detected and the 13 C data, with a quantitative estimate of the ZVI-PRB efficiency of less than 10% for PCE. Dual element 13 C- 37 Cl isotopic plots confirmed that biodegradation was the main process at the site including the ZVI-PRB area. Based on the carbon isotope data, approximately 45% and 71% of PCE and TCE, respectively, were estimated to be removed by biodegradation. 2 H combined with 13 C and 37 Cl seems to have identified two discrete sources contributing to the contaminant plume, indicating the potential of δ 2 H to discriminate whether a compound is of industrial origin, or whether a compound is formed as a daughter product during degradation.

The radiological hazard of plutonium isotopes and specific plutonium mixtures

International Nuclear Information System (INIS)

Heindel, G.; Clow, J.; Inkret, W.; Miller, G.

1995-11-01

The US Department of Energy defines the hazard categories of its nuclear facilities based upon the potential for accidents to have significant effects on specific populations and the environment. In this report, the authors consider the time dependence of hazard category 2 (significant on-site effects) for facilities with inventories of plutonium isotopes and specific weapons-grade and heat-source mixtures of plutonium isotopes. The authors also define relative hazard as the reciprocal of the hazard category 2 threshold value and determine its time dependence. The time dependence of both hazard category 2 thresholds and relative hazards are determined and plotted for 10,000 years to provide useful information for planning long-term storage or disposal facilities

Compound-Specific Chlorine Isotope Analysis of Tetrachloromethane and Trichloromethane by Gas Chromatography-Isotope Ratio Mass Spectrometry vs Gas Chromatography-Quadrupole Mass Spectrometry: Method Development and Evaluation of Precision and Trueness.

Science.gov (United States)

Heckel, Benjamin; Rodríguez-Fernández, Diana; Torrentó, Clara; Meyer, Armin; Palau, Jordi; Domènech, Cristina; Rosell, Mònica; Soler, Albert; Hunkeler, Daniel; Elsner, Martin

2017-03-21

Compound-specific chlorine isotope analysis of tetrachloromethane (CCl 4 ) and trichloromethane (CHCl 3 ) was explored by both, gas chromatography-isotope ratio mass spectrometry (GC-IRMS) and GC-quadrupole MS (GC-qMS), where GC-qMS was validated in an interlaboratory comparison between Munich and Neuchâtel with the same type of commercial GC-qMS instrument. GC-IRMS measurements analyzed CCl isotopologue ions, whereas GC-qMS analyzed the isotopologue ions CCl 3 , CCl 2 , CCl (of CCl 4 ) and CHCl 3 , CHCl 2 , CHCl (of CHCl 3 ), respectively. Lowest amount dependence (good linearity) was obtained (i) in H-containing fragment ions where interference of 35 Cl- to 37 Cl-containing ions was avoided; (ii) with tuning parameters favoring one predominant rather than multiple fragment ions in the mass spectra. Optimized GC-qMS parameters (dwell time 70 ms, 2 most abundant ions) resulted in standard deviations of 0.2‰ (CHCl 3 ) and 0.4‰ (CCl 4 ), which are only about twice as large as 0.1‰ and 0.2‰ for GC-IRMS. To compare also the trueness of both methods and laboratories, samples from CCl 4 and CHCl 3 degradation experiments were analyzed and calibrated against isotopically different reference standards for both CCl 4 and CHCl 3 (two of each). Excellent agreement confirms that true results can be obtained by both methods provided that a consistent set of isotopically characterized reference materials is used.

Is it really organic? – Multi-isotopic analysis as a tool to discriminate between organic and conventional plants

DEFF Research Database (Denmark)

Laursen, K.H.; Mihailova, A.; Kelly, S.D.

2013-01-01

for discrimination of organically and conventionally grown plants. The study was based on wheat, barley, faba bean and potato produced in rigorously controlled long-term field trials comprising 144 experimental plots. Nitrogen isotope analysis revealed the use of animal manure, but was unable to discriminate between......Novel procedures for analytical authentication of organic plant products are urgently needed. Here we present the first study encompassing stable isotopes of hydrogen, carbon, nitrogen, oxygen, magnesium and sulphur as well as compound-specific nitrogen and oxygen isotope analysis of nitrate...... plants that were fertilised with synthetic nitrogen fertilisers or green manures from atmospheric nitrogen fixing legumes. This limitation was bypassed using oxygen isotope analysis of nitrate in potato tubers, while hydrogen isotope analysis allowed complete discrimination of organic and conventional...

Applications of compound-specific carbon isotope ratios in organic contaminant studies

International Nuclear Information System (INIS)

Aravena, R.; Hunkeler, D.; Bloom, Y.; Frape, S.K.; Butler, B.; Edwards, E.; Cox, E.

1999-01-01

In this paper results are presented on the application of compound-specific isotope ratios measurements to assess biodegradation of chlorinated solvents, in particularly on microbial dechlorination of tetrachloroethene (PCE) and trichloroethene (TCE). Analytical aspects and isotope data from laboratory and field studies are discussed. The analytical tests showed that both headspace and SPME techniques provide accurate δ 13 C values with a similar precision for a wide range of chlorinated solvents. However, the SPME method is generally more sensitive. The microcosm experiments show that a significant isotopic fractionation occurs during dechlorination of PCE and TCE to ethene. The largest fractionation factors are observed in the steps DCE-VC and VC-Ethene. In general, the δ 13 C of each dechlorination product was always more negative than the δ 13 C of the corresponding precursor. In addition, the δ 13 C values of each compound increased with time. A similar pattern was observed for dechlorination of PCE at a field site. These results show that compound-specific carbon isotope ratios technology is a very sensitive tool for evaluation of natural attenuation of chlorinated solvents in groundwater. (author)

Calcium Isotope Analysis by Mass Spectrometry

Science.gov (United States)

Boulyga, S.; Richter, S.

2010-12-01

The variations in the isotopic composition of calcium caused by fractionation in heterogeneous systems and by nuclear reactions can provide insight into numerous biological, geological, and cosmic processes, and therefore isotopic analysis finds a wide spectrum of applications in cosmo- and geochemistry, paleoclimatic, nutritional, and biomedical studies. The measurement of calcium isotopic abundances in natural samples has challenged the analysts for more than three decades. Practically all Ca isotopes suffer from significant isobaric interferences, whereas low-abundant isotopes can be particularly affected by neighboring major isotopes. The extent of natural variations of stable isotopes appears to be relatively limited, and highly precise techniques are required to resolve isotopic effects. Isotope fractionation during sample preparation and measurements and instrumental mass bias can significantly exceed small isotope abundance variations in samples, which have to be investigated. Not surprisingly, a TIMS procedure developed by Russell et al. (Russell et al., 1978. Geochim Cosmochim Acta 42: 1075-1090) for Ca isotope measurements was considered as revolutionary for isotopic measurements in general, and that approach is used nowadays (with small modifications) for practically all isotopic systems and with different mass spectrometric techniques. Nevertheless, despite several decades of calcium research and corresponding development of mass spectrometers, the available precision and accuracy is still not always sufficient to achieve the challenging goals. This presentation discusses figures of merits of presently used analytical methods and instrumentation, and attempts to critically assess their limitations. Additionally, the availability of Ca isotope reference materials will be discussed.

Monitoring of the aerobe biodegradation of chlorinated organic solvents by stable isotope analysis

Science.gov (United States)

Horváth, Anikó; Futó, István; Palcsu, László

2014-05-01

Our chemical-biological basic research aims to eliminate chlorinated environmental contaminants from aquifers around industrial areas in the frame of research program supported by the European Social Fund (TÁMOP-4.2.2.A-11/1/KONV-2012-0043). The most careful and simplest way includes the in situ biodegradation with the help of cultured and compound specific strains. Numerous members of Pseudomonas bacteria are famous about function of bioremediation. They can metabolism the environmental hazardous chemicals like gas oils, dyes, and organic solvents. Our research based on the Pseudomonas putida F1 strain, because its ability to degrade halogenated hydrocarbons such as trichloroethylene. Several methods were investigated to estimate the rate of biodegradation, such as the measurement of the concentration of the pollutant along the contamination pathway, the microcosm's studies or the compound specific stable isotope analysis. In this area in the Transcarpathian basin we are pioneers in the stable isotope monitoring of biodegradation. The main goal is to find stable isotope fractionation factors by stable isotope analysis, which can help us to estimate the rate and effectiveness of the biodegradation. The subsequent research period includes the investigation of the method, testing its feasibility and adaptation in the environment. Last but not least, the research gives an opportunity to identify the producer of the contaminant based on the stable isotope composition of the contaminant.

Potential of isotope analysis (C, Cl) to identify dechlorination mechanisms

Science.gov (United States)

Cretnik, Stefan; Thoreson, Kristen; Bernstein, Anat; Ebert, Karin; Buchner, Daniel; Laskov, Christine; Haderlein, Stefan; Shouakar-Stash, Orfan; Kliegman, Sarah; McNeill, Kristopher; Elsner, Martin

2013-04-01

Chloroethenes are commonly used in industrial applications, and detected as carcinogenic contaminants in the environment. Their dehalogenation is of environmental importance in remediation processes. However, a detailed understanding frequently accounted problem is the accumulation of toxic degradation products such as cis-dichloroethylene (cis-DCE) at contaminated sites. Several studies have addressed the reductive dehalogenation reactions using biotic and abiotic model systems, but a crucial question in this context has remained open: Do environmental transformations occur by the same mechanism as in their corresponding in vitro model systems? The presented study shows the potential to close this research gap using the latest developments in compound specific chlorine isotope analysis, which make it possible to routinely measure chlorine isotope fractionation of chloroethenes in environmental samples and complex reaction mixtures.1,2 In particular, such chlorine isotope analysis enables the measurement of isotope fractionation for two elements (i.e., C and Cl) in chloroethenes. When isotope values of both elements are plotted against each other, different slopes reflect different underlying mechanisms and are remarkably insensitive towards masking. Our results suggest that different microbial strains (G. lovleyi strain SZ, D. hafniense Y51) and the isolated cofactor cobalamin employ similar mechanisms of reductive dechlorination of TCE. In contrast, evidence for a different mechanism was obtained with cobaloxime cautioning its use as a model for biodegradation. The study shows the potential of the dual isotope approach as a tool to directly compare transformation mechanisms of environmental scenarios, biotic transformations, and their putative chemical lab scale systems. Furthermore, it serves as an essential reference when using the dual isotope approach to assess the fate of chlorinated compounds in the environment.

Mercury speciation analysis in seafood by species-specific isotope dilution: method validation and occurrence data

Energy Technology Data Exchange (ETDEWEB)

Clemens, Stephanie; Guerin, Thierry [Agence Nationale de Securite Sanitaire de l' Alimentation, Laboratoire de Securite des Aliments de Maisons-Alfort, Unite des Contaminants Inorganiques et Mineraux de l' Environnement, ANSES, Maisons-Alfort (France); Monperrus, Mathilde; Donard, Olivier F.X.; Amouroux, David [IPREM UMR 5254 CNRS - Universite de Pau et des Pays de l' Adour, Laboratoire de Chimie Analytique Bio-Inorganique et Environnement, Institut des Sciences Analytiques et de Physico-chimie pour l' Environnement et les Materiaux, Pau Cedex (France)

2011-11-15

Methylmercury (MeHg) and total mercury (THg) in seafood were determined using species-specific isotope dilution analysis and gas chromatography combined with inductively coupled plasma mass spectrometry. Sample preparation methods (extraction and derivation step) were evaluated on certified reference materials using isotopically enriched Hg species. Solid-liquid extraction, derivation by propylation and automated agitation gave excellent accuracy and precision results. Satisfactory figures of merit for the selected method were obtained in terms of limit of quantification (1.2 {mu}g Hg kg{sup -1} for MeHg and 1.4 {mu}g Hg kg{sup -1} for THg), repeatability (1.3-1.7%), intermediate precision reproducibility (1.5% for MeHg and 2.2% for THg) and trueness (bias error less than 7%). By means of a recent strategy based on accuracy profiles ({beta}-expectation tolerance intervals), the selected method was successfully validated in the range of approximately 0.15-5.1 mg kg{sup -1} for MeHg and 0.27-5.2 mg kg{sup -1} for THg. Probability {beta} was set to 95% and the acceptability limits to {+-}15%. The method was then applied to 62 seafood samples representative of consumption in the French population. The MeHg concentrations were generally low (1.9-588 {mu}g kg{sup -1}), and the percentage of MeHg varied from 28% to 98% in shellfish and from 84% to 97% in fish. For all real samples tested, methylation and demethylation reactions were not significant, except in one oyster sample. The method presented here could be used for monitoring food contamination by MeHg and inorganic Hg in the future to more accurately assess human exposure. (orig.)

Reconstructing hydroclimatic variations using compound-specific hydrogen isotope analysis of biomarkers from a maar lake in the Central Highlands, Vietnam

Science.gov (United States)

Doiron, K. E.; Stevens, L. R.; Sauer, P. E.

2017-12-01

Monsoonal variation in Southeast Asia affects a significant portion of the global population, but knowledge regarding response of the monsoon system to changing boundary conditions is limited. The paleoclimatic tool of compound-specific isotope analysis(CSIA) provides the ability to reconstruct past precipitation using a diverse set of biomarkers preserved in the sedimentary record. Limited proxies in tropical southeast Asia and difficult site access have led to a deficit in paleoclimate records. Ia M'He (14°10'45" N, 107°52' E) is a shallow volcanic crater (maar) lake, approximately 57 ha, located in the Central Highlands of Vietnam. Precipitation in the Central Highlands is sensitive to reorganizations of major climatic features, such as the migration of the ITCZ and the coupled Indo-Asian monsoon, ENSO and related shifts in the Pacific Walker Circulation and typhoon frequency. To examine this complex behavior, this pilot study aims to provide a 500-year record of effective moisture inferred from CSIA of hydrogen isotopes on biomarkers. This study highlights the use of hydrogen isotopes of C28 n-alkanoic acid and dominant n-alkane chain lengths of C27 and C29, associated with terrestrial plant leaf waxes, as tracers for precipitation. The hydrogen isotope ratios of the plant wax components provide a proxy for paleo precipitation in a region where rainfall and droughts heavily influence population dynamics and create social discord. The CSIA record is expected to correlate with records from northern Vietnam, the South China Sea and Indonesia, with greater precipitation during the Little Ice Age. The CSIA data of terrestrial plant leaf waxes will be compared with secondary proxies including: diatoms, C/N and biogenic silica.

Isotopic Abundance and Chemical Purity Analysis of Stable Isotope Deuterium Labeled Sudan I

Directory of Open Access Journals (Sweden)

CAI Yin-ping;LEI Wen;ZHENG Bo;DU Xiao-ning

2014-02-01

Full Text Available It is important that to analysis of the isotopic abundance and chemical purity of Sudan I-D5, which is the internal standard of isotope dilution mass spectrometry. The isotopic abundance of Sudan I-D5 is detected by “mass cluster” classification method and LC-MS. The repeatability and reproducibility experiments were carried out by using different mass spectrometers and different operators. The RSD was less than 0.1%, so the repeatability and reproducibility were satisfactory. The accuracy and precision of the isotopic abundance analysis method was good with the results of F test and t test. The high performance liquid chromatography (HPLC had been used for detecting the chemical purity of Sudan I-D5 as external standard method.

Simultaneous speciation of mercury and butyltin compounds in natural waters and snow by propylation and species-specific isotope dilution mass spectrometry analysis

Energy Technology Data Exchange (ETDEWEB)

Monperrus, M.; Tessier, E.; Veschambre, S.; Amouroux, D.; Donard, O. [Universite de Pau et des Pays de L' Adour, Laboratoire de Chimie Analytique Bio-inorganique et Environnement, CNRS UMR 5034, Helioparc, Pau (France)

2005-02-01

A robust method has been developed for simultaneous determination of mercury and butyltin compounds in aqueous samples. This method is capable of providing accurate results for analyte concentrations in the picogram per liter to nanogram per liter range. The simultaneous determination of the mercury and tin compounds is achieved by species-specific isotope dilution, derivatization, and gas chromatography-inductively coupled plasma mass spectrometer (GC-ICP-MS). In derivatization by ethylation and propylation, reaction conditions such as pH and the effect of chloride were carefully studied. Ethylation was found to be more sensitive to matrix effects, especially for mercury compounds. Propylation was thus the preferred derivatization method for simultaneous determination of organomercury and organotin compounds in environmental samples. The analytical method is highly accurate and precise, with RSD values of 1 and 3% for analyte concentrations in the picogram per liter to nanogram per liter range. By use of cleaning procedures and SIDMS blank measurements, detection limits in the range 10-60 pg L{sup -1} were achieved; these are suitable for determination of background levels of these contaminants in environmental samples. This was demonstrated by using the method for analysis of real snow and seawater samples. This work illustrates the great advantage of species-specific isotope dilution for the validation of an analytical speciation method - the possibility of overcoming species transformations and non-quantitative recovery. Analysis time is saved by use of the simultaneous method, because of the use of a single sample-preparation procedure and one analysis. (orig.)

Study and validity of 13C stable carbon isotopic ratio analysis by mass spectrometry and 2H site-specific natural isotopic fractionation by nuclear magnetic resonance isotopic measurements to characterize and control the authenticity of honey

International Nuclear Information System (INIS)

Cotte, J.F.; Casabianca, H.; Lheritier, J.; Perrucchietti, C.; Sanglar, C.; Waton, H.; Grenier-Loustalot, M.F.

2007-01-01

Honey samples were analyzed by stable carbon isotopic ratio analysis by mass spectrometry (SCIRA-MS) and site-specific natural isotopic fractionation measured by nuclear magnetic resonance (SNIF-NMR) to first determine their potentials for characterizing the substance and then to combat adulteration. Honey samples from several geographic and botanical origins were analyzed. The δ 13 C parameter was not significant for characterizing an origin, while the (D/H) I ratio could be used to differentiate certain single-flower varieties. Application of the official control method of adding a C 4 syrup (AOAC official method 998.12) to our authentic samples revealed anomalies resulting from SCIRA indices that were more negative than -1 per mille (permil). A filtration step was added to the experimental procedure and provided results that were compliant with Natural origin of our honey samples. In addition, spiking with a C 4 syrup could be detected starting at 9-10%. The use of SNIF-NMR is limited by the detection of a syrup spike starting only at 20%, which is far from satisfying

Applications of stable isotope analysis in mammalian ecology.

Science.gov (United States)

Walter, W David; Kurle, Carolyn M; Hopkins, John B

2014-01-01

In this editorial, we provide a brief introduction and summarize the 10 research articles included in this Special Issue on Applications of stable isotope analysis in mammalian ecology. The first three articles report correction and discrimination factors that can be used to more accurately estimate the diets of extinct and extant mammals using stable isotope analysis. The remaining seven applied research articles use stable isotope analysis to address a variety of wildlife conservation and management questions from the oceans to the mountains.

Measurement of isotope abundance variations in nature by gravimetric spiking isotope dilution analysis (GS-IDA).

Science.gov (United States)

Chew, Gina; Walczyk, Thomas

2013-04-02

Subtle variations in the isotopic composition of elements carry unique information about physical and chemical processes in nature and are now exploited widely in diverse areas of research. Reliable measurement of natural isotope abundance variations is among the biggest challenges in inorganic mass spectrometry as they are highly sensitive to methodological bias. For decades, double spiking of the sample with a mix of two stable isotopes has been considered the reference technique for measuring such variations both by multicollector-inductively coupled plasma mass spectrometry (MC-ICPMS) and multicollector-thermal ionization mass spectrometry (MC-TIMS). However, this technique can only be applied to elements having at least four stable isotopes. Here we present a novel approach that requires measurement of three isotope signals only and which is more robust than the conventional double spiking technique. This became possible by gravimetric mixing of the sample with an isotopic spike in different proportions and by applying principles of isotope dilution for data analysis (GS-IDA). The potential and principle use of the technique is demonstrated for Mg in human urine using MC-TIMS for isotopic analysis. Mg is an element inaccessible to double spiking methods as it consists of three stable isotopes only and shows great potential for metabolically induced isotope effects waiting to be explored.

Isotope specific resolution recovery image reconstruction in high resolution PET imaging

OpenAIRE

Kotasidis Fotis A.; Kotasidis Fotis A.; Angelis Georgios I.; Anton-Rodriguez Jose; Matthews Julian C.; Reader Andrew J.; Reader Andrew J.; Zaidi Habib; Zaidi Habib; Zaidi Habib

2014-01-01

Purpose: Measuring and incorporating a scanner specific point spread function (PSF) within image reconstruction has been shown to improve spatial resolution in PET. However due to the short half life of clinically used isotopes other long lived isotopes not used in clinical practice are used to perform the PSF measurements. As such non optimal PSF models that do not correspond to those needed for the data to be reconstructed are used within resolution modeling (RM) image reconstruction usuall...

Stable isotope analysis

International Nuclear Information System (INIS)

Tibari, Elghali; Taous, Fouad; Marah, Hamid

2014-01-01

This report presents results related to stable isotopes analysis carried out at the CNESTEN DASTE in Rabat (Morocco), on behalf of Senegal. These analyzes cover 127 samples. These results demonstrate that Oxygen-18 and Deuterium in water analysis were performed by infrared Laser spectroscopy using a LGR / DLT-100 with Autosampler. Also, the results are expressed in δ values (‰) relative to V-SMOW to ± 0.3 ‰ for oxygen-18 and ± 1 ‰ for deuterium.

Origin of Xylitol in Chewing Gum: A Compound-Specific Isotope Technique for the Differentiation of Corn- and Wood-Based Xylitol by LC-IRMS.

Science.gov (United States)

Köster, Daniel; Wolbert, Jens-Benjamin; Schulte, Marcel S; Jochmann, Maik A; Schmidt, Torsten C

2018-02-28

The sugar replacement compound xylitol has gained increasing attention because of its use in many commercial food products, dental-hygiene articles, and pharmaceuticals. It can be classified by the origin of the raw material used for its production. The traditional "birch xylitol" is considered a premium product, in contrast to xylitol produced from agriculture byproducts such as corn husks or sugar-cane straw. Bulk stable-isotope analysis (BSIA) and compound-specific stable-isotope analysis (CSIA) by liquid-chromatography isotope-ratio mass spectrometry (LC-IRMS) of chewing-gum extracts were used to determine the δ 13 C isotope signatures for xylitol. These were applied to elucidate the original plant type the xylitol was produced from on the basis of differences in isotope-fractionation processes of photosynthetic CO 2 fixation. For the LC-IRMS analysis, an organic-solvent-free extraction protocol and HPLC method for the separation of xylitol from different artificial sweeteners and sugar-replacement compounds was successfully developed and applied to the analysis of 21 samples of chewing gum, from which 18 could be clearly related to the raw-material plant class.

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.

New Isotope Analysis Method: Atom Trap Mass Spectrometry

International Nuclear Information System (INIS)

Ko, Kwang Hoon; Park, Hyun Min; Han, Jae Min; Kim, Taek Soo; Cha, Yong Ho; Lim, Gwon; Jeong, Do Young

2011-01-01

Trace isotope analysis has been an important role in science, archaeological dating, geology, biology and nuclear industry. Some fission products such as Sr-90, Cs-135 and Kr-85 can be released to the environment when nuclear accident occurs and the reprocessing factory operates. Thus, the analysis of artificially produced radioactive isotopes has been of interest in nuclear industry. But it is difficult to detect them due to low natural abundance less then 10 -10 . In general, radio-chemical method has been applied to detect ultra-trace radio isotopes. But this method has disadvantages of long measurement time for long lived radioisotopes and toxic chemical process for the purification. The Accelerator Mass Spectrometer has high isotope selectivity, but the system is huge and its selectivity is affected by isobars. The laser based method, such as RIMS (Resonance Ionization Mass Spectrometry) has the advantage of isobar-effect free characteristics. But the system size is still huge for high isotope selective system. Recently, ATTA (Atom Trap Trace Analysis) has been successfully applied to detect ultra-trace isotope, Kr-81 and Kr-85. ATTA is the isobar-effect free detection with high isotope selectivity and the system size is small. However, it requires steady atomic beam source during detection, and is not allowed simultaneous detection of several isotopes. In this presentation, we introduce new isotope detection method which is a coupled method of Atom Trap Mass Spectrometry (ATMS). We expect that it can overcome the disadvantage of ATTA while it has both advantages of ATTA and mass spectrometer. The basic concept and the system design will be presented. In addition, the experimental status of ATMS will also be presented

Individual-specific transgenerational marking of fish populations based on a barium dual-isotope procedure.

Science.gov (United States)

Huelga-Suarez, Gonzalo; Moldovan, Mariella; Garcia-Valiente, America; Garcia-Vazquez, Eva; Alonso, J Ignacio Garcia

2012-01-03

The present study focuses on the development and evaluation of an individual-specific transgenerational marking procedure using two enriched barium isotopes, (135)Ba and (137)Ba, mixed at a given and selectable molar ratio. The method is based on the deconvolution of the isotope patterns found in the sample into four molar contribution factors: natural xenon (Xe nat), natural barium (Ba nat), Ba135, and Ba137. The ratio of molar contributions between Ba137 and Ba135 is constant and independent of the contribution of natural barium in the sample. This procedure was tested in brown trout ( Salmo trutta ) kept in captivity. Trout were injected with three different Ba137/Ba135 isotopic signatures ca. 7 months and 7 days before spawning to compare the efficiency of the marking procedure at long and short term, respectively. The barium isotopic profiles were measured in the offspring by means of inductively coupled plasma mass spectrometry. Each of the three different isotopic signatures was unequivocally identified in the offspring in both whole eggs and larvae. For 9 month old offspring, the characteristic barium isotope signatures could also be detected in the otoliths even in the presence of a high and variable amount of barium of natural isotope abundance. In conclusion, it can be stated that the proposed dual-isotope marking is inheritable and can be detected after both long-term and short-term marking. Furthermore, the dual-isotope marking can be made individual-specific, so that it allows identification of offspring from a single individual or a group of individuals within a given fish group. © 2011 American Chemical Society

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

Stable isotope analysis in primatology: a critical review.

Science.gov (United States)

Sandberg, Paul A; Loudon, James E; Sponheimer, Matt

2012-11-01

Stable isotope analysis has become an important tool in ecology over the last 25 years. A wealth of ecological information is stored in animal tissues in the relative abundances of the stable isotopes of several elements, particularly carbon and nitrogen, because these isotopes navigate through ecological processes in predictable ways. Stable carbon and nitrogen isotopes have been measured in most primate taxonomic groups and have yielded information about dietary content, dietary variability, and habitat use. Stable isotopes have recently proven useful for addressing more fine-grained questions about niche dynamics and anthropogenic effects on feeding ecology. Here, we discuss stable carbon and nitrogen isotope systematics and critically review the published stable carbon and nitrogen isotope data for modern primates with a focus on the problems and prospects for future stable isotope applications in primatology. © 2012 Wiley Periodicals, Inc.

Pyrolysis compound specific isotopic analysis (δ13C and δD Py-CSIA) of soil organic matter size fractions under four vegetation covers.

Science.gov (United States)

Jiménez-Morillo, Nicasio T.; González-Vila, Francisco J.; Almendros, Gonzalo; De la Rosa, José M.; González-Pérez, José A.

2015-04-01

A chemical characterization of soil organic matter (SOM) under different ground cover from a Mediterranean climate (Doñana National Park, Andalusia, Spain) is approached using bulk δ15N, δ13C, δ18O and δD isotopic analysis (C/TC-IRMS) and δ13C and δD pyrolysis compound specific isotopic analysis (Py-CSIA: Py-GC-C/TC-IRMS). Soil samples were collected in sandy soils, Arenosols (WRB 2006) from the Doñana National Park (SW Spain) under different vegetation cover: cork oak (Quercus suber, QS), eagle fern (Pteridium aquilinum, PA), pine (Pinus pinea, PP) and rockrose (Halimium halimifolium, HH). Two size fractions; coarse (C: 1-2 mm) and fine (F: studied from each soil. A complete conventional analytical pyrolysis (Py-GC/MS) of these samples have been studied in detail (Jiménez-Morillo et al., 2015). Bulk isotopic analysis of stable light elements (δ15N, δ13C, δ18O and δD) revealed particular isotopic signatures showing differences related with the main vegetation cover and the different soil size fraction. All samples had a carbon isotopic signature between -26 and -29 ‰, which indicated that the organic matter in the two fractions of each soil sample derived from C3-type plants. The bulk δD isotopic signature in whole soil sample indicate a lower deuterium fractionation occurs in SOM under arboreal than under no-arboreal vegetation, this can be caused by the occurrence of a higher water evaporation rate under bush vegetation and/or to differences due to leaf morphology as previously described (Leaney et al., 1985). A δ15N vs. δ18O chart may provide some clues about N origin in the soil and particularly about the original source of nitrates (Kendall et al., 1996). In in all sample and size fractions our values are in the chart area corresponding to NO3 in precipitation, with lighter δ18O (c. 20 ‰) values compatible with fertilizers may be from adjacent crops. In addition we were able to assign δ13C and δD values for a number of specific SOM

Tracking transformation processes of organic micropollutants in aquatic environments using multi-element isotope fractionation analysis

International Nuclear Information System (INIS)

Hofstetter, Thomas B.; Bolotin, Jakov; Skarpeli-Liati, Marita; Wijker, Reto; Kurt, Zohre; Nishino, Shirley F.; Spain, Jim C.

2011-01-01

The quantitative description of enzymatic or abiotic transformations of man-made organic micropollutants in rivers, lakes, and groundwaters is one of the major challenges associated with the risk assessment of water resource contamination. Compound-specific isotope analysis enables one to identify (bio)degradation pathways based on changes in the contaminants' stable isotope ratios even if multiple reactive and non-reactive processes cause concentrations to decrease. Here, we investigated how the magnitude and variability of isotope fractionation in some priority pollutants is determined by the kinetics and mechanisms of important enzymatic and abiotic redox reactions. For nitroaromatic compounds and substituted anilines, we illustrate that competing transformation pathways can be assessed via trends of N and C isotope signatures.

The CSSIAR v.1.00 Software: A new tool based on SIAR to assess soil redistribution using Compound Specific Stable Isotopes

Directory of Open Access Journals (Sweden)

de los Santos-Villalobos Sergio

2017-01-01

Full Text Available Soil erosion is one of the biggest challenges for food production around the world. Many techniques have been used to evaluate and mitigate soil degradation. Nowadays isotopic techniques are becoming a powerful tool to assess soil apportionment. One of the innovative techniques used is the Compound Specific Stable Isotopes (CSSI analysis, which has been used to track down sediments and specify their sources by the isotopic signature of δ13C in specific fatty acids. The application of this technique on soil apportionment has been recently developed, however there is a lack of user-friendly Software for data processing and interpretation. The aim of this article is to introduce a new open source tool for working with data sets generated by the use of the CSSI technique to assess soil apportionment, called the CSSIARv1.00 Software

The CSSIAR v.1.00 Software: A new tool based on SIAR to assess soil redistribution using Compound Specific Stable Isotopes

Science.gov (United States)

Sergio, de los Santos-Villalobos; Claudio, Bravo-Linares; dos Anjos Roberto, Meigikos; Renan, Cardoso; Max, Gibbs; Andrew, Swales; Lionel, Mabit; Gerd, Dercon

Soil erosion is one of the biggest challenges for food production around the world. Many techniques have been used to evaluate and mitigate soil degradation. Nowadays isotopic techniques are becoming a powerful tool to assess soil apportionment. One of the innovative techniques used is the Compound Specific Stable Isotopes (CSSI) analysis, which has been used to track down sediments and specify their sources by the isotopic signature of δ13 C in specific fatty acids. The application of this technique on soil apportionment has been recently developed, however there is a lack of user-friendly Software for data processing and interpretation. The aim of this article is to introduce a new open source tool for working with data sets generated by the use of the CSSI technique to assess soil apportionment, called the CSSIARv1.00 Software

Compound-Specific Isotope Analysis (CSIA Application for Source Apportionment and Natural Attenuation Assessment of Chlorinated Benzenes

Directory of Open Access Journals (Sweden)

Luca Alberti

2017-11-01

Full Text Available In light of the complex management of chlorobenzene (CB contaminated sites, at which a hydraulic barrier (HB for plumes containment is emplaced, compound-specific stable isotope analysis (CSIA has been applied for source apportionment, for investigating the relation between the upgradient and downgradient of the HB, and to target potential CB biodegradation processes. The isotope signature of all the components potentially involved in the degradation processes has been expressed using the concentration-weighted average δ13C of CBs + benzene (δ13Csum. Upgradient of the HB, the average δ13Csum of −25.6‰ and −29.4‰ were measured for plumes within the eastern and western sectors, respectively. Similar values were observed for the potential sources, with δ13Csum values of −26.5‰ for contaminated soils and −29.8‰ for the processing water pipeline in the eastern and western sectors, respectively, allowing for apportioning of these potential sources to the respective contaminant plumes. For the downgradient of the HB, similar CB concentrations but enriched δ13Csum values between −24.5‰ and −25.9‰ were measured. Moreover, contaminated soils showed a similar δ13Csum signature of −24.5‰, thus suggesting that the plumes likely originate from past activities located in the downgradient of the HB. Within the industrial property, significant δ13C enrichments were measured for 1,2,4-trichlorobenzene (TCB, 1,2-dichlorobenzene (DCB, 1,3-DCB, and 1,4-DCBs, thus suggesting an important role for anaerobic biodegradation. Further degradation of monochlorobenzene (MCB and benzene was also demonstrated. CSIA was confirmed to be an effective approach for site characterization, revealing the proper functioning of the HB and demonstrating the important role of natural attenuation processes in reducing the contamination upgradient of the HB.

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

Stable isotope analysis indicates a lack of inter- and intra-specific dietary redundancy among ecologically important coral reef fishes

Science.gov (United States)

Plass-Johnson, J. G.; McQuaid, C. D.; Hill, J. M.

2013-06-01

Parrotfish are critical consumers on coral reefs, mediating the balance between algae and corals, and are often categorised into three functional groups based on adult morphology and feeding behaviour. We used stable isotope analysis (δ13C, δ15N) to investigate size-related ontogenetic dietary changes in multiple species of parrotfish on coral reefs around Zanzibar. We compared signatures among species and functional groups (scrapers, excavators and browsers) as well as ontogenetic stages (immature, initial and terminal phase) within species. Stable isotope analysis suggests that ontogenetic dietary shifts occurred in seven of the nine species examined; larger individuals had enriched δ13C values, with no relationship between size and δ15N. The relationship between fish length and δ13C signature was maintained when species were categorised as scrapers and excavators, but was more pronounced for scrapers than excavators, indicating stronger ontogenetic changes. Isotopic mixing models classified the initial phase of both the most abundant excavator ( Chlorurus sordidus) as a scraper and the immature stage of the scraper Scarus ghobban (the largest species) as an excavator, indicating that diet relates to size rather than taxonomy. The results indicate that parrotfish may show similar intra-group changes in diet with length, but that their trophic ecology is more complex than suggested by morphology alone. Stable isotope analyses indicate that feeding ecology may differ among species within functional groups, and according to ontogenetic stage within a species.

Isotope analysis of lithium by thermionic mass spectrometry

International Nuclear Information System (INIS)

Kakazu, M.H.; Sarkis, J.E.S.

1991-04-01

An analytical mass spectrometric method for the isotope analysis of lithium has been studied. The analysis were carried out by using a single focusing thermoionic mass spectrometer Varian Mat TH5 with 90 sup(0) magnetic sector field and 21.4 cm deflection radius, equipped with a dual Re-filament thermal ionization ion source. The effect of different lithium chemical forms, such as, carbonate, chloride, nitrate and sulfate upon the isotopic ratios sup(6)Li/ sup(7)Li has been studied. Isotopic fractionation of lithium was studied in terms of the time of analysis. The results obtained with lithium carbonate yielded a precision of ±0.1% and an accuracy of ± 0.6%, whereas with other chemical forms yielded precisions of ±0.5% and accuracies of ±2%. A fractionation correction factor, K=1.005, was obtained for different samples of lithium carbonate isotopic standard CBNM IRM 016, which has been considered constant. (author)

Basic methods of isotope analysis; Osnovnye metody analiza izotopov

Energy Technology Data Exchange (ETDEWEB)

Ochkin, A V; Rozenkevich, M B

2000-07-01

The bases of the most applied methods of the isotope analysis are briefly presented. The possibilities and analytical characteristics of the mass-spectrometric, spectral, radiochemical and special methods of the isotope analysis, including application of the magnetic resonance, chromatography and refractometry, are considered.

Application of compound specific 13C isotope investigations of chlorinated hydrocarbons in contaminated groundwaters

International Nuclear Information System (INIS)

Osenbrueck, K.; Heidinger, M.; Voropaev, A.; Ertl, S.; Eichinger, L.

2002-01-01

Full text: Chlorinated hydrocarbons are one of the most common pollutants found in groundwater. Due to complex contamination situations with overlapping contamination plumes the assessment of the organic contaminants requires the installation of expensive observation wells and high analytical effort. Here the determination of the stable isotope ratio 13 C/ 12 C of the organic compounds offers a promising and efficient tool to investigate the origin and the biodegradation characteristics of the chlorinated hydrocarbons in groundwater. The application of the method is based on characteristic isotope fingerprints, differing in chlorinated solvents. This isotope fingerprint is derived from different production pathways and is not influenced by transport or by retardation processes in the underground. Due to the fact, that two different contaminations can easily be distinguished by isotope ratios, an improved distinction of spatially and temporally different contamination plumes might be possible. In course of biologically mediated degradation processes a shift of the isotope ratios between the precursor and the product can frequently be observed, such as with denitrification or sulfate reduction processes. The isotope fractionation is due to a preferential reaction of the bonds formed by the lighter isotopes and leads to a progressive enrichment of the heavy isotopes in the precursor while the product becomes depleted in the heavy isotopes. Biological degradation of the highly chlorinated hydrocarbons is due to a co-metabolic dechlorinisation. Tetrachloroethene (PCE) for example degrades under anoxic conditions via trichloroethene (TCE) to cis-1,2-dichloroethene (cDCE). Subsequent degradation to vinyl chloride (VC) and ethene may appear under aerobic as well as reducing environments depending on the site specific conditions. In several laboratory studies it has been shown, that biodegradation of the chlorinated hydrocarbons is accompanied by an isotope fractionation of

Isotope analysis in petroleum exploration

International Nuclear Information System (INIS)

Rodrigues, R.

1982-01-01

The study about isotopic analysis in petroleum exploration performed at Petrobras Research Center is showed. The results of the petroleum recuperation in same Brazilian basin and shelves are comented. (L.H.L.L.) [pt

Analysis of barium by isotope mass spectrometry

International Nuclear Information System (INIS)

Long Kaiming; Jia Baoting; Liu Xuemei

2004-01-01

The isotopic abundance ratios for barium at sub-microgram level are analyzed by thermal surface ionization mass spectrometry (TIMS). Rhenium trips used for sample preparation are firstly treated to eliminate possible barium background interference. During the preparation of barium samples phosphoric acid is added as an emitting and stabilizing reagent. The addition of phosphoric acid increases the collection efficiency and ion current strength and stability for barium. A relative standard deviation of 0.02% for the isotopic abundance ratio of 137 Ba to 138 Ba is achieved when the 138 Ba ion current is (1-3) x 10 -12 A. The experimental results also demonstrate that the isotope fractionation effect is negligibly small in the isotopic analysis of barium

Congener-specific accumulation and trophic transfer of polychlorinated biphenyls in spider crab food webs revealed by stable isotope analysis

Energy Technology Data Exchange (ETDEWEB)

Bodin, N. [IFREMER, DCN-BE, Technopole Brest-Iroise, Pointe du Diable, 29280 Plouzane (France); LPTC-UMR 5472 CNRS, Universite de Bordeaux 1, 351 cours de la Liberation, 33400 Talence (France)], E-mail: bodin.nathalie@caramail.com; Le Loc' h, F. [IRD, UR 070 RAP, Centre de Recherche Halieutique, Avenue Jean Monnet, B.P. 171, 34203 Sete Cedex (France); Caisey, X.; Le Guellec, A.-M.; Abarnou, A.; Loizeau, V. [IFREMER, DCN-BE, Technopole Brest-Iroise, Pointe du Diable, 29280 Plouzane (France); Latrouite, D. [IFREMER, DCB-STH, Technopole Brest-Iroise, Pointe du Diable, 29280 Plouzane (France)

2008-01-15

Polychlorobiphenyls (PCB) and stable isotopes ({delta}{sup 15}N and {delta}{sup 13}C) were analyzed in the spider crab (Maja brachydactyla) food web from the Iroise Sea (Western Brittany) and the Seine Bay (Eastern English Channel). PCB concentrations were all significantly higher in organisms from the Seine Bay than those from the Iroise Sea. PCB patterns were strongly related to the feeding mode of the species, and increased influence of higher chlorinated congeners was highlighted with trophic position of the organisms. PCB concentrations (lipid normalized) were significantly related to the isotopically derived trophic level (TL) in spider crab food webs. The highest trophic magnification factors (TMFs) were calculated for the congeners with 2,4,5-substitution, and were lower in the Seine Bay compared to the Iroise Sea. The confrontation of PCB and TL data also revealed biotransformation capacity of decapod crustaceans for specific congeners based on structure-activity relations. - The influence of feeding mode and trophic position on the fate of PCBs in spider crab food webs is discussed by using a stable isotopic approach.

Branched GDGTs in Lacustrine Environments: Tracing Allochthonous and Autochthonous Sources Using Compound-Specific Stable Carbon Isotope Analysis

Science.gov (United States)

Weber, Y.; S Sinninghe Damsté, J.; Lehmann, M. F.; Niemann, H.; Schubert, C. J.

2015-12-01

allochthonous (i.e., soil) source. Our data demonstrate the great potential of compound-specific C isotope analysis to constrain the origin of brGDGTs in lake sediments, possibly allowing the identification of freshwater environments that are particularly suited for brGDGT-based paleoenvironmental reconstructions.

Using stable isotope analysis to discriminate gasoline on the basis of its origin.

Science.gov (United States)

Heo, Su-Young; Shin, Woo-Jin; Lee, Sin-Woo; Bong, Yeon-Sik; Lee, Kwang-Sik

2012-03-15

Leakage of gasoline and diesel from underground tanks has led to a severe environmental problem in many countries. Tracing the production origin of gasoline and diesel is required to enable the development of dispute resolution and appropriate remediation strategies for the oil-contaminated sites. We investigated the bulk and compound-specific isotopic compositions of gasoline produced by four oil companies in South Korea: S-Oil, SK, GS and Hyundai. The relative abundance of several compounds in gasoline was determined by the peak height of the major ion (m/z 44). The δ(13)C(Bulk) and δD(Bulk) values of gasoline produced by S-Oil were significantly different from those of SK, GS and Hyundai. In particular, the compound-specific isotopic value (δ(13)C(CSIA)) of methyl tert-butyl ether (MTBE) in S-Oil gasoline was significantly lower than that of gasoline produced by other oil companies. The abundance of several compounds in gasoline, such as n-pentane, MTBE, n-hexane, toluene, ethylbenzene and o-xylene, differed widely among gasoline from different oil companies. This study shows that gasoline can be forensically discriminated according to the oil company responsible for its manufacture using stable isotope analysis combined with multivariate statistical analysis. Copyright © 2012 John Wiley & Sons, Ltd.

Optical spectroscopy of laser-produced plasmas for standoff isotopic analysis

Science.gov (United States)

Harilal, S. S.; Brumfield, B. E.; LaHaye, N. L.; Hartig, K. C.; Phillips, M. C.

2018-06-01

Rapid, in-field, and non-contact isotopic analysis of solid materials is extremely important to a large number of applications, such as nuclear nonproliferation monitoring and forensics, geochemistry, archaeology, and biochemistry. Presently, isotopic measurements for these and many other fields are performed in laboratory settings. Rapid, in-field, and non-contact isotopic analysis of solid material is possible with optical spectroscopy tools when combined with laser ablation. Laser ablation generates a transient vapor of any solid material when a powerful laser interacts with a sample of interest. Analysis of atoms, ions, and molecules in a laser-produced plasma using optical spectroscopy tools can provide isotopic information with the advantages of real-time analysis, standoff capability, and no sample preparation requirement. Both emission and absorption spectroscopy methods can be used for isotopic analysis of solid materials. However, applying optical spectroscopy to the measurement of isotope ratios from solid materials presents numerous challenges. Isotope shifts arise primarily due to variation in nuclear charge distribution caused by different numbers of neutrons, but the small proportional nuclear mass differences between nuclei of various isotopes lead to correspondingly small differences in optical transition wavelengths. Along with this, various line broadening mechanisms in laser-produced plasmas and instrumental broadening generated by the detection system are technical challenges frequently encountered with emission-based optical diagnostics. These challenges can be overcome by measuring the isotope shifts associated with the vibronic emission bands from molecules or by using the techniques of laser-based absorption/fluorescence spectroscopy to marginalize the effect of instrumental broadening. Absorption and fluorescence spectroscopy probe the ground state atoms existing in the plasma when it is cooler, which inherently provides narrower

Essentials of iron, chromium, and calcium isotope analysis of natural materials by thermal ionization mass spectrometry

Science.gov (United States)

Fantle, M.S.; Bullen, T.D.

2009-01-01

The use of isotopes to understand the behavior of metals in geological, hydrological, and biological systems has rapidly expanded in recent years. One of the mass spectrometric techniques used to analyze metal isotopes is thermal ionization mass spectrometry, or TIMS. While TIMS has been a useful analytical technique for the measurement of isotopic composition for decades and TIMS instruments are widely distributed, there are significant difficulties associated with using TIMS to analyze isotopes of the lighter alkaline earth elements and transition metals. Overcoming these difficulties to produce relatively long-lived and stable ion beams from microgram-sized samples is a non-trivial task. We focus here on TIMS analysis of three geologically and environmentally important elements (Fe, Cr, and Ca) and present an in-depth look at several key aspects that we feel have the greatest potential to trouble new users. Our discussion includes accessible descriptions of different analytical approaches and issues, including filament loading procedures, collector cup configurations, peak shapes and interferences, and the use of isotopic double spikes and related error estimation. Building on previous work, we present quantitative simulations, applied specifically in this study to Fe and Ca, that explore the effects of (1) time-variable evaporation of isotopically homogeneous spots from a filament and (2) interferences on the isotope ratios derived from a double spike subtraction routine. We discuss how and to what extent interferences at spike masses, as well as at other measured masses, affect the double spike-subtracted isotope ratio of interest (44Ca/40Ca in the case presented, though a similar analysis can be used to evaluate 56Fe/54Fe and 53Cr/52Cr). The conclusions of these simulations are neither intuitive nor immediately obvious, making this examination useful for those who are developing new methodologies. While all simulations are carried out in the context of a

Calculation of radiation production of high specific activity isotopes 192Ir and 60Co

International Nuclear Information System (INIS)

Zhou Quan; Zhong Wenfa; Xu Xiaolin

1997-01-01

The high specific activity isotopes: 192 Ir and 60 Co in the high neutron flux reactor are calculated with the method of reactor physics. The results of calculation are analyzed in two aspects: the production of isotopes and the influence to parameters of the reactor, and hence a better case is proposed as a reference to the production

Assessing connectivity of estuarine fishes based on stable isotope ratio analysis

Science.gov (United States)

Herzka, Sharon Z.

2005-07-01

Assessing connectivity is fundamental to understanding the population dynamics of fishes. I propose that isotopic analyses can greatly contribute to studies of connectivity in estuarine fishes due to the high diversity of isotopic signatures found among estuarine habitats and the fact that variations in isotopic composition at the base of a food web are reflected in the tissues of consumers. Isotopic analysis can be used for identifying nursery habitats and estimating their contribution to adult populations. If movement to a new habitat is accompanied by a shift to foods of distinct isotopic composition, recent immigrants and residents can be distinguished based on their isotopic ratios. Movement patterns thus can be reconstructed based on information obtained from individuals. A key consideration is the rate of isotopic turnover, which determines the length of time that an immigrant to a given habitat will be distinguishable from a longtime resident. A literature survey indicated that few studies have measured turnover rates in fishes and that these have focused on larvae and juveniles. These studies reveal that biomass gain is the primary process driving turnover rates, while metabolic turnover is either minimal or undetectable. Using a simple dilution model and biomass-specific growth rates, I estimated that young fishes with fast growth rates will reflect the isotopic composition of a new diet within days or weeks. Older or slower-growing individuals may take years or never fully equilibrate. Future studies should evaluate the factors that influence turnover rates in fishes during various stages of the life cycle and in different tissues, as well as explore the potential for combining stable isotope and otolith microstructure analyses to examine the relationship between demographic parameters, movement and connectivity.

Advanced concepts for gamma-ray isotopic analysis and instrumentation

International Nuclear Information System (INIS)

Buckley, W.M.; Carlson, J.B.

1994-07-01

The Safeguards Technology Program at the Lawrence Livermore National Laboratory is developing actinide isotopic analysis technologies in response to needs that address issues of flexibility of analysis, robustness of analysis, ease-of-use, automation and portability. Recent developments such as the Intelligent Actinide Analysis System (IAAS), begin to address these issues. We are continuing to develop enhancements on this and other instruments that improve ease-of-use, automation and portability. Requests to analyze samples with unusual isotopics, contamination, or containers have made us aware of the need for more flexible and robust analysis. We have modified the MGA program to extend its plutonium isotopic analysis capability to samples with greater 241 Am content or U isotopics. We are looking at methods for dealing with tantalum or lead contamination and contamination with high-energy gamma emitters, such as 233 U. We are looking at ways to allow the program to use additional information about the sample to further extend the domain of analyzable samples. These unusual analyses will come from the domain of samples that need to be measured because of complex reconfiguration or environmental cleanup

Compound-specific isotopic analyses: a novel tool for reconstruction of ancient biogeochemical processes

Science.gov (United States)

Hayes, J. M.; Freeman, K. H.; Popp, B. N.; Hoham, C. H.

1990-01-01

Patterns of isotopic fractionation in biogeochemical processes are reviewed and it is suggested that isotopic fractionations will be small when substrates are large. If so, isotopic compositions of biomarkers will reflect those of their biosynthetic precursors. This prediction is tested by consideration of results of analyses of geoporphyrins and geolipids from the Greenhorn Formation (Cretaceous, Western Interior Seaway of North America) and the Messel Shale (Eocene, lacustrine, southern Germany). It is shown (i) that isotopic compositions of porphyrins that are related to a common source, but which have been altered structurally, cluster tightly and (ii) that isotopic differences between geolipids and porphyrins related to a common source are equal to those observed in modern biosynthetic products. Both of these observations are consistent with preservation of biologically controlled isotopic compositions during diagenesis. Isotopic compositions of individual compounds can thus be interpreted in terms of biogeochemical processes in ancient depositional environments. In the Cretaceous samples, isotopic compositions of n-alkanes are covariant with those of total organic carbon, while delta values for pristane and phytane are covariant with those of porphyrins. In this unit representing an open marine environment, the preserved acyclic polyisoprenoids apparently derive mainly from primary material, while the extractable, n-alkanes derive mainly from lower levels of the food chain. In the Messel Shale, isotopic compositions of individual biomarkers range from -20.9 to -73.4% vs PDB. Isotopic compositions of specific compounds can be interpreted in terms of origin from methylotrophic, chemautotrophic, and chemolithotrophic microorganisms as well as from primary producers that lived in the water column and sediments of this ancient lake.

Ion Mobility Mass Spectrometry Direct Isotope Abundance Analysis

International Nuclear Information System (INIS)

Manard, Manuel J.; Weeks, Stephan; Kyle, Kevin

2010-01-01

The nuclear forensics community is currently engaged in the analysis of illicit nuclear or radioactive material for the purposes of non-proliferations and attribution. One technique commonly employed for gathering nuclear forensics information is isotope analysis. At present, the state-of-the-art methodology for obtaining isotopic distributions is thermal ionization mass spectrometry (TIMS). Although TIMS is highly accurate at determining isotope distributions, the technique requires an elementally pure sample to perform the measurement. The required radiochemical separations give rise to sample preparation times that can be in excess of one to two weeks. Clearly, the nuclear forensics community is in need of instrumentation and methods that can expedite their decision making process in the event of a radiological release or nuclear detonation. Accordingly, we are developing instrumentation that couples a high resolution IM drift cell to the front end of a MS. The IM cell provides a means of separating ions based upon their collision cross-section and mass-to-charge ratio (m/z). Two analytes with the same m/z, but with different collision cross-sections (shapes) would exit the cell at different times, essentially enabling the cell to function in a similar manner to a gas chromatography (GC) column. Thus, molecular and atomic isobaric interferences can be effectively removed from the ion beam. The mobility selected chemical species could then be introduced to a MS for high-resolution mass analysis to generate isotopic distributions of the target analytes. The outcome would be an IM/MS system capable of accurately measuring isotopic distributions while concurrently eliminating isobaric interferences and laboratory radiochemical sample preparation. The overall objective of this project is developing instrumentation and methods to produce near real-time isotope distributions with a modular mass spectrometric system that performs the required gas-phase chemistry and

A Paleoevaporation Proxy Using Compound Specific Stable Isotope Measurements from Peatland Biomarkers

Science.gov (United States)

Wang, J.; Nichols, J. E.; Huang, Y.

2009-12-01

It is important to understand how evaporation from wetlands changes with climate. To do this, we have developed a paleoevaporation proxy for use in ombrotrophic peatland sediments. Using compound specific hydrogen isotopic ratios of vascular plant and Sphagnum biomarkers, we can quantitatively reconstruct past changes in evaporation. The contrast in H isotopic ratios of water available to living Sphagnum and water in the acrotelm can be used to estimate “f”—the fraction of water remaining after evaporation. Vascular plant leaf waxes record H isotopic ratios of precipitation which is little affected by evaporation, whereas the Sphagnum biomarker, C23 n-alkane, records H isotopic ratios of the water inside its cells and between its leaves, which is strongly affected by evaporation at the bog surface. Evaporation changes can then be calculated with the H-isotopic ratios of the two types of biomarkers. We calibrated the apparent fractionation of D/H ratios from source water to C23 n-alkane with lab-grown Sphagnum. We also present several reconstructions of paleoevaporation from peatlands throughout eastern North America. By comparison with overall hydrologic balance, we are able to understand the varying role of evaporation in the hydrologic system in both time and space.

Amino acid compositions in heated carbonaceous chondrites and their compound-specific nitrogen isotopic ratios

Science.gov (United States)

Chan, Queenie Hoi Shan; Chikaraishi, Yoshito; Takano, Yoshinori; Ogawa, Nanako O.; Ohkouchi, Naohiko

2016-01-01

A novel method has been developed for compound-specific nitrogen isotope compositions with an achiral column which was previously shown to offer high precision for nitrogen isotopic analysis. We applied the method to determine the amino acid contents and stable nitrogen isotopic compositions of individual amino acids from the thermally metamorphosed (above 500 °C) Antarctic carbonaceous chondrites Ivuna-like (CI)1 (or CI-like) Yamato (Y) 980115 and Ornans-like (CO)3.5 Allan Hills (ALH) A77003 with the use of gas chromatography/combustion/isotope ratio mass spectrometry. ALHA77003 was deprived of amino acids due to its extended thermal alteration history. Amino acids were unambiguously identified in Y-980115, and the δ15N values of selected amino acids (glycine +144.8 ‰; α-alanine +121.2 ‰) are clearly extraterrestrial. Y-980115 has experienced an extended period of aqueous alteration as indicated by the presence of hydrous mineral phases. It has also been exposed to at least one post-hydration short-lived thermal metamorphism. Glycine and alanine were possibly produced shortly after the accretion event of the asteroid parent body during the course of an extensive aqueous alteration event and have abstained from the short-term post-aqueous alteration heating due to the heterogeneity of the parent body composition and porosity. These carbonaceous chondrite samples are good analogs that offer important insights into the target asteroid Ryugu of the Hayabusa-2 mission, which is a C-type asteroid likely composed of heterogeneous materials including hydrated and dehydrated minerals.

Selective laser ionization for mass-spectral isotopic analysis

International Nuclear Information System (INIS)

Miller, C.M.; Nogar, N.S.; Downey, S.W.

1983-01-01

Resonant enhancement of the ionization process can provide a high degree of elemental selectivity, thus eliminating or drastically reducing the interference problem. In addition, extension of this method to isotopically selective ionization has the potential for greatly increasing the range of isotope ratios that can be determined experimentally. This gain can be realized by reducing or eliminating the tailing of the signal from the high-abundance isotope into that of the low-abundance isotope, augmenting the dispersion of the mass spectrometer. We briefly discuss the hardware and techniques used in both our pulsed and cw RIMS experiments. Results are presented for both cw ionization experiments on Lu/Yb mixtures, and spectroscopic studies of multicolor RIMS of Tc. Lastly, we discuss practical limits of cw RIMS analysis in terms of detection limits and measurable isotope ratios

Development of a code for the isotopic analysis of Uranium

Energy Technology Data Exchange (ETDEWEB)

Kim, J. H.; Kang, M. Y.; Kim, Jinhyeong; Choi, H. D. [Seoul National Univ., Seoul (Korea, Republic of)

2013-05-15

To strengthen the national nuclear nonproliferation regime by an establishment of nuclear forensic system, the techniques for nuclear material analysis and the categorization of important domestic nuclear materials are being developed. MGAU and FRAM are commercial software for the isotopic analysis of Uranium by using γ-spectroscopy, but the diversity of detection geometry and some effects - self attenuation, coincidence summing, etc. - suggest an analysis tool under continual improvement and modification. Hence, developing another code for HPGe γ- and x-ray spectrum analysis is started in this study. The analysis of the 87-101 keV region of Uranium spectrum is attempted based on the isotopic responses similar to those developed in MGAU. The code for isotopic analysis of Uranium is started from a fitting.

Enhanced understanding of ectoparasite: host trophic linkages on coral reefs through stable isotope analysis

Science.gov (United States)

Demopoulos, Amanda W. J.; Sikkel, Paul C.

2015-01-01

Parasitism, although the most common type of ecological interaction, is usually ignored in food web models and studies of trophic connectivity. Stable isotope analysis is widely used in assessing the flow of energy in ecological communities and thus is a potentially valuable tool in understanding the cryptic trophic relationships mediated by parasites. In an effort to assess the utility of stable isotope analysis in understanding the role of parasites in complex coral-reef trophic systems, we performed stable isotope analysis on three common Caribbean reef fish hosts and two kinds of ectoparasitic isopods: temporarily parasitic gnathiids (Gnathia marleyi) and permanently parasitic cymothoids (Anilocra). To further track the transfer of fish-derived carbon (energy) from parasites to parasite consumers, gnathiids from host fish were also fed to captive Pederson shrimp (Ancylomenes pedersoni) for at least 1 month. Parasitic isopods had δ13C and δ15N values similar to their host, comparable with results from the small number of other host–parasite studies that have employed stable isotopes. Adult gnathiids were enriched in 15N and depleted in13C relative to juvenile gnathiids, providing insights into the potential isotopic fractionation associated with blood-meal assimilation and subsequent metamorphosis. Gnathiid-fed Pedersen shrimp also had δ13C values consistent with their food source and enriched in 15N as predicted due to trophic fractionation. These results further indicate that stable isotopes can be an effective tool in deciphering cryptic feeding relationships involving parasites and their consumers, and the role of parasites and cleaners in carbon transfer in coral-reef ecosystems specifically.

Enhanced understanding of ectoparasite–host trophic linkages on coral reefs through stable isotope analysis

Directory of Open Access Journals (Sweden)

Amanda W.J. Demopoulos

2015-04-01

Full Text Available Parasitism, although the most common type of ecological interaction, is usually ignored in food web models and studies of trophic connectivity. Stable isotope analysis is widely used in assessing the flow of energy in ecological communities and thus is a potentially valuable tool in understanding the cryptic trophic relationships mediated by parasites. In an effort to assess the utility of stable isotope analysis in understanding the role of parasites in complex coral-reef trophic systems, we performed stable isotope analysis on three common Caribbean reef fish hosts and two kinds of ectoparasitic isopods: temporarily parasitic gnathiids (Gnathia marleyi and permanently parasitic cymothoids (Anilocra. To further track the transfer of fish-derived carbon (energy from parasites to parasite consumers, gnathiids from host fish were also fed to captive Pederson shrimp (Ancylomenes pedersoni for at least 1 month. Parasitic isopods had δ13C and δ15N values similar to their host, comparable with results from the small number of other host–parasite studies that have employed stable isotopes. Adult gnathiids were enriched in 15N and depleted in 13C relative to juvenile gnathiids, providing insights into the potential isotopic fractionation associated with blood-meal assimilation and subsequent metamorphosis. Gnathiid-fed Pedersen shrimp also had δ13C values consistent with their food source and enriched in 15N as predicted due to trophic fractionation. These results further indicate that stable isotopes can be an effective tool in deciphering cryptic feeding relationships involving parasites and their consumers, and the role of parasites and cleaners in carbon transfer in coral-reef ecosystems specifically.

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

Advances in isotopic analysis for food authenticity testing

DEFF Research Database (Denmark)

Laursen, Kristian Holst; Bontempo, L.; Camin, Federica

2016-01-01

Abstract Stable isotope analysis has been used for food authenticity testing for more than 30 years and is today being utilized on a routine basis for a wide variety of food commodities. During the past decade, major analytical method developments have been made and the fundamental understanding...... authenticity testing is currently developing even further. In this chapter, we aim to provide an overview of the latest developments in stable isotope analysis for food authenticity testing. As several review articles and book chapters have recently addressed this topic, we will primarily focus on relevant...... literature from the past 5 years. We will focus on well-established methods for food authenticity testing using stable isotopes but will also include recent methodological developments, new applications, and current and future challenges....

Compound- and position-specific carbon isotopic signatures of abiogenic hydrocarbons from on-land serpentinite-hosted Hakuba Happo hot spring in Japan

Science.gov (United States)

Suda, Konomi; Gilbert, Alexis; Yamada, Keita; Yoshida, Naohiro; Ueno, Yuichiro

2017-06-01

by compound-specific isotopic analysis.

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 gas chromatography/isotope ratio mass spectrometry and liquid chromatography/isotope ratio mass spectrometry for carbon stable-isotope analysis of carbohydrates

NARCIS (Netherlands)

Moerdijk-Poortvliet, Tanja C. W.; Schierbeek, Henk; Houtekamer, Marco; van Engeland, Tom; Derrien, Delphine; Stal, Lucas J.; Boschker, Henricus T. S.

2015-01-01

We compared gas chromatography/isotope ratio mass spectrometry (GC/IRMS) and liquid chromatography/isotope ratio mass spectrometry (LC/IRMS) for the measurement of δ(13)C values in carbohydrates. Contrary to GC/IRMS, no derivatisation is needed for LC/IRMS analysis of carbohydrates. Hence, although

Comparison of gas chromatography/isotope ratio mass spectrometry and liquid chromatography/isotope ratio mass spectrometry for carbon stable-isotope analysis of carbohydrates

NARCIS (Netherlands)

Moerdijk-Poortvliet, T.C.W.; Schierbeek, H.; Houtekamer, M.; van Engeland, T.; Derrien, D.; Stal, L.J.; Boschker, H.T.S.

2015-01-01

We compared gas chromatography/isotope ratio mass spectrometry (GC/IRMS) and liquid chromatography/isotope ratio mass spectrometry (LC/IRMS) for the measurement of d13C values in carbohydrates. Contrary to GC/IRMS, no derivatisation is needed for LC/IRMS analysis of carbohydrates. Hence, although

Comparison of gas chromatography/isotope ratio mass spectrometry and liquid chromatography/isotope ratio mass spectrometry for carbon stable-isotope analysis of carbohydrates

NARCIS (Netherlands)

Moerdijk-Poortvliet, T.C.W.; Schierbeek, H.; Houtekamer, M.; van Engeland, T.; Derrien, D.; Stal, L.J.; Boschker, H.T.S.

2015-01-01

Rationale: We compared gas chromatography/isotope ratio mass spectrometry (GC/IRMS) and liquid chromatography/isotope ratio mass spectrometry (LC/IRMS) for the measurement of δ13C values in carbohydrates. Contrary to GC/IRMS, no derivatisation is needed for LC/IRMS analysis of carbohydrates. Hence,

Suitability of selected free-gas and dissolved-gas sampling containers for carbon isotopic analysis.

Science.gov (United States)

Eby, P; Gibson, J J; Yi, Y

2015-07-15

Storage trials were conducted for 2 to 3 months using a hydrocarbon and carbon dioxide gas mixture with known carbon isotopic composition to simulate typical hold times for gas samples prior to isotopic analysis. A range of containers (both pierced and unpierced) was periodically sampled to test for δ(13)C isotopic fractionation. Seventeen containers were tested for free-gas storage (20°C, 1 atm pressure) and 7 containers were tested for dissolved-gas storage, the latter prepared by bubbling free gas through tap water until saturated (20°C, 1 atm) and then preserved to avoid biological activity by acidifying to pH 2 with phosphoric acid and stored in the dark at 5°C. Samples were extracted using valves or by piercing septa, and then introduced into an isotope ratio mass spectrometer for compound-specific δ(13)C measurements. For free gas, stainless steel canisters and crimp-top glass serum bottles with butyl septa were most effective at preventing isotopic fractionation (pierced and unpierced), whereas silicone and PTFE-butyl septa allowed significant isotopic fractionation. FlexFoil and Tedlar bags were found to be effective only for storage of up to 1 month. For dissolved gas, crimp-top glass serum bottles with butyl septa were again effective, whereas silicone and PTFE-butyl were not. FlexFoil bags were reliable for up to 2 months. Our results suggest a range of preferred containers as well as several that did not perform very well for isotopic analysis. Overall, the results help establish better QA/QC procedures to avoid isotopic fractionation when storing environmental gas samples. Recommended containers for air transportation include steel canisters and glass serum bottles with butyl septa (pierced and unpierced). Copyright © 2015 John Wiley & Sons, Ltd.

A site-specific and multi-element isotopic approach to origin inference of sugars in foods and beverages

International Nuclear Information System (INIS)

Martin, M.L.; Martin, G.J.; Guillou, C.

1991-01-01

A strategy is presented for the characterization of sugars according to their botanical origin. The samples fermented in standardized conditions can be described in the multi-dimensional space of the overall carbon isotope ratio of ethanol measured by isotope ratio mass spectrometry (IRMS) and of the specific hydrogen isotope parameters of the methyl and methylene sites derived from nuclear magnetic resonance investigation of site-specific natural isotope fractionation (SNIF-NMR method). In the comparison of natural juices, the deuterium and oxygen-18 parameters of water extracted from the juice and from the end fermentation medium also contain information on the origin of the product. The isotopic effects of the concentration processes leading to concentrated juices, musts and syrups can be estimated and taken into account in interpreting the data. The classification power of this multi-element and multi-site approach is illustrated by discriminant analyses involving selected isotopic variables associated with pineapple, apple and barley sugars, compared to beet and cane sugars which are common sources of enrichment. The ability of the method to detect adulteration by exogenous sugars is improved when environmental conditions can be taken into account. (authors)

Isotopic analysis of radioactive waste packages (an inexpensive approach)

International Nuclear Information System (INIS)

Padula, D.A.; Richmond, J.S.

1983-01-01

A computer printout of the isotopic analysis for all radioactive waste packages containing resins, or other aqueous filter media is now required at the disposal sites at Barnwell, South Carolina, and Beatty, Nevada. Richland, Washington requires an isotopic analysis for all radioactive waste packages. The NRC (Nuclear Regulatory Commission), through 10 CFR 61, will require shippers of radioactive waste to classify and label for disposal all radioactive waste forms. These forms include resins, filters, sludges, and dry active waste (trash). The waste classification is to be based upon 10 CFR 61 (Section 1-7). The isotopes upon which waste classification is to be based are tabulated. 7 references, 8 tables

Dual element ((15)N/(14)N, (13)C/(12)C) isotope analysis of glyphosate and AMPA by derivatization-gas chromatography isotope ratio mass spectrometry (GC/IRMS) combined with LC/IRMS.

Science.gov (United States)

Mogusu, Emmanuel O; Wolbert, J Benjamin; Kujawinski, Dorothea M; Jochmann, Maik A; Elsner, Martin

2015-07-01

To assess sources and degradation of the herbicide glyphosate [N-(phosphonomethyl) glycine] and its metabolite AMPA (aminomethylphosphonic acid), concentration measurements are often inconclusive and even (13)C/(12)C analysis alone may give limited information. To advance isotope ratio analysis of an additional element, we present compound-specific (15)N/(14)N analysis of glyphosate and AMPA by a two step derivatization in combination with gas chromatography/isotope ratio mass spectrometry (GC/IRMS). The N-H group was derivatized with isopropyl chloroformate (iso-PCF), and remaining acidic groups were subsequently methylated with trimethylsilyldiazomethane (TMSD). Iso-PCF treatment at pH 10 indicated decomposition of the derivative. At pH 10, and with an excess of iso-PCF by 10-24, greatest yields and accurate (15)N/(14)N ratios were obtained (deviation from elemental analyzer-IRMS: -0.2 ± 0.9% for glyphosate; -0.4 ± 0.7% for AMPA). Limits for accurate δ(15)N analysis of glyphosate and AMPA were 150 and 250 ng injected, respectively. A combination of δ(15)N and δ(13)C analysis by liquid chromatography/isotope ratio mass spectrometry (LC/IRMS) (1) enabled an improved distinction of commercial glyphosate products and (2) showed that glyphosate isotope values during degradation by MnO2 clearly fell outside the commercial product range. This highlights the potential of combined carbon and nitrogen isotopes analysis to trace sources and degradation of glyphosate.

Measurement system analysis (MSA) of the isotopic ratio for uranium isotope enrichment process control

Energy Technology Data Exchange (ETDEWEB)

Medeiros, Josue C. de; Barbosa, Rodrigo A.; Carnaval, Joao Paulo R., E-mail: josue@inb.gov.br, E-mail: rodrigobarbosa@inb.gov.br, E-mail: joaocarnaval@inb.gov.br [Industrias Nucleares do Brasil (INB), Rezende, RJ (Brazil)

2013-07-01

Currently, one of the stages in nuclear fuel cycle development is the process of uranium isotope enrichment, which will provide the amount of low enriched uranium for the nuclear fuel production to supply 100% Angra 1 and 20% Angra 2 demands. Determination of isotopic ration n({sup 235}U)/n({sup 238}U) in uranium hexafluoride (UF{sub 6} - used as process gas) is essential in order to control of enrichment process of isotopic separation by gaseous centrifugation cascades. The uranium hexafluoride process is performed by gas continuous feeding in separation unit which uses the centrifuge force principle, establishing a density gradient in a gas containing components of different molecular weights. The elemental separation effect occurs in a single ultracentrifuge that results in a partial separation of the feed in two fractions: an enriched on (product) and another depleted (waste) in the desired isotope ({sup 235}UF{sub 6}). Industrias Nucleares do Brasil (INB) has used quadrupole mass spectrometry (QMS) by electron impact (EI) to perform isotopic ratio n({sup 235}U)/n({sup 238}U) analysis in the process. The decision of adjustments and change te input variables are based on the results presented in these analysis. A study of stability, bias and linearity determination has been performed in order to evaluate the applied method, variations and systematic errors in the measurement system. The software used to analyze the techniques above was the Minitab 15. (author)

Isotopic analysis of uranium by thermoionic mass spectrometry

International Nuclear Information System (INIS)

Moraes, N.M.P. de.

1979-01-01

Uranium isotopic ratio measurements by thermoionic spectrometry are presented. Emphasis is given upon the investigation of the parameters that directly affect the precision and accuracy of the results. Optimized procedures, namely, chemical processing, sample loading on the filaments, vaporization, ionization and measurements of ionic currents, are established. Adequate statistical analysis of the data for the calculation of the internal and external variances and mean standard deviation are presented. These procedures are applied to natural and NBS isotopic standard uranium samples. The results obtained agree with the certified values within specified limits. 235 U/ 238 U isotopic ratios values determined for NBS-U500, and a series of standard samples with variable isotopic compositon, are used to calculate mass discrimination factor [pt

Hydrogen isotope analysis of amino acids and whole cells reflects biosynthetic processing of nutrient- and water-derived hydrogen

Science.gov (United States)

Griffin, P.; Newsome, S.; Steele, A.; Fogel, M. L.

2011-12-01

Hydrogen (H) isotopes serve as sensitive tracers of biochemical processes that can be exploited to answer critical questions in biogeochemistry, ecology, and microbiology. Despite this apparent utility, relatively little is known about the specific mechanisms of H isotope fractionation involved in biosynthesis. In order to understand how organisms incorporate hydrogen from their chemical milieu into biomass, we have cultured the model bacterium E. coli MG1655 in a variety of media composed of deuterium-labeled nutrients and waters. Isotopic analysis of bulk cell mass reveals that the H fractionation between media water and cell material varies as a function of the nutrient source, with commonly used organic food sources (glucose and tryptone) leading to far smaller fractionation signals than non-standard ones (such as formamide, adenine, and urea). In addition, we have completed compound specific isotope analysis of amino acids using combined GC-IRMS. Amino acids harvested from E. coli cultured on glucose in water of varied D/H composition posses an extraordinary range of isotopic compositions (400-600 %). Furthermore, these amino acids follow a systematic distribution of D/H where proline is always heaviest and glycine is always lightest. However, when the short-chain peptide tryptone is used in place of glucose, only the non-essential amino acids reflect media water D/H values, suggesting the direct incorporation of some media-borne amino acids into cellular protein. These observations provide a foundation for understanding the cellular routing of hydrogen obtained from food and water sources and indicate that D/H analysis can serve as a powerful probe of biological function.

ATTA - A new method of ultrasensitive isotope trace analysis

International Nuclear Information System (INIS)

Bailey, K.; Chen, C.Y.; Du, X.; Li, Y.M.; Lu, Z.-T.; O'Connor, T.P.; Young, L.

2000-01-01

A new method of ultrasensitive isotope trace analysis has been developed. This method, based on the technique of laser manipulation of neutral atoms, has been used to count individual 85 Kr and 81 Kr atoms present in a natural krypton gas sample with isotopic abundances in the range of 10 -11 and 10 -13 , respectively. This method is free of contamination from other isotopes and elements and can be applied to various different isotope tracers for a wide range of applications. The demonstrated detection efficiency is 1x10 -7 . System improvements could increase the efficiency by many orders of magnitude

Assessing microbial degradation of o-xylene at field-scale from the reduction in mass flow rate combined with compound-specific isotope analyses

Science.gov (United States)

Peter, A.; Steinbach, A.; Liedl, R.; Ptak, T.; Michaelis, W.; Teutsch, G.

2004-07-01

In recent years, natural attenuation (NA) has evolved into a possible remediation alternative, especially in the case of BTEX spills. In order to be approved by the regulators, biodegradation needs to be demonstrated which requires efficient site investigation and monitoring tools. Three methods—the Integral Groundwater Investigation method, the compound-specific isotope analysis (CSIA) and a newly developed combination of both—were used in this work to quantify at field scale the biodegradation of o-xylene at a former gasworks site which is heavily contaminated with BTEX and PAHs. First, the Integral Groundwater Investigation method [Schwarz, R., Ptak, T., Holder, T., Teutsch, G., 1998. Groundwater risk assessment at contaminated sites: a new investigation approach. In: Herbert, M. and Kovar, K. (Editors), GQ'98 Groundwater Quality: Remediation and Protection. IAHS Publication 250, pp. 68-71; COH 4 (2000) 170] was applied, which allows the determination of mass flow rates of o-xylene by integral pumping tests. Concentration time series obtained during pumping at two wells were used to calculate inversely contaminant mass flow rates at the two control planes that are defined by the diameter of the maximum isochrone. A reactive transport model was used within a Monte Carlo approach to identify biodegradation as the dominant process for reduction in the contaminant mass flow rate between the two consecutive control planes. Secondly, compound-specific carbon isotope analyses of o-xylene were performed on the basis of point-scale samples from the same two wells. The Rayleigh equation was used to quantify the degree of biodegradation that occurred between the wells. Thirdly, a combination of the Integral Groundwater Investigation method and the compound-specific isotope analysis was developed and applied. It comprises isotope measurements during the integral pumping tests and the evaluation of δ13C time series by an inversion algorithm to obtain spatially

Stable isotope analysis of Dacryoconarid carbonate microfossils: a new tool for Devonian oxygen and carbon isotope stratigraphy.

Science.gov (United States)

Frappier, Amy Benoit; Lindemann, Richard H; Frappier, Brian R

2015-04-30

Dacryoconarids are extinct marine zooplankton known from abundant, globally distributed calcite microfossils in the Devonian, but their shell stable isotope composition has not been previously explored. Devonian stable isotope stratigraphy is currently limited to less common invertebrates or bulk rock analyses of uncertain provenance. As with Cenozoic planktonic foraminifera, isotopic analysis of dacryoconarid shells could facilitate higher-resolution, geographically widespread stable isotope records of paleoenvironmental change, including marine hypoxia events, climate changes, and biocrises. We explored the use of Dacryoconarid isotope stratigraphy as a viable method in interpreting paleoenvironments. We applied an established method for determining stable isotope ratios (δ(13) C, δ(18) O values) of small carbonate microfossils to very well-preserved dacryoconarid shells. We analyzed individual calcite shells representing five common genera using a Kiel carbonate device coupled to a MAT 253 isotope ratio mass spectrometer. Calcite shell δ(13) C and δ(18) O values were compared by taxonomic group, rock unit, and locality. Single dacryoconarid calcite shells are suitable for stable isotope analysis using a Kiel-IRMS setup. The dacryoconarid shell δ(13) C values (-4.7 to 2.3‰) and δ(18) O values (-10.3 to -4.8‰) were consistent across taxa, independent of shell size or part, but varied systematically through time. Lower fossil δ(18) O values were associated with warmer water temperature and more variable δ(13) C values were associated with major bioevents. Dacryoconarid δ(13) C and δ(18) O values differed from bulk rock carbonate values. Dacryoconarid individual microfossil δ(13) C and δ(18) O values are highly sensitive to paleoenvironmental changes, thus providing a promising avenue for stable isotope chemostratigraphy to better resolve regional to global paleoceanographic changes throughout the upper Silurian to the upper Devonian. Our results

TPASS: a gamma-ray spectrum analysis and isotope identification computer code

International Nuclear Information System (INIS)

Dickens, J.K.

1981-03-01

The gamma-ray spectral data-reduction and analysis computer code TPASS is described. This computer code is used to analyze complex Ge(Li) gamma-ray spectra to obtain peak areas corrected for detector efficiencies, from which are determined gamma-ray yields. These yields are compared with an isotope gamma-ray data file to determine the contributions to the observed spectrum from decay of specific radionuclides. A complete FORTRAN listing of the code and a complex test case are given

Transformation of chlorpyrifos in integrated recirculating constructed wetlands (IRCWs) as revealed by compound-specific stable isotope (CSIA) and microbial community structure analysis.

Science.gov (United States)

Tang, Xiaoyan; Yang, Yang; Huang, Wenda; McBride, Murray B; Guo, Jingjing; Tao, Ran; Dai, Yunv

2017-06-01

Carbon isotope analysis and 454 pyrosequencing methods were used to investigate in situ biodegradation of chlorpyrifos during its transport through three model integrated recirculating constructed wetlands (IRCWs). Results show that plant and Fe-impregnated biochar promoted degradation of chlorpyrifos and its metabolite 3,5,6-trichloro-2-pyridinol (TCP). Carbon isotope ratios in the IRCWs shifted to -31.24±0.58‰ (IRCW1, plant free), -26.82±0.60‰ (IRCW2, with plant) and -24.76±0.94‰ (IRCW3, with plant and Fe-biochar). The enrichment factors (Ɛ bulk,c ) were determined as -0.69±0.06‰ (IRCW1), -0.91±0.07‰ (IRCW2) and -1.03±0.09‰ (IRCW3). Microbial community analysis showed that IRCW3 was dominated by members of Bacillus, which can utilize and degrade chlorpyrifos. These results reveal that plant and Fe-biochar can induce carbon isotope fractionation and have a positive impact on the chlorpyrifos degradation efficiency by influencing the development of beneficial microbial communities. Copyright © 2017. Published by Elsevier Ltd.

Automatic measurement system for light element isotope analysis

International Nuclear Information System (INIS)

Satake, Hiroshi; Ikegami, Kouichi.

1990-01-01

The automatic measurement system for the light element isotope analysis was developed by installing the specially designed inlet system which was controlled by a computer. The microcomputer system contains specific interface boards for the inlet system and the mass spectrometer, Micromass 602 E. All the components of the inlet and the computer system installed are easily available in Japan. Ten samples can be automatically measured as a maximum of. About 160 minutes are required for 10 measurements of δ 18 O values of CO 2 . Thus four samples can be measured per an hour using this system, while usually three samples for an hour using the manual operation. The automatized analysis system clearly has an advantage over the conventional method. This paper describes the details of this automated system, such as apparatuses used, the control procedure and the correction for reliable measurement. (author)

Deuterium, carbon and nitrogen isotopic analysis of natural and synthetic caffeines. Authentication of coffees and coffee extracts

International Nuclear Information System (INIS)

Danho, D.; Naulet, N.; Martin, G.J.

1992-01-01

Isotope ratio mass spectrometry (IRMS) was used to determine the δ( 13 C) and δ( 15 N) values of a series of caffeine samples extracted from coffee beans or obtained by synthesis, 2 H NMR spectra were recorded in order to compute the site-specific isotope ratios of caffeine. The set of the five isotope ratios measured for the 26 different samples was studied by multi-variate analysis (principal component and discriminant analyse) and it is shown that the synthetic samples are clearly distinguishable from the natural caffeines which in turn can be classified with complete accuracy as of either American or African origin

Carnivore specific bone bioapatite and collagen carbon isotope fractionations: Case studies of modern and fossil grey wolf populations

Science.gov (United States)

Fox-Dobbs, K.; Wheatley, P. V.; Koch, P. L.

2006-12-01

Stable isotope analyses of modern and fossil biogenic tissues are routinely used to reconstruct present and past vertebrate foodwebs. Accurate isotopic dietary reconstructions require a consumer and tissue specific understanding of how isotopes are sorted, or fractionated, between trophic levels. In this project we address the need for carnivore specific isotope variables derived from populations that are ecologically well- characterized. Specifically, we investigate the trophic difference in carbon isotope values between mammalian carnivore (wolf) bone bioapatite and herbivore (prey) bone bioapatite. We also compare bone bioapatite and collagen carbon isotope values collected from the same individuals. We analyzed bone specimens from two modern North American grey wolf (Canis lupus) populations (Isle Royale National Park, Michigan and Yellowstone National Park, Wyoming), and the ungulate herbivores that are their primary prey (moose and elk, respectively). Because the diets of both wolf populations are essentially restricted to a single prey species, there were no confounding effects due to carnivore diet variability. We measured a trophic difference of approximately -1.3 permil between carnivore (lower value) and herbivore (higher value) bone bioapatite carbon isotope values, and an average inter-tissue difference of 5.1 permil between carnivore bone collagen (lower value) and bioapatite (higher value) carbon isotope values. Both of these isotopic differences differ from previous estimates derived from a suite of African carnivores; our carnivore-herbivore bone bioapatite carbon isotope spacing is smaller (-1.3 vs. -4.0 permil), and our carnivore collagen-bioapatite carbon difference is larger (5.1 vs. 3.0 permil). These discrepancies likely result from comparing values measured from a single hypercarnivore (wolf) to average values calculated from several carnivore species, some of which are insectivorous or partly omnivorous. The trophic and inter

Monitoring biodegradation of ethene and bioremediation of chlorinated ethenes at a contaminated site using compound-specific isotope analysis (CSIA).

Science.gov (United States)

Mundle, Scott O C; Johnson, Tiffany; Lacrampe-Couloume, Georges; Pérez-de-Mora, Alfredo; Duhamel, Melanie; Edwards, Elizabeth A; McMaster, Michaye L; Cox, Evan; Révész, Kinga; Sherwood Lollar, Barbara

2012-02-07

Chlorinated ethenes are commonly found in contaminated groundwater. Remediation strategies focus on transformation processes that will ultimately lead to nontoxic products. A major concern with these strategies is the possibility of incomplete dechlorination and accumulation of toxic daughter products (cis-1,2-dichloroethene (cDCE), vinyl chloride (VC)). Ethene mass balance can be used as a direct indicator to assess the effectiveness of dechlorination. However, the microbial processes that affect ethene are not well characterized and poor mass balance may reflect biotransformation of ethene rather than incomplete dechlorination. Microbial degradation of ethene is commonly observed in aerobic systems but fewer cases have been reported in anaerobic systems. Limited information is available on the isotope enrichment factors associated with these processes. Using compound-specific isotope analysis (CSIA) we determined the enrichment factors associated with microbial degradation of ethene in anaerobic microcosms (ε = -6.7‰ ± 0.4‰, and -4.0‰ ± 0.8‰) from cultures collected from the Twin Lakes wetland area at the Savannah River site in Georgia (United States), and in aerobic microcosms (ε = -3.0‰ ± 0.3‰) from Mycobacterium sp. strain JS60. Under anaerobic and aerobic conditions, CSIA can be used to determine whether biotransformation of ethene is occurring in addition to biodegradation of the chlorinated ethenes. Using δ(13)C values determined for ethene and for chlorinated ethenes at a contaminated field site undergoing bioremediation, this study demonstrates how CSIA of ethene can be used to reduce uncertainty and risk at a site by distinguishing between actual mass balance deficits during reductive dechlorination and apparent lack of mass balance that is related to biotransformation of ethene.

SIMS analysis of isotopic impurities in ion implants

International Nuclear Information System (INIS)

Sykes, D.E.; Blunt, R.T.

1986-01-01

The n-type dopant species Si and Se used for ion implantation in GaAs are multi-isotopic with the most abundant isotope not chosen because of potential interferences with residual gases. SIMS analysis of a range of 29 Si implants produced by several designs of ion implanter all showed significant 28 Si impurity with a different depth distribution from that of the deliberately implanted 29 Si isotope. This effect was observed to varying degrees with all fifteen implanters examined and in every 29 Si implant analysed to date 29 Si + , 29 Si ++ and 30 Si implants all show the same effect. In the case of Se implantation, poor mass resolution results in the implantation of all isotopes with the same implant distribution (i.e. energy), whilst implants carried out with good mass resolution show the implantation of all isotopes with the characteristic lower depth distribution of the impurity isotopes as found in the Si implants. This effect has also been observed in p-type implants into GaAs (Mg) and for Ga implanted in Si. A tentative explanation of the effect is proposed. (author)

Sensing site-specific structural characteristics and chirality using vibrational circular dichroism of isotope labeled peptides.

Science.gov (United States)

Keiderling, Timothy A

2017-12-01

Isotope labeling has a long history in chemistry as a tool for probing structure, offering enhanced sensitivity, or enabling site selection with a wide range of spectroscopic tools. Chirality sensitive methods such as electronic circular dichroism are global structural tools and have intrinsically low resolution. Consequently, they are generally insensitive to modifications to enhance site selectivity. The use of isotope labeling to modify vibrational spectra with unique resolvable frequency shifts can provide useful site-specific sensitivity, and these methods have been recently more widely expanded in biopolymer studies. While the spectral shifts resulting from changes in isotopic mass can provide resolution of modes from specific parts of the molecule and can allow detection of local change in structure with perturbation, these shifts alone do not directly indicate structure or chirality. With vibrational circular dichroism (VCD), the shifted bands and their resultant sign patterns can be used to indicate local conformations in labeled biopolymers, particularly if multiple labels are used and if their coupling is theoretically modeled. This mini-review discusses selected examples of the use of labeling specific amides in peptides to develop local structural insight with VCD spectra. © 2017 Wiley Periodicals, Inc.

Krypton isotope analysis using near-resonant stimulated Raman spectroscopy

International Nuclear Information System (INIS)

Whitehead, C.A.; Cannon, B.D.; Wacker, J.F.

1994-12-01

A method for measuring low relative abundances of 85 Kr in one liter or less samples of air has been under development here at Pacific Northwest Laboratory. The goal of the Krypton Isotope Laser Analysis (KILA) method is to measure ratios of 10 -10 or less of 85 Kr to more abundant stable krypton. Mass spectrometry and beta counting are the main competing technologies used in rare-gas trace analysis and are limited in application by such factors as sample size, counting times, and selectivity. The use of high-resolution lasers to probe hyperfine levels to determine isotopic abundance has received much attention recently. In this study, we report our progress on identifying and implementing techniques for trace 85 Kr analysis on small gas samples in a static cell as well as limitations on sensitivity and selectivity for the technique. High-resolution pulsed and cw lasers are employed in a laser-induced fluorescence technique that preserves the original sample. This technique, is based on resonant isotopic depletion spectroscopy (RIDS) in which one isotope is optically depleted while preserving the population of a less abundant isotope. The KILA method consists of three steps. In the first step, the 1s 5 metastable level of krypton is populated via radiative cascade following two-photon excitation of the 2p 6 energy level. Next, using RBDS, the stable krypton isotopes are optically depleted to the ground state through the 1s 4 level with the bulk of the 85 Kr population being preserved. Finally, the remaining metastable population is probed to determine 85 Kr concentration. The experimental requirements for each of these steps are outlined below

Isotopically modified compounds

International Nuclear Information System (INIS)

Kuruc, J.

2009-01-01

In this chapter the nomenclature of isotopically modified compounds in Slovak language is described. This chapter consists of following parts: (1) Isotopically substituted compounds; (2) Specifically isotopically labelled compounds; (3) Selectively isotopically labelled compounds; (4) Non-selectively isotopically labelled compounds; (5) Isotopically deficient compounds.

Assessing chlorinated ethene degradation in a large scale contaminant plume by dual carbon–chlorine isotope analysis and quantitative PCR

DEFF Research Database (Denmark)

Hunkeler, D.; Abe, Y.; Broholm, Mette Martina

2011-01-01

The fate of chlorinated ethenes in a large contaminant plume originating from a tetrachloroethene (PCE) source in a sandy aquifer in Denmark was investigated using novel methods including compound-specific carbon and chlorine isotope analysis and quantitative real-time polymerase chain reaction (q...... reduction by pyrite as indicated by the formation of cDCE and stable carbon isotope data. TCE and cDCE showed carbon isotope trends typical for reductive dechlorination with an initial depletion of 13C in the daughter products followed by an enrichment of 13C as degradation proceeded. At 1000 m downgradient......DCE. The significant enrichment of 13C in VC indicates that VC was transformed further, although the mechanismcould not be determined. The transformation of cDCEwas the rate limiting step as no accumulation of VC occurred. In summary, the study demonstrates that carbon–chlorine isotope analysis and qPCR combinedwith...

Intramolecular carbon and nitrogen isotope analysis by quantitative dry fragmentation of the phenylurea herbicide isoproturon in a combined injector/capillary reactor prior to GC separation.

Science.gov (United States)

Penning, Holger; Elsner, Martin

2007-11-01

Potentially, compound-specific isotope analysis may provide unique information on source and fate of pesticides in natural systems. Yet for isotope analysis, LC-based methods that are based on the use of organic solvents often cannot be used and GC-based analysis is frequently not possible due to thermolability of the analyte. A typical example of a compound with such properties is isoproturon (3-(4-isopropylphenyl)-1,1-dimethylurea), belonging to the worldwide extensively used phenylurea herbicides. To make isoproturon accessible to carbon and nitrogen isotope analysis, we developed a GC-based method during which isoproturon was quantitatively fragmented to dimethylamine and 4-isopropylphenylisocyanate. Fragmentation occurred only partially in the injector but was mainly achieved on a heated capillary column. The fragments were then chromatographically separated and individually measured by isotope ratio mass spectrometry. The reliability of the method was tested in hydrolysis experiments with three isotopically different batches of isoproturon. For all three products, the same isotope fractionation factors were observed during conversion and the difference in isotope composition between the batches was preserved. This study demonstrates that fragmentation of phenylurea herbicides does not only make them accessible to isotope analysis but even enables determination of intramolecular isotope fractionation.

U and Pb isotope analysis of uraninite and galena by ion microprobe

Energy Technology Data Exchange (ETDEWEB)

Evins, L.Z.; Sunde, T.; Schoeberg, H. [Swedish Museum of Natural History, Stockholm (Sweden). Laboratory for Isotope Geology; Fayek, M. [Univ. of Tennessee, Knoxville, TN (United States). Dept. of Geological Sciences

2001-10-01

Accurate isotopic analysis of minerals by ion microprobe, or SIMS (Secondary Ion Mass Spectrometry) usually requires a standard to correct for instrumental mass bias effects that occur during analysis. We have calibrated two uraninite crystals and one galena crystal to be used as ion probe standards. As part of this study we describe the analytical procedures and problems encountered while trying to establish fractionation factors for U and Pb isotopes measured in galena and uraninite. Only the intra-element isotopic mass fractionation is considered and not the interelement fractionation. Galena and uraninite were analysed with TIMS (Thermal Ionisation Mass Spectrometry) prior to SIMS. One uraninite crystal (P88) comes from Sweden and is ca 900 Ma old, the other from Maine, USA (LAMNH-30222) and is ca 350 Ma old. The galena sample comes from the Paleoproterozoic ore district Bergslagen in Sweden. SIMS analyses were performed at two different laboratories: the NORDSM facility in Stockholm, which has a high resolution Cameca IMS 1270 ion microprobe, and the Oak Ridge National Laboratory (ORNL) in Tennessee, which has a Cameca IMS 4f ion microprobe. The results show that during the analysis of galena, Pb isotopes fractionate in favour of the lighter isotope by as much as 0.5%/amu. A Pb isotope fractionation factor for uraninite was more difficult to calculate, probably due to the formation of hydride interferences encountered during analysis with the Cameca IMS 1270 ion microprobe. However, drying the sample in vacuum prior to analysis, and using high-energy filtering and a cold trap during analysis can minimise these hydride interferences. A large fractionation of U isotopes of ca 1.4%/amu in favour of the lighter isotope was calculated for uraninite.

U and Pb isotope analysis of uraninite and galena by ion microprobe

International Nuclear Information System (INIS)

Evins, L.Z.; Sunde, T.; Schoeberg, H.; Fayek, M.

2001-10-01

Accurate isotopic analysis of minerals by ion microprobe, or SIMS (Secondary Ion Mass Spectrometry) usually requires a standard to correct for instrumental mass bias effects that occur during analysis. We have calibrated two uraninite crystals and one galena crystal to be used as ion probe standards. As part of this study we describe the analytical procedures and problems encountered while trying to establish fractionation factors for U and Pb isotopes measured in galena and uraninite. Only the intra-element isotopic mass fractionation is considered and not the interelement fractionation. Galena and uraninite were analysed with TIMS (Thermal Ionisation Mass Spectrometry) prior to SIMS. One uraninite crystal (P88) comes from Sweden and is ca 900 Ma old, the other from Maine, USA (LAMNH-30222) and is ca 350 Ma old. The galena sample comes from the Paleoproterozoic ore district Bergslagen in Sweden. SIMS analyses were performed at two different laboratories: the NORDSM facility in Stockholm, which has a high resolution Cameca IMS 1270 ion microprobe, and the Oak Ridge National Laboratory (ORNL) in Tennessee, which has a Cameca IMS 4f ion microprobe. The results show that during the analysis of galena, Pb isotopes fractionate in favour of the lighter isotope by as much as 0.5%/amu. A Pb isotope fractionation factor for uraninite was more difficult to calculate, probably due to the formation of hydride interferences encountered during analysis with the Cameca IMS 1270 ion microprobe. However, drying the sample in vacuum prior to analysis, and using high-energy filtering and a cold trap during analysis can minimise these hydride interferences. A large fractionation of U isotopes of ca 1.4%/amu in favour of the lighter isotope was calculated for uraninite

Comparison of gas chromatography/isotope ratio mass spectrometry and liquid chromatography/isotope ratio mass spectrometry for carbon stable-isotope analysis of carbohydrates.

Science.gov (United States)

Moerdijk-Poortvliet, Tanja C W; Schierbeek, Henk; Houtekamer, Marco; van Engeland, Tom; Derrien, Delphine; Stal, Lucas J; Boschker, Henricus T S

2015-07-15

We compared gas chromatography/isotope ratio mass spectrometry (GC/IRMS) and liquid chromatography/isotope ratio mass spectrometry (LC/IRMS) for the measurement of δ(13)C values in carbohydrates. Contrary to GC/IRMS, no derivatisation is needed for LC/IRMS analysis of carbohydrates. Hence, although LC/IRMS is expected to be more accurate and precise, no direct comparison has been reported. GC/IRMS with the aldonitrile penta-acetate (ANPA) derivatisation method was compared with LC/IRMS without derivatisation. A large number of glucose standards and a variety of natural samples were analysed for five neutral carbohydrates at natural abundance as well as at (13)C-enriched levels. Gas chromatography/chemical ionisation mass spectrometry (GC/CIMS) was applied to check for incomplete derivatisation of the carbohydrate, which would impair the accuracy of the GC/IRMS method. The LC/IRMS technique provided excellent precision (±0.08‰ and ±3.1‰ at natural abundance and enrichment levels, respectively) for the glucose standards and this technique proved to be superior to GC/IRMS (±0.62‰ and ±19.8‰ at natural abundance and enrichment levels, respectively). For GC/IRMS measurements the derivatisation correction and the conversion of carbohydrates into CO2 had a considerable effect on the measured δ(13)C values. However, we did not find any significant differences in the accuracy of the two techniques over the full range of natural δ(13)C abundances and (13)C-labelled glucose. The difference in the performance of GC/IRMS and LC/IRMS diminished when the δ(13)C values were measured in natural samples, because the chromatographic performance and background correction became critical factors, particularly for LC/IRMS. The derivatisation of carbohydrates for the GC/IRMS method was complete. Although both LC/IRMS and GC/IRMS are reliable techniques for compound-specific stable carbon isotope analysis of carbohydrates (provided that derivatisation is complete and the

A versatile method for simultaneous stable carbon isotope analysis of DNA and RNA nucleotides by liquid chromatography/isotope ratio mass spectrometry

NARCIS (Netherlands)

Moerdijk-Poortvliet, T.C.W.; Brasser, J.; de Ruiter, G.; Houtekamer, M.; Bolhuis, H.; Stal, L.J.; Boschker, H.T.S.

2014-01-01

RATIONALELiquid chromatography/isotope ratio mass spectrometry (LC/IRMS) is currently the most accurate and precise technique for the measurement of compound-specific stable carbon isotope ratios (C-13/C-12) in biological metabolites, at their natural abundance. However, until now this technique

Food certification based on isotopic analysis, according to the European standards

International Nuclear Information System (INIS)

Costinel, Diana; Ionete, Roxana Elena; Vremera, Raluca; Stanciu, Vasile; Iordache, Andreea

2007-01-01

Full text: Under current EU research projects, several public research institutions, universities and private companies are collaborating to develop new methods of evidencing food adulteration and consequently assessing food safety. The use of mass spectrometry (MS) to determine the ratio of stable isotopes in bio-molecules now provides the means to prove the natural origin of a wide variety of foodstuffs - and therefore, to identify the fraud and consequently to reject the improper products or certify the food quality. Isotope analysis has been officially adopted by the EU as a means of controlling adulteration of some food stuffs. A network of research organizations developed the use of isotopic analysis to support training and technology transfer to encourage uptake of the technique. There were also developed proficiency-testing schemes to ensure the correct use of isotopic techniques in national testing laboratories. In addition, ensuring the food quality and safety is a requirement, which must be fulfilled for the integration in EU. The present paper emphasizes the isotopic analysis for D/H, 18 O/ 16 O, 13 C/ 12 C from food (honey, juice, wines) using a new generation Isotope Ratio MS, Finnigan Delta V Plus, coupled to a three flexible continuous flow preparation device (GasBench II, TC Elemental Analyser and GC-C/TC). (authors)

Quantitative analysis of deuterium using the isotopic effect on quaternary {sup 13}C NMR chemical shifts

Energy Technology Data Exchange (ETDEWEB)

Darwish, Tamim A., E-mail: tamim.darwish@ansto.gov.au [National Deuteration Facility, Australian Nuclear Science and Technology Organisation, Locked Bag 21, Kirrawee DC, NSW 2232 (Australia); Yepuri, Nageshwar Rao; Holden, Peter J. [National Deuteration Facility, Australian Nuclear Science and Technology Organisation, Locked Bag 21, Kirrawee DC, NSW 2232 (Australia); James, Michael [Australian Synchrotron, 800 Blackburn Road, Clayton, Victoria 3168 (Australia)

2016-07-13

Quantitative analysis of specifically deuterated compounds can be achieved by a number of conventional methods, such as mass spectroscopy, or by quantifying the residual {sup 1}H NMR signals compared to signals from internal standards. However, site specific quantification using these methods becomes challenging when dealing with non-specifically or randomly deuterated compounds that are produced by metal catalyzed hydrothermal reactions in D{sub 2}O, one of the most convenient deuteration methods. In this study, deuterium-induced NMR isotope shifts of quaternary {sup 13}C resonances neighboring deuterated sites have been utilized to quantify the degree of isotope labeling of molecular sites in non-specifically deuterated molecules. By probing {sup 13}C NMR signals while decoupling both proton and deuterium nuclei, it is possible to resolve {sup 13}C resonances of the different isotopologues based on the isotopic shifts and the degree of deuteration of the carbon atoms. We demonstrate that in different isotopologues, the same quaternary carbon, neighboring partially deuterated carbon atoms, are affected to an equal extent by relaxation. Decoupling both nuclei ({sup 1}H, {sup 2}H) resolves closely separated quaternary {sup 13}C signals of the different isotopologues, and allows their accurate integration and quantification under short relaxation delays (D1 = 1 s) and hence fast accumulative spectral acquisition. We have performed a number of approaches to quantify the deuterium content at different specific sites to demonstrate a convenient and generic analysis method for use in randomly deuterated molecules, or in cases of specifically deuterated molecules where back-exchange processes may take place during work up. - Graphical abstract: The relative intensities of quaternary {sup 13}C {"1H,"2H} resonances are equal despite the different relaxation delays, allowing the relative abundance of the different deuterated isotopologues to be calculated using NMR fast

Differential Isotope Labeling of Glycopeptides for Accurate Determination of Differences in Site-Specific Glycosylation.

Science.gov (United States)

Pabst, Martin; Benešová, Iva; Fagerer, Stephan R; Jacobsen, Mathias; Eyer, Klaus; Schmidt, Gregor; Steinhoff, Robert; Krismer, Jasmin; Wahl, Fabian; Preisler, Jan; Zenobi, Renato

2016-01-04

We introduce a stable isotope labeling approach for glycopeptides that allows a specific glycosylation site in a protein to be quantitatively evaluated using mass spectrometry. Succinic anhydride is used to specifically label primary amino groups of the peptide portion of the glycopeptides. The heavy form (D4(13)C4) provides an 8 Da mass increment over the light natural form (H4(12)C4), allowing simultaneous analysis and direct comparison of two glycopeptide profiles in a single MS scan. We have optimized a protocol for an in-solution trypsin digestion, a one-pot labeling procedure, and a post-labeling solid-phase extraction to obtain purified and labeled glycopeptides. We provide the first demonstration of this approach by comparing IgG1 Fc glycopeptides from polyclonal IgG samples with respect to their galactosylation and sialylation patterns using MALDI MS and LC-ESI-MS.

Complementing approaches to demonstrate chlorinated solvent biodegradation in a complex pollution plume: Mass balance, PCR and compound-specific stable isotope analysis

Science.gov (United States)

Courbet, Christelle; Rivière, Agnès; Jeannottat, Simon; Rinaldi, Sandro; Hunkeler, Daniel; Bendjoudi, Hocine; de Marsily, Ghislain

2011-11-01

This work describes the use of different complementing methods (mass balance, polymerase chain reaction assays and compound-specific stable isotope analysis) to demonstrate the existence and effectiveness of biodegradation of chlorinated solvents in an alluvial aquifer. The solvent-contaminated site is an old chemical factory located in an alluvial plain in France. As most of the chlorinated contaminants currently found in the groundwater at this site were produced by local industries at various times in the past, it is not enough to analyze chlorinated solvent concentrations along a flow path to convincingly demonstrate biodegradation. Moreover, only a few data were initially available to characterize the geochemical conditions at this site, which were apparently complex at the source zone due to (i) the presence of a steady oxygen supply to the groundwater by irrigation canal losses and river infiltration and (ii) an alkaline pH higher than 10 due to former underground lime disposal. A demonstration of the existence of biodegradation processes was however required by the regulatory authority within a timeframe that did not allow a full geochemical characterization of such a complex site. Thus a combination of different fast methods was used to obtain a proof of the biodegradation occurrence. First, a mass balance analysis was performed which revealed the existence of a strong natural attenuation process (biodegradation, volatilization or dilution), despite the huge uncertainty on these calculations. Second, a good agreement was found between carbon isotopic measurements and PCR assays (based on 16S RNA gene sequences and functional genes), which clearly indicated reductive dechlorination of different hydrocarbons (Tetrachloroethene—PCE-, Trichloroethene—TCE-, 1,2- cisDichloroethene— cis-1,2-DCE-, 1,2- transDichloroethene— trans-1,2-DCE-, 1,1-Dichloroethene—1,1-DCE-, and Vinyl Chloride—VC) to ethene. According to these carbon isotope measurements

Molecular Isotopic Distribution Analysis (MIDAs) with adjustable mass accuracy.

Science.gov (United States)

Alves, Gelio; Ogurtsov, Aleksey Y; Yu, Yi-Kuo

2014-01-01

In this paper, we present Molecular Isotopic Distribution Analysis (MIDAs), a new software tool designed to compute molecular isotopic distributions with adjustable accuracies. MIDAs offers two algorithms, one polynomial-based and one Fourier-transform-based, both of which compute molecular isotopic distributions accurately and efficiently. The polynomial-based algorithm contains few novel aspects, whereas the Fourier-transform-based algorithm consists mainly of improvements to other existing Fourier-transform-based algorithms. We have benchmarked the performance of the two algorithms implemented in MIDAs with that of eight software packages (BRAIN, Emass, Mercury, Mercury5, NeutronCluster, Qmass, JFC, IC) using a consensus set of benchmark molecules. Under the proposed evaluation criteria, MIDAs's algorithms, JFC, and Emass compute with comparable accuracy the coarse-grained (low-resolution) isotopic distributions and are more accurate than the other software packages. For fine-grained isotopic distributions, we compared IC, MIDAs's polynomial algorithm, and MIDAs's Fourier transform algorithm. Among the three, IC and MIDAs's polynomial algorithm compute isotopic distributions that better resemble their corresponding exact fine-grained (high-resolution) isotopic distributions. MIDAs can be accessed freely through a user-friendly web-interface at http://www.ncbi.nlm.nih.gov/CBBresearch/Yu/midas/index.html.

Development and application of liquid chromatography coupled to isotope ratio mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Zhang, Lijun

2014-02-19

Stable isotope analysis has found widespread applications in various disciplines such as archaeology, geochemistry, biology, food authenticity, and forensic science. Coupling chromatography to isotope ratio mass spectrometry for compound-specific isotope analysis (CSIA) is a trend, as it provides several advantages over bulk isotope analysis, e.g., relatively simple sample preparation, the ability to measure individual compounds in a complex mixture in one run, and the reduced sample size required for precise isotope analysis. Gas chromatography coupled to isotope ratio mass spectrometry (GC/IRMS) has been well-established for compound-specific isotope analysis of volatile organic compounds within the last two decades. However, an interface combining liquid chromatography with isotope ratio mass spectrometry (LC/IRMS) was not commercially available until 2004. The current design of the interface requires using a carbon-free eluent in chromatographic separation. This requirement limits the application of the most frequently used reversed-phase liquid chromatography in CSIA, because the elution strength of water at room temperature is too low to serve as mobile phase in reversed-phase separations. In order to increase the elution strength of water, we propose using high temperature water for chromatographic elution. The polarity of water decreases with an increase of temperature, yielding increased elution strength in reversed-phase columns. Therefore, high temperature water can be used as eluent instead of organic solvent for combining reversed-phase liquid chromatography with isotope ratio mass spectrometry (RPLC/IRMS). Additionally, temperature gradients can replace organic solvent gradients to increase chromatographic resolution. This is very important for LC/IRMS analysis, as precise isotope analysis requires baseline separation of analytes. In this thesis, high-temperature reversed-phase liquid chromatography was coupled to, and for the first time carefully

Development and application of liquid chromatography coupled to isotope ratio mass spectrometry

International Nuclear Information System (INIS)

Zhang, Lijun

2014-01-01

Stable isotope analysis has found widespread applications in various disciplines such as archaeology, geochemistry, biology, food authenticity, and forensic science. Coupling chromatography to isotope ratio mass spectrometry for compound-specific isotope analysis (CSIA) is a trend, as it provides several advantages over bulk isotope analysis, e.g., relatively simple sample preparation, the ability to measure individual compounds in a complex mixture in one run, and the reduced sample size required for precise isotope analysis. Gas chromatography coupled to isotope ratio mass spectrometry (GC/IRMS) has been well-established for compound-specific isotope analysis of volatile organic compounds within the last two decades. However, an interface combining liquid chromatography with isotope ratio mass spectrometry (LC/IRMS) was not commercially available until 2004. The current design of the interface requires using a carbon-free eluent in chromatographic separation. This requirement limits the application of the most frequently used reversed-phase liquid chromatography in CSIA, because the elution strength of water at room temperature is too low to serve as mobile phase in reversed-phase separations. In order to increase the elution strength of water, we propose using high temperature water for chromatographic elution. The polarity of water decreases with an increase of temperature, yielding increased elution strength in reversed-phase columns. Therefore, high temperature water can be used as eluent instead of organic solvent for combining reversed-phase liquid chromatography with isotope ratio mass spectrometry (RPLC/IRMS). Additionally, temperature gradients can replace organic solvent gradients to increase chromatographic resolution. This is very important for LC/IRMS analysis, as precise isotope analysis requires baseline separation of analytes. In this thesis, high-temperature reversed-phase liquid chromatography was coupled to, and for the first time carefully

Isotopic analysis of plutonium by computer controlled mass spectrometry

International Nuclear Information System (INIS)

1974-01-01

Isotopic analysis of plutonium chemically purified by ion exchange is achieved using a thermal ionization mass spectrometer. Data acquisition from and control of the instrument is done automatically with a dedicated system computer in real time with subsequent automatic data reduction and reporting. Separation of isotopes is achieved by varying the ion accelerating high voltage with accurate computer control

Optical spectroscopy of laser-produced plasmas for standoff isotopic analysis

Energy Technology Data Exchange (ETDEWEB)

Harilal, Sivanandan S.; Brumfield, Brian E.; LaHaye, Nicole L.; Hartig, Kyle C.; Phillips, Mark C.

2018-04-20

This review article covers the present status of isotope detection through emission, absorption, and fluorescence spectroscopy of atoms and molecules in a laser-produced plasma formed from a solid sample. A description of the physics behind isotope shifts in atoms and molecules is presented, followed by the physics behind solid sampling of laser ablation plumes, optical methods for isotope measurements, the suitable physical conditions of laser-produced plasma plumes for isotopic analysis, and the current status. Finally, concluding remarks will be made on the existing gaps between previous works in the literature and suggestions for future work.

System and method for high precision isotope ratio destructive analysis

Science.gov (United States)

Bushaw, Bruce A; Anheier, Norman C; Phillips, Jon R

2013-07-02

A system and process are disclosed that provide high accuracy and high precision destructive analysis measurements for isotope ratio determination of relative isotope abundance distributions in liquids, solids, and particulate samples. The invention utilizes a collinear probe beam to interrogate a laser ablated plume. This invention provides enhanced single-shot detection sensitivity approaching the femtogram range, and isotope ratios that can be determined at approximately 1% or better precision and accuracy (relative standard deviation).

From position-specific isotope labeling towards soil fluxomics: a novel toolbox to assess the microbial impact on biogeochemical cycles

Science.gov (United States)

Apostel, C.; Dippold, M. A.; Kuzyakov, Y.

2015-12-01

Understanding the microbial impact on C and nutrient cycles is one of the most important challenges in terrestrial biogeochemistry. Transformation of low molecular weight organic substances (LMWOS) is a key step in all biogeochemical cycles because 1) all high molecular substances pass the LMWOS pool during their degradation and 2) only LMWOS can be taken up by microorganisms intact. Thus, the transformations of LMWOS are dominated by biochemical pathways of the soil microorganisms. Thus, understanding fluxes and transformations in soils requires a detailed knowledge on the microbial metabolic network and its control mechanism. Tracing C fate in soil by isotopes became on of the most applied and promising biogeochemistry tools but studies were nearly exclusively based on uniformly labeled substances. However, such tracers do not allow the differentiation of the intact use of the initial substances from its transformation to metabolites. The novel tool of position-specific labeling enables to trace molecule atoms separately and thus to determine the cleavage of molecules - a prerequisite for metabolic tracing. Position-specific labeling of basic metabolites and quantification of isotope incorporation in CO2 and bulk soil enabled following the basic metabolic pathways of microorganisms. However, the combination of position-specific 13C labeling with compound-specific isotope analysis of microbial biomarkers and metabolites like phospholipid fatty acids (PLFA) or amino sugars revealed new insights into the soil fluxome: First, it enables tracing specific anabolic pathways in diverse microbial communities in soils e.g. carbon starvation pathways versus pathways reflecting microbial growth. Second, it allows identification of specific pathways of individual functional microbial groups in soils in situ. Tracing metabolic pathways and understanding their regulating factors are crucial for soil C fluxomics i.e. the unravaling of the complex network of C transformations

Authentication of organically grown plants - advantages and limitations of atomic spectroscopy for multi-element and stable isotope analysis

DEFF Research Database (Denmark)

Laursen, Kristian Holst; Schjørring, Jan Kofod; Kelly, S.D.

2014-01-01

Organic food products are believed to be healthier, safer and more environment-friendly than their conventional counterparts and are sold at premium prices. Consequently, adulteration of organic plants and fraudulent activities for economic profit are increasing. This has spurred the development...... plant tissue, and compound-specific isotope analysis based on isotope ratio-mass spectrometry are promising tools for documenting the fertilization history of organic plants. However, these techniques are challenged by the potential diversity of fertilization practices of organic and conventional plant...

Hg stable isotope analysis by the double-spike method.

Science.gov (United States)

Mead, Chris; Johnson, Thomas M

2010-06-01

Recent publications suggest great potential for analysis of Hg stable isotope abundances to elucidate sources and/or chemical processes that control the environmental impact of mercury. We have developed a new MC-ICP-MS method for analysis of mercury isotope ratios using the double-spike approach, in which a solution containing enriched (196)Hg and (204)Hg is mixed with samples and provides a means to correct for instrumental mass bias and most isotopic fractionation that may occur during sample preparation and introduction into the instrument. Large amounts of isotopic fractionation induced by sample preparation and introduction into the instrument (e.g., by batch reactors) are corrected for. This may greatly enhance various Hg pre-concentration methods by correcting for minor fractionation that may occur during preparation and removing the need to demonstrate 100% recovery. Current precision, when ratios are normalized to the daily average, is 0.06 per thousand, 0.06 per thousand, 0.05 per thousand, and 0.05 per thousand (2sigma) for (202)Hg/(198)Hg, (201)Hg/(198)Hg, (200)Hg/(198)Hg, and (199)Hg/(198)Hg, respectively. This is slightly better than previously published methods. Additionally, this precision was attained despite the presence of large amounts of other Hg isotopes (e.g., 5.0% atom percent (198)Hg) in the spike solution; substantially better precision could be achieved if purer (196)Hg were used.

Results of Am isotopic ratio analysis in irradiated MOX fuels

Energy Technology Data Exchange (ETDEWEB)

Koyama, Shin-ichi; Osaka, Masahiko; Mitsugashira, Toshiaki; Konno, Koichi [Power Reactor and Nuclear Fuel Development Corp., Oarai, Ibaraki (Japan). Oarai Engineering Center; Kajitani, Mikio

1997-04-01

For analysis of a small quantity of americium, it is necessary to separate from curium which has similar chemical property. As a chemical separation method for americium and curium, the oxidation of americium with pentavalent bismuth and subsequent co-precipitation of trivalent curium with BIP O{sub 4} were applied to analyze americium in irradiated MOX fuels which contained about 30wt% plutonium and 0.9wt% {sup 241}Am before irradiation and were irradiated up to 26.2GWd/t in the experimental fast reactor Joyo. The purpose of this study is to measure isotopic ratio of americium and to evaluate the change of isotopic ratio with irradiation. Following results are obtained in this study. (1) The isotopic ratio of americium ({sup 241}Am, {sup 242m}Am and {sup 243}Am) can be analyzed in the MOX fuels by isolating americium. The isotopic ratio of {sup 242m}Am and {sup 243}Am increases up to 0.62at% and 0.82at% at maximum burnup, respectively, (2) The results of isotopic analysis indicates that the contents of {sup 241}Am decreases, whereas {sup 242m}Am, {sup 243}Am increase linearly with increasing burnup. (author)

Gas chromatographic isolation technique for compound-specific radiocarbon analysis

International Nuclear Information System (INIS)

Uchida, M.; Kumamoto, Y.; Shibata, Y.; Yoneda, M.; Morita, M.; Kawamura, K.

2002-01-01

Full text: We present here a gas chromatographic isolation technique for the compound-specific radiocarbon analysis of biomarkers from the marine sediments. The biomarkers of fatty acids, hydrocarbon and sterols were isolated with enough amount for radiocarbon analysis using a preparative capillary gas chromatograph (PCGC) system. The PCGC systems used here is composed of an HP 6890 GC with FID, a cooled injection system (CIS, Gerstel, Germany), a zero-dead-volume effluent splitter, and a cryogenic preparative collection device (PFC, Gerstel). For AMS analysis, we need to separate and recover sufficient quantity of target individual compounds (>50 μgC). Yields of target compounds from C 14 n-alkanes to C 40 to C 30 n-alkanes and approximately that of 80% for higher molecular weights compounds more than C 30 n-alkanes. Compound specific radiocarbon analysis of organic compounds, as well as compound-specific stable isotope analysis, provide valuable information on the origins and carbon cycling in marine system. Above PCGC conditions, we applied compound-specific radiocarbon analysis to the marine sediments from western north Pacific, which showed the possibility of a useful chronology tool for estimating the age of sediment using organic matter in paleoceanographic study, in the area where enough amounts of planktonic foraminifera for radiocarbon analysis by accelerator mass spectrometry (AMS) are difficult to obtain due to dissolution of calcium carbonate. (author)

Cavity Ring-down Spectroscopy for Carbon Isotope Analysis with 2 μm Diode Laser

International Nuclear Information System (INIS)

Hiromoto, K.; Tomita, H.; Watanabe, K.; Kawarabayashi, J.; Iguchi, T.

2009-01-01

We have made a prototype based on CRDS with 2 μm diode laser for carbon isotope analysis of CO 2 in air. The carbon isotope ratio was obtained to be (1.085±0.012)x10 -2 which shows good agreement with the isotope ratio measured by the magnetic sector-type mass spectrometer within uncertainty. Hence, we demonstrated the carbon isotope analysis based on CRDS with 2 μm tunable diode laser.

On the interference of Kr during carbon isotope analysis of methane using continuous-flow combustion–isotope ratio mass spectrometry

NARCIS (Netherlands)

Schmitt, J.; Seth, B.; Bock, M; van der Veen, C.; Möller, L.; Sapart, C.J.; Prokopiou, M.; Sowers, T.; Röckmann, T.; Fischer, H

2013-01-01

Stable carbon isotope analysis of methane ( 13C of CH4) on atmospheric samples is one key method to constrain the current and past atmospheric CH4 budget. A frequently applied measurement technique is gas chromatography (GC) isotope ratio mass spectrometry (IRMS) coupled to a

Chlorine isotope effects from isotope ratio mass spectrometry suggest intramolecular C-Cl bond competition in trichloroethene (TCE) reductive dehalogenation.

Science.gov (United States)

Cretnik, Stefan; Bernstein, Anat; Shouakar-Stash, Orfan; Löffler, Frank; Elsner, Martin

2014-05-20

Chlorinated ethenes are prevalent groundwater contaminants. To better constrain (bio)chemical reaction mechanisms of reductive dechlorination, the position-specificity of reductive trichloroethene (TCE) dehalogenation was investigated. Selective biotransformation reactions (i) of tetrachloroethene (PCE) to TCE in cultures of Desulfitobacterium sp. strain Viet1; and (ii) of TCE to cis-1,2-dichloroethene (cis-DCE) in cultures of Geobacter lovleyi strain SZ were investigated. Compound-average carbon isotope effects were -19.0‰ ± 0.9‰ (PCE) and -12.2‰ ± 1.0‰ (TCE) (95% confidence intervals). Using instrumental advances in chlorine isotope analysis by continuous flow isotope ratio mass spectrometry, compound-average chorine isotope effects were measured for PCE (-5.0‰ ± 0.1‰) and TCE (-3.6‰ ± 0.2‰). In addition, position-specific kinetic chlorine isotope effects were determined from fits of reactant and product isotope ratios. In PCE biodegradation, primary chlorine isotope effects were substantially larger (by -16.3‰ ± 1.4‰ (standard error)) than secondary. In TCE biodegradation, in contrast, the product cis-DCE reflected an average isotope effect of -2.4‰ ± 0.3‰ and the product chloride an isotope effect of -6.5‰ ± 2.5‰, in the original positions of TCE from which the products were formed (95% confidence intervals). A greater difference would be expected for a position-specific reaction (chloride would exclusively reflect a primary isotope effect). These results therefore suggest that both vicinal chlorine substituents of TCE were reactive (intramolecular competition). This finding puts new constraints on mechanistic scenarios and favours either nucleophilic addition by Co(I) or single electron transfer as reductive dehalogenation mechanisms.

Applications of stable isotope analysis in foodstuffs surveillance and environmental research

International Nuclear Information System (INIS)

Pichlmayer, F.; Blochberger, F.

1991-12-01

The instrumental coupling of Elemental Analysis and Mass Spectrometry, constituting a convenient tool for isotope ratio measurements of the bioelements in solid or liquid samples is now well established. Advantages of this technique compared with the so far usual wet chemistry sample preparation are: speed of analysis, easy operation and minor sample consumption. The performance of the system is described and some applications are given. Detection of foodstuffs adulterations is mainly based on the natural carbon isotope differences between C 3 - and C 4 -plants. In the field of environmental research the existing small isotopic variations of carbon, nitrogen and sulfur in nature, which depend on substance origin and history, are used as intrinsic signature of the considered sample. Examples of source appointment or exclusion by help of this natural isotopic tracer method are dealt with. (authors)

Apportioning sources of organic matter in streambed sediments: An integrated molecular and compound-specific stable isotope approach

Energy Technology Data Exchange (ETDEWEB)

Cooper, Richard J., E-mail: Richard.J.Cooper@uea.ac.uk [School of Environmental Sciences, University of East Anglia, Norwich Research Park, Norwich NR4 7TJ (United Kingdom); Pedentchouk, Nikolai; Hiscock, Kevin M.; Disdle, Paul [School of Environmental Sciences, University of East Anglia, Norwich Research Park, Norwich NR4 7TJ (United Kingdom); Krueger, Tobias [IRI THESys, Humboldt University, 10099 Berlin (Germany); Rawlins, Barry G. [British Geological Survey, Keyworth, Nottingham NG12 5GG (United Kingdom)

2015-07-01

We present a novel application for quantitatively apportioning sources of organic matter in streambed sediments via a coupled molecular and compound-specific isotope analysis (CSIA) of long-chain leaf wax n-alkane biomarkers using a Bayesian mixing model. Leaf wax extracts of 13 plant species were collected from across two environments (aquatic and terrestrial) and four plant functional types (trees, herbaceous perennials, and C{sub 3} and C{sub 4} graminoids) from the agricultural River Wensum catchment, UK. Seven isotopic (δ{sup 13}C{sub 27}, δ{sup 13}C{sub 29}, δ{sup 13}C{sub 31}, δ{sup 13}C{sub 27–31}, δ{sup 2}H{sub 27}, δ{sup 2}H{sub 29}, and δ{sup 2}H{sub 27–29}) and two n-alkane ratio (average chain length (ACL), carbon preference index (CPI)) fingerprints were derived, which successfully differentiated 93% of individual plant specimens by plant functional type. The δ{sup 2}H values were the strongest discriminators of plants originating from different functional groups, with trees (δ{sup 2}H{sub 27–29} = − 208‰ to − 164‰) and C{sub 3} graminoids (δ{sup 2}H{sub 27–29} = − 259‰ to − 221‰) providing the largest contrasts. The δ{sup 13}C values provided strong discrimination between C{sub 3} (δ{sup 13}C{sub 27–31} = − 37.5‰ to − 33.8‰) and C{sub 4} (δ{sup 13}C{sub 27–31} = − 23.5‰ to − 23.1‰) plants, but neither δ{sup 13}C nor δ{sup 2}H values could uniquely differentiate aquatic and terrestrial species, emphasizing a stronger plant physiological/biochemical rather than environmental control over isotopic differences. ACL and CPI complemented isotopic discrimination, with significantly longer chain lengths recorded for trees and terrestrial plants compared with herbaceous perennials and aquatic species, respectively. Application of a comprehensive Bayesian mixing model for 18 streambed sediments collected between September 2013 and March 2014 revealed considerable temporal variability in the

Tracing carbon flow in an arctic marine food web using fatty acid-stable isotope analysis.

Science.gov (United States)

Budge, S M; Wooller, M J; Springer, A M; Iverson, S J; McRoy, C P; Divoky, G J

2008-08-01

Global warming and the loss of sea ice threaten to alter patterns of productivity in arctic marine ecosystems because of a likely decline in primary productivity by sea ice algae. Estimates of the contribution of ice algae to total primary production range widely, from just 3 to >50%, and the importance of ice algae to higher trophic levels remains unknown. To help answer this question, we investigated a novel approach to food web studies by combining the two established methods of stable isotope analysis and fatty acid (FA) analysis--we determined the C isotopic composition of individual diatom FA and traced these biomarkers in consumers. Samples were collected near Barrow, Alaska and included ice algae, pelagic phytoplankton, zooplankton, fish, seabirds, pinnipeds and cetaceans. Ice algae and pelagic phytoplankton had distinctive overall FA signatures and clear differences in delta(13)C for two specific diatom FA biomarkers: 16:4n-1 (-24.0+/-2.4 and -30.7+/-0.8 per thousand, respectively) and 20:5n-3 (-18.3+/-2.0 and -26.9+/-0.7 per thousand, respectively). Nearly all delta(13)C values of these two FA in consumers fell between the two stable isotopic end members. A mass balance equation indicated that FA material derived from ice algae, compared to pelagic diatoms, averaged 71% (44-107%) in consumers based on delta(13)C values of 16:4n-1, but only 24% (0-61%) based on 20:5n-3. Our estimates derived from 16:4n-1, which is produced only by diatoms, probably best represented the contribution of ice algae relative to pelagic diatoms. However, many types of algae produce 20:5n-3, so the lower value derived from it likely represented a more realistic estimate of the proportion of ice algae material relative to all other types of phytoplankton. These preliminary results demonstrate the potential value of compound-specific isotope analysis of marine lipids to trace C flow through marine food webs and provide a foundation for future work.

Amino acid specific stable nitrogen isotope values in avian tissues: Insights from captive American kestrels and wild herring gulls

Science.gov (United States)

Hebert, Craig E.; Popp, B.N.; Fernie, K.J.; Ka'apu-Lyons, C.; Rattner, Barnett A.; Wallsgrove, N.

2016-01-01

Through laboratory and field studies, the utility of amino acid compound-specific nitrogen isotope analysis (AA-CSIA) in avian studies is investigated. Captive American kestrels (Falco sparverius) were fed an isotopically characterized diet and patterns in δ15N values of amino acids (AAs) were compared to those in their tissues (muscle and red blood cells) and food. Based upon nitrogen isotope discrimination between diet and kestrel tissues, AAs could mostly be categorized as source AAs (retaining baseline δ15N values) and trophic AAs (showing 15N enrichment). Trophic discrimination factors based upon the source (phenylalanine, Phe) and trophic (glutamic acid, Glu) AAs were 4.1 (muscle) and 5.4 (red blood cells), lower than those reported for metazoan invertebrates. In a field study involving omnivorous herring gulls (Larus argentatus smithsonianus), egg AA isotopic patterns largely retained those observed in the laying female’s tissues (muscle, red blood cells, and liver). Realistic estimates of gull trophic position were obtained using bird Glu and Phe δ15N values combined with β values (difference in Glu and Phe δ15N in primary producers) for aquatic and terrestrial food webs. Egg fatty acids were used to weight β values for proportions of aquatic and terrestrial food in gull diets. This novel approach can be applied to generalist species that feed across ecosystem boundaries.

Quantitative analysis of 39 polybrominated diphenyl ethers by isotope dilution GC/low-resolution MS.

Science.gov (United States)

Ackerman, Luke K; Wilson, Glenn R; Simonich, Staci L

2005-04-01

A GC/low-resolution MS method for the quantitative isotope dilution analysis of 39 mono- to heptabrominated diphenyl ethers was developed. The effects of two different ionization sources, electron impact (EI) and electron capture negative ionization (ECNI), and the effects of their parameters on production of high-mass fragment ions [M - xH - yBr](-) specific to PBDEs were investigated. Electron energy, emission current, source temperature, ECNI system pressure, and choice of ECNI reagent gases were optimized. Previously unidentified enhancement of PBDE high-mass fragment ion [M - xH - yBr](-) abundance was achieved. Electron energy had the largest impact on PBDE high-mass fragment ion abundance for both the ECNI and EI sources. By monitoring high-mass fragment ions of PBDEs under optimized ECNI source conditions, quantitative isotope dilution analysis of 39 PBDEs was conducted using nine (13)C(12) labeled PBDEs on a low-resolution MS with low picogram to femtogram instrument detection limits.

Enantioselective stable isotope analysis (ESIA) — A new concept to evaluate the environmental fate of chiral organic contaminants

International Nuclear Information System (INIS)

Badea, Silviu-Laurentiu; Danet, Andrei-Florin

2015-01-01

Since 2011, the enantiospecific stable carbon isotope analysis (ESIA) has emerged as an innovative technique to assess the environmental fate of chiral emerging compounds by combining in one experimental technique both compound specific isotope analysis (CSIA) and enantioselective analysis. To date, the ESIA was applied for four classes of compounds: α-hexachlorocyclohexane (α-HCH), polar herbicides (phenoxy acids), synthetic polycyclic musk galaxolide (HHCB), and phenoxyalkanoic methyl herbicides. From an analytical point of view there are factors that are hindering the application of ESIA methods for the field samples: (i.e. amounts of target analyte, matrix effects, GC resolution) and overcoming these factors is challenging. While ESIA was shown as a mature technique for the first three abovementioned class of compounds, no isotope analysis of individual enantiomers could be performed for phenoxyalkanoic methyl herbicides. With respect to field studies, one study showed that ESIA might be a promising tool to distinguish between biotic and abiotic transformation pathways of chiral organic contaminants and even to differentiate between their aerobic and anaerobic biotransformation pathways. The development of ESIA methods for new chiral emerging contaminants in combination with development of multi-element isotope analysis will contribute to a better characterization of transformation pathways of chiral organic contaminants. - Highlights: • ESIA is an innovative technique to assess the environmental fate of chiral pollutants • Overcoming the analytical limitations of ESIA is challenging • Development of ESIA methods for new chiral emerging contaminants is needed

Enantioselective stable isotope analysis (ESIA) — A new concept to evaluate the environmental fate of chiral organic contaminants

Energy Technology Data Exchange (ETDEWEB)

Badea, Silviu-Laurentiu, E-mail: badeasilviu@gmail.com [Department of Chemistry, Umeå University, SE-901 87 Umeå (Sweden); Danet, Andrei-Florin [Department of Analytical Chemistry, University of Bucharest, Faculty of Chemistry, 90-92 Panduri Str., Bucharest 050657 (Romania)

2015-05-01

Since 2011, the enantiospecific stable carbon isotope analysis (ESIA) has emerged as an innovative technique to assess the environmental fate of chiral emerging compounds by combining in one experimental technique both compound specific isotope analysis (CSIA) and enantioselective analysis. To date, the ESIA was applied for four classes of compounds: α-hexachlorocyclohexane (α-HCH), polar herbicides (phenoxy acids), synthetic polycyclic musk galaxolide (HHCB), and phenoxyalkanoic methyl herbicides. From an analytical point of view there are factors that are hindering the application of ESIA methods for the field samples: (i.e. amounts of target analyte, matrix effects, GC resolution) and overcoming these factors is challenging. While ESIA was shown as a mature technique for the first three abovementioned class of compounds, no isotope analysis of individual enantiomers could be performed for phenoxyalkanoic methyl herbicides. With respect to field studies, one study showed that ESIA might be a promising tool to distinguish between biotic and abiotic transformation pathways of chiral organic contaminants and even to differentiate between their aerobic and anaerobic biotransformation pathways. The development of ESIA methods for new chiral emerging contaminants in combination with development of multi-element isotope analysis will contribute to a better characterization of transformation pathways of chiral organic contaminants. - Highlights: • ESIA is an innovative technique to assess the environmental fate of chiral pollutants • Overcoming the analytical limitations of ESIA is challenging • Development of ESIA methods for new chiral emerging contaminants is needed.

In vivo synthesized 34S enriched amino acid standards for species specific isotope dilution of proteins

DEFF Research Database (Denmark)

Hermann, Gerrit; Moller, Laura Hyrup; Gammelgaard, Bente

2016-01-01

(ICP-MS) combined to anion exchange showed that very high concentrated spike material could be produced with [small mu ]mol amounts of proteinogenic sulfur containing amino acids per g cell dry weight. An enrichment of 34S to 96.3 +/- 0.4% (n = 3) and 98.5 +/- 0.4% (n = 3) for cysteic acid...... with the concept of species specific isotope dilution analysis (IDA). The method relies on the determination of the two sulfur containing amino acids, cysteine and methionine by sulfur speciation analysis and is hence applicable to any protein containing sulfur. In vivo synthesis using 34S as sulfur source...... and methionine sulfone, respectively, was assessed. The established IDA method was validated for the absolute quantification of commercially available lysozyme and ceruloplasmin standards including the calculation of a total combined uncertainty budget....

Optical spectroscopy versus mass spectrometry: The race for fieldable isotopic analysis

International Nuclear Information System (INIS)

Barshick, C.M.; Young, J.P.; Shaw, R.W.

1995-01-01

Several techniques have been developed to provide on-site isotopic analyses, including decay-counting and mass spectrometry, as well as methods that rely on the accessibility of optical transitions for isotopic selectivity (e.g., laser-induced fluorescence and optogalvanic spectroscopy). The authors have been investigating both mass spectrometry and optogalvanic spectroscopy for several years. Although others have considered these techniques for isotopic analysis, the authors have focussed on the use of a dc glow discharge for atomization and ionization, and a demountable discharge cell for rapid sample exchange. The authors' goal is a fieldable instrument that provides useful uranium isotope ratio information

The use of stable isotopes in medicinal chemistry

International Nuclear Information System (INIS)

Halliday, D.; Thompson, G.N.

1988-01-01

Stable isotopes have been employed increasingly as tracers over the last decade both to provide the clinician with the opportunity to broaden, in a quantitative manner, discrete areas of diagnosis and research, and the clinical chemist with definitive methodology for specific analyte analysis. These non-radioactive 'heavy' isotopes contain one or more extra neutrons in the nucleus compared with their more abundant 'lighter' analogues. Impetus in the application of stable isotopes for in vivo studies has come from an increased awareness of the possible harmful effects in the use of radionuclides, and a realisation of several positive advantages conferred by the use of stable isotopes in their own right - certain elements of clinical importance (especially nitrogen) lack a useable radio-nuclide equivalent; use of a 'cocktail' of stable isotopes permits a range of studies to be performed in the same patient simultaneously and, within specific constraints, serial studies can be performed in the same patients. (author)

Direct uranium isotope ratio analysis of single micrometer-sized glass particles

International Nuclear Information System (INIS)

Kappel, Stefanie; Boulyga, Sergei F.; Prohaska, Thomas

2012-01-01

We present the application of nanosecond laser ablation (LA) coupled to a ‘Nu Plasma HR’ multi collector inductively coupled plasma mass spectrometer (MC-ICP-MS) for the direct analysis of U isotope ratios in single, 10–20 μm-sized, U-doped glass particles. Method development included studies with respect to (1) external correction of the measured U isotope ratios in glass particles, (2) the applied laser ablation carrier gas (i.e. Ar versus He) and (3) the accurate determination of lower abundant 236 U/ 238 U isotope ratios (i.e. 10 −5 ). In addition, a data processing procedure was developed for evaluation of transient signals, which is of potential use for routine application of the developed method. We demonstrate that the developed method is reliable and well suited for determining U isotope ratios of individual particles. Analyses of twenty-eight S1 glass particles, measured under optimized conditions, yielded average biases of less than 0.6% from the certified values for 234 U/ 238 U and 235 U/ 238 U ratios. Experimental results obtained for 236 U/ 238 U isotope ratios deviated by less than −2.5% from the certified values. Expanded relative total combined standard uncertainties U c (k = 2) of 2.6%, 1.4% and 5.8% were calculated for 234 U/ 238 U, 235 U/ 238 U and 236 U/ 238 U, respectively. - Highlights: ► LA-MC-ICP-MS was fully validated for the direct analysis of individual particles. ► Traceability was established by using an IRMM glass particle reference material. ► Measured U isotope ratios were in agreement with the certified range. ► A comprehensive total combined uncertainty evaluation was performed. ► The analysis of 236 U/ 238 U isotope ratios was improved by using a deceleration filter.

Chlorine Isotope Effects from Isotope Ratio Mass Spectrometry Suggest Intramolecular C-Cl Bond Competition in Trichloroethene (TCE Reductive Dehalogenation

Directory of Open Access Journals (Sweden)

Stefan Cretnik

2014-05-01

Full Text Available Chlorinated ethenes are prevalent groundwater contaminants. To better constrain (biochemical reaction mechanisms of reductive dechlorination, the position-specificity of reductive trichloroethene (TCE dehalogenation was investigated. Selective biotransformation reactions (i of tetrachloroethene (PCE to TCE in cultures of Desulfitobacterium sp. strain Viet1; and (ii of TCE to cis-1,2-dichloroethene (cis-DCE in cultures of Geobacter lovleyi strain SZ were investigated. Compound-average carbon isotope effects were −19.0‰ ± 0.9‰ (PCE and −12.2‰ ± 1.0‰ (TCE (95% confidence intervals. Using instrumental advances in chlorine isotope analysis by continuous flow isotope ratio mass spectrometry, compound-average chorine isotope effects were measured for PCE (−5.0‰ ± 0.1‰ and TCE (−3.6‰ ± 0.2‰. In addition, position-specific kinetic chlorine isotope effects were determined from fits of reactant and product isotope ratios. In PCE biodegradation, primary chlorine isotope effects were substantially larger (by −16.3‰ ± 1.4‰ (standard error than secondary. In TCE biodegradation, in contrast, the product cis-DCE reflected an average isotope effect of −2.4‰ ± 0.3‰ and the product chloride an isotope effect of −6.5‰ ± 2.5‰, in the original positions of TCE from which the products were formed (95% confidence intervals. A greater difference would be expected for a position-specific reaction (chloride would exclusively reflect a primary isotope effect. These results therefore suggest that both vicinal chlorine substituents of TCE were reactive (intramolecular competition. This finding puts new constraints on mechanistic scenarios and favours either nucleophilic addition by Co(I or single electron transfer as reductive dehalogenation mechanisms.

Retroconversion is a minor contributor to increases in eicosapentaenoic acid following docosahexaenoic acid feeding as determined by compound specific isotope analysis in rat liver.

Science.gov (United States)

Metherel, Adam H; Chouinard-Watkins, Raphaël; Trépanier, Marc-Olivier; Lacombe, R J Scott; Bazinet, Richard P

2017-01-01

Dietary docosahexaenoic acid (DHA, 22:6n-3) not only increases blood and tissue levels of DHA, but also eicosapentaenoic acid (EPA, 20:5n-3). It is generally believed that this increase is due to DHA retroconversion to EPA, however, a slower conversion of α-linolenic acid (ALA, 18:3n-3) derived EPA to downstream metabolic products (i.e. slower turnover of EPA) is equally plausible. In this study, 21-day old Long Evans rats were weaned onto an ALA only or DHA + ALA diet for 12 weeks. Afterwards, livers were collected and the natural abundance 13 C-enrichment was determined by compound specific isotope analysis (CSIA) of liver EPA by isotope ratio mass-spectrometry and compared to dietary ALA and DHA 13 C-enrichment. Isotopic signatures (per mil, ‰) for liver EPA were not different ( p  > 0.05) between the ALA only diet (-25.89 ± 0.39 ‰, mean ± SEM) and the DHA + ALA diet (-26.26 ± 0.40 ‰), suggesting the relative contribution from dietary ALA and DHA to liver EPA did not change. However, with DHA feeding estimates of absolute EPA contribution from ALA increased 4.4-fold (147 ± 22 to 788 ± 153 nmol/g) compared to 3.2-fold from DHA (91 ± 14 to 382 ± 13 nmol/g), respectively. In conclusion, CSIA of liver EPA in rats following 12-weeks of dietary DHA suggests that retroconversion of DHA to EPA is a relatively small contributor to increases in EPA, and that this increase in EPA is largely coming from elongation/desaturation of ALA.

[Trophic niche partitioning of pelagic sharks in Central Eastern Pacific inferred from stable isotope analysis.

Science.gov (United States)

Li, Yun Kai; Gao, Xiao di; Wang, Lin Yu; Fang, Lin

2018-01-01

As the apex predators of the open ocean ecosystems, pelagic sharks play important roles in stabilizing the marine food web through top-down control. Stable isotope analysis is a powerful tool to investigate the feeding ecology. The carbon and nitrogen isotope ratios can be used to trace food source and evaluate the trophic position of marine organisms. In this study, the isotope values of 130 pelagic sharks from 8 species in Central Eastern Pacific were analyzed and their trophic position and niche were calculated to compare the intra/inter-specific resource partitioning in the Central Eastern Pacific ecosystem. The results exhibited significant differences in both carbon and nitrogen isotope values among the shark species. The trophic levels ranged from 4.3 to 5.4 in the Central Eastern Pacific shark community. The trophic niche of blue sharks and shortfin mako sharks showed no overlap with the other shark species, exhibiting unique ecological roles in the open ocean food web. These data highlighted the diverse roles among pelagic sharks, supporting previous findings that this species is not trophically redundant and the trophic niche of pelagic sharks can not be simply replaced by those of other top predator species.

Oxygen isotope analysis of plant water without extraction procedure

International Nuclear Information System (INIS)

Gan, K.S.; Wong, S.C.; Farquhar, G.D.; Yong, J.W.H.

2001-01-01

Isotopic analyses of plant water (mainly xylem, phloem and leaf water) are gaming importance as the isotopic signals reflect plant-environment interactions, affect the oxygen isotopic composition of atmospheric O 2 and CO 2 and are eventually incorporated into plant organic matter. Conventionally, such isotopic measurements require a time-consuming process of isolating the plant water by azeotropic distillation or vacuum extraction, which would not complement the speed of isotope analysis provided by continuous-flow IRMS (Isotope-Ratio Mass Spectrometry), especially when large data sets are needed for statistical calculations in biological studies. Further, a substantial amount of plant material is needed for water extraction and leaf samples would invariably include unenriched water from the fine veins. To measure sub-microlitre amount of leaf mesophyll water, a new approach is undertaken where a small disc of fresh leaf is cut using a specially designed leaf punch, and pyrolysed directly in an IRMS. By comparing with results from pyrolysis of the dry matter of the same leaf, the 18 O content of leaf water can be determined without extraction from fresh leaves. This method is validated using a range of cellulose-water mixtures to simulate the constituents of fresh leaf. Cotton leaf water δ 18 O obtained from both methods of fresh leaf pyrolysis and azeotropic distillation will be compared. The pyrolysis technique provides a robust approach to measure the isotopic content of water or any volatile present in a homogeneous solution or solid hydrous substance

Site-Specific Hydrogen Isotope Composition of Propane: Mass spectrometric methods, equilibrium temperature dependence, and kinetics of exchange

Science.gov (United States)

Xie, H.; Ponton, C.; Kitchen, N.; Lloyd, M. K.; Lawson, M.; Formolo, M. J.; Eiler, J. M.

2016-12-01

Intramolecular isotope ordering can constrain temperatures of synthesis, mechanisms of formation, and/or source substrates of organic compounds. Here we explore site-specific hydrogen isotope variations of propane. Statistical thermodynamic models predict that at equilibrium methylene hydrogen (-CH2-) in propane will be 10's of per mil higher in D/H ratio than methyl hydrogen (-CH3) at geologically relevant temperatures, and that this difference is highly temperature dependent ( 0.5-1 ‰/°C). Chemical-kinetic controls on site-specific D/H in propane could constrain the mechanisms, conditions and extents of propane synthesis or destruction. We have developed a method for measuring the difference in D/H ratio between methylene and methyl hydrogen in propane by gas source mass spectrometry. The data were measured using the Thermo Fisher Double Focusing Sector high resolution mass spectrometer (DFS), and involve comparison of the D/H ratios of molecular ion (C3H8+) and the ethyl fragmental ion (C2H5+). We demonstrate the accuracy and precision of this method through analysis of D-labeled and independently analyzed propanes. In the exchange experiments, propane was heated (100-200 oC) either alone or in the presence of D-enriched water (δD=1,1419 ‰ SMOW), with or without one of several potentially catalytic substrates for hours to weeks. Propane was found to exchange hydrogen with water vigorously at 200 °C in the presence of metal catalysts. In the presence of Ni catalyst, methylene hydrogen exchanges 2.5 times faster than methyl hydrogen. Hydrogen exchange in the presence of Pd catalyst is more effective and can equilibrate hydrogen isotope distribution on propane on the order of 7 days. Isotopic exchange in the presence of natural materials have also been tested, but is only measurable in the methylene group at 200 °C. High catalytic activity of Pd permits attainment of a bracketed, time-invariant equilibrium state that we use to calibrate the site-specific

Maintaining high precision of isotope ratio analysis over extended periods of time.

Science.gov (United States)

Brand, Willi A

2009-06-01

Stable isotope ratios are reliable and long lasting process tracers. In order to compare data from different locations or different sampling times at a high level of precision, a measurement strategy must include reliable traceability to an international stable isotope scale via a reference material (RM). Since these international RMs are available in low quantities only, we have developed our own analysis schemes involving laboratory working RM. In addition, quality assurance RMs are used to control the long-term performance of the delta-value assignments. The analysis schemes allow the construction of quality assurance performance charts over years of operation. In this contribution, the performance of three typical techniques established in IsoLab at the MPI-BGC in Jena is discussed. The techniques are (1) isotope ratio mass spectrometry with an elemental analyser for delta(15)N and delta(13)C analysis of bulk (organic) material, (2) high precision delta(13)C and delta(18)O analysis of CO(2) in clean-air samples, and (3) stable isotope analysis of water samples using a high-temperature reaction with carbon. In addition, reference strategies on a laser ablation system for high spatial resolution delta(13)C analysis in tree rings is exemplified briefly.

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.

Diets of nesting laughing gulls (Larus atricilla) at the Virginia Coast Reserve: observations from stable isotope analysis

Science.gov (United States)

Knoff, A.J.; Macko, S.A.; Erwin, R.M.

2001-01-01

Food web studies often ignore details of temporal, spatial, and intrapopulation dietary variation in top-level consumers. In this study, intrapopulation dietary variation of a dominant carnivore, the Laughing Gull (Larus atricilla), was examined using carbon, nitrogen, and sulfur isotope analysis of gull tissues as well as their prey (fish, invertebrates, and insects) from the Virginia Coast Reserve estuarine system. As earlier traditional diet studies found evidence of individual dietary specialization within gull populations, this study used stable isotope analysis to assess specialization in a coastal Laughing Gull population. Specifically, blood, muscle, and feather isotope values indicated significant intrapopulation dietary specialization. Some gulls relied more heavily on estuarine prey (mean blood δ13C = -17.5, δ15N = 12.6, and δ34S = 9.3), whereas others appeared to consume more foods of marine origin (mean blood δ13C = -19.4, δ15N = 14.8, and δ34S = 10.4). It is important to account for such dietary variability when assessing trophic linkages in dynamic estuarine systems.

Development of isotope dilution gamma-ray spectrometry for plutonium analysis

Energy Technology Data Exchange (ETDEWEB)

Li, T.K.; Parker, J.L. (Los Alamos National Lab., NM (United States)); Kuno, Y.; Sato, S.; Kurosawa, A.; Akiyama, T. (Power Reactor and Nuclear Fuel Development Corp., Tokai, Ibaraki (Japan))

1991-01-01

We are studying the feasibility of determining the plutonium concentration and isotopic distribution of highly radioactive, spent-fuel dissolver solutions by employing high-resolution gamma-ray spectrometry. The study involves gamma-ray plutonium isotopic analysis for both dissolver and spiked dissolver solution samples, after plutonium is eluted through an ion-exchange column and absorbed in a small resin bead bag. The spike is well characterized, dry plutonium containing {approximately}98% of {sup 239}Pu. By using measured isotopic information, the concentration of elemental plutonium in the dissolver solution can be determined. Both the plutonium concentration and the isotopic composition of the dissolver solution obtained from this study agree well with values obtained by traditional isotope dilution mass spectrometry (IDMS). Because it is rapid, easy to operate and maintain, and costs less, this new technique could be an alternative method to IDMS for input accountability and verification measurements in reprocessing plants. 7 refs., 4 figs., 4 tabs.

Isotopic analysis of boron by thermal ionization mass spectrometry

International Nuclear Information System (INIS)

Kakazu, M.H.; Sarkis, J.E.S.; Souza, I.M.S.

1991-07-01

This paper presents a methodology for isotopic analysis of boron by thermal ionization mass spectrometry technique through the ion intensity measurement of Na 2 BO + 2 in H 3 BO 3 , B o and B 4 C. The samples were loaded on single tantalum filaments by different methods. In the case of H 3 BO 3 , the method of neutralization with NaOH was used. For B 4 C the alcaline fusion with Na 2 CO 3 and for B o dissolution with 1:1 nitric sulfuric acid mixture followed by neutralization with NaOH was used. The isotopic ratio measurements were obtained by the use of s Faraday cup detector with external precision of ±0,4% and accuracy of ±0,1%, relative to H 3 BO 3 isotopic standard NBS 951. The effects of isotopic fractionation was studied in function of the time during the analyses and the different chemical forms of deposition. (author)

Characterization of wines according the geographical origin by analysis of isotopes and minerals and the influence of harvest on the isotope values.

Science.gov (United States)

Dutra, S V; Adami, L; Marcon, A R; Carnieli, G J; Roani, C A; Spinelli, F R; Leonardelli, S; Vanderlinde, R

2013-12-01

We studied Brazilian wines produced by microvinification from Cabernet Sauvignon and Merlot grapes, vintages 2007 and 2008, from the Serra Gaúcha, Campanha and Serra do Sudeste regions, in order to differentiate them according to geographical origin by using isotope and mineral element analyses. In addition, the influence of vintage production in isotope values was verified. Isotope analysis was performed by isotope ratio mass spectrometry (IRMS), and the determination of minerals was by flame atomic absorption (FAA). The best parameters to classify the wines in the 2008 vintage were Rb and Li. The results of the δ(13)C of wine ethanol, Rb and Li showed a significant difference between the varieties regardless of the region studied. The δ(18)O values of water and δ(13)C of ethanol showed significant differences, regardless of the variety. Discriminant analysis of isotope and minerals values allowed to classify approximately 80% of the wines from the three regions studied. Copyright © 2013 Elsevier Ltd. All rights reserved.

Isotope analysis of micro metal particles by adopting laser-ablation mass spectrometry

International Nuclear Information System (INIS)

Song, Kyu Seok; Ha, Young Kyung; Han, Sun Ho; Park, Yong Joon; Kim, Won Ho

2005-01-01

The isotope analysis of microparticles in environmental samples as well as laboratory samples is an important task. A special concern is necessary in particle analysis of swipe samples. Micro particles are normally analyzed either by dissolving particles in the solvents and adopting conventional analytical methods or direct analysis method such as a laser-ablation ICP mass spectrometry (LA-ICP-MS), SIMS, and SNMS (sputtered neutral mass spectrometry). But the LA-ICPMS uses large amount of samples because normally laser beam is tightly focused on the target particle for the complete ablation. The SIMS and SNMS utilize ion beams for the generation of sample ions from the particle. But the number of ions generated by an ion beam is less than 5% of the total generated particles in SIMS. The SNMS is also an excellent analytical technique for particle analysis, however, ion beam and frequency tunable laser system are required for the analysis. Recently a direct analysis of elements as well as isotopes by using laser-ablation is recognized one of the most efficient detection technology for particle samples. The laser-ablation mass spectrometry requires only one laser source without frequency tuneability with no sample pretreatment. Therefore this technique is one of the simplest analysis techniques for solid samples as well as particles. In this study as a part of the development of the new isotope analysis techniques for particles samples, a direct laser-ablation is adopted with mass spectrometry. Zinc and gadolinium were chosen as target samples, since these elements have isotopes with minor abundance (0.62% for Zn, and 0.2% for Gd). The preliminary result indicates that isotopes of these two elements are analyzed within 10% of natural abundance with good mass resolution by using direct laser-ablation mass spectrometry

Bulk and compound-specific isotope analysis of long-chain n-alkanes from a 85,000 year sediment core from Lake Peten Petén Itzá, Guatemala

Science.gov (United States)

Mays, J.; Brenner, M.; Curtis, J. H.; Curtis, K.; Hodell, D. A.; Correa-Metrio, A.; Escobar, J.; Dutton, A. L.; Zimmerman, A. R.; Guilderson, T. P.

2013-12-01

Sediment core PI-6 from Lake Petén Itzá, Guatemala possesses an 85-ka record of climate from lowland Central America. Variations in sediment lithology suggest large, abrupt changes in precipitation during the last glacial and deglacial periods, and into the early Holocene. Study of cores from nearby Lake Quexil demonstrated the utility of using the carbon isotopic composition of leaf wax n-alkanes to infer changes in terrestrial vegetation (Huang et al. 2001). Forty-nine samples were taken from composite Petén Itzá core PI-6 to measure carbon isotopes of bulk organic carbon and long-chain n alkanes. Changes in δ13C values indicate shifts in the relative proportion of C3 to C4 biomass. The record shows largest δ13C variations are associated with Heinrich Events. Carbon isotope values in sediments deposited during the Last Glacial Maximum (LGM) indicate moderate precipitation and little rainfall fluctuation. The deglacial was a period of pronounced climate variability, e.g. the Bölling-Allerod and Younger Dryas. Arid times of the deglacial were inferred from samples with the greatest δ13C values in organic matter, reflecting the largest proportion of C4 plants. Such inferences are supported by stable isotope measurements on ostracod shells and analysis of pollen from the same sample depths in core PI-6. Carbon stable isotope measures on bulk organic carbon and n alkane compounds show similar trends throughout the record and the C:N ratio of Petén Itzá sediments indicates a predominantly allochthonous source for bulk organic matter. Hence, isotope measures on bulk organic carbon (δ13CTOC) in sediments from this lake are sufficient to infer climate-driven shifts in vegetation, making n-alkane extraction and isotope analysis superfluous.

High burn-up plutonium isotopic compositions recommended for use in shielding analysis

International Nuclear Information System (INIS)

Zimmerman, M.G.

1977-06-01

Isotopic compositions for plutonium generated and recycled in LWR's were estimated for use in shielding calculations. The values were obtained by averaging isotopic values from many sources in the literature. These isotopic values should provide the basis for a reasonable prediction of exposure rates from the range of LWR fuel expected in the future. The isotopic compositions given are meant to be used for shielding calculations, and the values are not necessarily applicable to other forms of analysis, such as inventory assessment or criticality safety. 11 tables, 2 figs

Spectral analysis software improves confidence in plant and soil water stable isotope analyses performed by isotope ratio infrared spectroscopy (IRIS).

Science.gov (United States)

West, A G; Goldsmith, G R; Matimati, I; Dawson, T E

2011-08-30

Previous studies have demonstrated the potential for large errors to occur when analyzing waters containing organic contaminants using isotope ratio infrared spectroscopy (IRIS). In an attempt to address this problem, IRIS manufacturers now provide post-processing spectral analysis software capable of identifying samples with the types of spectral interference that compromises their stable isotope analysis. Here we report two independent tests of this post-processing spectral analysis software on two IRIS systems, OA-ICOS (Los Gatos Research Inc.) and WS-CRDS (Picarro Inc.). Following a similar methodology to a previous study, we cryogenically extracted plant leaf water and soil water and measured the δ(2)H and δ(18)O values of identical samples by isotope ratio mass spectrometry (IRMS) and IRIS. As an additional test, we analyzed plant stem waters and tap waters by IRMS and IRIS in an independent laboratory. For all tests we assumed that the IRMS value represented the "true" value against which we could compare the stable isotope results from the IRIS methods. Samples showing significant deviations from the IRMS value (>2σ) were considered to be contaminated and representative of spectral interference in the IRIS measurement. Over the two studies, 83% of plant species were considered contaminated on OA-ICOS and 58% on WS-CRDS. Post-analysis, spectra were analyzed using the manufacturer's spectral analysis software, in order to see if the software correctly identified contaminated samples. In our tests the software performed well, identifying all the samples with major errors. However, some false negatives indicate that user evaluation and testing of the software are necessary. Repeat sampling of plants showed considerable variation in the discrepancies between IRIS and IRMS. As such, we recommend that spectral analysis of IRIS data must be incorporated into standard post-processing routines. Furthermore, we suggest that the results from spectral analysis be

HTSSIP: An R package for analysis of high throughput sequencing data from nucleic acid stable isotope probing (SIP experiments.

Directory of Open Access Journals (Sweden)

Nicholas D Youngblut

Full Text Available Combining high throughput sequencing with stable isotope probing (HTS-SIP is a powerful method for mapping in situ metabolic processes to thousands of microbial taxa. However, accurately mapping metabolic processes to taxa is complex and challenging. Multiple HTS-SIP data analysis methods have been developed, including high-resolution stable isotope probing (HR-SIP, multi-window high-resolution stable isotope probing (MW-HR-SIP, quantitative stable isotope probing (qSIP, and ΔBD. Currently, there is no publicly available software designed specifically for analyzing HTS-SIP data. To address this shortfall, we have developed the HTSSIP R package, an open-source, cross-platform toolset for conducting HTS-SIP analyses in a straightforward and easily reproducible manner. The HTSSIP package, along with full documentation and examples, is available from CRAN at https://cran.r-project.org/web/packages/HTSSIP/index.html and Github at https://github.com/buckleylab/HTSSIP.

High precision analysis of trace lithium isotope by thermal ionization mass spectrometry

International Nuclear Information System (INIS)

Tang Lei; Liu Xuemei; Long Kaiming; Liu Zhao; Yang Tianli

2010-01-01

High precision analysis method of ng lithium by thermal ionization mass spectrometry is developed. By double-filament measurement,phosphine acid ion enhancer and sample pre-baking technique,the precision of trace lithium analysis is improved. For 100 ng lithium isotope standard sample, relative standard deviation is better than 0.086%; for 10 ng lithium isotope standard sample, relative standard deviation is better than 0.90%. (authors)

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

Protein-based stable isotope probing.

Science.gov (United States)

Jehmlich, Nico; Schmidt, Frank; Taubert, Martin; Seifert, Jana; Bastida, Felipe; von Bergen, Martin; Richnow, Hans-Hermann; Vogt, Carsten

2010-12-01

We describe a stable isotope probing (SIP) technique that was developed to link microbe-specific metabolic function to phylogenetic information. Carbon ((13)C)- or nitrogen ((15)N)-labeled substrates (typically with >98% heavy label) were used in cultivation experiments and the heavy isotope incorporation into proteins (protein-SIP) on growth was determined. The amount of incorporation provides a measure for assimilation of a substrate, and the sequence information from peptide analysis obtained by mass spectrometry delivers phylogenetic information about the microorganisms responsible for the metabolism of the particular substrate. In this article, we provide guidelines for incubating microbial cultures with labeled substrates and a protocol for protein-SIP. The protocol guides readers through the proteomics pipeline, including protein extraction, gel-free and gel-based protein separation, the subsequent mass spectrometric analysis of peptides and the calculation of the incorporation of stable isotopes into peptides. Extraction of proteins and the mass fingerprint measurements of unlabeled and labeled fractions can be performed in 2-3 d.

Isotopic neutron sources for neutron activation analysis

International Nuclear Information System (INIS)

Hoste, J.

1988-06-01

This User's Manual is an attempt to provide for teaching and training purposes, a series of well thought out demonstrative experiments in neutron activation analysis based on the utilization of an isotopic neutron source. In some cases, these ideas can be applied to solve practical analytical problems. 19 refs, figs and tabs

Microcalorimeter Q-spectroscopy for rapid isotopic analysis of trace actinide samples

Energy Technology Data Exchange (ETDEWEB)

Croce, M.P., E-mail: mpcroce@lanl.gov [Los Alamos National Laboratory, Los Alamos, NM (United States); Bond, E.M.; Hoover, A.S.; Kunde, G.J.; Mocko, V.; Rabin, M.W.; Weisse-Bernstein, N.R.; Wolfsberg, L.E. [Los Alamos National Laboratory, Los Alamos, NM (United States); Bennett, D.A.; Hays-Wehle, J.; Schmidt, D.R.; Ullom, J.N. [National Institute of Standards and Technology, Boulder, CO (United States)

2015-06-01

We are developing superconducting transition-edge sensor (TES) microcalorimeters that are optimized for rapid isotopic analysis of trace actinide samples by Q-spectroscopy. By designing mechanically robust TESs and simplified detector assembly methods, we have developed a detector for Q-spectroscopy of actinides that can be assembled in minutes. We have characterized the effects of each simplification and present the results. Finally, we show results of isotopic analysis of plutonium samples with Q-spectroscopy detectors and compare the results to mass spectrometry.

Microcalorimeter Q-spectroscopy for rapid isotopic analysis of trace actinide samples

International Nuclear Information System (INIS)

Croce, M.P.; Bond, E.M.; Hoover, A.S.; Kunde, G.J.; Mocko, V.; Rabin, M.W.; Weisse-Bernstein, N.R.; Wolfsberg, L.E.; Bennett, D.A.; Hays-Wehle, J.; Schmidt, D.R.; Ullom, J.N.

2015-01-01

We are developing superconducting transition-edge sensor (TES) microcalorimeters that are optimized for rapid isotopic analysis of trace actinide samples by Q-spectroscopy. By designing mechanically robust TESs and simplified detector assembly methods, we have developed a detector for Q-spectroscopy of actinides that can be assembled in minutes. We have characterized the effects of each simplification and present the results. Finally, we show results of isotopic analysis of plutonium samples with Q-spectroscopy detectors and compare the results to mass spectrometry

Potential application of gas chromatography to the analysis of hydrogen isotopes

International Nuclear Information System (INIS)

Warner, D.K.; Sprague, R.E.; Bohl, D.R.

1976-01-01

Gas chromatography is used at Mound Laboratory for the analysis of hydrogen isotopic impurities in gas mixtures. This instrumentation was used to study the applicability of the gas chromatography technique to the determination of the major components of hydrogen isotopic gas mixtures. The results of this study, including chromatograms and precision data, are presented

Discrimination of ginseng cultivation regions using light stable isotope analysis.

Science.gov (United States)

Kim, Kiwook; Song, Joo-Hyun; Heo, Sang-Cheol; Lee, Jin-Hee; Jung, In-Woo; Min, Ji-Sook

2015-10-01

Korean ginseng is considered to be a precious health food in Asia. Today, thieves frequently compromise ginseng farms by pervasive theft. Thus, studies regarding the characteristics of ginseng according to growth region are required in order to deter ginseng thieves and prevent theft. In this study, 6 regions were selected on the basis of Korea regional criteria (si, gun, gu), and two ginseng-farms were randomly selected from each of the 6 regions. Then 4-6 samples of ginseng were acquired from each ginseng farm. The stable isotopic compositions of H, O, C, and N of the collected ginseng samples were analyzed. As a result, differences in the hydrogen isotope ratios could be used to distinguish regional differences, and differences in the nitrogen isotope ratios yielded characteristic information regarding the farms from which the samples were obtained. Thus, stable isotope values could be used to differentiate samples according to regional differences. Therefore, stable isotope analysis serves as a powerful tool to discriminate the regional origin of Korean ginseng samples from across Korea. Copyright © 2015 Elsevier Ireland Ltd. All rights reserved.

Dissolution of barite for the analysis of strontium isotopes and other chemical and isotopic variations using aqueous sodium carbonate

Science.gov (United States)

Breit, G.N.; Simmons, E.C.; Goldhaber, M.B.

1985-01-01

A simple procedure for preparing barite samples for chemical and isotopic analysis is described. Sulfate ion, in barite, in the presence of high concentrations of aqueous sodium carbonate, is replaced by carbonate. This replacement forms insoluble carbonates with the cations commonly in barite: Ba, Sr, Ca and Pb. Sulfate is released into the solution by the carbonate replacement and is separated by filtration. The aqueous sulfate can then be reprecipitated for analysis of the sulfur and oxygen isotopes. The cations in the carbonate phase can be dissolved by acidifying the solid residue. Sr can be separated from the solution for Sr isotope analysis by ion-exchange chromatography. The sodium carbonate used contains amounts of Sr which will affect almost all barite 87Sr 86Sr ratios by less than 0.00001 at 1.95?? of the mean. The procedure is preferred over other techniques used for preparing barite samples for the determination of 87Sr 86Sr ratios because it is simple, rapid and enables simultaneous determination of many compositional parameters on the same material. ?? 1985.

Sensitive and substrate-specific detection of metabolically active microorganisms in natural microbial consortia using community isotope arrays.

Science.gov (United States)

Tourlousse, Dieter M; Kurisu, Futoshi; Tobino, Tomohiro; Furumai, Hiroaki

2013-05-01

The goal of this study was to develop and validate a novel fosmid-clone-based metagenome isotope array approach - termed the community isotope array (CIArray) - for sensitive detection and identification of microorganisms assimilating a radiolabeled substrate within complex microbial communities. More specifically, a sample-specific CIArray was used to identify anoxic phenol-degrading microorganisms in activated sludge treating synthetic coke-oven wastewater in a single-sludge predenitrification-nitrification process. Hybridization of the CIArray with DNA from the (14) C-phenol-amended sample indicated that bacteria assimilating (14) C-atoms, presumably directly from phenol, under nitrate-reducing conditions were abundant in the reactor, and taxonomic assignment of the fosmid clone end sequences suggested that they belonged to the Gammaproteobacteria. The specificity of the CIArray was validated by quantification of fosmid-clone-specific DNA in density-resolved DNA fractions from samples incubated with (13) C-phenol, which verified that all CIArray-positive probes stemmed from microorganisms that assimilated isotopically labeled carbon. This also demonstrated that the CIArray was more sensitive than DNA-SIP, as the former enabled positive detection at a phenol concentration that failed to yield a 'heavy' DNA fraction. Finally, two operational taxonomic units distantly related to marine Gammaproteobacteria were identified to account for more than half of 16S rRNA gene clones in the 'heavy' DNA library, corroborating the CIArray-based identification. © 2013 Federation of European Microbiological Societies. Published by Blackwell Publishing Ltd. All rights reserved.

Analysis of anaerobic BTX biodegradation in a subarctic aquifer using isotopes and benzylsuccinates.

Science.gov (United States)

McKelvie, Jennifer R; Lindstrom, Jon E; Beller, Harry R; Richmond, Sharon A; Sherwood Lollar, Barbara

2005-12-01

In situ biodegradation of benzene, toluene, and xylenes in a petroleum hydrocarbon contaminated aquifer near Fairbanks, Alaska was assessed using carbon and hydrogen compound specific isotope analysis (CSIA) of benzene and toluene and analysis of signature metabolites for toluene (benzylsuccinate) and xylenes (methylbenzylsuccinates). Carbon and hydrogen isotope ratios of benzene were between -25.9 per thousand and -26.8 per thousand for delta13C and -119 per thousand and -136 per thousand for delta2H, suggesting that biodegradation of benzene is unlikely at this site. However, biodegradation of both xylenes and toluene were documented in this subarctic aquifer. Biodegradation of xylenes was indicated by the presence of methylbenzylsuccinates with concentrations of 17-50 microg/L in three wells. Anaerobic toluene biodegradation was also indicated by benzylsuccinate concentrations of 10-49 microg/L in the three wells with the highest toluene concentrations (1500-5000 microg/L toluene). Since benzylsuccinate typically accounts for a very small fraction of the toluene present in groundwater (generally data is particularly valuable given the challenge of verifying biodegradation in subarctic environments where degradation rates are typically much slower than in temperate environments.

Progress in the analysis and interpretation of N2O isotopes: Potential and future challenges

Science.gov (United States)

Mohn, Joachim; Tuzson, Béla; Zellweger, Christoph; Harris, Eliza; Ibraim, Erkan; Yu, Longfei; Emmenegger, Lukas

2017-04-01

In recent years, research on nitrous oxide (N2O) stable isotopes has significantly advanced, addressing an increasing number of research questions in biogeochemical and atmospheric sciences [1]. An important milestone was the development of quantum cascade laser based spectroscopic devices [2], which are inherently specific for structural isomers (15N14N16O vs. 14N15N16O) and capable to collect real-time data with high temporal resolution, complementary to the well-established isotope-ratio mass-spectrometry (IRMS) method. In combination with automated preconcentration, optical isotope ratio spectroscopy (OIRS) has been applied to disentangle source processes in suburban, rural and pristine environments [e.g. 3, 4]. Within the European Metrology Research Programme (EMRP) ENV52 project "Metrology for high-impact greenhouse gases (HIGHGAS)", the quality of N2O stable isotope analysis by OIRS, the comparability between laboratories, and the traceability to the international isotope ratio scales have been addressed. An inter-laboratory comparison between eleven IRMS and OIRS laboratories, organised within HIGHGAS, indicated limited comparability for 15N site preference, i.e. the difference between 15N abundance in central (N*NO) and end (*NNO) position [5]. In addition, the accuracy of the NH4NO3 decomposition reaction, which provides the link between 15N site preference and the international 15N/14N scale, was found to be limited by non-quantitative NH4NO3 decomposition in combination with substantially different isotope enrichment factors for both nitrogen atoms [6]. Results of the HIGHGAS project indicate that the following research tasks have to be completed to foster research on N2O isotopes: 1) develop improved techniques to link the 15N and 18O abundance and the 15N site preference in N2O to the international stable isotope ratio scales; 2) provide N2O reference materials, pure and diluted in an air matrix, to improve inter-laboratory compatibility. These tasks

System design specification Brayton Isotope Power System (BIPS) Flight System (FS), and Ground Demonstration System (GDS)

International Nuclear Information System (INIS)

1976-01-01

The system design specification for ground demonstration, development, and flight qualification of a Brayton Isotope Power System (BIPS) is presented. The requirements for both a BIPS conceptual Flight System (FS) and a Ground Demonstration System (GDS) are defined

Principles of isotopic analysis by mass spectrometry

International Nuclear Information System (INIS)

Herrmann, M.

1980-01-01

The use of magnetic sector field mass spectrometers in isotopic analysis, especially for nitrogen gas, is outlined. Two measuring methods are pointed out: the scanning mode for significantly enriched samples and the double collector method for samples near the natural abundance of 15 N. The calculation formulas are derived and advice is given for corrections. (author)

Cooperation on Improved Isotopic Identification and Analysis Software for Portable, Electrically Cooled High-Resolution Gamma Spectrometry Systems Final Report

Energy Technology Data Exchange (ETDEWEB)

Dreyer, Jonathan G. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Wang, Tzu-Fang [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Vo, Duc T. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Funk, Pierre F. [Inst. for Radiological Protection and Nuclear Safety (IRSN), Fontenay-aux-Roses (France); Weber, Anne-Laure [Inst. for Radiological Protection and Nuclear Safety (IRSN), Fontenay-aux-Roses (France)

2017-07-20

Under a 2006 agreement between the Department of Energy (DOE) of the United States of America and the Institut de Radioprotection et de Sûreté Nucléaire (IRSN) of France, the National Nuclear Security Administration (NNSA) within DOE and IRSN initiated a collaboration to improve isotopic identification and analysis of nuclear material [i.e., plutonium (Pu) and uranium (U)]. The specific aim of the collaborative project was to develop new versions of two types of isotopic identification and analysis software: (1) the fixed-energy response-function analysis for multiple energies (FRAM) codes and (2) multi-group analysis (MGA) codes. The project is entitled Action Sheet 4 – Cooperation on Improved Isotopic Identification and Analysis Software for Portable, Electrically Cooled, High-Resolution Gamma Spectrometry Systems (Action Sheet 4). FRAM and MGA/U235HI are software codes used to analyze isotopic ratios of U and Pu. FRAM is an application that uses parameter sets for the analysis of U or Pu. MGA and U235HI are two separate applications that analyze Pu or U, respectively. They have traditionally been used by safeguards practitioners to analyze gamma spectra acquired with high-resolution gamma spectrometry (HRGS) systems that are cooled by liquid nitrogen. However, it was discovered that these analysis programs were not as accurate when used on spectra acquired with a newer generation of more portable, electrically cooled HRGS (ECHRGS) systems. In response to this need, DOE/NNSA and IRSN collaborated to update the FRAM and U235HI codes to improve their performance with newer ECHRGS systems. Lawrence Livermore National Laboratory (LLNL) and Los Alamos National Laboratory (LANL) performed this work for DOE/NNSA.

Quantifying inter-laboratory variability in stable isotope analysis of ancient skeletal remains.

Directory of Open Access Journals (Sweden)

William J Pestle

Full Text Available Over the past forty years, stable isotope analysis of bone (and tooth collagen and hydroxyapatite has become a mainstay of archaeological and paleoanthropological reconstructions of paleodiet and paleoenvironment. Despite this method's frequent use across anthropological subdisciplines (and beyond, the present work represents the first attempt at gauging the effects of inter-laboratory variability engendered by differences in a sample preparation, and b analysis (instrumentation, working standards, and data calibration. Replicate analyses of a 14C-dated ancient human bone by twenty-one archaeological and paleoecological stable isotope laboratories revealed significant inter-laboratory isotopic variation for both collagen and carbonate. For bone collagen, we found a sizeable range of 1.8‰ for δ13Ccol and 1.9‰ for δ15Ncol among laboratories, but an interpretatively insignificant average pairwise difference of 0.2‰ and 0.4‰ for δ13Ccol and δ15Ncol respectively. For bone hydroxyapatite the observed range increased to a troublingly large 3.5‰ for δ13Cap and 6.7‰ for δ18Oap, with average pairwise differences of 0.6‰ for δ13Cap and a disquieting 2.0‰ for δ18Oap. In order to assess the effects of preparation versus analysis on isotopic variability among laboratories, a subset of the samples prepared by the participating laboratories were analyzed a second time on the same instrument. Based on this duplicate analysis, it was determined that roughly half of the isotopic variability among laboratories could be attributed to differences in sample preparation, with the other half resulting from differences in analysis (instrumentation, working standards, and data calibration. These findings have serious implications for choices made in the preparation and extraction of target biomolecules, the comparison of results obtained from different laboratories, and the interpretation of small differences in bone collagen and hydroxyapatite

Quantifying inter-laboratory variability in stable isotope analysis of ancient skeletal remains.

Science.gov (United States)

Pestle, William J; Crowley, Brooke E; Weirauch, Matthew T

2014-01-01

Over the past forty years, stable isotope analysis of bone (and tooth) collagen and hydroxyapatite has become a mainstay of archaeological and paleoanthropological reconstructions of paleodiet and paleoenvironment. Despite this method's frequent use across anthropological subdisciplines (and beyond), the present work represents the first attempt at gauging the effects of inter-laboratory variability engendered by differences in a) sample preparation, and b) analysis (instrumentation, working standards, and data calibration). Replicate analyses of a 14C-dated ancient human bone by twenty-one archaeological and paleoecological stable isotope laboratories revealed significant inter-laboratory isotopic variation for both collagen and carbonate. For bone collagen, we found a sizeable range of 1.8‰ for δ13Ccol and 1.9‰ for δ15Ncol among laboratories, but an interpretatively insignificant average pairwise difference of 0.2‰ and 0.4‰ for δ13Ccol and δ15Ncol respectively. For bone hydroxyapatite the observed range increased to a troublingly large 3.5‰ for δ13Cap and 6.7‰ for δ18Oap, with average pairwise differences of 0.6‰ for δ13Cap and a disquieting 2.0‰ for δ18Oap. In order to assess the effects of preparation versus analysis on isotopic variability among laboratories, a subset of the samples prepared by the participating laboratories were analyzed a second time on the same instrument. Based on this duplicate analysis, it was determined that roughly half of the isotopic variability among laboratories could be attributed to differences in sample preparation, with the other half resulting from differences in analysis (instrumentation, working standards, and data calibration). These findings have serious implications for choices made in the preparation and extraction of target biomolecules, the comparison of results obtained from different laboratories, and the interpretation of small differences in bone collagen and hydroxyapatite isotope values

Chromatographic speciation of Cr(III)-species, inter-species equilibrium isotope fractionation and improved chemical purification strategies for high-precision isotope analysis.

Science.gov (United States)

Larsen, K K; Wielandt, D; Schiller, M; Bizzarro, M

2016-04-22

Chromatographic purification of chromium (Cr), which is required for high-precision isotope analysis, is complicated by the presence of multiple Cr-species with different effective charges in the acid digested sample aliquots. The differing ion exchange selectivity and sluggish reaction rates of these species can result in incomplete Cr recovery during chromatographic purification. Because of large mass-dependent inter-species isotope fractionation, incomplete recovery can affect the accuracy of high-precision Cr isotope analysis. Here, we demonstrate widely differing cation distribution coefficients of Cr(III)-species (Cr(3+), CrCl(2+) and CrCl2(+)) with equilibrium mass-dependent isotope fractionation spanning a range of ∼1‰/amu and consistent with theory. The heaviest isotopes partition into Cr(3+), intermediates in CrCl(2+) and the lightest in CrCl2(+)/CrCl3°. Thus, for a typical reported loss of ∼25% Cr (in the form of Cr(3+)) through chromatographic purification, this translates into 185 ppm/amu offset in the stable Cr isotope ratio of the residual sample. Depending on the validity of the mass-bias correction during isotope analysis, this further results in artificial mass-independent effects in the mass-bias corrected (53)Cr/(52)Cr (μ(53)Cr* of 5.2 ppm) and (54)Cr/(52)Cr (μ(54)Cr* of 13.5 ppm) components used to infer chronometric and nucleosynthetic information in meteorites. To mitigate these fractionation effects, we developed strategic chemical sample pre-treatment procedures that ensure high and reproducible Cr recovery. This is achieved either through 1) effective promotion of Cr(3+) by >5 days exposure to HNO3H2O2 solutions at room temperature, resulting in >∼98% Cr recovery for most types of sample matrices tested using a cationic chromatographic retention strategy, or 2) formation of Cr(III)-Cl complexes through exposure to concentrated HCl at high temperature (>120 °C) for several hours, resulting in >97.5% Cr recovery using a

Lead isotopic compositions of environmental certified reference materials for an inter-laboratory comparison of lead isotope analysis

International Nuclear Information System (INIS)

Aung, Nyein Nyein; Uryu, Tsutomu; Yoshinaga, Jun

2004-01-01

Lead isotope ratios, viz. 207 Pb/ 206 Pb and 208 Pb/ 206 Pb, of the commercially available certified reference materials (CRMs) issued in Japan are presented with an objective to provide a data set, which will be useful for the quality assurance of analytical procedures, instrumental performance and method validation of the laboratories involved in environmental lead isotope ratio analysis. The analytical method used in the present study was inductively coupled plasma quadrupole mass spectrometry (ICPQMS) presented by acid digestion and with/without chemical separation of lead from the matrix. The precision of the measurements in terms of the relative standard deviation (RSD) of triplicated analyses was 0.19% and 0.14%, for 207 Pb/ 206 Pb and 208 Pb/ 206 Pb, respectively. The trueness of lead isotope ratio measurements of the present study was tested with a few CRMs, which have been analyzed by other analytical methods and reported in various literature. The lead isotopic ratios of 18 environmental matrix CRMs (including 6 CRMs analyzed for our method validation) are presented and the distribution of their ratios is briefly discussed. (author)

Comparison of mass-spectrometry and α-counting in analysis of uranium and plutonium isotopes in environmental samples

International Nuclear Information System (INIS)

Irleweck, K.; Pichlmayer, F.

1980-01-01

The determination of trace amounts of U and Pu isotopes is of interest in environmental and personal monitoring programmes. Commonly after preconcentration and separation of the radionuclides a proper sample is prepared electrolytically and the measurements are performed by alpha spectrometry. Some investigations on uranium isotopic abundances and on plutonium fallout deposition in soil have been carried out in this way. It is impossible to distinguish between the isotopes 239 Pu and 240 Pu by alpha spectrometry, however, because their α-energies are too close together. Such determinations can only be carried out by mass spectrometry. Specific Pu emissions, e.g. from nuclear production plants, can be discriminated from the global fallout level. Mass spectrometry is the more sensitive method for measuring long-lived nuclides compared with α-spectrometry. In the case of soil analysis, however, Pu detection is obstructed by the high natural uranium content, usually in the range 0.2 to 2.0 ppm which exceeds the trace amounts of plutonium by several orders of magnitude. This work describes a chemical procedure which separates U/Pu sufficiently for alpha spectrometry as well as for mass spectrometry, and compares results of environmental analysis applying both methods. (author)

Penguin Proxies: Deciphering Millennial-Scale Antarctic Ecosystem Change using Amino Acid Stable Isotope Analysis.

Science.gov (United States)

Michelson, C.; McMahon, K.; Emslie, S. D.; Patterson, W. P.; McCarthy, M. D.; Polito, M. J.

2017-12-01

The Southern Ocean ecosystem is undergoing rapid environmental change due to ongoing and historic anthropogenic impacts such as climate change and marine mammal harvesting. These disturbances may have cascading effects through the Antarctic food webs, resulting in profound shifts in the sources and cycling of organic matter supporting higher-trophic organisms, such as penguins. For example, bulk stable isotope analyses of modern and ancient preserved penguin tissues suggest variations in penguin feeding ecology throughout the Holocene with dramatic isotopic shifts in the last 200 years. However, it is not clear whether these isotopic shifts resulted from changes at the base of the food web, dietary shifts in penguins, or some combination of both factors. Newly developed compound-specific stable nitrogen isotope analysis of individual amino acids (CSIA-AA) may provide a powerful new tool to tease apart these confounding variables. Stable nitrogen isotope values of trophic amino acids (e.g., glutamic acid) increase substantially with each trophic transfer in the food web, while source amino acid (e.g., phenylalanine) stable nitrogen isotope values remain relatively unchanged and reflect ecosystem baselines. As such, we can use this CSIA-AA approach to decipher between baseline and dietary shifts in penguins over time from modern and ancient eggshells of Pygoscelis penguins in the Antarctic Peninsula and the Ross Sea regions of Antarctica. In order to accurately apply this CSIA-AA approach, we first characterized the trophic fractionation factors of individual amino acids between diet and penguin consumers in a long-term controlled penguin feeding experiment. We then applied these values to modern and ancient eggshells from the Antarctic Peninsula and Ross Sea to evaluate shifts in penguin trophic dynamics as a function of climate and anthropogenic interaction throughout much of the Holocene. This work develops a cutting edge new molecular geochemistry approach

Analysis of growth and tissue replacement rates by stable sulfur isotope turnover.

Science.gov (United States)

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

2003-12-01

Stable isotope analysis has become a powerful tool to study animal ecology. Analysis of stable isotope ratios of elements such as carbon, nitrogen, sulfur, hydrogen, oxygen and others have been used to trace migratory routes, reconstruct dietary sources and determine the physiological condition of individual animals. The isotopes most commonly used are carbon, due to differential carbon fractionation in C3 and C4 plants, and nitrogen, due to the approximately 3% enrichment in 15N per trophic level. Although all cells express sulfur-containing compounds, such as cysteine, methionine, and coenzyme A, the turnover rate of sulfur in tissues has not been examined in most studies, owing to the difficulty in determining the δ 34S signature. In this study, we have assessed the rate of sulfur isotopic turnover in mouse tissues following a diet change from terrestrial (7%) to marine (19%) source. Turnover models reflecting both growth rate and metabolic tissue replacement will be developed for blood, liver, fat and muscle tissues.

In Situ Carbon Isotope Analysis by Laser Ablation MC-ICP-MS.

Science.gov (United States)

Chen, Wei; Lu, Jue; Jiang, Shao-Yong; Zhao, Kui-Dong; Duan, Deng-Fei

2017-12-19

Carbon isotopes have been widely used in tracing a wide variety of geological and environmental processes. The carbon isotope composition of bulk rocks and minerals was conventionally analyzed by isotope ratio mass spectrometry (IRMS), and, more recently, secondary ionization mass spectrometry (SIMS) has been widely used to determine carbon isotope composition of carbon-bearing solid materials with good spatial resolution. Here, we present a new method that couples a RESOlution S155 193 nm laser ablation system with a Nu Plasma II MC-ICP-MS, with the aim of measuring carbon isotopes in situ in carbonate minerals (i.e., calcite and aragonite). Under routine operating conditions for δ 13 C analysis, instrumental bias generally drifts by 0.8‰-2.0‰ in a typical analytical session of 2-3 h. Using a magmatic calcite as the standard, the carbon isotopic composition was determined for a suite of calcite samples with δ 13 C values in the range of -6.94‰ to 1.48‰. The obtained δ 13 C data are comparable to IRMS values. The combined standard uncertainty for magmatic calcite is ICP-MS can serve as an appropriate method to analyze carbon isotopes of carbonate minerals in situ.

13C metabolic flux analysis: optimal design of isotopic labeling experiments.

Science.gov (United States)

Antoniewicz, Maciek R

2013-12-01

Measuring fluxes by 13C metabolic flux analysis (13C-MFA) has become a key activity in chemical and pharmaceutical biotechnology. Optimal design of isotopic labeling experiments is of central importance to 13C-MFA as it determines the precision with which fluxes can be estimated. Traditional methods for selecting isotopic tracers and labeling measurements did not fully utilize the power of 13C-MFA. Recently, new approaches were developed for optimal design of isotopic labeling experiments based on parallel labeling experiments and algorithms for rational selection of tracers. In addition, advanced isotopic labeling measurements were developed based on tandem mass spectrometry. Combined, these approaches can dramatically improve the quality of 13C-MFA results with important applications in metabolic engineering and biotechnology. Copyright © 2013 Elsevier Ltd. All rights reserved.

Impact analysis of a hydrogen isotopes container

International Nuclear Information System (INIS)

Lee, M. S.; Hwang, C. S.; Jeong, H. S.

2003-01-01

The container used for the radioactive materials, containing hydrogen isotopes is evaluated in a view of hypothetical accident. The computational analysis is a cost effective tool to minimize testing and streamline the regulatory procedures, and supports experimental programs to qualify the container for the safe transport of radioactive materials. The numerical analysis of 9m free-drop onto a flat unyielding, horizontal surface has been performed using the explicit finite element computer program ABAQUS. Especially free-drop simulations for 30 .deg. C tilted condition are precisely estimated

The Potential of Isotope Ratio Mass Spectrometry (IRMS) and Gas Chromatography-IRMS Analysis of Triacetone Triperoxide in Forensic Explosives Investigations.

Science.gov (United States)

Bezemer, Karlijn D B; Koeberg, Mattijs; van der Heijden, Antoine E D M; van Driel, Chris A; Blaga, Cornelia; Bruinsma, Jildert; van Asten, Arian C

2016-09-01

Studying links between triacetone triperoxide (TATP) samples from crime scenes and suspects can assist in criminal investigations. Isotope ratio mass spectrometry (IRMS) and gas chromatography (GC)-IRMS were used to measure the isotopic compositions of TATP and its precursors acetone and hydrogen peroxide. In total, 31 TATP samples were synthesized with different raw material combinations and reaction conditions. For carbon, a good differentiation and a linear relationship were observed for acetone-TATP combinations. The extent of negative (δ(13) C) fractionation depended on the reaction yield. Limited enrichment was observed for the hydrogen isotope (δ(2) H) values of the TATP samples probably due to a constant exchange of hydrogen atoms in aqueous solution. For oxygen (δ(18) O), the small isotopic range and excess of water in hydrogen peroxide resulted in poor differentiation. GC-IRMS and IRMS data were comparable except for one TATP sample prepared with high acid concentration demonstrating the potential of compound-specific isotope analysis. Carbon IRMS has practical use in forensic TATP investigations. © 2016 American Academy of Forensic Sciences.

Isotope dilution analysis of environmental samples

International Nuclear Information System (INIS)

Tolgyessy, J.; Lesny, J.; Korenova, Z.; Klas, J.; Klehr, E.H.

1986-01-01

Isotope dilution analysis has been used for the determination of several trace elements - especially metals - in a variety of environmental samples, including aerosols, water, soils, biological materials and geological materials. Variations of the basic concept include classical IDA, substoichiometric IDA, and more recently, sub-superequivalence IDA. Each variation has its advantages and limitations. A periodic chart has been used to identify those elements which have been measured in environmental samples using one or more of these methods. (author)

Carbon and hydrogen isotope fractionation during aerobic biodegradation of quinoline and 3-methylquinoline.

Science.gov (United States)

Cui, Mingchao; Zhang, Wenbing; Fang, Jun; Liang, Qianqiong; Liu, Dongxuan

2017-08-01

Compound-specific isotope analysis has been used extensively to investigate the biodegradation of various organic pollutants. To date, little isotope fractionation information is available for the biodegradation of quinolinic compounds. In this study, we report on the carbon and hydrogen isotope fractionation during quinoline and 3-methylquinoline aerobic microbial degradation by a Comamonas sp. strain Q10. Degradation of quinoline and 3-methylquinoline was accompanied by isotope fractionation. Large hydrogen and small carbon isotope fractionation was observed for quinoline while minor carbon and hydrogen isotope fractionation effects occurred for 3-methylquinoline. Bulk carbon and hydrogen enrichment factors (ε bulk ) for quinoline biodegradation were -1.2 ± 0.1 and -38 ± 1‰, respectively, while -0.7 ± 0.1 and -5 ± 1‰ for 3-methylquinoline, respectively. This reveals a potential advantage for employing quinoline as the model compound and hydrogen isotope analysis for assessing aerobic biodegradation of quinolinic compounds. The apparent kinetic isotope effects (AKIE C ) values of carbon were 1.008 ± 0.0005 for quinoline and 1.0048 ± 0.0005 for 3-methylquinoline while AKIE H values of hydrogen of 1.264 ± 0.011 for quinoline and 1.0356 ± 0.0103 for 3-methylquinoline were obtained. The combined evaluation of carbon and hydrogen isotope fractionation yields Λ values (Λ = Δδ 2 H/Δδ 13 C ≈ εH bulk /εC bulk ) of 29 ± 2 for quinoline and 8 ± 2 for 3-methylquinoline. The results indicate that the substrate specificity may have a significant influence on the isotope fractionation for the biodegradation of quinolinic compounds. The substrate-specific isotope enrichment factors would be important for assessing the behavior and fate of quinolinic compounds in the environment.

Hanford Isotope Project strategic business analysis Cesium-137 (Cs-137)

Energy Technology Data Exchange (ETDEWEB)

NONE

1995-10-01

The purpose of this business analysis is to address the beneficial reuse of Cesium 137 (Cs-137) in order to utilize a valuable national asset and possibly save millions of tax dollars. Food irradiation is the front runner application along with other uses. This business analysis supports the objectives of the Department of Energy National Isotope Strategy distributed in August 1994 which describes the DOE plans for the production and distribution of isotope products and services. As part of the Department`s mission as stated in that document. ``The Department of Energy will also continue to produce and distribute other radioisotopes and enriched stable isotopes for medical diagnostics and therapeutics, industrial, agricultural, and other useful applications on a businesslike basis. This is consistent with the goals and objectives of the National Performance Review. The Department will endeavor to look at opportunities for private sector to co-fund or invest in new ventures. Also, the Department will seek to divest from ventures that can more profitably or reliably be operated by the private sector.``

Hanford Isotope Project strategic business analysis Cesium-137 (Cs-137)

International Nuclear Information System (INIS)

1995-10-01

The purpose of this business analysis is to address the beneficial reuse of Cesium 137 (Cs-137) in order to utilize a valuable national asset and possibly save millions of tax dollars. Food irradiation is the front runner application along with other uses. This business analysis supports the objectives of the Department of Energy National Isotope Strategy distributed in August 1994 which describes the DOE plans for the production and distribution of isotope products and services. As part of the Department's mission as stated in that document. ''The Department of Energy will also continue to produce and distribute other radioisotopes and enriched stable isotopes for medical diagnostics and therapeutics, industrial, agricultural, and other useful applications on a businesslike basis. This is consistent with the goals and objectives of the National Performance Review. The Department will endeavor to look at opportunities for private sector to co-fund or invest in new ventures. Also, the Department will seek to divest from ventures that can more profitably or reliably be operated by the private sector.''

Comparison of GC-ICP-MS and HPLC-ICP-MS for species-specific isotope dilution analysis of tributyltin in sediment after accelerated solvent extraction

International Nuclear Information System (INIS)

Wahlen, Raimund; Wolff-Briche, Celine

2003-01-01

This study describes a direct comparison of GC and HPLC hyphenated to ICP-MS determination of tributyltin (TBT) in sediment by species-specific isotope dilution analysis (SS-IDMS). The certified reference sediment PACS-2 (NRC, Canada) and a candidate reference sediment (P-18/HIPA-1) were extracted using an accelerated solvent extraction (ASE) procedure. For comparison of GC and LC methods an older bottle of PACS-2 was used, whilst a fresh bottle was taken for demonstration of the accuracy of the methods. The data obtained show good agreement between both methods for both the PACS-2 sediment (LC-ICP-IDMS 828±87 ng g -1 TBT as Sn, GC-ICP-IDMS 848±39 ng g -1 TBT as Sn) and the P-18/ HIPA-1 sediment (LC-ICP-IDMS 78.0±9.7 ng g -1 TBT as Sn, GC-ICP-IDMS 79.2±3.8 ng g -1 TBT as Sn). The analysis by GC-ICP-IDMS offers a greater signal-to-noise ratio and hence a superior detection limit of 0.03 pg TBT as Sn, in the sediment extracts compared to HPLC-ICP-IDMS (3 pg TBT as Sn). A comparison of the uncertainties associated with both methods indicates superior precision of the GC approach. This is related to the better reproducibility of the peak integration, which affects the isotope ratio measurements used for IDMS. The accuracy of the ASE method combined with HPLC-ICP-IDMS was demonstrated during the international interlaboratory comparison P-18 organised by the Comite Consultatif pour la Quantite de Matiere (CCQM). The results obtained by GC-ICP-IDMS for a newly opened bottle of PACS-2 were 1087±77 ng g -1 Sn for DBT and 876±51 ng g -1 Sn for TBT (expanded uncertainties with a coverage factor of 2), which are in good agreement with the certified values of 1090±150 ng g -1 Sn and 980±130 ng g -1 Sn, respectively. (orig.)

Stable Isotope Quantitative N-Glycan Analysis by Liquid Separation Techniques and Mass Spectrometry.

Science.gov (United States)

Mittermayr, Stefan; Albrecht, Simone; Váradi, Csaba; Millán-Martín, Silvia; Bones, Jonathan

2017-01-01

Liquid phase separation analysis and subsequent quantitation remains a challenging task for protein-derived oligosaccharides due to their inherent structural complexity and diversity. Incomplete resolution or co-detection of multiple glycan species complicates peak area-based quantitation and associated statistical analysis when optical detection methods are used. The approach outlined herein describes the utilization of stable isotope variants of commonly used fluorescent tags that allow for mass-based glycan identification and relative quantitation following separation by liquid chromatography (LC) or capillary electrophoresis (CE). Comparability assessment of glycoprotein-derived oligosaccharides is performed by derivatization with commercially available isotope variants of 2-aminobenzoic acid or aniline and analysis by LC- and CE-mass spectrometry. Quantitative information is attained from the extracted ion chromatogram/electropherogram ratios generated from the light and heavy isotope clusters.

Integrating stomach content and stable isotope analyses to quantify the diets of pygoscelid penguins.

Directory of Open Access Journals (Sweden)

Michael J Polito

Full Text Available Stomach content analysis (SCA and more recently stable isotope analysis (SIA integrated with isotopic mixing models have become common methods for dietary studies and provide insight into the foraging ecology of seabirds. However, both methods have drawbacks and biases that may result in difficulties in quantifying inter-annual and species-specific differences in diets. We used these two methods to simultaneously quantify the chick-rearing diet of Chinstrap (Pygoscelis antarctica and Gentoo (P. papua penguins and highlight methods of integrating SCA data to increase accuracy of diet composition estimates using SIA. SCA biomass estimates were highly variable and underestimated the importance of soft-bodied prey such as fish. Two-source, isotopic mixing model predictions were less variable and identified inter-annual and species-specific differences in the relative amounts of fish and krill in penguin diets not readily apparent using SCA. In contrast, multi-source isotopic mixing models had difficulty estimating the dietary contribution of fish species occupying similar trophic levels without refinement using SCA-derived otolith data. Overall, our ability to track inter-annual and species-specific differences in penguin diets using SIA was enhanced by integrating SCA data to isotopic mixing modes in three ways: 1 selecting appropriate prey sources, 2 weighting combinations of isotopically similar prey in two-source mixing models and 3 refining predicted contributions of isotopically similar prey in multi-source models.

Transition-state analysis of a Vmax mutant of AMP nucleosidase by the application of heavy-atom kinetic isotope effects

International Nuclear Information System (INIS)

Parkin, D.W.; Mentch, F.; Banks, G.A.; Horenstein, B.A.; Schramm, V.L.

1991-01-01

The transition state of the V max mutant of AMP nucleosidase from Azotobacter vinelandii has been characterized by heavy-atom kinetic isotope effects in the presence and absence of MgATP, the allosteric activator. The enzyme catalyzes hydrolysis of the N-glycosidic bond of AMP at approximately 2% of the rate of the normal enzyme with only minor changes in the K m for substrate, the activation constant for MgATP, and the K i for formycin 5'-phosphate, a tight-binding competitive inhibitor. Isotope effects were measured as a function of the allosteric activator concentration that increases the turnover number of the enzyme from 0.006 s -1 . The kinetic isotope effects were measured with the substrates [1'- 3 H]AMP, [2'- 2 H]AMP, [9- 15 N]AMP, and [1',9- 14 C, 15 N]AMP. All substrates gave significant kinetic isotope effects in a pattern that establishes that the reaction expresses intrinsic kinetic isotope effects in the presence or absence of MgATP. Transition-state analysis using bond-energy and bond-order vibrational analysis indicated that the transition state for the mutant enzyme has a similar position in the reaction coordinate compared to that for the normal enzyme. The mutant enzyme is less effective in stabilizing the carbocation-like intermediate and in the ability to protonate N7 of adenine to create a better leaving group. This altered transition-state structure was confirmed by an altered substrate specificity for the mutant protein

Quantitative mass-spectrometric analysis of hydrogen helium isotope mixtures

International Nuclear Information System (INIS)

Langer, U.

1998-12-01

This work deals with the mass-spectrometric method for the quantitative analysis of hydrogen-helium-isotope mixtures, with special attention to fusion plasma diagnostics. The aim was to use the low-resolution mass spectrometry, a standard measuring method which is well established in science and industry. This task is solved by means of the vector mass spectrometry, where a mass spectrum is repeatedly measured, but with stepwise variation of the parameter settings of a quadruple mass spectrometer. In this way, interfering mass spectra can be decomposed and, moreover, it is possible to analyze underestimated mass spectra of complex hydrogen-helium-isotope mixtures. In this work experimental investigations are presented which show that there are different parameters which are suitable for the UMS-method. With an optimal choice of the parameter settings hydrogen-helium-isotope mixtures can be analyzed with an accuracy of 1-3 %. In practice, a low sensitivity for small helium concentration has to be noted. To cope with this task, a method for selective hydrogen pressure reduction has been developed. Experimental investigations and calculations show that small helium amounts (about 1 %) in a hydrogen atmosphere can be analyzed with an accuracy of 3 - 10 %. Finally, this work deals with the effects of the measuring and calibration error on the resulting error in spectrum decomposition. This aspect has been investigated both in general mass-spectrometric gas analysis and in the analysis of hydrogen-helium-mixtures by means of the vector mass spectrometry. (author)

Amino acid δ13C analysis of hair proteins and bone collagen using liquid chromatography/isotope ratio mass spectrometry

DEFF Research Database (Denmark)

Raghavan, Maanasa; McCullagh, James S. O.; Lynnerup, Niels

2010-01-01

We report a novel method for the chromatographic separation and measurement of stable carbon isotope ratios (delta(13)C) of individual amino acids in hair proteins and bone collagen using the LC-IsoLink system, which interfaces liquid chromatography (LC) with isotope ratio mass spectrometry (IRMS......). This paper provides baseline separation of 15 and 13 of the 18 amino acids in bone collagen and hair proteins, respectively. We also describe an approach to analysing small hair samples for compound-specific analysis of segmental hair sections. The LC/IRMS method is applied in a historical context...... by the delta(13)C analysis of hair proteins and bone collagen recovered from six individuals from Uummannaq in Greenland. The analysis of hair and bone amino acids from the same individual, compared for the first time in this study, is of importance in palaeodietary reconstruction. If hair proteins can be used...

Hydrology of Bishop Creek, California: An Isotopic Analysis

Science.gov (United States)

Michael L. Space; John W. Hess; Stanley D. Smith

1989-01-01

Five power generation plants along an eleven kilometer stretch divert Bishop Creek water for hydro-electric power. Stream diversion may be adversely affecting the riparian vegetation. Stable isotopic analysis is employed to determine surface water/ground-water interactions along the creek. surface water originates primarily from three headwater lakes. Discharge into...

Recent developments in application of stable isotope analysis on agro-product authenticity and traceability.

Science.gov (United States)

Zhao, Yan; Zhang, Bin; Chen, Gang; Chen, Ailiang; Yang, Shuming; Ye, Zhihua

2014-02-15

With the globalisation of agro-product markets and convenient transportation of food across countries and continents, the potential for distribution of mis-labelled products increases accordingly, highlighting the need for measures to identify the origin of food. High quality food with identified geographic origin is a concern not only for consumers, but also for agriculture farmers, retailers and administrative authorities. Currently, stable isotope ratio analysis in combination with other chemical methods gradually becomes a promising approach for agro-product authenticity and traceability. In the last five years, a growing number of research papers have been published on tracing agro-products by stable isotope ratio analysis and techniques combining with other instruments. In these reports, the global variety of stable isotope compositions has been investigated, including light elements such as C, N, H, O and S, and heavy isotopes variation such as Sr and B. Several factors also have been considered, including the latitude, altitude, evaporation and climate conditions. In the present paper, an overview is provided on the authenticity and traceability of the agro-products from both animal and plant sources by stable isotope ratio analysis. Copyright © 2013 Elsevier Ltd. All rights reserved.

Lead isotope ratio analysis of bullet samples by using quadrupole ICP-MS

International Nuclear Information System (INIS)

Tamura, Shu-ichi; Hokura, Akiko; Nakai, Izumi; Oishi, Masahiro

2006-01-01

The measurement conditions for the precise analysis of the lead stable isotope ratio by using an ICP-MS equipped with a quadrupole mass spectrometer were studied in order to apply the technique to the forensic identification of bullet samples. The values of the relative standard deviation obtained for the ratio of 208 Pb/ 206 Pb, 207 Pb/ 206 Pb and 204 Pb/ 206 Pb were lower than 0.2% after optimization of the analytical conditions, including the optimum lead concentration of the sample solution to be about 70 ppb and an integration time for 1 m/s of 15 s. This method was applied to an analysis of lead in bullets for rifles and handguns; a stable isotope ratio of lead was found to be suitable for the identification of bullets. This study has demonstrated that the lead isotope ratio measured by using a quadrupole ICP-MS was useful for a practical analysis of bullet samples in forensic science. (author)

Hydrogen isotope analysis by quadrupole mass spectrometry

International Nuclear Information System (INIS)

Ellefson, R.E.; Moddeman, W.E.; Dylla, H.F.

1981-03-01

The analysis of isotopes of hydrogen (H, D, T) and helium ( 3 He, 4 He) and selected impurities using a quadrupole mass spectrometer (QMS) has been investigated as a method of measuring the purity of tritium gas for injection into the Tokamak Fusion Test Reactor (TFTR). A QMS was used at low resolution, m/Δm 3 He, and 4 He in HT/D 2

Effects of euthanasia method on stable-carbon and stable-nitrogen isotope analysis for an ectothermic vertebrate.

Science.gov (United States)

Atwood, Meredith A

2013-04-30

Stable isotope analysis is a critical tool for understanding ecological food webs; however, results can be sensitive to sample preparation methods. To limit the possibility of sample contamination, freezing is commonly used to euthanize invertebrates and preserve non-lethal samples from vertebrates. For destructive sampling of vertebrates, more humane euthanasia methods are preferred to freezing and it is essential to evaluate how these euthanasia methods affect stable isotope results. Stable isotope ratios and elemental composition of carbon and nitrogen were used to evaluate whether the euthanasia method compromised the integrity of the sample for analysis. Specifically, the stable isotope and C:N ratios were compared for larval wood frogs (Rana sylvatica  =  Lithobates sylvaticus), an ectothermic vertebrate, that had been euthanized by freezing with four different humane euthanasia methods: CO2, benzocaine, MS-222 (tricaine methanesulfonate), and 70% ethanol. The euthanasia method was not related to the δ(13)C or δ(15)N values and the comparisons revealed no differences between freezing and any of the other treatments. However, there were slight (non-significant) differences in the isotope ratios of benzocaine and CO2 when each was compared with freezing. The elemental composition was altered by the euthanasia method employed. The percentage nitrogen was higher in CO2 treatments than in freezing, and similar (non-significant) trends were seen for ethanol treatments relative to freezing. The resulting C:N ratios were higher for benzocaine treatments than for both CO2 and ethanol. Similar (non-significant) trends suggested that the C:N ratios were also higher for animals euthanized by freezing than for both CO2 and ethanol euthanasia methods. The euthanasia method had a larger effect on elemental composition than stable isotope ratios. The percentage nitrogen and the subsequent C:N ratios were most affected by the CO2 and ethanol euthanasia methods, whereas

Isotope separation process

International Nuclear Information System (INIS)

Wexler, Sol; Young, C.E.

1976-01-01

Description is given of method for separating a specific isotope from a mixture of isotopes of an actinide element present as MF 6 , wherein M is the actinide element. It comprises: preparing a feed gas mixture of MF 6 in a propellant gas; passing the feed gas mixture under pressure through an expansion nozzle while heating the mixture to about 600 0 C; releasing the heated gas mixture from the nozzle into an exhaust chamber having a reduced pressure, whereby a gas jet of MF 6 molecules, MF 6 molecular clusters and propellant gas molecules is formed, the MF 6 molecules having a translational energy of about 3 eV; converting the MF 6 molecules to MF 6 ions by passing the jet through a cross jet of electron donor atoms so that an electron transfer takes place between the MF 6 - molecules and the electron donor atoms whereby the jet is now quasi-neutral, containing negative MF 6 - ions and positive donor ions; passing the quasi-neutral jet through a radiofrequency mass filter tuned to separate the MF 6 ions containing the specific isotope from the MF 6 - ions of the other isotopes and neutralizing and collecting the MF 6 molecules of the specific isotope [fr

Isotope analysis by emission spectroscopy; Analyse isotopique par spectroscopie d'emission

Energy Technology Data Exchange (ETDEWEB)

Artaud, J; Gerstenkorn, S [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires; Blaise, J [Centre National de la Recherche Scientifique (CNRS), Lab. Aime Cotton, 92 - Meudon-Bellevue (France)

1959-07-01

Quantitative analysis of isotope mixtures by emission spectroscopy is resulting from the phenomenon called 'isotope shift', say from the fact that spectral lines produced by a mixture of isotopes of a same element are complex. Every spectral line is, indeed, resulting from several lines respectively corresponding to each isotope. Then isotopic components are near one to others, and their separation is effected by means of Fabry-Perot calibration standard: the apparatus allowing to measure abundances is the Fabry-Perot photo-electric spectrometer, designed in 1948 by MM. JACQUINOT and DUFOUR. This method has been used to make abundance determination in the case of helium, lithium, lead and uranium. In the case of lithium, the utilised analysis line depends on the composition of examined isotopic mixture. For mixtures containing 7 to 93 pour cent of one of isotopes of lithium, this line is the lithium blue line: {lambda} = 4603 angstrom. In other cases the red line {lambda} = 6707 angstrom is preferable, though it allows to do easily nothing but relative determinations. Helium shows no particular difficulty and the analysis line selected was {lambda} = 6678 angstrom. For lead the line {lambda} = 5201 angstrom gives the possibility to determine the isotope abundance for the four isotopes of lead notwithstanding the presence of hyperfine structure of {sup 207}Pb. For uranium, line {lambda} 5027 angstrom is used, and this method allows to determine the composition of isotope mixtures, the content of which in {sup 235}U may shorten to 0,1 per cent. Relative precision is about 2 per cent for contents in {sup 235}U over 1 per cent. For lower contents, this line {lambda} = 5027 angstrom will allow relative measures when using previously dosed mixtures. (author) [French] L'analyse quantitative des melanges isotopiques par spectroscopie d'emission doit son existence au phenomene appele 'deplacement isotopique', c'est-a-dire au fait que les raies spectrales emises par un

Stable isotope analysis of precipitation samples obtained via crowdsourcing reveals the spatiotemporal evolution of Superstorm Sandy.

Directory of Open Access Journals (Sweden)

Stephen P Good

Full Text Available Extra-tropical cyclones, such as 2012 Superstorm Sandy, pose a significant climatic threat to the northeastern United Sates, yet prediction of hydrologic and thermodynamic processes within such systems is complicated by their interaction with mid-latitude water patterns as they move poleward. Fortunately, the evolution of these systems is also recorded in the stable isotope ratios of storm-associated precipitation and water vapor, and isotopic analysis provides constraints on difficult-to-observe cyclone dynamics. During Superstorm Sandy, a unique crowdsourced approach enabled 685 precipitation samples to be obtained for oxygen and hydrogen isotopic analysis, constituting the largest isotopic sampling of a synoptic-scale system to date. Isotopically, these waters span an enormous range of values (> 21‰ for δ(18O, > 160‰ for δ(2H and exhibit strong spatiotemporal structure. Low isotope ratios occurred predominantly in the west and south quadrants of the storm, indicating robust isotopic distillation that tracked the intensity of the storm's warm core. Elevated values of deuterium-excess (> 25‰ were found primarily in the New England region after Sandy made landfall. Isotope mass balance calculations and Lagrangian back-trajectory analysis suggest that these samples reflect the moistening of dry continental air entrained from a mid-latitude trough. These results demonstrate the power of rapid-response isotope monitoring to elucidate the structure and dynamics of water cycling within synoptic-scale systems and improve our understanding of storm evolution, hydroclimatological impacts, and paleo-storm proxies.

Stable isotope analysis of precipitation samples obtained via crowdsourcing reveals the spatiotemporal evolution of Superstorm Sandy.

Science.gov (United States)

Good, Stephen P; Mallia, Derek V; Lin, John C; Bowen, Gabriel J

2014-01-01

Extra-tropical cyclones, such as 2012 Superstorm Sandy, pose a significant climatic threat to the northeastern United Sates, yet prediction of hydrologic and thermodynamic processes within such systems is complicated by their interaction with mid-latitude water patterns as they move poleward. Fortunately, the evolution of these systems is also recorded in the stable isotope ratios of storm-associated precipitation and water vapor, and isotopic analysis provides constraints on difficult-to-observe cyclone dynamics. During Superstorm Sandy, a unique crowdsourced approach enabled 685 precipitation samples to be obtained for oxygen and hydrogen isotopic analysis, constituting the largest isotopic sampling of a synoptic-scale system to date. Isotopically, these waters span an enormous range of values (> 21‰ for δ(18)O, > 160‰ for δ(2)H) and exhibit strong spatiotemporal structure. Low isotope ratios occurred predominantly in the west and south quadrants of the storm, indicating robust isotopic distillation that tracked the intensity of the storm's warm core. Elevated values of deuterium-excess (> 25‰) were found primarily in the New England region after Sandy made landfall. Isotope mass balance calculations and Lagrangian back-trajectory analysis suggest that these samples reflect the moistening of dry continental air entrained from a mid-latitude trough. These results demonstrate the power of rapid-response isotope monitoring to elucidate the structure and dynamics of water cycling within synoptic-scale systems and improve our understanding of storm evolution, hydroclimatological impacts, and paleo-storm proxies.

Nanometer-scale isotope analysis of bulk diamond by atom probe tomography

NARCIS (Netherlands)

Schirhagl, R.; Raatz, N.; Meijer, J.; Markham, M.; Gerstl, S. S. A.; Degen, C. L.

2015-01-01

Atom-probe tomography (APT) combines field emission of atoms with mass spectrometry to reconstruct three-dimensional tomograms of materials with atomic resolution and isotope specificity. Despite significant recent progress in APT technology, application to wide-bandgap materials with strong

Certification of methylmercury in cod fish tissue certified reference material by species-specific isotope dilution mass spectrometric analysis

Energy Technology Data Exchange (ETDEWEB)

Inagaki, Kazumi; Kuroiwa, Takayoshi; Narukawa, Tomohiro; Yarita, Takashi; Takatsu, Akiko; Okamoto, Kensaku; Chiba, Koichi [National Metrology Institute of Japan (NMIJ), National Institute of Advanced Industrial Science and Technology (AIST), Environmental Standard Section, Tsukuba, Ibaraki (Japan)

2008-07-15

A new cod fish tissue certified reference material, NMIJ CRM 7402-a, for methylmercury analysis was certified by the National Metrological Institute of Japan in the National Institute of Advanced Industrial Science and Technology (NMIJ/AIST). Cod fish was collected from the sea close to Japan. The cod muscle was powdered by freeze-pulverization and was placed into 600 glass bottles (10 g each), which were sterilized with {gamma}-ray irradiation. The certification was carried out using species-specific isotope dilution gas chromatography inductively coupled plasma mass spectrometry (SSID-GC-ICPMS), where {sup 202}Hg-enriched methylmercury (MeHg) was used as the spike compound. In order to avoid any possible analytical biases caused by nonquantitative extraction, degradation and/or formation of MeHg in sample preparations, two different extraction methods (KOH/methanol and HCl/methanol extractions) were performed, and one of these extraction methods utilized two different derivatization methods (ethylation and phenylation). A double ID method was adopted to minimize the uncertainty arising from the analyses. In order to ensure not only the reliability of the analytical results but also traceability to SI units, the standard solution of MeHg used for the reverse-ID was prepared from high-purity MeHg chloride and was carefully assayed as follows: the total mercury was determined by ID-ICPMS following aqua regia digestion, and the ratio of Hg as MeHg to the total Hg content was estimated by GC-ICPMS. The certified value given for MeHg is 0.58 {+-} 0.02 mg kg{sup -1} as Hg. (orig.)

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

Estimation of the specific mass effect in the isotope shifts of energy levels in the optical spectrum of Ba I and Ba II

International Nuclear Information System (INIS)

Pendrill, L.R.

1984-01-01

A graphical method for separating mass and volume effects from purely optical isotope shift data is presented and compared with King's ''bunching'' method. Recent experimental data on isotope shifts for a wide range of spectral lines in the naturally abundant isotopes of Ba I and Ba II are analysed. Some agreement is found with muonic X-ray data concerning the nuclear size for the isotopes 136, 137 and 138, but there is disagreement (over 20%) for the other isotopes. The level isotope shifts are further parameterised in terms of a linear model, and the specific mass effect is decomposed into sums of one-electron and two-electron shift parameters with respect to the inert-gas like ground state of Ba III. (orig.)

Specific equilibrium behavior of hydrogen isotopes adsorbed onto synthetic zeolite A-type governed by lithium cations

International Nuclear Information System (INIS)

Takashima, Shoji; Kotoh, Kenji

2013-01-01

Highlights: • Isotherms for H 2 and D 2 adsorbed onto SZ-LiA at 77.4 K are shown. • The adsorption isotherms exhibit specific deviation in the range lower than 10 Pa. • SZ-LiA indicates the power of several 100-times at 0.1 Pa, compared with SZ-NaA. • Experimental isotherms are described empirically by a dual-site Langmuir equation. • The isotope effect on adsorption isotherms appears in the Langmuir constants. -- Abstract: Since synthetic zeolites (SZs) are powerfully adsorptive for hydrogen isotopes at cryogenic temperatures such as liquefied nitrogen, adsorption processes using these have been considered applicable to such as recovery of tritium from the lithium blanket of DT fusion reactor system. Onto these zeolites the adsorptions isotherms for hydrogen isotopes onto SZ-NaA, SZ-CaA and SZ-NaX at 77.4 K were already clarified experimentally and analytically. These isotherms exhibit similar profiles of Langmuir type. In this work, adsorption isotherms were examined for H 2 and D 2 on SZ-LiA at 77.4 K. SZ-LiA was made from SZ-NaA by exchanging its sodium ions for lithium ones, provided by TOSOH Corp. The experimental results demonstrate the specific equilibrium behavior of hydrogen isotopes adsorbed on SZ-LiA, deviating from isothermal profiles on SZ-CaA and SZ-NaX. SZ-LiA show the isothermal profiles of adsorption for H 2 and D 2 similar to on the conventional zeolites in the range from around 1 kPa to the atmospheric pressure, but exhibit a plateau around 1 mol/kg between 0.1 Pa and 100 Pa, while other zeolites show linearly profiling isotherms. This deviation indicates the adsorptive power of SZ-LiA remarkably greater than that of the others

Growth history of cultured pearl oysters based on stable oxygen isotope analysis

Science.gov (United States)

Nakashima, R.; Furuta, N.; Suzuki, A.; Kawahata, H.; Shikazono, N.

2007-12-01

We investigated the oxygen isotopic ratio in shells of the pearl oyster Pinctada martensii cultivated in embayments in Mie Prefecture, central Japan, to evaluate the biomineralization of shell structures of the species and its pearls in response to environmental change. Microsamples for oxygen isotope analysis were collected from the surfaces of shells (outer, middle, and inner shell layers) and pearls. Water temperature variations were estimated from the oxygen isotope values of the carbonate. Oxygen isotope profiles of the prismatic calcite of the outer shell layer reflected seasonal variations of water temperature, whereas those of nacreous aragonites of the middle and inner shell layers and pearls recorded temperatures from April to November, June to September, and July to September, respectively. Lower temperatures in autumn and winter might slow the growth of nacreous aragonites. The oxygen isotope values are controlled by both variations of water temperature and shell structures; the prismatic calcite of this species is useful for reconstructing seasonal changes of calcification temperature.

Metal/glass composites for analysis of hydrogen isotopes by gas-chromatography

International Nuclear Information System (INIS)

Nicolae, Constantin Adrian; Sisu, Claudia; Stefanescu, Doina; Stanciu, Vasile

1999-01-01

The separation process of hydrogen isotopes by cryogenic distillation or thermal diffusion is a key technology for tritium separation from heavy water in CANDU reactor and for tritium fuel cycle in thermonuclear fusion reactor. In each process, analytical techniques for analyzing the hydrogen isotope mixture are required. An extensive experimental research has been carried out in order to produce the most suitable adsorbents and to establish the best operating conditions for selective separation and analysis of hydrogen isotopes by gas-chromatography. This paper describes the preparation of adsorbent materials used as stationary phases in the gas-chromatographic column for hydrogen isotope separation and the treatment (activation) of stationary phases. Modified thermoresisting glass with Fe(NH 4 ) 2 (SO 4 ) 2 ·6H 2 O and Cr 2 O 3 respectively have been experimentally investigated at 77 K for H 2 , HD and D 2 separation and the results of chromatographic runs are reported and discussed. The gas-chromatographic apparatus used in this study is composed of a Hewlett-Packard 7620A gas-chromatograph equipped with a gas carrier flow rate controller and a thermal conductivity detector. The apparatus comprises also a Dewar vessel containing the separation column. The hydrogen isotopes, H 2 , HD, D 2 , and their mixture have been obtained in our laboratories. The best operating conditions and parameters of the Fe 3+ /glass adsorbent column , i.e. granulometry, column length, pressure-drop along the column, carrier gas flow rate and sample volume have been studied by means of the analysis of the retention times, separation factors and HETP. (authors)

Carbon isotope analysis of carbonaceous compounds in Puget Sound and Lake Washington

International Nuclear Information System (INIS)

Swanson, J.R.

1980-01-01

A new method has been developed and tested for determining chronological profiles of organic pollutants. This method, Carbon Isotope Analysis (CIA), involves measurements of 12 C, 13 C and 14 C in carbonaceous compounds found in layers of sediment. Lipids, total aliphatic hydrocarbons (TAHs) and polycyclic aromatic hydrocarbons (PAHs) are separated from kg quantities of sediment. Large Soxhlet extractors are used to remove the extractable organics, using ultra-pure benzene-methanol solution and having an extraction efficiency of about 86% for compounds with boiling points higher than n-tetradecane (n-C 14 ). The basic steps in compound separation include freeze-drying, extraction, fractionation, column chromatography and evaporation. Isolating the TAH and PAH fractions is accomplished by eluting samples from Sephadex and alumina/silica-gel columns. The amount of each fraction recovered is determined by converting the hydrocarbons to carbon dioxide and measuring this gas manometrically. Variations in 12 C and 13 C abundances for carbonaceous compounds are primarily due to thermodynamic, photosynthetic and metabolic fractionation processes. Thus, the source of a particular organic compound can often be determined by measuring its 13 C/ 12 C ratio. Combining the information from both the 13 C analysis and 14 C analysis makes source identification more certain. In addition, this investigation reviews carbon isotopic data and carbon cycling and analyzes organic pollution in two limited ecosystems (Puget Sound and Lake Washington). Specifically, distinct carbonaceous species are analyzed for pollution in sediments of Lake Washington, Elliott Bay, Commencement Bay, central Puget Sound and northern Puget Sound near the Cherry Point oil refineries

Study of medical isotope production facility stack emissions and noble gas isotopic signature using automatic gamma-spectra analysis platform

Science.gov (United States)

Zhang, Weihua; Hoffmann, Emmy; Ungar, Kurt; Dolinar, George; Miley, Harry; Mekarski, Pawel; Schrom, Brian; Hoffman, Ian; Lawrie, Ryan; Loosz, Tom

2013-04-01

The nuclear industry emissions of the four CTBT (Comprehensive Nuclear-Test-Ban Treaty) relevant radioxenon isotopes are unavoidably detected by the IMS along with possible treaty violations. Another civil source of radioxenon emissions which contributes to the global background is radiopharmaceutical production companies. To better understand the source terms of these background emissions, a joint project between HC, ANSTO, PNNL and CRL was formed to install real-time detection systems to support 135Xe, 133Xe, 131mXe and 133mXe measurements at the ANSTO and CRL 99Mo production facility stacks as well as the CANDU (CANada Deuterium Uranium) primary coolant monitoring system at CRL. At each site, high resolution gamma spectra were collected every 15 minutes using a HPGe detector to continuously monitor a bypass feed from the stack or CANDU primary coolant system as it passed through a sampling cell. HC also conducted atmospheric monitoring for radioxenon at approximately 200 km distant from CRL. A program was written to transfer each spectrum into a text file format suitable for the automatic gamma-spectra analysis platform and then email the file to a server. Once the email was received by the server, it was automatically analysed with the gamma-spectrum software UniSampo/Shaman to perform radionuclide identification and activity calculation for a large number of gamma-spectra in a short period of time (less than 10 seconds per spectrum). The results of nuclide activity together with other spectrum parameters were saved into the Linssi database. This database contains a large amount of radionuclide information which is a valuable resource for the analysis of radionuclide distribution within the noble gas fission product emissions. The results could be useful to identify the specific mechanisms of the activity release. The isotopic signatures of the various radioxenon species can be determined as a function of release time. Comparison of 133mXe and 133Xe activity

An estimation of Central Iberian Peninsula atmospheric δ13C and water δD in the Upper Cretaceous using pyrolysis compound specific isotopic analysis (Py-CSIA) of a fossil conifer.

Science.gov (United States)

González-Pérez, José A.; Jiménez-Morillo, Nicasio T.; De la Rosa, José M.; Almendros, Gonzalo; González-Vila, Francisco J.

2015-04-01

Frenelopsis is a frequently found genus of the Cretaceous floras adapted to dry, saline and in general to environmental conditions marked by severe water stress [1]. Stable isotope analysis of fossil organic materials can be used to infer palaeoenvironmental variables helpful to reconstruct plant paleohabitats [2]. In this study stable isotope analysis of organic fossil remains (FR) and humic fractions (FA, HA and humin) of Frenelopsis oligiostomata are studied in bulk (C, H, O, N IRMS) and in specific compounds released by pyrolysis (C, H, Py-CSIA). Well preserved F. oligiostomata fossils were handpicked from a limestone included in compacted marls from Upper Cretaceous (Senonian c. 72 Mya) in Guadalix de la Sierra (Madrid, Spain) [3]. The fossils were decarbonated with 6M HCl. Humic substances were extracted from finely ground fossil remains (FR) by successive treatments with 0.1M Na4P2O7 + NaOH [4]. The extract was acidified resulting into insoluble HA and soluble FA fractions. The HA and FA were purified as in [5] and [6] respectively. Bulk stable isotopic analysis (δ13C, δD, δ18O, δ15N IRMS) was done in an elemental micro-analyser coupled to a continuous flow Delta V Advantage isotope ratio mass spectrometer (IRMS). Pyrolysis compound specific isotopic analysis Py-CSIA (δ13C, δD): was done by coupling a double-shot pyrolyzer to a chromatograph connected to an IRMS. Structural features of specific peaks were inferred by comparing/matching mass spectra from conventional Py-GC/MS (data not shown) with Py-GC/IRMS chromatograms obtained using the same chromatographic conditions. Bulk C isotopic signature found for FR (-20.5±0.02 ‰) was in accordance with previous studies [2, 7-9]. This heavy isotopic δ13C signature indicates a depleted stomatal conductance and paleoenvironmental growth conditions of water and salt stress. This is in line with the morphological and depositional characteristics [3] confirming that F. oligostomata was adapted to highly xeric

Feeding preferences of West Indian manatees in Florida, Belize, and Puerto Rico as indicated by stable isotope analysis

Science.gov (United States)

Alves-Stanley, Christy D.; Worthy, Graham A.J.; Bonde, Robert K.

2010-01-01

The endangered West Indian manatee Trichechus manatus has 2 recognized subspecies: the Florida T. m. latirostris and Antillean T. m. manatus manatee, both of which are found in freshwater, estuarine, and marine habitats. A better understanding of manatee feeding preferences and habitat use is essential to establish criteria on which conservation plans can be based. Skin from manatees in Florida, Belize, and Puerto Rico, as well as aquatic vegetation from their presumed diet, were analyzed for stable carbon and nitrogen isotope ratios. This is the first application of stable isotope analysis to Antillean manatees. Stable isotope ratios for aquatic vegetation differed by plant type (freshwater, estuarine, and marine), collection location, and in one instance, season. Carbon and nitrogen isotope ratios for manatee skin differed between collection location and in one instance, season, but did not differ between sex or age class. Signatures in the skin of manatees sampled in Belize and Puerto Rico indicated a diet composed primarily of seagrasses, whereas those of Florida manatees exhibited greater regional variation. Mixing model results indicated that manatees sampled from Crystal River and Homosassa Springs (Florida, USA) ate primarily freshwater vegetation, whereas manatees sampled from Big Bend Power Plant, Ten Thousand Islands, and Warm Mineral Springs (Florida) fed primarily on seagrasses. Possible diet-tissue discrimination values for 15N were estimated to range from 1.0 to 1.5 per mil. Stable isotope analysis can be used to interpret manatee feeding behavior over a long period of time, specifically the use of freshwater vegetation versus seagrasses, and can aid in identifying critical habitats and improving conservation efforts.

Study of the matrix specific mass discrimination effects during inductively coupled plasma mass spectrometry isotope ratio measurements

International Nuclear Information System (INIS)

Vassileva, E.; Quetel, Ch.R.

2004-01-01

Sample matrix related effects on mass discrimination during inductively coupled plasma mass spectrometry (ICP-MS) isotope ratio measurements have only been rarely reported. However, they can lead to errors larger than the uncertainty claimed on the ratio results when not properly taken into account or corrected for. These matrix specific affects were experienced during an Isotope Dilution Mass Spectrometry (IDMS) campaign we carried out for the certification of the Cd amount content in some food digest samples (7% acidity and salts content around 450μg g -1 ). Dilution was not possible for Cd only present at the low ng g -1 level. Up to 1% difference was observed on Cd isotope ratio results between measurements performed directly or after matrix separation. This was a significant difference considering that less than 1.5% relative combined uncertainty was eventually estimated for these IDMS measurements. Similar results could be obtained either way after the implementation of necessary corrections. The direct measurement approach associated to a correction for mass discrimination effects using the food digest sample itself (and the IUPAC table values as reference for the natural Cd isotopic composition) was preferred as it was the easiest. Consequently, the impact of matrix effects on mass discrimination during isotope ratio measurements with two types of ICP- MS (quadrupole and magnetic sector instruments) was studied for 4 elements (Li, Cu, Cd and Tl). Samples of varying salinity (up to 0.25%) and acidity (up to 7%) characteristics were prepared using isotopic certified reference materials of these elements. The long term and short-term stability, respectively reproducibility and repeatability, of the results, as well as the evolution of the difference to certified ratio values were monitored. As expected the 13 investigated isotopic ratios were all sensitive to variations in salt and acid concentrations. Our experiments also showed that simultaneous variation

Calcium Isotope Analysis with "Peak Cut" Method on Column Chemistry

Science.gov (United States)

Zhu, H.; Zhang, Z.; Liu, F.; Li, X.

2017-12-01

To eliminate isobaric interferences from elemental and molecular isobars (e.g., 40K+, 48Ti+, 88Sr2+, 24Mg16O+, 27Al16O+) on Ca isotopes during mass determination, samples should be purified through ion-exchange column chemistry before analysis. However, large Ca isotopic fractionation has been observed during column chemistry (Russell and Papanastassiou, 1978; Zhu et al., 2016). Therefore, full recovery during column chemistry is greatly needed, otherwise uncertainties would be caused by poor recovery (Zhu et al., 2016). Generally, matrix effects could be enhanced by full recovery, as other elements might overlap with Ca cut during column chemistry. Matrix effects and full recovery are difficult to balance and both need to be considered for high-precision analysis of stable Ca isotopes. Here, we investigate the influence of poor recovery on δ44/40Ca using TIMS with the double spike technique. The δ44/40Ca values of IAPSO seawater, ML3B-G and BHVO-2 in different Ca subcats (e.g., 0-20, 20-40, 40-60, 60-80, 80-100%) with 20% Ca recovery on column chemistry display limited variation after correction by the 42Ca-43Ca double spike technique with the exponential law. Notably, δ44/40Ca of each Ca subcut is quite consistent with δ44/40Ca of Ca cut with full recovery within error. Our results indicate that the 42Ca-43Ca double spike technique can simultaneously correct both of the Ca isotopic fractionation that occurred during column chemistry and thermal ionization mass spectrometry (TIMS) determination properly, because both of the isotopic fractionation occurred during analysis follow the exponential law well. Therefore, we propose the "peak cut" method on Ca column chemistry for samples with complex matrix effects. Briefly, for samples with low Ca contents, we can add the double spike before column chemistry, and only collect the middle of the Ca eluate and abandon the both sides of Ca eluate that might overlap with other elements (e.g., K, Sr). This method would

Analysis of stable isotope assisted metabolomics data acquired by GC-MS

International Nuclear Information System (INIS)

Wei, Xiaoli; Shi, Biyun; Koo, Imhoi; Yin, Xinmin; Lorkiewicz, Pawel; Suhail, Hamid; Rattan, Ramandeep; Giri, Shailendra; McClain, Craig J.

2017-01-01

Stable isotope assisted metabolomics (SIAM) measures the abundance levels of metabolites in a particular pathway using stable isotope tracers (e.g., 13 C, 18 O and/or 15 N). We report a method termed signature ion approach for analysis of SIAM data acquired on a GC-MS system equipped with an electron ionization (EI) ion source. The signature ion is a fragment ion in EI mass spectrum of a derivatized metabolite that contains all atoms of the underivatized metabolite, except the hydrogen atoms lost during derivatization. In this approach, GC-MS data of metabolite standards were used to recognize the signature ion from the EI mass spectra acquired from stable isotope labeled samples, and a linear regression model was used to deconvolute the intensity of overlapping isotopologues. A mixture score function was also employed for cross-sample chromatographic peak list alignment to recognize the chromatographic peaks generated by the same metabolite in different samples, by simultaneously evaluating the similarity of retention time and EI mass spectrum of two chromatographic peaks. Analysis of a mixture of 16 13 C-labeled and 16 unlabeled amino acids showed that the signature ion approach accurately identified and quantified all isotopologues. Analysis of polar metabolite extracts from cells respectively fed with uniform 13 C-glucose and 13 C-glutamine further demonstrated that this method can also be used to analyze the complex data acquired from biological samples. - Highlights: • A signature ion approach is developed for analysis of stable isotope GC-MS data. • GC-MS data of compound standards are used for selection of the signature ion. • Linear regression model is used to deconvolute the overlapping isotopologue peaks. • The developed method was tested by known compounds and biological samples.

Rapid-swept CW cavity ring-down laser spectroscopy for carbon isotope analysis

International Nuclear Information System (INIS)

Tomita, Hideki; Watanabe, Kenichi; Takiguchi, Yu; Kawarabayashi, Jun; Iguchi, Tetsuo

2006-01-01

With the aim of developing a portable system for an in field isotope analysis, we investigate an isotope analysis based on rapid-swept CW cavity ring-down laser spectroscopy, in which the concentration of a chemical species is derived from its photo absorbance. Such a system can identify the isotopomer and still be constructed as a quite compact system. We have made some basic experimental measurements of the overtone absorption lines of carbon dioxide ( 12 C 16 O 2 , 13 C 16 O 2 ) by rapid-swept cavity ring-down spectroscopy with a CW infrared diode laser at 6,200 cm -1 (1.6 μm). The isotopic ratio has been obtained as (1.07±0.13)x10 -2 , in good agreement with the natural abundance within experimental uncertainty. The detection sensitivity in absorbance has been estimated to be 3x10 -8 cm -1 . (author)

Calculation of Site-specific Carbon-isotope Fractionation in Pedogenic Oxide Minerals

Energy Technology Data Exchange (ETDEWEB)

Rustad, James R.; Zarzycki, Piotr

2008-07-29

Ab initio molecular dynamics and quantum chemistry techniques are used to calculate the structure, vibrational frequencies, and carbon-isotope fractionation factors of the carbon dioxide component [CO2(m)] of soil (oxy)hydroxide minerals goethite, diaspore, and gibbsite. We have identified two possible pathways of incorporation of CO2(m) into (oxy)hydroxide crystal structures: one in which the C4+ substitutes for four H+ [CO2(m)A] and another in which C4+ substitutes for (Al3+,Fe3+) + H+ [CO2(m)B]. Calculations of isotope fractionation factors give large differences between the two structures, with the CO2(m)A being isotopically lighter than CO2(m)B by ≈10 per mil in the case of gibbsite and nearly 20 per mil in the case of goethite. The reduced partition function ratio of CO2(m)B structure in goethite differs from CO2(g) by <1 per mil. The predicted fractionation for gibbsite is >10 per mil higher, close to those measured for calcite and aragonite. The surprisingly large difference in the carbon-isotope fractionation factor between the CO2(m)A and CO2(m)B structures within a given mineral suggests that the isotopic signatures of soil (oxy)hydroxide could be heterogeneous.

Isotope analysis (δ13C of pulpy whole apple juice

Directory of Open Access Journals (Sweden)

Ricardo Figueira

2011-09-01

Full Text Available The objectives of this study were to develop the method of isotope analysis to quantify the carbon of C3 photosynthetic cycle in pulpy whole apple juice and to measure the legal limits based on Brazilian legislation in order to identify the beverages that do not conform to the Ministry of Agriculture, Livestock and Food Supply (MAPA. This beverage was produced in a laboratory according to the Brazilian law. Pulpy juices adulterated by the addition of sugarcane were also produced. The isotope analyses measured the relative isotope enrichment of the juices, their pulpy fractions (internal standard and purified sugar. From those results, the quantity of C3 source was estimated by means of the isotope dilution equation. To determine the existence of adulteration in commercial juices, it was necessary to create a legal limit according to the Brazilian law. Three brands of commercial juices were analyzed. One was classified as adulterated. The legal limit enabled to clearly identify the juice that was not in conformity with the Brazilian law. The methodology developed proved efficient for quantifying the carbon of C3 origin in commercial pulpy apple juices.

Source Attribution of Cyanides using Anionic Impurity Profiling, Stable Isotope Ratios, Trace Elemental Analysis and Chemometrics

Energy Technology Data Exchange (ETDEWEB)

Mirjankar, Nikhil S.; Fraga, Carlos G.; Carman, April J.; Moran, James J.

2016-01-08

Chemical attribution signatures (CAS) for chemical threat agents (CTAs) are being investigated to provide an evidentiary link between CTAs and specific sources to support criminal investigations and prosecutions. In a previous study, anionic impurity profiles developed using high performance ion chromatography (HPIC) were demonstrated as CAS for matching samples from eight potassium cyanide (KCN) stocks to their reported countries of origin. Herein, a larger number of solid KCN stocks (n = 13) and, for the first time, solid sodium cyanide (NaCN) stocks (n = 15) were examined to determine what additional sourcing information can be obtained through anion, carbon stable isotope, and elemental analyses of cyanide stocks by HPIC, isotope ratio mass spectrometry (IRMS), and inductively coupled plasma optical emission spectroscopy (ICP-OES), respectively. The HPIC anion data was evaluated using the variable selection methods of Fisher-ratio (F-ratio), interval partial least squares (iPLS), and genetic algorithm-based partial least squares (GAPLS) and the classification methods of partial least squares discriminate analysis (PLSDA), K nearest neighbors (KNN), and support vector machines discriminate analysis (SVMDA). In summary, hierarchical cluster analysis (HCA) of anion impurity profiles from multiple cyanide stocks from six reported country of origins resulted in cyanide samples clustering into three groups: Czech Republic, Germany, and United States, independent of the associated alkali metal (K or Na). The three country groups were independently corroborated by HCA of cyanide elemental profiles and corresponded to countries with known solid cyanide factories. Both the anion and elemental CAS are believed to originate from the aqueous alkali hydroxides used in cyanide manufacture. Carbon stable isotope measurements resulted in two clusters: Germany and United States (the single Czech stock grouped with United States stocks). The carbon isotope CAS is believed to

Isotope dilution analysis for urinary fentanyl and its main metabolite, norfentanyl, in patients by isotopic fractionation using capillary gas chromatography

Energy Technology Data Exchange (ETDEWEB)

Sera, Shoji; Goromaru, Tsuyoshi [Fukuyama Univ., Hiroshima (Japan). Faculty of Pharmacy and Pharmaceutical Sciences; Sameshima, Teruko; Kawasaki, Koichi; Oda, Toshiyuki

1998-07-01

Isotope dilution analysis was applied to determine urinary excretion of fentanyl (FT) and its main metabolite, norfentanyl (Nor-FT), by isotopic fractionation using a capillary gas chromatograph equipped with a surface ionization detector (SID). Urinary FT was determined quantitatively in the range of 0.4-40 ng/ml using deuterium labeled FT (FT-{sup 2}H{sub 19}), as an internal standard. We also performed isotope dilution analysis of Nor-FT in urine. N-Alkylation was necessary to sensitively detect Nor-FT with SID. Methyl derivative was selected from 3 kinds of N-alkyl derivatives to increase sensitivity and peak resolution, and to prevent interference with urinary compound. Nor-FT concentration was quantitatively determined in the range of 10-400 ng/ml using deuterium labeled Nor-FT (Nor-FT-{sup 2}H{sub 10}). No endogenous compounds or concomitant drugs interfered with the detection of FT and Nor-FT in the urine of patients. The present method will be useful for pharmacokinetic studies and the evaluation of drug interactions in FT metabolism. (author)

Isotope dilution analysis for urinary fentanyl and its main metabolite, norfentanyl, in patients by isotopic fractionation using capillary gas chromatography

International Nuclear Information System (INIS)

Sera, Shoji; Goromaru, Tsuyoshi; Sameshima, Teruko; Kawasaki, Koichi; Oda, Toshiyuki

1998-01-01

Isotope dilution analysis was applied to determine urinary excretion of fentanyl (FT) and its main metabolite, norfentanyl (Nor-FT), by isotopic fractionation using a capillary gas chromatograph equipped with a surface ionization detector (SID). Urinary FT was determined quantitatively in the range of 0.4-40 ng/ml using deuterium labeled FT (FT- 2 H 19 ), as an internal standard. We also performed isotope dilution analysis of Nor-FT in urine. N-Alkylation was necessary to sensitively detect Nor-FT with SID. Methyl derivative was selected from 3 kinds of N-alkyl derivatives to increase sensitivity and peak resolution, and to prevent interference with urinary compound. Nor-FT concentration was quantitatively determined in the range of 10-400 ng/ml using deuterium labeled Nor-FT (Nor-FT- 2 H 10 ). No endogenous compounds or concomitant drugs interfered with the detection of FT and Nor-FT in the urine of patients. The present method will be useful for pharmacokinetic studies and the evaluation of drug interactions in FT metabolism. (author)

Isotope ratio analysis by a combination of element analyzer and mass spectrometer

International Nuclear Information System (INIS)

Pichlmayer, F.

1987-06-01

The use of stable isotope ratios of carbon, nitrogen and sulfur as analytical tool in many fields of research is of growing interest. A method has therefore been developed, consisting in essential of coupling an Elemental Analyzer with an Isotope Mass Spectrometer, which enables the gas preparation of carbon dioxide, nitrogen and sulfur dioxide from any solid or liquid sample in a fast and easy way. Results of carbon isotope measurements in food analysis are presented, whereat it is possible to check origin and treatment of sugar, oils, fats, mineral waters, spirituous liquors etc. and to detect adulterations as well. Also applications in the field of environmental research are given. (Author)

Chemically modified glasses for analysis of hydrogen isotopes by gas-chromatography

International Nuclear Information System (INIS)

Stanciu, Vasile; Stefanescu, Doina

1999-01-01

Hydrogen isotope separation process by such methods as cryogenic distillation or thermal diffusion method is one of the key technologies of the tritium separation from heavy water of CANDU reactors and in the tritium fuel cycle for a thermonuclear fusion reactor. In each process, the analytical techniques for measuring contents of hydrogen isotope mixture are necessary. An extensive experimental research has been carried out in order to produce the most suitable absorbent and define the best operating conditions for selective separation and analysis of hydrogen isotope by gas-chromatography. This paper describes the preparation of adsorbent materials utilised as stationary phase in the gas-chromatographic column for hydrogen isotope separation and treatment (activation) of stationary phase. Modified thermo-resisting glass with Fe(NH 4 ) 2 (SO 4 ) 2 6H 2 O and Cr 2 O 3 , respectively, have been experimentally investigated at 77 K for H 2 , HD and D 2 separation and the results of chromatographic runs are also reported and discussed. The gas-chromatographic apparatus used is composed of a Hewlett-Packard 7620A gas-chromatograph equipped with a gas carrier flow rate controller and a thermal conductivity detector (TCD). The apparatus comprises also a Dewar vessel containing the separation column. The hydrogen isotopes H 2 , HD, D 2 and their mixture have been obtained in our laboratories. The best operating conditions of the adsorbent column Fe (III)/glass and Cr 2 O 3 /glass, i.e. granulometry, column length, pressure-drop along the column, carrier gas flow rate, sample volume have been studied by means of the analysis of the retention times, separation factors and HETP. (authors)

ISODEP, A Fuel Depletion Analysis Code for Predicting Isotopic ...

African Journals Online (AJOL)

The trend of results was found to be consistent with those obtained by analytical and other numerical methods. Discovery and Innovation Vol. 13 no. 3/4 December (2001) pp. 184-195. KEY WORDS: depletion analysis, code, research reactor, simultaneous equations, decay of nuclides, radionuclitides, isotope. Résumé

Carbon isotopic analysis of atmospheric methane by isotope-ratio-monitoring gas chromatography-mass spectrometry

Science.gov (United States)

Merritt, Dawn A.; Hayes, J. M.; Des Marais, David J.

1995-01-01

Less than 15 min are required for the determination of delta C(sub PDB)-13 with a precision of 0.2 ppt(1 sigma, single measurement) in 5-mL samples of air containing CH4 at natural levels (1.7 ppm). An analytical system including a sample-introduction unit incorporating a preparative gas chromatograph (GC) column for separation of CH4 from N2, O2, and Ar is described. The 15-min procedure includes time for operation of that system, high-resolution chromatographic separation of the CH4, on-line combustion and purification of the products, and isotopic calibration. Analyses of standards demonstrate that systematic errors are absent and that there is no dependence of observed values of delta on sample size. For samples containing 100 ppm or more CH4, preconcentration is not required and the analysis time is less than 5 min. The system utilizes a commercially available, high-sensitivity isotope-ratio mass spectrometer. For optimal conditions of smaple handling and combustion, performance of the system is within a factor of 2 of the shot-noise limit. The potential exists therefore for analysis of samples as small as 15 pmol CH4 with a standard deviation of less than 1 ppt.

First stable isotope analysis of Asiatic wild ass tail hair from the Mongolian Gobi.

Science.gov (United States)

Horacek, Micha; Sturm, Martina Burnik; Kaczensky, Petra

Stable isotope analysis has become a powerful tool to study feeding ecology, water use or movement pattern in contemporary, historic and ancient species. Certain hair and teeth grow continuously, and when sampled longitudinally can provide temporally explicit information on dietary regime and movement pattern. In an initial trial, we analysed a tail sample of an Asiatic wild ass ( Equus hemionus ) from the Mongolian Gobi. We found seasonal variations in H, C and N isotope patterns, likely being the result of temporal variations in available feeds, water supply and possibly physiological status. Thus stable isotope analysis shows promise to study the comparative ecology of the three autochthonous equid species in the Mongolian Gobi.

In-situ Isotopic Analysis at Nanoscale using Parallel Ion Electron Spectrometry: A Powerful New Paradigm for Correlative Microscopy

Science.gov (United States)

Yedra, Lluís; Eswara, Santhana; Dowsett, David; Wirtz, Tom

2016-01-01

Isotopic analysis is of paramount importance across the entire gamut of scientific research. To advance the frontiers of knowledge, a technique for nanoscale isotopic analysis is indispensable. Secondary Ion Mass Spectrometry (SIMS) is a well-established technique for analyzing isotopes, but its spatial-resolution is fundamentally limited. Transmission Electron Microscopy (TEM) is a well-known method for high-resolution imaging down to the atomic scale. However, isotopic analysis in TEM is not possible. Here, we introduce a powerful new paradigm for in-situ correlative microscopy called the Parallel Ion Electron Spectrometry by synergizing SIMS with TEM. We demonstrate this technique by distinguishing lithium carbonate nanoparticles according to the isotopic label of lithium, viz. 6Li and 7Li and imaging them at high-resolution by TEM, adding a new dimension to correlative microscopy. PMID:27350565

Development of a new method for hydrogen isotope analysis of trace hydrocarbons in natural gas samples

Directory of Open Access Journals (Sweden)

Xibin Wang

2016-12-01

Full Text Available A new method had been developed for the analysis of hydrogen isotopic composition of trace hydrocarbons in natural gas samples by using solid phase microextraction (SPME combined with gas chromatography-isotope ratio mass spectrometry (GC/IRMS. In this study, the SPME technique had been initially introduced to achieve the enrichment of trace content of hydrocarbons with low abundance and coupled to GC/IRMS for hydrogen isotopic analysis. The main parameters, including the equilibration time, extraction temperature, and the fiber type, were systematically optimized. The results not only demonstrated that high extraction yield was true but also shows that the hydrogen isotopic fractionation was not observed during the extraction process, when the SPME device fitted with polydimethylsiloxane/divinylbenzene/carbon molecular sieve (PDMS/DVB/CAR fiber. The applications of SPME-GC/IRMS method were evaluated by using natural gas samples collected from different sedimentary basins; the standard deviation (SD was better than 4‰ for reproducible measurements; and also, the hydrogen isotope values from C1 to C9 can be obtained with satisfying repeatability. The SPME-GC/IRMS method fitted with PDMS/DVB/CAR fiber is well suited for the preconcentration of trace hydrocarbons, and provides a reliable hydrogen isotopic analysis for trace hydrocarbons in natural gas samples.

Error analysis of isotope dilution mass spectrometry method with internal standard

International Nuclear Information System (INIS)

Rizhinskii, M.W.; Vitinskii, M.Y.

1989-02-01

The computation algorithms of the normalized isotopic ratios and element concentration by isotope dilution mass spectrometry with internal standard are presented. A procedure based on the Monte-Carlo calculation is proposed for predicting the magnitude of the errors to be expected. The estimation of systematic and random errors is carried out in the case of the certification of uranium and plutonium reference materials as well as for the use of those reference materials in the analysis of irradiated nuclear fuels. 4 refs, 11 figs, 2 tabs

Direct uranium isotope ratio analysis of single micrometer-sized glass particles

OpenAIRE

Kappel, Stefanie; Boulyga, Sergei F.; Prohaska, Thomas

2012-01-01

We present the application of nanosecond laser ablation (LA) coupled to a ‘Nu Plasma HR’ multi collector inductively coupled plasma mass spectrometer (MC-ICP-MS) for the direct analysis of U isotope ratios in single, 10–20 μm-sized, U-doped glass particles. Method development included studies with respect to (1) external correction of the measured U isotope ratios in glass particles, (2) the applied laser ablation carrier gas (i.e. Ar versus He) and (3) the accurate determination of lower abu...

Total and species-specific quantitative analyses of trace elements in sediment by isotope dilution inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Inagaki, Kazumi; Takatsu, Akiko; Yarita, Takashi; Okamoto, Kensaku; Chiba, Koichi

2009-01-01

Isotope dilution inductively coupled plasma mass spectrometry (ID-ICP-MS) is one of the reliable methods for total and species-specific quantitative analysis of trace elements. However, several technical problems (e.g. spectral interference caused from sample constituents) should be overcome to obtain reliable analytical results when environmental samples are analyzed by ID-ICP-MS. In our laboratory, various methods based on ID-ICP-MS have been investigated for reliable quantitative analyses of trace elements in environmental samples. In this paper, coprecipitate separation/ID-ICP-MS for the determination of trace elements in sediment, cation exchange disk filtration/ID-ICP-MS for the determination of selenium in sediment, species-specific ID-ICP-MS using 118 Sn/labeled organotin compounds for the determination of butyltins and phenyltins, and the application of the ID-ICP-MS methods to the certification of sediment reference materials are described. (author)

Optimization and Validation of the Developed Uranium Isotopic Analysis Code

Energy Technology Data Exchange (ETDEWEB)

Kim, J. H.; Kang, M. Y.; Kim, Jinhyeong; Choi, H. D. [Seoul National Univ., Seoul (Korea, Republic of)

2014-10-15

γ-ray spectroscopy is a representative non-destructive assay for nuclear material, and less time-consuming and less expensive than the destructive analysis method. The destructive technique is more precise than NDA technique, however, there is some correction algorithm which can improve the performance of γ-spectroscopy. For this reason, an analysis code for uranium isotopic analysis is developed by Applied Nuclear Physics Group in Seoul National University. Overlapped γ- and x-ray peaks in the 89-101 keV X{sub α}-region are fitted with Gaussian and Lorentzian distribution peak functions, tail and background functions. In this study, optimizations for the full-energy peak efficiency calibration and fitting parameters of peak tail and background are performed, and validated with 24 hour acquisition of CRM uranium samples. The optimization of peak tail and background parameters are performed with the validation by using CRM uranium samples. The analysis performance is improved in HEU samples, but more optimization of fitting parameters is required in LEU sample analysis. In the future, the optimization research about the fitting parameters with various type of uranium samples will be performed. {sup 234}U isotopic analysis algorithms and correction algorithms (coincidence effect, self-attenuation effect) will be developed.

Analysis of transuranic isotopes in irradiated U3Si2-Al fuel by alpha spectrometry

International Nuclear Information System (INIS)

Dian Anggraini; Aslina B Ginting; Arif Nugroho

2011-01-01

Separation and analysis of transuranic isotopes (uranium and plutonium) in irradiated U 3 Si 2 -Al plate has been done. The analysis experiment includes sample preparation (i.e. cutting, dissolving, filtering, dilution), fission products separation from heavy elements, and analysis of transuranic isotopes content with alpha spectrometer. The separation of transuranic isotopes (U, Pu) was done by two methods, i.e. direct method and ion exchanger method with zeolite. Measurement of standard transuranic isotope (AMR 43) and standard U 3 O 8 was done in advance in order to determine percentage of 235 U recovery and detector efficiency. Recovery of 235 U isotope was obtained as much as 92,58%, which fulfills validation requirement, and the detector efficiency was 0.314. Based on the measured recovery and detector efficiency, the separation was done by direct electrodeposition method of 250 µL irradiated U 3 Si 2 -Al solution. The deposited sample was subsequently analyzed with alpha spectrometer. The separation with ion exchanger was done by mixing and shaking of 300 µL irradiated U 3 Si 2 -Al solution and 0.5 gram zeolite to separate the liquid phase from the solid phase. The liquid phase was electrodeposited and analyzed with alpha spectrometer. The analysis of transuranic isotopes (U, Pu) by both methods shows different results. Heavy element ( 238 U, 236 U, 234 U, 239 Pu) content obtained by direct method was 0.0525 g/g and 235 U= 0.0076 g/g, while the separation using zeolite ion exchanger resulted in Heavy element = 0.0253 g/g and 235 U = 0.0092 g/g. (author)

Carbon isotope analysis in apple nectar beverages

Directory of Open Access Journals (Sweden)

Ricardo Figueira

2013-03-01

Full Text Available The aims of this study were to use the isotope analysis method to quantify the carbon of C3 photosynthetic cycle in commercial apple nectars and to determine the legal limit to identify the beverages that do not conform to the safety standards established by the Brazilian Ministry of Agriculture, Livestock and Food Supply. These beverages (apple nectars were produced in the laboratory according to the Brazilian legislation. Adulterated nectars were also produced with an amount of pulp juice below the permitted threshold limit value. The δ13C values of the apple nectars and their fractions (pulp and purified sugar were measured to quantify the C3 source percentage. In order to demonstrate the existence of adulteration, the values found were compared to the limit values established by the Brazilian Law. All commercial apple nectars analyzed were within the legal limits, which enabled to identify the nectars that were in conformity with the Brazilian Law. The isotopic methodology developed proved efficient to quantify the carbon of C3 origin in commercial apple nectars.

Review: Current applications and challenges for liquid chromatography coupled to isotope ratio mass spectrometry (LC/IRMS).

Science.gov (United States)

Godin, Jean-Philippe; McCullagh, James S O

2011-10-30

High-precision isotope analysis is recognized as an essential research tool in many fields of study. Until recently, continuous flow isotope ratio mass spectrometry (CF-IRMS) was available via an elemental analyzer or a gas chromatography inlet system for compound-specific analysis of light stable isotopes. In 2004, however, an interface that coupled liquid chromatography with IRMS (LC/IRMS) became commercially available for the first time. This brought the capability for new areas of application, in particular enabling compound-specific δ(13)C analysis of non-volatile, aqueous soluble, compounds from complex mixtures. The interface design brought with it several analytical constraints, however, in particular a lack of compatibility with certain types of chromatography as well as limited flow rates and mobile phase compositions. Routine LC/IRMS methods have, however, been established for measuring the δ(13)C isotopic ratios of underivatized individual compounds for application in archeology, nutrition and physiology, geochemistry, hydrology, soil science and food authenticity. Seven years after its introduction, we review the technical advances and constraints, methodological developments and new applications of liquid chromatography coupled to isotope ratio mass spectrometry. Copyright © 2011 John Wiley & Sons, Ltd.

Direct U isotope analysis in μm-sized particles by LA-MC-ICPMS

International Nuclear Information System (INIS)

Kappel, S.; Boulyga, S.F.; Prohaska, T.

2009-01-01

Full text: The knowledge of the isotopic composition of individual μm-sized hot particles is of great interest especially for strengthened nuclear safeguards in order to identify undeclared nuclear activities. We present the potential of a 'Nu Plasma HR' MC-ICPMS coupled to a New Wave 'UP 193' laser ablation (LA) system for the direct analysis of U isotope abundance ratios in individual μm-sized particles. The ability to determine 234 U/ 238 U and 235 U/ 238 U isotope ratios was successfully demonstrated in the NUSIMEP-6 interlaboratory comparison, which was organized by the IRMM (Geel, Belgium). (author)

Stable isotopes labelled compounds

International Nuclear Information System (INIS)

1982-09-01

The catalogue on stable isotopes labelled compounds offers deuterium, nitrogen-15, and multiply labelled compounds. It includes: (1) conditions of sale and delivery, (2) the application of stable isotopes, (3) technical information, (4) product specifications, and (5) the complete delivery programme

Stable isotope separation by thermal diffusion

International Nuclear Information System (INIS)

Vasaru, Gheorghe

2001-01-01

Thermal diffusion in both gaseous and liquid phase has been subject of extensive experimental and theoretical investigations, especially after the invention of K. Clusius and G. Dickel of the thermal diffusion column, sixty three years ago. This paper gives a brief overview of the most important research and developments performed during the time at the National Institute for Research and Development for Isotopic and Molecular Technology (ITIM) at Cluj - Napoca, Romania in the field of separation of stable isotopes by thermal diffusion. An retrospective analysis of the research and results concerning isotope separation by thermal diffusion entails the following conclusions: - thermal diffusion is an adequate method for hydrogen isotope separation (deuterium and tritium) and for noble gas isotope separation (He, Ne, Ar, Kr, Xe); - thermal diffusion is attractive also for 13 C enrichment using methane as raw material for separation, when annual yields of up to 100 g are envisaged; - lately, the thermal diffusion appears to be chosen as a final enrichment step for 17 O. An obvious advantage of this method is its non-specificity, i.e. the implied equipment can be utilized for isotope separation of other chemical elements too. Having in view the low investment costs for thermal diffusion cascades the method appears economically attractive for obtaining low-scale, laboratory isotope production. The paper has the following content: 1. The principle of method; 2. The method's application; 3. Research in the field of thermal diffusion at ITIM; 4. Thermal diffusion cascades for N, C, Ne, Ar and Kr isotope separation; 5. Conclusion

Isotopic analysis of bullet lead samples

International Nuclear Information System (INIS)

Sankar Das, M.; Venkatasubramanian, V.S.; Sreenivas, K.

1976-01-01

The possibility of using the isotopic composition of lead for the identification of bullet lead is investigated. Lead from several spent bullets were converted to lead sulphide and analysed for the isotopic abundances using an MS-7 mass spectrometer. The abundances are measured relative to that for Pb 204 was too small to permit differentiation, while the range of variation of Pb 206 and Pb 207 and the better precision in their analyses permitted differentiating samples from one another. The correlation among the samples examined has been pointed out. The method is complementary to characterisation of bullet leads by the trace element composition. The possibility of using isotopically enriched lead for tagging bullet lead is pointed out. (author)

Application of stable isotope analysis to study temporal changes in foraging ecology in a highly endangered amphibian.

Directory of Open Access Journals (Sweden)

J Hayley Gillespie

Full Text Available Understanding dietary trends for endangered species may be essential to assessing the effects of ecological disturbances such as habitat modification, species introductions or global climate change. Documenting temporal variation in prey selection may also be crucial for understanding population dynamics. However, the rarity, secretive behaviours and obscure microhabitats of some endangered species can make direct foraging observations difficult or impossible. Furthermore, the lethality or invasiveness of some traditional methods of dietary analysis (e.g. gut contents analysis, gastric lavage makes them inappropriate for such species. Stable isotope analysis facilitates non-lethal, indirect analysis of animal diet that has unrealized potential in the conservation of endangered organisms, particularly amphibians.I determined proportional contributions of aquatic macroinvertebrate prey to the diet of an endangered aquatic salamander Eurycea sosorum over a two-year period using stable isotope analysis of (13/12C and (15/14N and the Bayesian stable isotope mixing model SIAR. I calculated Strauss' dietary electivity indices by comparing these proportions with changing relative abundance of potential prey species through time. Stable isotope analyses revealed that a previously unknown prey item (soft-bodied planarian flatworms in the genus Dugesia made up the majority of E. sosorum diet. Results also demonstrate that E. sosorum is an opportunistic forager capable of diet switching to include a greater proportion of alternative prey when Dugesia populations decline. There is also evidence of intra-population dietary variation.Effective application of stable isotope analysis can help circumvent two key limitations commonly experienced by researchers of endangered species: the inability to directly observe these species in nature and the invasiveness or lethality of traditional methods of dietary analysis. This study illustrates the feasibility of stable

Copper and tin isotopic analysis of ancient bronzes for archaeological investigation: development and validation of a suitable analytical methodology.

Science.gov (United States)

Balliana, Eleonora; Aramendía, Maite; Resano, Martin; Barbante, Carlo; Vanhaecke, Frank

2013-03-01

Although in many cases Pb isotopic analysis can be relied on for provenance determination of ancient bronzes, sometimes the use of "non-traditional" isotopic systems, such as those of Cu and Sn, is required. The work reported on in this paper aimed at revising the methodology for Cu and Sn isotope ratio measurements in archaeological bronzes via optimization of the analytical procedures in terms of sample pre-treatment, measurement protocol, precision, and analytical uncertainty. For Cu isotopic analysis, both Zn and Ni were investigated for their merit as internal standard (IS) relied on for mass bias correction. The use of Ni as IS seems to be the most robust approach as Ni is less prone to contamination, has a lower abundance in bronzes and an ionization potential similar to that of Cu, and provides slightly better reproducibility values when applied to NIST SRM 976 Cu isotopic reference material. The possibility of carrying out direct isotopic analysis without prior Cu isolation (with AG-MP-1 anion exchange resin) was investigated by analysis of CRM IARM 91D bronze reference material, synthetic solutions, and archaeological bronzes. Both procedures (Cu isolation/no Cu isolation) provide similar δ (65)Cu results with similar uncertainty budgets in all cases (±0.02-0.04 per mil in delta units, k = 2, n = 4). Direct isotopic analysis of Cu therefore seems feasible, without evidence of spectral interference or matrix-induced effect on the extent of mass bias. For Sn, a separation protocol relying on TRU-Spec anion exchange resin was optimized, providing a recovery close to 100 % without on-column fractionation. Cu was recovered quantitatively together with the bronze matrix with this isolation protocol. Isotopic analysis of this Cu fraction provides δ (65)Cu results similar to those obtained upon isolation using AG-MP-1 resin. This means that Cu and Sn isotopic analysis of bronze alloys can therefore be carried out after a single chromatographic

Optimization of the solvent-based dissolution method to sample volatile organic compound vapors for compound-specific isotope analysis.

Science.gov (United States)

Bouchard, Daniel; Wanner, Philipp; Luo, Hong; McLoughlin, Patrick W; Henderson, James K; Pirkle, Robert J; Hunkeler, Daniel

2017-10-20

The methodology of the solvent-based dissolution method used to sample gas phase volatile organic compounds (VOC) for compound-specific isotope analysis (CSIA) was optimized to lower the method detection limits for TCE and benzene. The sampling methodology previously evaluated by [1] consists in pulling the air through a solvent to dissolve and accumulate the gaseous VOC. After the sampling process, the solvent can then be treated similarly as groundwater samples to perform routine CSIA by diluting an aliquot of the solvent into water to reach the required concentration of the targeted contaminant. Among solvents tested, tetraethylene glycol dimethyl ether (TGDE) showed the best aptitude for the method. TGDE has a great affinity with TCE and benzene, hence efficiently dissolving the compounds during their transition through the solvent. The method detection limit for TCE (5±1μg/m 3 ) and benzene (1.7±0.5μg/m 3 ) is lower when using TGDE compared to methanol, which was previously used (385μg/m 3 for TCE and 130μg/m 3 for benzene) [2]. The method detection limit refers to the minimal gas phase concentration in ambient air required to load sufficient VOC mass into TGDE to perform δ 13 C analysis. Due to a different analytical procedure, the method detection limit associated with δ 37 Cl analysis was found to be 156±6μg/m 3 for TCE. Furthermore, the experimental results validated the relationship between the gas phase TCE and the progressive accumulation of dissolved TCE in the solvent during the sampling process. Accordingly, based on the air-solvent partitioning coefficient, the sampling methodology (e.g. sampling rate, sampling duration, amount of solvent) and the final TCE concentration in the solvent, the concentration of TCE in the gas phase prevailing during the sampling event can be determined. Moreover, the possibility to analyse for TCE concentration in the solvent after sampling (or other targeted VOCs) allows the field deployment of the sampling

Isotopic analysis using optical spectroscopy (1963)

International Nuclear Information System (INIS)

Gerstenkorn, S.

1963-01-01

The isotopic displacement in the atomic lines of certain elements (H, He, Li, Ne, Sr, Hg, Pb, U, Pu) is used for dosing these elements isotopically. The use of the Fabry-Perot photo-electric interference spectrometer is shown to be particularly adapted for this sort of problem: in each case we give on the one hand the essential results obtained with this apparatus, and on the other hand the results previously obtained with a conventional apparatus (grating, photographic plate). These results together give an idea of the possibilities of optical spectroscopy: in the best case, the precision which may be expected is of the order of 1 to 2 per cent for isotopes whose concentration is about 1 per cent. (author) [fr

Trophodynamics and functional feeding groups of North Sea fauna: a combined stable isotope and fatty acid approach

NARCIS (Netherlands)

Kürten, B.; Frutos, I.; Struck, U.; Painting, S.J.; Polunin, N.V.C.; Middelburg, J.J.

The trophodynamics of pelagic and benthic animals of the North Sea, North Atlantic shelf, were assessed using stable isotope analysis (SIA) of natural abundance carbon and nitrogen isotopes, lipid fingerprinting and compound-specific SIA (CSIA) of phospholipid-derived fatty acids (PLFAs).

Trophodynamics and functional feeding groups of North Sea fauna: a combined stable isotope and fatty acid approach

NARCIS (Netherlands)

Kürten, B.; Frutos, I.; Struck, U.; Painting, S.J.; Polunin, N.V.C.; Middelburg, J.J.

2013-01-01

The trophodynamics of pelagic and benthic animals of the North Sea, North Atlantic shelf, were assessed using stable isotope analysis (SIA) of natural abundance carbon and nitrogen isotopes, lipid fingerprinting and compound-specific SIA (CSIA) of phospholipid-derived fatty acids (PLFAs).

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)

Spectrum analysis in lead spectrometer for isotopic fissile assay in used fuel

International Nuclear Information System (INIS)

Lee, Y.D.; Park, C.J.; Kim, H.D.; Song, K.C.

2014-01-01

The LSDS system is under development for analyzing isotopic fissile content applicable in a hot cell for the pyro process. The fuel assay area and nuclear material composition were selected for simulation. The source mechanism for efficient neutron generation was also determined. A neutron is produced at the Ta target by hitting it from accelerated electron. The parameters for an electron accelerator are being researched for cost effectiveness, easy maintenance, and compact size. The basic principle of LSDS is that isotopic fissile has its own fission structure below the unresolved resonance region. The source neutron interacts with a lead medium and produces continuous neutron energy, which generates dominant fission at each fissile. Therefore, a spectrum analysis is very important at a lead medium and fuel area for system working. The energy spectrum with respect to slowing down energy and the energy resolution were investigated in lead. A spectrum analysis was done by the existence of surrounding detectors. In particular, high resonance energy was considered. The spectrum was well organized at each slowing down energy and the energy resolution was acceptable to distinguish isotopic fissile fissions. Additionally, LSDS is applicable for the optimum design of spent fuel storage and management.The isotopic fissile content assay will increase the transparency and credibility for spent fuel storage and its re-utilization, as demanded internationally. (author)

A Practical Cryogen-Free CO2 Purification and Freezing Technique for Stable Isotope Analysis.

Science.gov (United States)

Sakai, Saburo; Matsuda, Shinichi

2017-04-18

Since isotopic analysis by mass spectrometry began in the early 1900s, sample gas for light-element isotopic measurements has been purified by the use of cryogens and vacuum-line systems. However, this conventional purification technique can achieve only certain temperatures that depend on the cryogens and can be sustained only as long as there is a continuous cryogen supply. Here, we demonstrate a practical cryogen-free CO 2 purification technique using an electrical operated cryocooler for stable isotope analysis. This approach is based on portable free-piston Stirling cooling technology and controls the temperature to an accuracy of 0.1 °C in a range from room temperature to -196 °C (liquid-nitrogen temperature). The lowest temperature can be achieved in as little as 10 min. We successfully purified CO 2 gas generated by carbonates and phosphoric acid reaction and found its sublimation point to be -155.6 °C at 0.1 Torr in the vacuum line. This means that the temperature required for CO 2 trapping is much higher than the liquid-nitrogen temperature. Our portable cooling system offers the ability to be free from the inconvenience of cryogen use for stable isotope analysis. It also offers a new cooling method applicable to a number of fields that use gas measurements.

Field ionization mass spectrometry (FIMS) applied to tracer studies and isotope dilution analysis

International Nuclear Information System (INIS)

Anbar, M.; Heck, H.d'A.; McReynolds, J.H.; St John, G.A.

1975-01-01

The nonfragmenting nature of field ionization mass spectrometry makes it a preferred technique for the isotopic analysis of multilabeled organic compounds. The possibility of field ionization of nonvolatile thermolabile materials significantly extends the potential uses of this technique beyond those of conventional ionization methods. Multilabeled tracers may be studied in biological systems with a sensitivity comparable to that of radioactive tracers. Isotope dilution analysis may be performed reliably by this technique down to picogram levels. These techniques will be illustrated by a number of current studies using multilabeled metabolites and drugs. The scope and limitations of the methodology are discussed

Stable isotope tracking of endangered sea turtles: validation with satellite telemetry and δ15N analysis of amino acids.

Directory of Open Access Journals (Sweden)

Jeffrey A Seminoff

Full Text Available Effective conservation strategies for highly migratory species must incorporate information about long-distance movements and locations of high-use foraging areas. However, the inherent challenges of directly monitoring these factors call for creative research approaches and innovative application of existing tools. Highly migratory marine species, such as marine turtles, regularly travel hundreds or thousands of kilometers between breeding and feeding areas, but identification of migratory routes and habitat use patterns remains elusive. Here we use satellite telemetry in combination with compound-specific isotope analysis of amino acids to confirm that insights from bulk tissue stable isotope analysis can reveal divergent migratory strategies and within-population segregation of foraging groups of critically endangered leatherback sea turtles (Dermochelys coriacea across the Pacific Ocean. Among the 78 turtles studied, we found a distinct dichotomy in δ(15N values of bulk skin, with distinct "low δ(15N" and "high δ(15N" groups. δ(15N analysis of amino acids confirmed that this disparity resulted from isotopic differences at the base of the food chain and not from differences in trophic position between the two groups. Satellite tracking of 13 individuals indicated that their bulk skin δ(15N value was linked to the particular foraging region of each turtle. These findings confirm that prevailing marine isoscapes of foraging areas can be reflected in the isotopic compositions of marine turtle body tissues sampled at nesting beaches. We use a Bayesian mixture model to show that between 82 and 100% of the 78 skin-sampled turtles could be assigned with confidence to either the eastern Pacific or western Pacific, with 33 to 66% of all turtles foraging in the eastern Pacific. Our forensic approach validates the use of stable isotopes to depict leatherback turtle movements over broad spatial ranges and is timely for establishing wise conservation

Stable isotope tracking of endangered sea turtles: validation with satellite telemetry and δ15N analysis of amino acids.

Science.gov (United States)

Seminoff, Jeffrey A; Benson, Scott R; Arthur, Karen E; Eguchi, Tomoharu; Dutton, Peter H; Tapilatu, Ricardo F; Popp, Brian N

2012-01-01

Effective conservation strategies for highly migratory species must incorporate information about long-distance movements and locations of high-use foraging areas. However, the inherent challenges of directly monitoring these factors call for creative research approaches and innovative application of existing tools. Highly migratory marine species, such as marine turtles, regularly travel hundreds or thousands of kilometers between breeding and feeding areas, but identification of migratory routes and habitat use patterns remains elusive. Here we use satellite telemetry in combination with compound-specific isotope analysis of amino acids to confirm that insights from bulk tissue stable isotope analysis can reveal divergent migratory strategies and within-population segregation of foraging groups of critically endangered leatherback sea turtles (Dermochelys coriacea) across the Pacific Ocean. Among the 78 turtles studied, we found a distinct dichotomy in δ(15)N values of bulk skin, with distinct "low δ(15)N" and "high δ(15)N" groups. δ(15)N analysis of amino acids confirmed that this disparity resulted from isotopic differences at the base of the food chain and not from differences in trophic position between the two groups. Satellite tracking of 13 individuals indicated that their bulk skin δ(15)N value was linked to the particular foraging region of each turtle. These findings confirm that prevailing marine isoscapes of foraging areas can be reflected in the isotopic compositions of marine turtle body tissues sampled at nesting beaches. We use a Bayesian mixture model to show that between 82 and 100% of the 78 skin-sampled turtles could be assigned with confidence to either the eastern Pacific or western Pacific, with 33 to 66% of all turtles foraging in the eastern Pacific. Our forensic approach validates the use of stable isotopes to depict leatherback turtle movements over broad spatial ranges and is timely for establishing wise conservation efforts in

Isotope selection for patients undergoing prostate brachytherapy

International Nuclear Information System (INIS)

Cha, Christine M.; Potters, Louis; Ashley, Richard; Freeman, Katherine; Wang Xiaohong; Waldbaum, Robert; Leibel, Steven

1999-01-01

Purpose: Ultrasound-guided trans perineal interstitial permanent prostate brachytherapy (TIPPB) is generally performed with either 103 Pd or 125 I. The use of 125 I for low Gleason score tumors and 103 Pd for higher Gleason scores has been suggested based on isotope dose rate and cell doubling time observed in in vitro studies. While many centers follow these isotope selection criteria, other centers have elected to use only a single isotope, regardless of Gleason score. No clinical data have been published comparing these isotopes. This study was undertaken to compare outcomes between 125 I and 103 Pd in a matched pair analysis for patients undergoing prostate brachytherapy. Methods and Materials: Six hundred forty-eight consecutively treated patients with clinically confined prostate cancer underwent TIPPB between June 1992 and February 1997. Five hundred thirty-two patients underwent TIPPB alone, whereas 116 received pelvic external beam irradiation and TIPPB. Ninety-three patients received androgen deprivation therapy prior to TIPPB. The prescribed doses for TIPPB were 160 Gy for 125 I (pre-TG43) and 120 Gy for 103 Pd. Patients treated with combination therapy received 41.4 or 45 Gy (1.8 Gy/fraction) external beam irradiation followed by a 3- to 5-week break and then received either a 120-Gy 125 I or a 90-Gy 103 Pd implant. Until November 1994, all patients underwent an 125 I implant after which the isotope selection was based on either Gleason score (Gleason score 2-5: 125 I; Gleason 5-8: 103 Pd) or isotope availability. A matched pair analysis was performed to assess any difference between isotopes. Two hundred twenty-two patients were matched according to Gleason score, prostate-specific antigen (PSA), and stage. PSA relapse-free survival (PSA-RFS) was calculated based on the American Society for Therapeutic Radiology and Oncology (ASTRO) Consensus Group definition of failure. Kaplan-Meier actuarial survival curves were compared to assess differences in

Blood-specific isotopic discrimination factors in the Magellanic penguin (Spheniscus magellanicus).

Science.gov (United States)

Ciancio, Javier E; Righi, Carina; Faiella, Adrián; Frere, Esteban

2016-08-30

The use of stable isotopes for ecological studies has increased exponentially in recent years. Isotopic trophic studies are based on the assumption that animals are what they eat plus a discrimination factor. The discrimination factor is affected by many variables and can be determined empirically. The Magellanic penguin is a highly abundant marine bird that plays a key role in the southern oceans. This study provides the first estimation of the Magellanic penguin blood discrimination factor for (13) C and (15) N. A two and a half month feeding experiment was performed, in which ten captive penguins were fed their main natural prey (anchovy Engraulis anchoita). The discrimination factors were estimated by comparing anchovy δ(13) C and δ(15) N values (obtained with isotope ratio mass spectrometry using lipid-extracted and bulk anchovy muscle) with penguin blood δ(13) C and δ(15) N values. Penguin blood was shown to be enriched, compared with anchovies, for (13) C and (15) N. No changes were observed in the stable isotope ratios of anchovies and discrimination factors during the experiment. The overall discrimination factors were 0.93 ± 0.12 (bulk) and 0.41 ± 0.12 (lipid-free) for (13) C; and 2.81 ± 0.17 (bulk) and 2.31 ± 0.17 (lipid-free) for (15) N. Having an accurate discrimination factor for the studied species is key in any trophic or food web isotopic study. Comparisons of estimated diet-to-blood discrimination factors with published values of aquatic piscivore birds showed that the (13) C discrimination factor is particularly variable, and therefore ecologists should be cautious when using a surrogate value from other species. In this study, the Magellanic penguin discrimination factor of a tissue that does not require euthanasia was obtained, a fundamental input for trophic isotopic modeling of the species. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

ANALYSIS OF RICIN TOXIN PREPARATIONS FOR CARBOHYDRATE AND FATTY ACID ABUNDANCE AND ISOTOPE RATIO INFORMATION

Energy Technology Data Exchange (ETDEWEB)

Wunschel, David S.; Kreuzer-Martin, Helen W.; Antolick, Kathryn C.; Colburn, Heather A.; Moran, James J.; Melville, Angela M.

2009-12-01

This report describes method development and preliminary evaluation for analyzing castor samples for signatures of purifying ricin. Ricin purification from the source castor seeds is essentially a problem of protein purification using common biochemical methods. Indications of protein purification will likely manifest themselves as removal of the non-protein fractions of the seed. Two major, non-protein, types of biochemical constituents in the seed are the castor oil and various carbohydrates. The oil comprises roughly half the seed weight while the carbohydrate component comprises roughly half of the remaining “mash” left after oil and hull removal. Different castor oil and carbohydrate components can serve as indicators of specific toxin processing steps. Ricinoleic acid is a relatively unique fatty acid in nature and is the most abundant component of castor oil. The loss of ricinoleic acid indicates a step to remove oil from the seeds. The relative amounts of carbohydrates and carbohydrate-like compounds, including arabinose, xylose, myo-inositol fucose, rhamnose, glucosamine and mannose detected in the sample can also indicate specific processing steps. For instance, the differential loss of arabinose relative to mannose and N-acetyl glucosamine indicates enrichment for the protein fraction of the seed using protein precipitation. The methods developed in this project center on fatty acid and carbohydrate extraction from castor samples followed by derivatization to permit analysis by gas chromatography-mass spectrometry (GC-MS). Method descriptions herein include: the source and preparation of castor materials used for method evaluation, the equipment and description of procedure required for chemical derivatization, and the instrument parameters used in the analysis. Two types of derivatization methods describe analysis of carbohydrates and one procedure for analysis of fatty acids. Two types of GC-MS analysis is included in the method development, one

A Compound-Specific Hydrogen Isotope Record at the Onset of Ocean Anoxic Event 2, Kaiparowits Plateau, Southern Utah

Science.gov (United States)

Todes, J.; Jones, M. M.; Sageman, B. B.; Osburn, M. R.

2017-12-01

Rhythmic lithologic variations (limestone-shale couplets) interpreted to reflect Milankovitch cycles occur at the onset of Ocean Anoxic Event 2 (OAE2) in deposits of the Western Interior Seaway. These couplets have been interpreted to reflect climate cycles: however, the physical mechanism(s) through which climate cycles were translated to the sedimentary record during peak greenhouse conditions remain unsettled. Although glacioeustasy has been considered, variance in surface ocean temperature, ocean circulation, or local hydrology may be more plausible options. Compound-specific hydrogen isotope ratios (δ2H) of n-alkanes and other biomarkers may provide a means to evaluate such mechanisms. Since sedimentary alkanes are direct products of plants and membrane lipid diagenesis and are resistant to secondary hydrogen exchange during thermal maturation at low (chain length distributions suggest low thermal maturity and the possible preservation of primary δ2H values. Short and long chain ­n-alkanes are potentially sourced from planktonic biomass and terrestrial plants, respectively, enabling a comparison of climatic processes between marine and terrestrial settings. Biomarkers, including both steranes and hopanes, are also preserved and reflect putative source organisms and local paleoenvironmental conditions. Facies-specific δ2H analysis will allow for evaluation of changes in the dominant source of atmospheric moisture in the Western Interior during orbitally-forced climate cycles. Organic matter deposited during periods of northerly Boreal influence would have a depleted 2H-isotope composition relative to those deposited during periods of more southerly Tethys influence. In this model, these variations are reflected by lithology - limestone deposition would occur during warm, evaporative Tethys-dominated times, while cooler, wetter Boreal periods would promote shale deposition.

Validation of multi-element isotope dilution ICPMS for the analysis of basalts

Energy Technology Data Exchange (ETDEWEB)

Willbold, M.; Jochum, K.P.; Raczek, I.; Amini, M.A.; Stoll, B.; Hofmann, A.W. [Max-Planck-Institut fuer Chemie, Mainz (Germany)

2003-09-01

In this study we have validated a newly developed multi-element isotope dilution (ID) ICPMS method for the simultaneous analysis of up to 12 trace elements in geological samples. By evaluating the analytical uncertainty of individual components using certified reference materials we have quantified the overall analytical uncertainty of the multi-element ID ICPMS method at 1-2%. Individual components include sampling/weighing, purity of reagents, purity of spike solutions, calibration of spikes, determination of isotopic ratios, instrumental sources of error, correction of mass discrimination effect, values of constants, and operator bias. We have used the ID-determined trace elements for internal standardization to improve indirectly the analysis of 14 other (mainly mono-isotopic trace elements) by external calibration. The overall analytical uncertainty for those data is about 2-3%. In addition, we have analyzed USGS and MPI-DING geological reference materials (BHVO-1, BHVO-2, KL2-G, ML3B-G) to quantify the overall bias of the measurement procedure. Trace element analysis of geological reference materials yielded results that agree mostly within about 2-3% relative to the reference values. Since these results match the conclusions obtained by the investigation of the overall analytical uncertainty, we take this as a measure for the validity of multi-element ID ICPMS. (orig.)

BENCHMARKING ORTEC ISOTOPIC MEASUREMENTS AND CALCULATIONS

Energy Technology Data Exchange (ETDEWEB)

Dewberry, R; Raymond Sigg, R; Vito Casella, V; Nitin Bhatt, N

2008-09-29

This report represents a description of compiled benchmark tests conducted to probe and to demonstrate the extensive utility of the Ortec ISOTOPIC {gamma}-ray analysis computer program. The ISOTOPIC program performs analyses of {gamma}-ray spectra applied to specific acquisition configurations in order to apply finite-geometry correction factors and sample-matrix-container photon absorption correction factors. The analysis program provides an extensive set of preset acquisition configurations to which the user can add relevant parameters in order to build the geometry and absorption correction factors that the program determines from calculus and from nuclear g-ray absorption and scatter data. The Analytical Development Section field nuclear measurement group of the Savannah River National Laboratory uses the Ortec ISOTOPIC analysis program extensively for analyses of solid waste and process holdup applied to passive {gamma}-ray acquisitions. Frequently the results of these {gamma}-ray acquisitions and analyses are to determine compliance with facility criticality safety guidelines. Another use of results is to designate 55-gallon drum solid waste as qualified TRU waste3 or as low-level waste. Other examples of the application of the ISOTOPIC analysis technique to passive {gamma}-ray acquisitions include analyses of standard waste box items and unique solid waste configurations. In many passive {gamma}-ray acquisition circumstances the container and sample have sufficient density that the calculated energy-dependent transmission correction factors have intrinsic uncertainties in the range 15%-100%. This is frequently the case when assaying 55-gallon drums of solid waste with masses of up to 400 kg and when assaying solid waste in extensive unique containers. Often an accurate assay of the transuranic content of these containers is not required, but rather a good defensible designation as >100 nCi/g (TRU waste) or <100 nCi/g (low level solid waste) is required. In

Extermination Of Uranium Isotopes Composition Using A Micro Computer With An IEEE-488 Interface For Mass Spectrometer Analysis

International Nuclear Information System (INIS)

Prajitno; Taftazani, Agus; Yusuf

1996-01-01

A mass spectrometry method can be used to make qualitative or quantitative analysis. For qualitative analysis, identification of unknown materials by a Mass Spectrometer requires definite assignment of mass number to peak on chart. In quantitative analysis, a mass spectrometer is used to determine isotope composition material in the sample. Analysis system of a Mass Spectrometer possession of PPNY-BATAN based on comparison ion current intensity which enter the collector, and have been used to analyse isotope composition. Calculation of isotope composition have been manually done. To increase the performance and to avoid manual data processing, a micro computer and IEEE-488 interface have been installed, also software packaged has been made. So that the determination of the isotope composition of material in the sample will be faster and more efficient. Tile accuracy of analysis using this program on sample standard U 3 O 8 NBS 010 is between 93,87% - 99,98%

New online method for water isotope analysis of speleothem fluid inclusions using laser absorption spectroscopy (WS-CRDS)

Science.gov (United States)

Affolter, S.; Fleitmann, D.; Leuenberger, M.

2014-07-01

A new online method to analyse water isotopes of speleothem fluid inclusions using a wavelength scanned cavity ring down spectroscopy (WS-CRDS) instrument is presented. This novel technique allows us simultaneously to measure hydrogen and oxygen isotopes for a released aliquot of water. To do so, we designed a new simple line that allows the online water extraction and isotope analysis of speleothem samples. The specificity of the method lies in the fact that fluid inclusions release is made on a standard water background, which mainly improves the δ D robustness. To saturate the line, a peristaltic pump continuously injects standard water into the line that is permanently heated to 140 °C and flushed with dry nitrogen gas. This permits instantaneous and complete vaporisation of the standard water, resulting in an artificial water background with well-known δ D and δ18O values. The speleothem sample is placed in a copper tube, attached to the line, and after system stabilisation it is crushed using a simple hydraulic device to liberate speleothem fluid inclusions water. The released water is carried by the nitrogen/standard water gas stream directly to a Picarro L1102-i for isotope determination. To test the accuracy and reproducibility of the line and to measure standard water during speleothem measurements, a syringe injection unit was added to the line. Peak evaluation is done similarly as in gas chromatography to obtain &delta D; and δ18O isotopic compositions of measured water aliquots. Precision is better than 1.5 ‰ for δ D and 0.4 ‰ for δ18O for water measurements for an extended range (-210 to 0 ‰ for δ D and -27 to 0 ‰ for δ18O) primarily dependent on the amount of water released from speleothem fluid inclusions and secondarily on the isotopic composition of the sample. The results show that WS-CRDS technology is suitable for speleothem fluid inclusion measurements and gives results that are comparable to the isotope ratio mass

The Importance of Zostera marina to a Local Food Web Based on the Analysis of Compound Specific Isotopes in Maquoit Bay, Gulf of Maine

Science.gov (United States)

Doolittle, H. A.; Johnson, B. J.; Ambrose, W. G.; Locke, W.; Harris, C. M.

2010-12-01

Zostera marina (also known as eelgrass) is an important primary producer in near shore ecosystems in the Gulf of Maine, providing both habitat and nutrients for a variety of organisms (e.g., crustaceans, polychaetes, gastropods, and fish). The purpose of this study is to use compound specific δ13C analyses of essential amino acids to determine the degree to which organic matter derived from isotopically distinct primary producers (e.g., eelgrass, phytoplankton, and epiphytic algae) contribute to the diets of snails, shrimp, and fish in an eelgrass system in Casco Bay. Maquoit Bay, located in northwestern Casco Bay, in the Gulf of Maine, is a shallow estuarine system that is characterized by silt and clay sized sediments and the presence of extensive eelgrass beds. Amino acid concentrations and δ13C compositions were determined for a variety of sample-types collected in July-August, 2010, from three sites in the study area, including muscle tissue from Tautogolabrus adspersus (cunner), Gasterosteus aculeatus (3-spined stickleback), Nassarius obsoletus (snail), and Mysis spp. (shrimp), seston (i.e., phytoplankton), Z. marina, and epiphytic algae. TFAA amino acid derivatives of the total hydrolyzate were analyzed by GC-FID for amino acid concentration, and by GC-c-IRMS- for carbon isotope composition. Muscle tissue was dominated by glutamic and aspartic acids, and leucine, whereas Zostera marina was dominated by aspartic and glutamic acids, and proline. Phenylalanine and leucine in Z. marina are approximately 10 ‰ enriched in 13C relative to these same amino acids in the seston. The carbon isotope values of these essential amino acids are significantly more enriched in 13C for N. obsoletus than for T. adspersus, G. aculeatus, and Mysis spp. These data suggest that organic matter derived from Z. marina and/or epiphytic algae is more important in the diets of N. obsoletus, and organic matter derived from seston is more important for the diets of T. adspersus, G

Bulk - Samples gamma-rays activation analysis (PGNAA) with Isotopic Neutron Sources

International Nuclear Information System (INIS)

HASSAN, A.M.

2009-01-01

An overview is given on research towards the Prompt Gamma-ray Neutron Activation Analysis (PGNAA) of bulk-samples. Some aspects in bulk-sample PGNAA are discussed, where irradiation by isotopic neutron sources is used mostly for in-situ or on-line analysis. The research was carried out in a comparative and/or qualitative way or by using a prior knowledge about the sample material. Sometimes we need to use the assumption that the mass fractions of all determined elements add up to 1. The sensitivity curves are also used for some elements in such complex samples, just to estimate the exact percentage concentration values. The uses of 252 Cf, 241 Arn/Be and 239 Pu/Be isotopic neutron sources for elemental investigation of: hematite, ilmenite, coal, petroleum, edible oils, phosphates and pollutant lake water samples have been mentioned.

Feasibility study of plutonium isotopic analysis of resin beads by nondestructive gamma-ray spectroscopy

International Nuclear Information System (INIS)

Li, T.K.

1985-01-01

We have initiated a feasibility study on the use of nondestructive low-energy gamma-ray spectroscopy for plutonium isotopic analysis on resin beads. Seven resin bead samples were measured, with each sample containing an average of 9 μg of plutonium; the isotopic compositions of the samples varied over a wide range. The gamma-ray spectroscopy results, obtained from 4-h counting-time measurements, were compared with mass spectrometry results. The average ratios of gamma-ray spectroscopy to mass spectrometry were 1.014 +- 0.025 for 238 Pu/ 239 Pu, 0.996 +- 0.018 for 240 Pu/ 239 Pu, and 0.980 +- 0.038 for 241 Pu/ 239 Pu. The rapid, automated, and accurate nondestructive isotopic analysis of resin beads may be very useful to process technicians and International Atomic Energy Agency inspectors. 3 refs., 1 fig., 3 tabs

On the interference of Kr during carbon isotope analysis of methane using continuous-flow combustion–isotope ratio mass spectrometry

Directory of Open Access Journals (Sweden)

J. Schmitt

2013-05-01

Full Text Available Stable carbon isotope analysis of methane (δ13C of CH4 on atmospheric samples is one key method to constrain the current and past atmospheric CH4 budget. A frequently applied measurement technique is gas chromatography (GC isotope ratio mass spectrometry (IRMS coupled to a combustion-preconcentration unit. This report shows that the atmospheric trace gas krypton (Kr can severely interfere during the mass spectrometric measurement, leading to significant biases in δ13C of CH4, if krypton is not sufficiently separated during the analysis. According to our experiments, the krypton interference is likely composed of two individual effects, with the lateral tailing of the doubly charged 86Kr peak affecting the neighbouring m/z 44 and partially the m/z 45 Faraday cups. Additionally, a broad signal affecting m/z 45 and especially m/z 46 is assumed to result from scattered ions of singly charged krypton. The introduced bias in the measured isotope ratios is dependent on the chromatographic separation, the krypton-to-CH4 mixing ratio in the sample, the focusing of the mass spectrometer as well as the detector configuration and can amount to up to several per mil in δ13C. Apart from technical solutions to avoid this interference, we present correction routines to a posteriori remove the bias.

Analytical developments in thermal ionization mass spectrometry for the isotopic analysis of very small amounts

International Nuclear Information System (INIS)

Mialle, S.

2011-01-01

In the framework of the French transmutation project of nuclear wastes, experiments consisted in the irradiation in a fast neutron reactor of few milligrams of isotopically enriched powders. Hence, the isotopic analysis of very small amount of irradiation products is one of the main issues. The aim of this study was to achieve analytical developments in thermal ionization mass spectrometry in order to accurately analyze these samples. Several axes were studied including the new total evaporation method, deposition techniques, electron multiplier potentialities and comparison between different isotope measurement techniques. Results showed that it was possible to drastically decrease the amounts needed for analysis, especially with Eu and Nd, while maintaining an uncertainty level in agreement with the project requirements. (author) [fr

Assessing the functional diversity of herbivorous reef fishes using a compound-specific stable isotope approach

KAUST Repository

Tietbohl, Matthew

2016-12-01

Herbivorous coral reef fishes play an important role in helping to structure their environment directly by consuming algae and indirectly by promoting coral health and growth. These fishes are generally separated into three broad groups: browsers, grazers, and excavators/scrapers, with these groupings often thought to have a fixed general function and all fishes within a group thought to have similar ecological roles. This categorization assumes a high level of functional redundancy within herbivorous fishes. However, recent evidence questions the use of this broad classification scheme, and posits that there may actually be more resource partitioning within these functional groupings. Here, I use a compound-specific stable isotope approach (CSIA) to show there appears to be a greater diversity of functional roles than previously assumed within broad functional groups. The δ13C signatures from essential amino acids of reef end-members (coral, macroalgae, detritus, and phytoplankton) and fish muscle were analyzed to investigate differences in resource use between fishes. Most end-members displayed clear isotopic differences, and most fishes within functional groups were dissimilar in their isotopic signature, implying differences in the resources they target. No grazers closely resembled each other isotopically, implying a much lower level of functional redundancy within this group; scraping parrotfish were also distinct from excavating parrotfish and to a lesser degree distinct between scrapers. This study highlights the potential of CSIA to help distinguish fine-scale ecological differences within other groups of reef organisms as well. These results question the utility of lumping nominally herbivorous fishes into broad groups with assumed similar roles. Given the apparent functional differences between nominally herbivorous reef fishes, it is important for managers to incorporate the diversity of functional roles these fish play.

Assessing the functional diversity of herbivorous reef fishes using a compound-specific stable isotope approach

KAUST Repository

Tietbohl, Matthew

2016-01-01

Herbivorous coral reef fishes play an important role in helping to structure their environment directly by consuming algae and indirectly by promoting coral health and growth. These fishes are generally separated into three broad groups: browsers, grazers, and excavators/scrapers, with these groupings often thought to have a fixed general function and all fishes within a group thought to have similar ecological roles. This categorization assumes a high level of functional redundancy within herbivorous fishes. However, recent evidence questions the use of this broad classification scheme, and posits that there may actually be more resource partitioning within these functional groupings. Here, I use a compound-specific stable isotope approach (CSIA) to show there appears to be a greater diversity of functional roles than previously assumed within broad functional groups. The δ13C signatures from essential amino acids of reef end-members (coral, macroalgae, detritus, and phytoplankton) and fish muscle were analyzed to investigate differences in resource use between fishes. Most end-members displayed clear isotopic differences, and most fishes within functional groups were dissimilar in their isotopic signature, implying differences in the resources they target. No grazers closely resembled each other isotopically, implying a much lower level of functional redundancy within this group; scraping parrotfish were also distinct from excavating parrotfish and to a lesser degree distinct between scrapers. This study highlights the potential of CSIA to help distinguish fine-scale ecological differences within other groups of reef organisms as well. These results question the utility of lumping nominally herbivorous fishes into broad groups with assumed similar roles. Given the apparent functional differences between nominally herbivorous reef fishes, it is important for managers to incorporate the diversity of functional roles these fish play.

Direct uranium isotope ratio analysis of single micrometer-sized glass particles.

Science.gov (United States)

Kappel, Stefanie; Boulyga, Sergei F; Prohaska, Thomas

2012-11-01

We present the application of nanosecond laser ablation (LA) coupled to a 'Nu Plasma HR' multi collector inductively coupled plasma mass spectrometer (MC-ICP-MS) for the direct analysis of U isotope ratios in single, 10-20 μm-sized, U-doped glass particles. Method development included studies with respect to (1) external correction of the measured U isotope ratios in glass particles, (2) the applied laser ablation carrier gas (i.e. Ar versus He) and (3) the accurate determination of lower abundant (236)U/(238)U isotope ratios (i.e. 10(-5)). In addition, a data processing procedure was developed for evaluation of transient signals, which is of potential use for routine application of the developed method. We demonstrate that the developed method is reliable and well suited for determining U isotope ratios of individual particles. Analyses of twenty-eight S1 glass particles, measured under optimized conditions, yielded average biases of less than 0.6% from the certified values for (234)U/(238)U and (235)U/(238)U ratios. Experimental results obtained for (236)U/(238)U isotope ratios deviated by less than -2.5% from the certified values. Expanded relative total combined standard uncertainties U(c) (k = 2) of 2.6%, 1.4% and 5.8% were calculated for (234)U/(238)U, (235)U/(238)U and (236)U/(238)U, respectively. Copyright © 2012 Elsevier Ltd. All rights reserved.

Spatially resolved δ13C analysis using laser ablation isotope ratio mass spectrometry

Science.gov (United States)

Moran, J.; Riha, K. M.; Nims, M. K.; Linley, T. J.; Hess, N. J.; Nico, P. S.

2014-12-01

Inherent geochemical, organic matter, and microbial heterogeneity over small spatial scales can complicate studies of carbon dynamics through soils. Stable isotope analysis has a strong history of helping track substrate turnover, delineate rhizosphere activity zones, and identifying transitions in vegetation cover, but most traditional isotope approaches are limited in spatial resolution by a combination of physical separation techniques (manual dissection) and IRMS instrument sensitivity. We coupled laser ablation sampling with isotope measurement via IRMS to enable spatially resolved analysis over solid surfaces. Once a targeted sample region is ablated the resulting particulates are entrained in a helium carrier gas and passed through a combustion reactor where carbon is converted to CO2. Cyrotrapping of the resulting CO2 enables a reduction in carrier gas flow which improves overall measurement sensitivity versus traditional, high flow sample introduction. Currently we are performing sample analysis at 50 μm resolution, require 65 ng C per analysis, and achieve measurement precision consistent with other continuous flow techniques. We will discuss applications of the laser ablation IRMS (LA-IRMS) system to microbial communities and fish ecology studies to demonstrate the merits of this technique and how similar analytical approaches can be transitioned to soil systems. Preliminary efforts at analyzing soil samples will be used to highlight strengths and limitations of the LA-IRMS approach, paying particular attention to sample preparation requirements, spatial resolution, sample analysis time, and the types of questions most conducive to analysis via LA-IRMS.

Isotope analysis reveals foraging area dichotomy for atlantic leatherback turtles.

Directory of Open Access Journals (Sweden)

Stéphane Caut

Full Text Available BACKGROUND: The leatherback turtle (Dermochelys coriacea has undergone a dramatic decline over the last 25 years, and this is believed to be primarily the result of mortality associated with fisheries bycatch followed by egg and nesting female harvest. Atlantic leatherback turtles undertake long migrations across ocean basins from subtropical and tropical nesting beaches to productive frontal areas. Migration between two nesting seasons can last 2 or 3 years, a time period termed the remigration interval (RI. Recent satellite transmitter data revealed that Atlantic leatherbacks follow two major dispersion patterns after nesting season, through the North Gulf Stream area or more eastward across the North Equatorial Current. However, information on the whole RI is lacking, precluding the accurate identification of feeding areas where conservation measures may need to be applied. METHODOLOGY/PRINCIPAL FINDINGS: Using stable isotopes as dietary tracers we determined the characteristics of feeding grounds of leatherback females nesting in French Guiana. During migration, 3-year RI females differed from 2-year RI females in their isotope values, implying differences in their choice of feeding habitats (offshore vs. more coastal and foraging latitude (North Atlantic vs. West African coasts, respectively. Egg-yolk and blood isotope values are correlated in nesting females, indicating that egg analysis is a useful tool for assessing isotope values in these turtles, including adults when not available. CONCLUSIONS/SIGNIFICANCE: Our results complement previous data on turtle movements during the first year following the nesting season, integrating the diet consumed during the year before nesting. We suggest that the French Guiana leatherback population segregates into two distinct isotopic groupings, and highlight the urgent need to determine the feeding habitats of the turtle in the Atlantic in order to protect this species from incidental take by

Pressurizer pump reliability analysis high flux isotope reactor

International Nuclear Information System (INIS)

Merryman, L.; Christie, B.

1993-01-01

During a prolonged outage from November 1986 to May 1990, numerous changes were made at the High Flux Isotope Reactor (HFIR). Some of these changes involved the pressurizer pumps. An analysis was performed to calculate the impact of these changes on the pressurizer system availability. The analysis showed that the availability of the pressurizer system dropped from essentially 100% to approximately 96%. The primary reason for the decrease in availability comes because off-site power grid disturbances sometimes result in a reactor trip with the present pressurizer pump configuration. Changes are being made to the present pressurizer pump configuration to regain some of the lost availability

Site-specific 13C content by quantitative isotopic 13C Nuclear Magnetic Resonance spectrometry: A pilot inter-laboratory study

International Nuclear Information System (INIS)

Chaintreau, Alain; Fieber, Wolfgang; Sommer, Horst; Gilbert, Alexis; Yamada, Keita; Yoshida, Naohiro; Pagelot, Alain; Moskau, Detlef; Moreno, Aitor; Schleucher, Jürgen; Reniero, Fabiano; Holland, Margaret; Guillou, Claude; Silvestre, Virginie; Akoka, Serge; Remaud, Gérald S.

2013-01-01

Graphical abstract: -- Highlights: •First ring test on isotopic 13 C NMR spectrometry. •Evaluation of the intra- and inter-variability of the NMR spectrometers used. •Definition of a protocol for qualification of the performance of the spectrometer. -- Abstract: Isotopic 13 C NMR spectrometry, which is able to measure intra-molecular 13 C composition, is of emerging demand because of the new information provided by the 13 C site-specific content of a given molecule. A systematic evaluation of instrumental behaviour is of importance to envisage isotopic 13 C NMR as a routine tool. This paper describes the first collaborative study of intra-molecular 13 C composition by NMR. The main goals of the ring test were to establish intra- and inter-variability of the spectrometer response. Eight instruments with different configuration were retained for the exercise on the basis of a qualification test. Reproducibility at the natural abundance of isotopic 13 C NMR was then assessed on vanillin from three different origins associated with specific δ 13 C i profiles. The standard deviation was, on average, between 0.9 and 1.2‰ for intra-variability. The highest standard deviation for inter-variability was 2.1‰. This is significantly higher than the internal precision but could be considered good in respect of a first ring test on a new analytical method. The standard deviation of δ 13 C i in vanillin was not homogeneous over the eight carbons, with no trend either for the carbon position or for the configuration of the spectrometer. However, since the repeatability for each instrument was satisfactory, correction factors for each carbon in vanillin could be calculated to harmonize the results

Linking cases of illegal shootings of the endangered California condor using stable lead isotope analysis

Energy Technology Data Exchange (ETDEWEB)

Finkelstein, Myra E., E-mail: myraf@ucsc.edu [Microbiology and Environmental Toxicology Department, University of California, Santa Cruz, CA 95064 (United States); Kuspa, Zeka E. [Microbiology and Environmental Toxicology Department, University of California, Santa Cruz, CA 95064 (United States); Welch, Alacia [National Park Service, Pinnacles National Park, 5000 Highway 146, Paicines, CA 95043 (United States); Eng, Curtis; Clark, Michael [Los Angeles Zoo and Botanical Gardens, 5333 Zoo Drive, Los Angeles, CA 90027 (United States); Burnett, Joseph [Ventana Wildlife Society, 19045 Portola Dr. Ste. F-1, Salinas, CA 93908 (United States); Smith, Donald R. [Microbiology and Environmental Toxicology Department, University of California, Santa Cruz, CA 95064 (United States)

2014-10-15

Lead poisoning is preventing the recovery of the critically endangered California condor (Gymnogyps californianus) and lead isotope analyses have demonstrated that ingestion of spent lead ammunition is the principal source of lead poisoning in condors. Over an 8 month period in 2009, three lead-poisoned condors were independently presented with birdshot embedded in their tissues, evidencing they had been shot. No information connecting these illegal shooting events existed and the timing of the shooting(s) was unknown. Using lead concentration and stable lead isotope analyses of feathers, blood, and recovered birdshot, we observed that: i) lead isotope ratios of embedded shot from all three birds were measurably indistinguishable from each other, suggesting a common source; ii) lead exposure histories re-constructed from feather analysis suggested that the shooting(s) occurred within the same timeframe; and iii) two of the three condors were lead poisoned from a lead source isotopically indistinguishable from the embedded birdshot, implicating ingestion of this type of birdshot as the source of poisoning. One of the condors was subsequently lead poisoned the following year from ingestion of a lead buckshot (blood lead 556 µg/dL), illustrating that ingested shot possess a substantially greater lead poisoning risk compared to embedded shot retained in tissue (blood lead ∼20 µg/dL). To our knowledge, this is the first study to use lead isotopes as a tool to retrospectively link wildlife shooting events. - Highlights: • We conducted a case-based analysis of illegal shootings of California condors. • Blood and feather Pb isotopes were used to reconstruct the illegal shooting events. • Embedded birdshot from the three condors had the same Pb isotope ratios. • Feather and blood Pb isotopes indicated that the condors were shot in a common event. • Ingested shot causes substantially greater lead exposure compared to embedded shot.

Isotopic provenance analysis and terrane tectonics: a warning about sediment transport distances

International Nuclear Information System (INIS)

Bassett, K.N.

1999-01-01

temporary storage. Sediment from the Amazon River can be found in the Barbados trench. transported ∼2000 km northward by near shore currents after more than 2500 km by the Amazon River from source. It's interesting to note that while large fluvial systems are helpful for transporting sediment very large distances, it is also possible by other mechanisms. Both the Bengal fan and the Barbados sediment have been transported at least 1500 km by purely marine sediment transport mechanisms. Similar transport distances occur in the Hikurangi submarine channel off the eastern coast of New Zealand (Lewis, 1999). There fine sands are transported ∼2000 km northward into the Kermadec trench by sediment gravity flow and deep water currents. Such modern examples of long distance sediment transport should be kept in mind when interpreting details of terrane translation. The possibility that the fine grained fraction may have been transported 2000-3000 km from their source makes their provenance of very little use when attempting to resolve controversies where distances of tectonic translation are on the same order of magnitude (Insular and Torlesse Superterranes). Thus detailed histories of terrane translation are best developed using coarse rather than fine size tractions. Gravels are transported over 10s to 100s of kilometers rather than the 1000s of kilometers possible for fine grained sediments. In addition, more detailed isotopic and geochemical provenance analysis is possible due to the larger grain size available allowing more specific characterization of the source area. However, truly effective characterization of sediment source rocks can only be accomplished as part of multidisciplinary research projects that would include provenance analysis by a variety of methods combined with basin analysis to understand facies relations and sediment dispersal paths. Copyright (1999) Geological Society of Australia

Dissipation kinetics of asparagine in soil measured by compound-specific analysis with metabolite tracking

DEFF Research Database (Denmark)

Czaban, Weronika; Rasmussen, Jim; Nicolaisen, Mogens

2016-01-01

labeled glutamic acid were detected in soil. This highlights the fast turnover of amino acid in soil and that the estimation of concentration of the formed compounds is important when evaluating plant available organic N. Efficiency of the compound-specific analysis showed to be a powerful technique......Estimating the potential for direct plant acquisition of organic N, in particular amino acids, requires assessment of their turnover times in soil. It is well known from 14C studies that mineralization of amino acids occurs within hours, but mineralization to 14CO2 does not indicate the rate...... of disappearance of the intact amino acid or the possible formation of metabolites during amino acid dissipation. We here used compound-specific isotope analysis with metabolite tracking to investigate the dissipation rate of universally labeled intact 13C15N-asparagine at two concentrations and the subsequent...

Synergistic effect of the simultaneous chemometric analysis of {sup 1}H NMR spectroscopic and stable isotope (SNIF-NMR, {sup 18}O, {sup 13}C) data: Application to wine analysis

Energy Technology Data Exchange (ETDEWEB)

Monakhova, Yulia B., E-mail: yul-monakhova@mail.ru [Chemisches und Veterinäruntersuchungsamt (CVUA) Karlsruhe, Weissenburger Strasse 3, Karlsruhe 76187 (Germany); Bruker Biospin GmbH, Silberstreifen, Rheinstetten 76287 (Germany); Department of Chemistry, Saratov State University, Astrakhanskaya Street 83, Saratov 410012 (Russian Federation); Godelmann, Rolf [Chemisches und Veterinäruntersuchungsamt (CVUA) Karlsruhe, Weissenburger Strasse 3, Karlsruhe 76187 (Germany); Hermann, Armin [Landesuntersuchungsamt -Institut für Lebensmittelchemie und Arzneimittelprüfung, Emy-Roeder-Straße 1, Mainz 55129 (Germany); Kuballa, Thomas [Chemisches und Veterinäruntersuchungsamt (CVUA) Karlsruhe, Weissenburger Strasse 3, Karlsruhe 76187 (Germany); Cannet, Claire; Schäfer, Hartmut; Spraul, Manfred [Bruker Biospin GmbH, Silberstreifen, Rheinstetten 76287 (Germany); Rutledge, Douglas N. [AgroParisTech, UMR 1145, Ingénierie Procédés Aliments, 16 rue Claude Bernard, Paris F-75005 (France)

2014-06-23

Highlights: • {sup 1}H NMR profilings of 718 wines were fused with stable isotope analysis data (SNIF-NMR, {sup 18}O, {sup 13}C). • The best improvement was obtained for prediction of the geographical origin of wine. • Certain enhancement was also obtained for the year of vintage (from 88 to 97% for {sup 1}H NMR to 99% for the fused data). • Independent component analysis was used as an alternative chemometric tool for classification. - Abstract: It is known that {sup 1}H NMR spectroscopy represents a good tool for predicting the grape variety, the geographical origin, and the year of vintage of wine. In the present study we have shown that classification models can be improved when {sup 1}H NMR profiles are fused with stable isotope (SNIF-NMR, {sup 18}O, {sup 13}C) data. Variable selection based on clustering of latent variables was performed on {sup 1}H NMR data. Afterwards, the combined data of 718 wine samples from Germany were analyzed using linear discriminant analysis (LDA), partial least squares-discriminant analysis (PLS-DA), factorial discriminant analysis (FDA) and independent components analysis (ICA). Moreover, several specialized multiblock methods (common components and specific weights analysis (ComDim), consensus PCA and consensus PLS-DA) were applied to the data. The best improvement in comparison with {sup 1}H NMR data was obtained for prediction of the geographical origin (up to 100% for the fused data, whereas stable isotope data resulted only in 60–70% correct prediction and {sup 1}H NMR data alone in 82–89% respectively). Certain enhancement was obtained also for the year of vintage (from 88 to 97% for {sup 1}H NMR to 99% for the fused data), whereas in case of grape varieties improved models were not obtained. The combination of {sup 1}H NMR data with stable isotope data improves efficiency of classification models for geographical origin and vintage of wine and can be potentially used for other food products as well.

2H Stable Isotope Analysis of Tooth Enamel: A Pilot Study

Science.gov (United States)

Holobinko, Anastasia; Kemp, Helen; Meier-Augenstein, Wolfram; Prowse, Tracy; Ford, Susan

2010-05-01

Stable isotope analysis of biogenic tissues such as tooth enamel and bone mineral has become a well recognized and increasingly important method for determining provenance of human remains, and has been used successfully in bioarchaeological studies as well as forensic investigations (Lee-Thorp, 2008; Meier-Augenstein and Fraser, 2008). Particularly, 18O and 2H stable isotopes are well established proxies as environmental indicators of climate (temperature) and source water and are therefore considered as indicators of geographic life trajectories of animals and humans (Hobson et al., 2004; Schwarcz and Walker, 2006). While methodology for 2H analysis of human hair, fingernails, and bone collagen is currently used to determine geographic origin and identify possible migration patterns, studies involving the analysis of 2H in tooth enamel appear to be nonexistent in the scientific literature. The apparent lack of research in this area is believed to have two main reasons. (1) Compared to the mineral calcium hydroxylapatite Ca10(PO4)6(OH)2, in tooth enamel forming bio-apatite carbonate ions replace some of the hydroxyl ions at a rate of one CO32 replacing two OH, yet published figures for the degree of substitution vary (Wopenka and Pasteris, 2005). (2) Most probably due to the aforementioned no published protocols exist for sample preparation and analytical method to obtain δ2H-values from the hydroxyl fraction of tooth enamel. This dilemma has been addressed through a pilot study to establish feasibility of 2H stable isotope analysis of ground tooth enamel by continuous-flow isotope ratio mass spectrometry (IRMS) coupled on-line to a high-temperature conversion elemental analyzer (TC/EA). An array of archaeological and modern teeth has been analyzed under different experimental conditions, and results from this pilot study are being presented. References: Lee-Thorp, J.A. (2008) Archaeometry, 50, 925-950 Meier-Augenstein, W. and Fraser, I. (2008) Science & Justice

High-Throughput Method for Strontium Isotope Analysis by Multi-Collector-Inductively Coupled Plasma-Mass Spectrometer

Energy Technology Data Exchange (ETDEWEB)

Wall, Andrew J. [National Energy Technology Lab. (NETL), Pittsburgh, PA, (United States); Capo, Rosemary C. [Univ. of Pittsburgh, PA (United States); Stewart, Brian W. [Univ. of Pittsburgh, PA (United States); Phan, Thai T. [Univ. of Pittsburgh, PA (United States); Jain, Jinesh C. [National Energy Technology Lab. (NETL), Pittsburgh, PA, (United States); Hakala, Alexandra [National Energy Technology Lab. (NETL), Pittsburgh, PA, (United States); Guthrie, George D. [National Energy Technology Lab. (NETL), Pittsburgh, PA, (United States)

2016-09-22

This technical report presents the details of the Sr column configuration and the high-throughput Sr separation protocol. Data showing the performance of the method as well as the best practices for optimizing Sr isotope analysis by MC-ICP-MS is presented. Lastly, this report offers tools for data handling and data reduction of Sr isotope results from the Thermo Scientific Neptune software to assist in data quality assurance, which help avoid issues of data glut associated with high sample throughput rapid analysis.

High-Throughput Method for Strontium Isotope Analysis by Multi-Collector-Inductively Coupled Plasma-Mass Spectrometer

Energy Technology Data Exchange (ETDEWEB)

Hakala, Jacqueline Alexandra [National Energy Technology Lab. (NETL), Morgantown, WV (United States)

2016-11-22

This technical report presents the details of the Sr column configuration and the high-throughput Sr separation protocol. Data showing the performance of the method as well as the best practices for optimizing Sr isotope analysis by MC-ICP-MS is presented. Lastly, this report offers tools for data handling and data reduction of Sr isotope results from the Thermo Scientific Neptune software to assist in data quality assurance, which help avoid issues of data glut associated with high sample throughput rapid analysis.

Preliminary results of oxygen isotope ratio measurement with a particle-gamma coincidence method

Energy Technology Data Exchange (ETDEWEB)

Borysiuk, Maciek, E-mail: maciek.borysiuk@pixe.lth.se; Kristiansson, Per; Ros, Linus; Abdel, Nassem S.; Elfman, Mikael; Nilsson, Charlotta; Pallon, Jan

2015-04-01

The possibility to study variations in the oxygen isotopic ratio with photon tagged nuclear reaction analysis (pNRA) is evaluated in the current work. The experiment described in the article was performed at Lund Ion Beam Analysis Facility (LIBAF) with a 2 MeV deuteron beam. Isotopic fractionation of light elements such as carbon, oxygen and nitrogen is the basis of many analytical tools in hydrology, geology, paleobiology and paleogeology. IBA methods provide one possible tool for measurement of isotopic content. During this experimental run we focused on measurement of the oxygen isotopic ratio. The measurement of stable isotopes of oxygen has a number of applications; the particular one driving the current investigation belongs to the field of astrogeology and specifically evaluation of fossil extraterrestrial material. There are three stable isotopes of oxygen: {sup 16}O, {sup 17}O and {sup 18}O. We procured samples highly enriched with all three isotopes. Isotopes {sup 16}O and {sup 18}O were easily detected in the enriched samples, but no significant signal from {sup 17}O was detected in the same samples. The measured yield was too low to detect {sup 18}O in a sample with natural abundances of oxygen isotopes, at least in the current experimental setup, but the spectral line from the reaction with {sup 16}O was clearly visible.

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.

Contribution of bulk mass spectrometry isotopic analysis to characterization of materials in the framework of CMX-4

International Nuclear Information System (INIS)

Kuchkin, A.; Stebelkov, V.; Zhizhin, K.; Lierse von Gostomski, Ch.; Kardinal, Ch.; Loi, E.; Keegan, E.; Kristo, M.J.

2018-01-01

Seven laboratories used the results of bulk uranium isotopic analysis by either inductively coupled plasma mass spectrometry (ICP-MS) or thermal ionization mass spectrometry (TIMS) for characterization of the samples in the Nuclear Forensic International Technical Working Group fourth international collaborative material exercise, CMX-4. Comparison of the measured isotopic compositions of uranium in three exercise samples is implemented for identifying any differences or similarities between the samples. The role of isotopic analyses in the context of a real nuclear forensic investigation is discussed. Several limitations in carrying out ICP-MS or TIMS analysis in CMX-4 are noted. (author)

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.)

Isotopic methods in hydrogeology and their application to the Underground Research Laboratory, Manitoba

International Nuclear Information System (INIS)

Gascoyne, M.; Kotzer, T.

1995-09-01

This review examines isotopic methods used to determine groundwater sources, residence times and processes of geochemical evolution that have been published in the international literature, with specific reference to AECL's experience in these methods and applications to groundwaters at the Underground Research Laboratory (URL), Manitoba. The program of groundwater sampling and analysis currently being planned for the URL area over the next several years will concentrate on specific isotopic measurements that may assist in understanding the groundwater flow system at the URL site. These results will add to the existing data for the URL area and indicate which isotopes are most useful when applied to the known groundwater flow system of the URL. This program of study is especially important because it not only uses standard geochemical and isotopic measurements (e.g., major ion, trace elements, 2 H/ 18 O, 14 C, 34 S) of groundwaters, but will determine values of more exotic and unusual ratios, such as 6 Li/ 7 Li, and B 11 /B 10 , whose potential for understanding groundwater geochemical evolution is largely unknown at present. In addition, the more established but equally complex methods of isotopic analysis, to determine 3 He/ 4 He, 36 Cl/Cl and 129 I/I, will be used to assess their potential for adding to the hydrogeochemical understanding of flow paths in crystalline rock. (author). 182 refs., 11 tabs., 27 figs

An isotopic analysis process with optical emission spectrometry on a laser-produced plasma

International Nuclear Information System (INIS)

Mauchien, P.; Pietsch, W.; Petit, A.; Briand, A.

1994-01-01

The sample that is to be analyzed is irradiated with a laser beam to produce a plasma at the sample surface; the spectrum of the light emitted by the plasma is analyzed and the isotope composition of the sample is derived from the spectrometry. The process is preferentially applied to uranium and plutonium; it is rapid, simpler and cheaper than previous methods, and may be applied to 'in-situ' isotopic analysis in nuclear industry. 2 figs

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

Trace, isotopic analysis of micron-sized grains -- Mo, Zr analysis of stardust (SiC and graphite grains).

Energy Technology Data Exchange (ETDEWEB)

Pellin, M. J.; Nicolussi, G. K.

1998-02-19

Secondary Neutral Mass Spectrometry using resonant laser ionization can provide for both high useful yields and high discrimination while maintaining high lateral and depth resolutions. An example of the power of the method is measurement of the isotopic composition of Mo and Zr in 1-5 {micro}m presolar SiC and graphite grains isolated from the Murchison CM2 meteorite for the first time. These grains have survived the formation of the Solar System and isotopic analysis reveals a record of the stellar nucleosynthesis present during their formation. Mo and Zr, though present at less than 10 ppm in some grains, are particularly useful in that among their isotopes are members that can only be formed by distinct nucleosynthetic processes known as s-, p-, and r-process. Successful isotopic analysis of these elements requires both high selectivity (since these are trace elements) and high efficiency (since the total number of atoms available are limited). Resonant Ionization Spectroscopy is particularly useful and flexible in this application. While the sensitivity of this t.edmique has often been reported in the past, we focus hereon the very low noise properties of the technique. We further demonstrate the efficacy of noise removal by two complimentary methods. First we use the resonant nature of the signal to subtract background signal. Second we demonstrate that by choosing the appropriate resonance scheme background can often be dramatically reduced.

Growth patterns of an intertidal gastropod as revealed by oxygen isotope analysis

Science.gov (United States)

Bean, J. R.; Hill, T. M.; Guerra, C.

2007-12-01

The size and morphology of mollusk shells are affected by environmental conditions. As a result, it is difficult to assess growth rate, population age structure, shell morphologies associated with ontogenetic stages, and to compare life history patterns across various environments. Oxygen isotope analysis is a useful tool for estimating minimum ages and growth rates of calcium carbonate secreting organisms. Calcite shell material from members of two northern California populations of the intertidal muricid gastropod Acanthinucella spirata was sampled for isotopic analysis. Individual shells were sampled from apex to margin, thus providing a sequential record of juvenile and adult growth. A. spirata were collected from a sheltered habitat in Tomales Bay and from an exposed reef in Bolinas. Abiotic factors, such as temperature, wave exposure, and substrate consistency, and biotic composition differ significantly between these sites, possibly resulting in local adaptations and variation in life history and growth patterns. Shell morphology of A. spirata changes with age as internal shell margin thickenings of denticle rows associated with external growth bands are irregularly accreted. It is not known when, either seasonally and/or ontogentically, these thickenings and bands form or whether inter or intra-populational variation exists. Preliminary results demonstrate the seasonal oxygen isotopic variability present at the two coastal sites, indicating 5-6 degC changes from winter to summertime temperatures; these data are consistent with local intertidal temperature records. Analysis of the seasonal patterns indicate that: 1) differences in growth rate and seasonal growth patterns at different ontogenetic stages within populations, and 2) differences in growth patterns and possibly age structure between the two A. spirata populations. These findings indicate that isotopic analyses, in addition to field observations and morphological measurements, are necessary to

Calibration and Data Processing in Gas Chromatography Combustion Isotope Ratio Mass Spectrometry

Science.gov (United States)

Zhang, Ying; Tobias, Herbert J.; Sacks, Gavin L.; Brenna, J. Thomas

2013-01-01

Compound-specific isotope analysis (CSIA) by gas chromatography combustion isotope ratio mass spectrometry (GCC-IRMS) is a powerful technique for the sourcing of substances, such as determination of the geographic or chemical origin of drugs and food adulteration, and it is especially invaluable as a confirmatory tool for detection of the use of synthetic steroids in competitive sport. We review here principles and practices for data processing and calibration of GCC-IRMS data with consideration to anti-doping analyses, with a focus on carbon isotopic analysis (13C/12C). After a brief review of peak definition, the isotopologue signal reduction methods of summation, curve-fitting, and linear regression are described and reviewed. Principles for isotopic calibration are considered in the context of the Δ13C = δ13CM – δ13CE difference measurements required for establishing adverse analytical findings for metabolites relative to endogenous reference compounds. Considerations for the anti-doping analyst are reviewed. PMID:22362612

Isotopic abundance analysis of carbon, nitrogen and sulfur with a combined elemental analyzer-mass spectrometer system

International Nuclear Information System (INIS)

Pichlmayer, F.; Blochberger, K.

1988-01-01

Stable isotope ratio measurements of carbon, nitrogen and sulfur are of growing interest as analytical tool in many fields of research, but applications were somewhat hindered in the past by the fact that cumbersome sample preparation was necessary. A method has therefore been developed, consisting in essential of coupling an elemental analyzer with an isotope mass spectrometer, enabling fast and reliable conversion of C-, N- and S-compounds in any solid or liquid sample into the measuring gases carbon dioxide, nitrogen and sulfur dioxide for on-line isotopic analysis. The experimental set-up and the main characteristics are described in short and examples of application in environmental research, food analysis and clinical diagnosis are given. (orig.)

Tracing fetal and childhood exposure to lead using isotope analysis of deciduous teeth

International Nuclear Information System (INIS)

Shepherd, Thomas J.; Dirks, Wendy; Roberts, Nick M.W.; Patel, Jaiminkumar G.; Hodgson, Susan; Pless-Mulloli, Tanja; Walton, Pamela; Parrish, Randall R.

2016-01-01

We report progress in using the isotopic composition and concentration of Pb in the dentine and enamel of deciduous teeth to provide a high resolution time frame of exposure to Pb during fetal development and early childhood. Isotope measurements (total Pb and 208 Pb/ 206 Pb, 207 Pb/ 206 Pb ratios) were acquired by laser ablation inductively coupled mass spectrometry at contiguous 100 micron intervals across thin sections of the teeth; from the outer enamel surface to the pulp cavity. Teeth samples (n=10) were selected from two cohorts of children, aged 5–8 years, living in NE England. By integrating the isotope data with histological analysis of the teeth, using the daily incremental lines in dentine, we were able to assign true estimated ages to each ablation point (first 2–3 years for molars, first 1–2 years for incisors+pre-natal growth). Significant differences were observed in the isotope composition and concentration of Pb between children, reflecting differences in the timing and sources of exposure during early childhood. Those born in 2000, after the withdrawal of leaded petrol in 1999, have the lowest dentine Pb levels (<0.2 µg Pb/g) with 208 Pb/ 206 Pb (mean ±2σ: 2.126–2.079) 208 Pb/ 206 Pb (mean ±2σ: 0.879–0.856) ratios that correlate very closely with modern day Western European industrial aerosols (PM 10 , PM 2.5 ) suggesting that diffuse airborne pollution was probably the primary source and exposure pathway. Legacy lead, if present, is insignificant. For those born in 1997, dentine lead levels are typically higher (>0.4 µgPb/g) with 208 Pb/ 206 Pb (mean ±2σ: 2.145–2.117) 208 Pb/ 206 Pb (mean ±2σ: 0.898–0.882) ratios that can be modelled as a binary mix between industrial aerosols and leaded petrol emissions. Short duration, high intensity exposure events (1–2 months) were readily identified, together with evidence that dentine provides a good proxy for childhood changes in the isotope composition of blood Pb. Our pilot

New on-line method for water isotope analysis of speleothem fluid inclusions using laser absorption spectroscopy (WS-CRDS)

Science.gov (United States)

Affolter, S.; Fleitmann, D.; Leuenberger, M.

2014-01-01

A new online method to analyse water isotopes of speleothem fluid inclusions using a wavelength scanned cavity ring down spectroscopy (WS-CRDS) instrument is presented. This novel technique allows us to simultaneously measure hydrogen and oxygen isotopes for a released aliquot of water. To do so, we designed a new simple line that allows the on-line water extraction and isotope analysis of speleothem samples. The specificity of the method lies in the fact that fluid inclusions release is made on a standard water background, which mainly improves the δD reliability. To saturate the line, a peristaltic pump continuously injects standard water into the line that is permanently heated to 140 °C and flushed with dry nitrogen gas. This permits instantaneous and complete vaporisation of the standard water resulting in an artificial water background with well-known δD and δ18O values. The speleothem sample is placed into a copper tube, attached to the line and after system stabilisation is crushed using a simple hydraulic device to liberate speleothem fluid inclusions water. The released water is carried by the nitrogen/standard water gas stream directly to a Picarro L1102-i for isotope determination. To test the accuracy and reproducibility of the line and to measure standard water during speleothem measurements a syringe injection unit was added to the line. Peak evaluation is done similarly as in gas chromatography to obtain δD and δ18O isotopic composition of measured water aliquots. Precision is better than 1.5‰ for δD and 0.4‰ for δ18O for water measurement for an extended range (-210 to 0‰ for δD and -27 to 0‰ for δ18O) primarily dependent on the amount of water released from speleothem fluid inclusions and secondarily on the isotopic composition of the sample. The results show that WS-CRDS technology is suitable for speleothem fluid inclusion measurements and gives results that are comparable to Isotope Ratio Mass Spectrometry (IRMS) technique.

Can a sponge fractionate isotopes?

Science.gov (United States)

Patel, B; Patel, S; Balani, M C

1985-03-22

The study has unequivocally demonstrated that siliceous sponges Spirastrella cuspidifera and Prostylyssa foetida from the same microecological niche exhibit a high degree of species specificity, while accumulating a host of heavy metal ions (Ni, Cr, Cd, Sn, Ti, Mo, Zr). S. cuspidifera accumulated, in addition, 60Co and 63Ni, showing discrimination against other radionuclides, 137Cs and 131I, present in the ambient waters receiving controlled low level waste discharges from a B.W.R. nuclear power station. P. foetida, on the other hand, accumulated only 131I and showed discrimination against other radionuclides including 60Co, although the stable iodine concentrations in both the sponges were the same. The specific activity of 60Co (in becquerels per gram of 59Co) in S. cuspidifera and 131I (in becquerels per gram of 127I) in P. foetida were at least two orders of magnitude greater than in the ambient sea water. That of 63Ni (in becquerels per gram of 62Ni) in S. cuspidifera, on the other hand, was lower by two orders of magnitude than in either abiotic matrices from the same environment. Thus, not only did both the species show bioaccumulation of a specific element, but also preferential uptake of isotopes of the same element, though they were equally available for intake. Such differential uptake of isotopes can possibly be explained in terms of two quite different mechanisms operating, each applicable in a particular case. One is that the xenobiotic isotope enters the environment in a physicochemical form or as a complex different from that of its natural counterpart. If equilibration with the latter is slow, so that the organism acquires the xenobiotic in an unfamiliar chemical context, it may treat it as a chemically distinct entity so that its concentration factor differs from that of stable isotope, thus changing the specific activity. Alternatively, if the xenobiotic is present in the same chemical form as the stable isotope, the only way in which specific

Modeling position-specific isotope fractionation of organic micropollutants degradation via different reaction pathways

DEFF Research Database (Denmark)

Jin, Biao; Rolle, Massimo

: dichlorobenzamide (BAM), isoproturon (IPU) and diclofenac (DCF). The model successfully reproduces the multi-element isotope data, and precisely captures the dual element isotope trends, characterizing the different degradation pathways. Besides illustrating the model capability of mechanistic evaluation...

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

Reconstructing diet by stable isotope analysis: Two case studies from Bronze Age and Early Medieval Lower Austria

International Nuclear Information System (INIS)

Rumpelmayr, K.

2012-01-01

Carbon and nitrogen stable isotope analysis is nowadays a method frequently applied for the reconstruction of past human diets. The principles of this technique were developed in the late 1970s and 1980s, when it was shown that the isotopic composition of an animal's body reflected that of its diet. Given that the investigated material (often bone collagen) is well enough preserved, several aspects of diet can be investigated by carbon and nitrogen isotopic signatures - expressed as δ13C- und δ15N-values - as e.g. whether nutrition was based on C3 or C4 plants. Furthermore, these signatures can be used for the detection of a marine component in the diet and they contain information about the trophic level of an individual. The goal of the work presented in this talk was to investigate certain aspects of diet using carbon and nitrogen stable isotope analysis of human and animal skeletal remains from Austrian archaeological sites. Two sites (both in Lower Austria) were selected for this study, the Bronze Age Cemetery of Gemeinlebarn and the Early Medieval settlement of Thunau/Gars am Kamp. Previous archaeological and anthropological examinations suggested that both sites were inhabited by socially differentiated populations. Hence, during the stable isotope analysis special attention was paid to the detection of variation in nutritional habits due to sociogenic or gender-related differences. δ13C- und δ15N-values were measured in collagen, extracted from bone samples, by means of elemental analyzer-isotope ratio mass spectrometry (EA-IRMS). The obtained stable isotope data were examined for significant differences between social groups and the sexes using statistical hypothesis testing (MANOVA and ANOVA). (author)

Evaluation of Kilauea Eruptions By Using Stable Isotope Analysis

Science.gov (United States)

Rahimi, K. E.; Bursik, M. I.

2016-12-01

Kilauea, on the island of Hawaii, is a large volcanic edifice with numerous named vents scattered across its surface. Halema`uma`u crater sits with Kilauea caldera, above the magma reservoir, which is the main source of lava feeding most vents on Kilauea volcano. Halema`uma`u crater produces basaltic explosive activity ranging from weak emission to sub-Plinian. Changes in the eruption style are thought to be due to the interplay between external water and magma (phreatomagmatic/ phreatic), or to segregation of gas from magma (magmatic) at shallow depths. Since there are three different eruption mechanisms (phreatomagmatic, phreatic, and magmatic), each eruption has its own isotope ratios. The aim of this study is to evaluate the eruption mechanism by using stable isotope analysis. Studying isotope ratios of D/H and δ18O within fluid inclusion and volcanic glass will provide an evidence of what driven the eruption. The results would be determined the source of water that drove an eruption by correlating the values with water sources (groundwater, rainwater, and magmatic water) since each water source has a diagnostic value of D/H and δ18O. These results will provide the roles of volatiles in eruptions. The broader application of this research is that these methods could help volcanologists forecasting and predicting the current volcanic activity by mentoring change in volatiles concentration within deposits.

High Resolution Gamma Ray Analysis of Medical Isotopes

Science.gov (United States)

Chillery, Thomas

2015-10-01

Compton-suppressed high-purity Germanium detectors at the University of Massachusetts Lowell have been used to study medical radioisotopes produced at Brookhaven Linac Isotope Producer (BLIP), in particular isotopes such as Pt-191 used for cancer therapy in patients. The ability to precisely analyze the concentrations of such radio-isotopes is essential for both production facilities such as Brookhaven and consumer hospitals across the U.S. Without accurate knowledge of the quantities and strengths of these isotopes, it is possible for doctors to administer incorrect dosages to patients, thus leading to undesired results. Samples have been produced at Brookhaven and shipped to UML, and the advanced electronics and data acquisition capabilities at UML have been used to extract peak areas in the gamma decay spectra. Levels of Pt isotopes in diluted samples have been quantified, and reaction cross-sections deduced from the irradiation parameters. These provide both cross checks with published work, as well as a rigorous quantitative framework with high quality state-of-the-art detection apparatus in use in the experimental nuclear physics community.

A reliable compound-specific nitrogen isotope analysis of amino acids by GC-C-IRMS following derivatisation into N-pivaloyl-iso-propyl (NPIP)esters for high-resolution food webs estimation.

Science.gov (United States)

Zhang, Zhongyi; Tian, Jing; Xiao, Hongwei; Zheng, Nengjian; Gao, Xiaofei; Zhu, Renguo; Xiao, Huayun

2016-10-15

The signatures of natural stable nitrogen isotopic composition (δ(15)N) of individual amino acid (AA) have been confirmed to be a potentially effective tool for elucidating nitrogen cycling and trophic position of various organisms in food webs. In the present study, a two-stage derivatisation approach of esterification followed by acylation was evaluated. The biological samples underwent acid hydrolysis and the released individual AA was derivatived into corresponding N-pivaloyl-isopropyl (NPIP) esters for nitrogen isotopic analysis in gas chromatography-combustion-isotope ratio mass spectrometry (GC-C-IRMS). Usually, 13 individual AA derivatives were separated with fine baseline resolution based on a nonpolar gas chromatography column (DB-5ms). The minimum sample amount required under the presented conditions is larger than 20ngN on column in order to accurately determine the δ(15)N values. The δ(15)N values determined by GC-C-IRMS with a precision of better than 1‰, were within 1‰ after empirical correction compared to the corresponding measured by element analysis (EA)-IRMS. Bland-Altman plot showed highly consistency of the δ(15)N values determined by the two measurement techniques. Cation-exchange chromatography was applied to remove interfering fraction from the extracts of plant and animal samples and without nitrogen isotope fractionation during the treatment procedure. Moreover, this approach was carried out to estimate the trophic level of various natural organisms in a natural lake environment. Results highly proved that the trophic level estimated via the presented AA method well reflected the actual food web structure in natural environments. Copyright © 2016 Elsevier B.V. All rights reserved.

Mobility and diet in Neolithic, Bronze Age and Iron Age Germany : evidence from multiple isotope analysis

NARCIS (Netherlands)

Oelze, Viktoria Martha

2012-01-01

Prehistoric human diet can be reconstructed by the analysis of carbon (C), nitrogen (N) and sulphur (S) stable isotopes in bone, whereas ancient mobility and provenance can be studied using the isotopes of strontium (Sr) and oxygen (O) in tooth enamel, and of sulphur in bone. Although thirty years

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

Molecular and stable carbon isotopic characterization of PAH contaminants at McMurdo Station, Antarctica

International Nuclear Information System (INIS)

Kim, Moonkoo . E-mail moonkoo.kim@wmich.edu; Kennicutt, Mahlon C.; Qian Yaorong

2006-01-01

The molecular and stable carbon isotopic compositions of contaminant polycyclic aromatic hydrocarbons (PAHs) at McMurdo Station, Antarctica were analyzed in samples collected from land and sub-tidal area. PAHs in the study areas were characterized by high amounts of naphthalene and alkylated naphthalenes from petroleum products introduced by human activities in the area. Principal component analysis (PCA) of PAH composition data identified multiple sources of PAH contamination in the study area. Compositional assignments of origins were confirmed using compound specific stable carbon isotopic analysis

Elemental and isotopic characterization of Japanese and Philippine polished rice samples using instrumental neutron activation analysis and isotope ratio mass spectrometry

International Nuclear Information System (INIS)

Pabroa, Preciosa Corazon B.; Sucgang, Raymond J.; Mendoza, Norman dS.; Ebihara, Mitsuru

2011-01-01

Rice is a staple food for most Asian countries such as the Philippines and Japan and as such its elemental and isotopic content are of interest to the consumers. Its elemental content may reflect the macro nutrient reduction during milling or probable toxic elements uptake. Three Japanese and four Philippine polished rice samples in his study mostly came from rice bought from supermarkets.These rice samples were washed, dried and ground to fine powder. Instrumental neutron activation analysis (INAA), a very sensitive non-destructive multi-element analytical technique, was used for the elemental analysis of the samples and isotope-ratio mass spectrometry (IRMS) was used to obtain the isotopic signatures of the samples. Results show that compared with the unpolished rice standard NIES CRM10b, the polished Japanese and Philippine rice sampled show reduced concentrations of elements by as much as 1/3 to 1/10 of Mg, Mn, K and Na. Levels of Ca and Zn are not greatly affected. Arsenic is found in all the Japanese rice tested at an average concentration of 0.103 μg/g and three out of four of the Philippine rice at an average concentration of 0.070 μg/g. Arsenic contamination may have been introduced from the fertilizer used in rice fields. Higher levels of Br are seen in two of the Philippine rice at 14 and 34 μg/g with the most probable source being the pesticide methyl bromide. Isotopic ratio of ae 13 C show signature of a C3 plant with possible narrow distinguishable signature of Japanese rice within -27.5 to -28.5 while Philippine rice within -29 to -30. More rice samples will be analyzed to gain better understanding of isotopic signatures to distinguish inter-varietal and/or geographical differences. Elemental composition of soil samples of rice samples sources will be determined for better understanding of uptake mechanisms. (author)

Redox substoichiometry in isotope dilution analysis Pt. 4

International Nuclear Information System (INIS)

Kambara, T.; Yoshioka, H.; Ugai, Y.

1980-01-01

The oxidation reaction of antimony(III) with potassium dichromate has been investigated radiometrically. The quantitative oxidation of antimony(III) was found to be not disturbed even in large amounts of tin(IV). On the basis of these results the redox substoichiometric isotope dilution analysis using potassium dichromate as the oxidizing agent was proposed for the determination of antimony in metallic tin. An antimony content of 1.22+-0.05 μg in metallic tin (10 mg) was determined without separation of the matrix element. (author)

Gamma-ray isotopic analysis development at Los Alamos

Energy Technology Data Exchange (ETDEWEB)

Thomas E. Sampson

1999-11-01

This report describes the development history and characteristics of software developed in the Safeguards Science and Technology group at Los Alamos for gamma-ray isotopic analysis. This software analyzes the gamma-ray spectrum from measurements performed on actinide samples (principally plutonium and uranium) of arbitrary size, geometry, and physical and chemical composition. The results are obtained without calibration using only fundamental tabulated nuclear constants. Characteristics of the current software versions are discussed in some detail and many examples of implemented measurement systems are shown.

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.)

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

Science.gov (United States)

Sahlstedt, Elina; Arppe, Laura

2017-04-01

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

Ar39 Detection at the 10-16 Isotopic Abundance Level with Atom Trap Trace Analysis

Science.gov (United States)

Jiang, W.; Williams, W.; Bailey, K.; Davis, A. M.; Hu, S.-M.; Lu, Z.-T.; O'Connor, T. P.; Purtschert, R.; Sturchio, N. C.; Sun, Y. R.; Mueller, P.

2011-03-01

Atom trap trace analysis, a laser-based atom counting method, has been applied to analyze atmospheric Ar39 (half-life=269yr), a cosmogenic isotope with an isotopic abundance of 8×10-16. In addition to the superior selectivity demonstrated in this work, the counting rate and efficiency of atom trap trace analysis have been improved by 2 orders of magnitude over prior results. The significant applications of this new analytical capability lie in radioisotope dating of ice and water samples and in the development of dark matter detectors.

Method and device for isotope separation

International Nuclear Information System (INIS)

Dawson, J.M.

1976-01-01

The method works with a converted Q machine. The plasma containing the isotopes to be separated is crossed by a magnetic field running in the direction of the plasma column. More energy is transfered to the chosen isotope by oscillating magnetic and/or electric fields or by sound waves by using the specific resonance frequency for the selected isotope. The isotopes thus heated to different extents can be separated according to various methods given in the patent claims. (GG) [de

Analysis and separation of boron isotopes; Analyse et separation des isotopes du bore

Energy Technology Data Exchange (ETDEWEB)

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

1966-11-01

The nuclear applications of boron-10 justify the study of a method of measurement of its isotopic abundance as well as of very small traces of boron in different materials. A systematic study of thermionic emission of BO{sub 2}Na{sub 2}{sup +} has been carried out. In the presence of a slight excess of alkalis, the thermionic emission is considerably reduced. On the other hand, the addition of a mixture of sodium hydroxide-glycerol (or mannitol) to borax permits to obtain an intense and stable beam. These results have permitted to establish an operative method for the analysis of traces of boron by isotopic dilution. In other respects, the needs of boron-10 in nuclear industry Justify the study of procedures of separation of isotopes of boron. A considerable isotopic effect has been exhibited in the chemical exchange reaction between methyl borate and borate salt in solution. In the case of exchange between methyl borate and sodium borate, the elementary separation factor {alpha} is: {alpha}=(({sup 11}B/{sup 10}B)vap.)/(({sup 11}B/{sup 10}B)liq.)=1.03{sub 3}. The high value of this elementary effect has been multiplied in a distillation column in which the problem of regeneration of the reactive has been resolved. An alternative procedure replacing the alkali borate by a borate of volatile base, for example diethylamine, has also been studied ({alpha}=1,02{sub 5} in medium hydro-methanolic with 2,2 per cent water). (author) [French] Les applications nucleaires du bore 10 justifient l'etude d'une methode de mesure de son abondance isotopique dans divers materiaux ainsi que le dosage de tres faibles traces de bore. Une etude systematique de l'emission thermoionique de BO{sub 2} Na{sub 2}{sup +} a ete effectuee. En presence d'un leger exces d'alcalins, l'emission thermoionique est considerablement reduite. Par contre l'addition au borax d'un melange soude-glycerol (ou mannitol) permet d'obtenir un faisceau stable et intense. Ces resultats ont permis d'etablir un mode

Compound-specific nitrogen and carbon isotope analysis of nitroaromatic compounds in aqueous samples using solid-phase microextraction coupled to GC/IRMS.

Science.gov (United States)

Berg, Michael; Bolotin, Jakov; Hofstetter, Thomas B

2007-03-15

Solid-phase microextraction (SPME) coupled to gas chromatography/isotope ratio mass spectrometry was used to determine the delta15N and delta13C signatures of selected nitroaromatic contaminants such as the explosive 2,4,6-trinitrotoluene (TNT) for derivation of isotopic enrichment factors of contaminant transformation. Parameters for efficient extraction of nitroaromatic compounds (NACs) and substituted anilines from water samples were evaluated by SPME-GC/MS. delta13C signatures determined by SPME-GC/IRMS and elemental analyzer IRMS (EA-IRMS) were in good agreement, generally within +/-0.7 per thousand, except for 2,4-dinitrotoluene (2,4-DNT) and TNT, which showed slight deviations (IRMS were between 73 and 780 microg L-1 and correlated with the extraction efficiencies of the compounds determined by SPME-GC/MS. Nitrogen isotope measurements by SPME-GC/IRMS were of similar precision (standard deviations IRMS within +/-1.3 per thousand (+2.5 per thousand for TNT), but no systematic trend was found for the deviations. LODs of delta15N measurements ranged from 1.6 to 9.6 mg L-1 for nitrotoluenes, chlorinated NACs and DNTs (22 mg L-1 for TNT). The SPME-GC/IRMS method is well suited for the determination of isotopic enrichment factors of various NAC transformation processes and provides so far unexplored possibilities to elucidate behavior and degradation mechanisms of nitroaromatic contaminants in soils and groundwaters.

Holocene Paleohydrological Changes in Northern Michigan: Interpretations of Biomarker Distributions and Compound Specific Stable Isotope Analysis from Peatlands

Science.gov (United States)

Nichols, J. E.; Booth, R. K.; Jackson, S. T.; Pendall, E. G.; Huang, Y.

2006-12-01

Sediments of ombrotrophic peatlands are excellent archives for reconstructing past changes in precipitation/evaporation (P/E) balance. Multiproxy analysis of these sediments is critical for better understanding of climatic events experienced by these highly sensitive systems, as each proxy may respond to different climate parameters. In this study, we use distributions of n-alkanes and δD of Sphagnum biomarkers to interpret paleohydrology from sediments of Irwin Smith Bog, northern Michigan. We then integrate these data with pollen data and testate amoebae-inferred water table depth. Sphagnum moss is the dominant peat former in ombrotrophic bogs, but vascular plants become abundant when water tables are drawn down. Thus, the abundance of Sphagnum relative to vascular plants is indicative of peatland hydrology. The n-alkanes produced by Sphagnum differ from vascular plants in the relative abundance of the different homologues, with the former having excess amounts of shorter chain C23 n-alkane. We use several measures (compound ratios, PCA) to show changes in then-alkane distributions in the sediments, and thus changes in the peatland plant community. Our data provide high- resolution, quantitative paleohydrological records for the study region that are consistent with other records. We also show that the relative abundance of a newly identified Sphagnum biomarker, 2-heptacosanone, can be used to reconstruct changing plant communities. Because ombrotrophic systems lose water by evaporation, drier/warmer conditions cause hydrogen isotopic enrichment of bog water and Sphagnum biomarkers. We measured the δD of C23 n-alkane and 2-heptacosanone to provide additional paleoclimate information. Our multiproxy approach allows us to better understand the climate changes during key intervals of the Holocene. For example, a sharp decrease in the abundance of Tsuga canadensis (hemlock) pollen has been previously identified in records from many places throughout eastern North

Isotopic Discrimination During Leaf Litter Decomposition

Science.gov (United States)

Ngao, J.; Rubino, M.

2006-12-01

Methods involving stable isotopes have been successfully applied since decades in various research fields. Tracing 13C natural abundance in ecosystem compartments greatly enhanced the understanding of the C fluxes in the plant-soil-atmosphere C exchanges when compartments present different C isotopic signatures (i.e. atmospheric CO2 vs photosynthetic leaves, C3 vs C4; etc.). However, the assumption that no isotopic discrimination occurs during respiration is commonly made in numbers of C isotope-based ecological studies. Furthermore, verifications of such assumption are sparse and not enough reliable. The aim of our study is to assess the potential isotopic discrimination that may occur during litter decomposition. Leaf litter from an Arbutus unedo (L.) stand (Tolfa, Italy) was incubated in 1L jars, under constant laboratory conditions (i.e. 25 ° C and 135% WC). During the entire incubation period, gravimetric mass loss, litter respiration rates and the isotopic composition of respired CO2 are monitored at regular intervals. Data from 7 months of incubation will be presented and discussed. After two months, the litter mass loss averaged 16% of initial dry mass. During the same time-period, the respiration rate decreased significantly by 58% of the initial respiration rate. Isotopic compositions of respired CO2 ranged between -27.95‰ and - 25.69‰. Mean values did not differ significantly among the sampling days, in spite of an apparent enrichment in 13C of respired CO2 with time. The significance of these isotopic enrichment will be determined at a longer time scale. They may reveal both/either a direct microbial discrimination during respiration processes and/or a use of different litter compounds as C source along time. Further chemical and compound-specific isotopic analysis of dry matter will be performed in order to clarify these hypotheses. This work is part of the "ALICE" project, funded by the European Union's Marie Curie Fellowship Actions that aims to

Position-specific 13C distributions within propane from experiments and natural gas samples

Science.gov (United States)

Piasecki, Alison; Sessions, Alex L.; Lawson, Michael; Ferreira, A.A.; Santos Neto, E. V.; Ellis, Geoffrey S.; Lewan, Michael; Eilers, J.M.

2018-01-01

Site-specific carbon isotope measurements of organic compounds potentially recover information that is lost in a conventional, ‘bulk’ isotopic analysis. Such measurements are useful because isotopically fractionating processes may have distinct effects at different molecular sites, and thermodynamically equilibrated populations of molecules tend to concentrate heavy isotopes in one molecular site versus another. Most recent studies of site-specific 13C in organics use specialized Nuclear Magnetic Resonance (NMR) techniques or complex chemical degradations prior to mass spectrometric measurements. Herein we present the first application of a new mass spectrometric technique that reconstructs the site-specific carbon isotope composition of propane based on measurements of the 13C/12C ratios of two or more fragment ions that sample different proportions of the terminal and central carbon sites. We apply this method to propane from laboratory experiments and natural gas samples to explore the relationships between site-specific carbon isotope composition, full-molecular δ13C, thermal maturity, and variation in organic matter precursors. Our goal is to advance the understanding of the sources and histories of short-chain alkanes within geologic systems. Our findings suggest that propane varies in its site-specific carbon isotope structure, which is correlated with increasing thermal maturity, first increasing in terminal position δ13C and then increasing in both center and terminal position δ13C. This pattern is observed in both experimental and natural samples, and is plausibly explained by a combination of site-specific, temperature-dependent isotope effects associated with conversion of different precursor molecules (kerogen, bitumen, and/or oil) to propane, differences in site-specific isotopic contents of those precursors, and possibly distillation of reactive components of those precursors with increasing maturity. We hypothesize that the largest changes in

Position-specific 13C distributions within propane from experiments and natural gas samples

Science.gov (United States)

Piasecki, Alison; Sessions, Alex; Lawson, Michael; Ferreira, A. A.; Santos Neto, E. V.; Ellis, Geoffrey S.; Lewan, Michael D.; Eiler, John M.

2018-01-01

Site-specific carbon isotope measurements of organic compounds potentially recover information that is lost in a conventional, 'bulk' isotopic analysis. Such measurements are useful because isotopically fractionating processes may have distinct effects at different molecular sites, and thermodynamically equilibrated populations of molecules tend to concentrate heavy isotopes in one molecular site versus another. Most recent studies of site-specific 13C in organics use specialized Nuclear Magnetic Resonance (NMR) techniques or complex chemical degradations prior to mass spectrometric measurements. Herein we present the first application of a new mass spectrometric technique that reconstructs the site-specific carbon isotope composition of propane based on measurements of the 13C/12C ratios of two or more fragment ions that sample different proportions of the terminal and central carbon sites. We apply this method to propane from laboratory experiments and natural gas samples to explore the relationships between site-specific carbon isotope composition, full-molecular δ13C, thermal maturity, and variation in organic matter precursors. Our goal is to advance the understanding of the sources and histories of short-chain alkanes within geologic systems. Our findings suggest that propane varies in its site-specific carbon isotope structure, which is correlated with increasing thermal maturity, first increasing in terminal position δ13C and then increasing in both center and terminal position δ13C. This pattern is observed in both experimental and natural samples, and is plausibly explained by a combination of site-specific, temperature-dependent isotope effects associated with conversion of different precursor molecules (kerogen, bitumen, and/or oil) to propane, differences in site-specific isotopic contents of those precursors, and possibly distillation of reactive components of those precursors with increasing maturity. We hypothesize that the largest changes in

Stable carbon isotope analysis (δ13C values) of polybrominated diphenyl ethers and their UV-transformation products

International Nuclear Information System (INIS)

Rosenfelder, Natalie; Bendig, Paul; Vetter, Walter

2011-01-01

Polybrominated diphenyl ethers (PBDEs) are frequently detected in food and environmental samples. We used compound specific isotope analysis to determine the δ 13 C values of individual PBDEs in two technical mixtures. Within the same technical product (DE-71 or DE-79), BDE congeners were the more depleted in 13 C the higher brominated they were. In contrast, the products of light-induced hydrodebromination of BDE 47 and technical DE-79 were more enriched in 13 C because of more stable bonds between 13 C and bromine. As a result, the δ 13 C values of the irradiated solution progressed diametrically compared to those of the technical synthesis. The ratio of the δ 13 C values of BDE 47 to BDE 99 and of BDE 99 to BDE 153 are thus suggested as indicators to distinguish native technical products from transformation products. Ratios 1) is typical of transformation products. - Highlights: → δ 13 C values of PBDEs were determined by means of compound specific isotope analysis. → PBDEs in technical mixtures were the more depleted in 13 C the higher they were brominated. → Solutions of individual PBDEs and technical PBDE mixtures were irradiated by UV light. → δ 13 C values of irradiated PBDEs and technical PBDEs progressed diametrically. → Ratios of the δ 13 C values were used to distinguish native from transformed PBDEs. - Diametrically progressing δ 13 C values in technical mixtures and UV-transformation products of DE-79 may be useful for source appointment of PBDEs in environmental samples

Forensic analysis of explosives using isotope ratio mass spectrometry (IRMS)--discrimination of ammonium nitrate sources.

Science.gov (United States)

Benson, Sarah J; Lennard, Christopher J; Maynard, Philip; Hill, David M; Andrew, Anita S; Roux, Claude

2009-06-01

An evaluation was undertaken to determine if isotope ratio mass spectrometry (IRMS) could assist in the investigation of complex forensic cases by providing a level of discrimination not achievable utilising traditional forensic techniques. The focus of the research was on ammonium nitrate (AN), a common oxidiser used in improvised explosive mixtures. The potential value of IRMS to attribute Australian AN samples to the manufacturing source was demonstrated through the development of a preliminary AN classification scheme based on nitrogen isotopes. Although the discrimination utilising nitrogen isotopes alone was limited and only relevant to samples from the three Australian manufacturers during the evaluated time period, the classification scheme has potential as an investigative aid. Combining oxygen and hydrogen stable isotope values permitted the differentiation of AN prills from three different Australian manufacturers. Samples from five different overseas sources could be differentiated utilising a combination of the nitrogen, oxygen and hydrogen isotope values. Limited differentiation between Australian and overseas prills was achieved for the samples analysed. The comparison of nitrogen isotope values from intact AN prill samples with those from post-blast AN prill residues highlighted that the nitrogen isotopic composition of the prills was not maintained post-blast; hence, limiting the technique to analysis of un-reacted explosive material.

Novel proxies for reconstructing paleohydrology from ombrotrophic peatlands: biomarker and compound-specific H and C stable isotope ratios

Science.gov (United States)

Wang, J.; Nichols, J. E.; Huang, Y.

2008-12-01

Ombrotrophic peatlands are excellent archives for paleohydrologic information because they are hydrologically isolated from their surroundings. However, quantitative proxies for deciphering peatland archives are lacking. Here, we present development and application of novel organic geochemical methods for quantitative reconstruction of paleohydrology from the ombrotrophic sediments, and comparison of organic geochemical data with conventional paleoecological proxies. Application of these methods to the sediments of several North American and European peatlands has revealed significant changes in the hydroclimate throughout the Holocene. The plant assemblage living at the surface of the peatland is tightly controlled by surface moisture. Under wet conditions, Sphagnum mosses, with no active mechanism for drawing water from below the surface of the peatland, are dominant. During dry conditions, vascular plants are more productive relative to Sphagnum. A ratio of the abundance of two biomarkers representing Sphagnum and vascular plants sensitively records changes in hydrologic balance (Nichols et al., 2006, Org. Geochem. 37, 1505-1513). We have further developed stable isotope models to compute climate parameters from compound-specific H and C isotope ratios of biomarkers to create a more comprehensive climate reconstruction. Vascular plant leaf waxes carry the D/H ratio signature of precipitation that is little affected by evaporation, whereas the Sphagnum biomarker records isotopic ratios of the water at the peatland surface, which is strongly enriched by evaporation. Evaporation amount can be calculated using the differences between D/H ratios of the two types of biomarkers. C isotope ratios of Sphagnum biomarkers can also be used to quantify surface wetness. Methanotrophic bacteria live symbiotically with Sphagnum, providing isotopically light carbon for photosynthesis. These bacteria are more active when the Sphagnum is wet, thus providing more 13C-depleted CO2

Field experimentation in isotope-aided studies

International Nuclear Information System (INIS)

Zapata, F.

1990-01-01

Isotopic-aided studies involve the application of isotopically labelled fertilizer as tracers for the quantitative and precise determination of the fate of specific nutrient elements in the soil/plant system. The planning of isotopic-aided studies requires a different approach from that followed in the design of normal fertilizer trials because of the cost and supply of isotopically labelled materials, the use of highly specialized equipment and the need for skillful trained staff in the use of isotope techniques both in the field/greenhouse and the laboratory. This report is intended to highlight the main points to be considered while applying those techniques in the field or greenhouse. It has been well established that nuclear techniques are a powerful tool in agricultural research. One should take advantage of the use of such techniques if the following criteria are met: The isotope method is the only way to solve a particular question or to obtain a specific piece of information. There are other methods available for such a purpose but the nuclear method provides a direct and quick means to obtain the needed information resulting in higher economic return

Isotope analysis of diamond-surface passivation effect of high-temperature H2O-grown atomic layer deposition-Al2O3 films

International Nuclear Information System (INIS)

Hiraiwa, Atsushi; Saito, Tatsuya; Matsumura, Daisuke; Kawarada, Hiroshi

2015-01-01

The Al 2 O 3 film formed using an atomic layer deposition (ALD) method with trimethylaluminum as Al precursor and H 2 O as oxidant at a high temperature (450 °C) effectively passivates the p-type surface conduction (SC) layer specific to a hydrogen-terminated diamond surface, leading to a successful operation of diamond SC field-effect transistors at 400 °C. In order to investigate this excellent passivation effect, we carried out an isotope analysis using D 2 O instead of H 2 O in the ALD and found that the Al 2 O 3 film formed at a conventional temperature (100 °C) incorporates 50 times more CH 3 groups than the high-temperature film. This CH 3 is supposed to dissociate from the film when heated afterwards at a higher temperature (550 °C) and causes peeling patterns on the H-terminated surface. The high-temperature film is free from this problem and has the largest mass density and dielectric constant among those investigated in this study. The isotope analysis also unveiled a relatively active H-exchange reaction between the diamond H-termination and H 2 O oxidant during the high-temperature ALD, the SC still being kept intact. This dynamic and yet steady H termination is realized by the suppressed oxidation due to the endothermic reaction with H 2 O. Additionally, we not only observed the kinetic isotope effect in the form of reduced growth rate of D 2 O-oxidant ALD but found that the mass density and dielectric constant of D 2 O-grown Al 2 O 3 films are smaller than those of H 2 O-grown films. This is a new type of isotope effect, which is not caused by the presence of isotopes in the films unlike the traditional isotope effects that originate from the presence of isotopes itself. Hence, the high-temperature ALD is very effective in forming Al 2 O 3 films as a passivation and/or gate-insulation layer of high-temperature-operation diamond SC devices, and the knowledge of the aforementioned new isotope effect will be a basis for further enhancing ALD

Nuclear and isotopic techniques underpinning probabilistic ecological risk analysis in coastal marine systems

International Nuclear Information System (INIS)

Szymczak, R.; Twining, J.; Hollins, S.; Hughes, C.; Mazumder, D.; Alquezar, R.

2006-01-01

Full text: The historical operation of manufacturing, chemical and other industries in the Sydney Harbour catchment over many decades has left a legacy of high chemical contamination in the surrounding catchment, such that a recent report describes Port Jackson as one of the most contaminated harbours in the world (Birch and Taylor, 2005). The legacy in Homebush Bay is amongst the worst in the harbour and presents a considerable management problem. Elucidation of environmental processes is the key to effective ecosystem management, however few tools are available to determine their inter-relationships, rates and directions. This study has four components: (1) determination of linkages between high trophic order species and different habitats resources using stable isotopic analyses of carbon and nitrogen. These studies identify trophic cascades forming the basis for selection of biota for contaminant transfer experiments; (2) short-term (weeks - months) chronology and geochemistry of sediment cores and traps in Homebush Bay to determine rates of sedimentation and resuspension (using environmental/cosmogenic Be). Models derived from these studies provide the contaminants levels against which risk is assessed; (3) biokinetic studies using proxy radiotracer isotopes (eg. 75 Se and 109 Cd for analogous stable metals) of the uptake and trophic transfer of contaminants by specific estaurine biota. Here we identify the rates and extent to which contaminants accumulated and transferred to predators/seafoods; and (4) application of a probabilistic ecological risk assessment model (AQUARISK) set to criteria determined by stakeholder consensus. In this study we analysed the distribution of natural isotopes and redistribution of artificial isotopes injected into ecological compartments to determine the key trophic linkages and contaminant pathways in an estuarine system and contribute to improving the accuracy and specificity of a probabilistic ecological risk assessment

Chromatographic speciation of Cr(III)-species, inter-species equilibrium isotope fractionation and improved chemical purification strategies for high-precision isotope analysis

DEFF Research Database (Denmark)

Larsen, Kirsten Kolbjørn; Wielandt, Daniel Kim Peel; Schiller, Martin

2016-01-01

Chromatographic purification of chromium (Cr), which is required for high-precision isotope analysis, is complicated by the presence of multiple Cr-species with different effective charges in the acid digested sample aliquots. The differing ion exchange selectivity and sluggish reaction rates of ...

Tracing fresh assimilates through Larix decidua exposed to elevated CO₂ and soil warming at the alpine treeline using compound-specific stable isotope analysis.

Science.gov (United States)

Streit, Kathrin; Rinne, Katja T; Hagedorn, Frank; Dawes, Melissa A; Saurer, Matthias; Hoch, Günter; Werner, Roland A; Buchmann, Nina; Siegwolf, Rolf T W

2013-02-01

How will carbon source-sink relations of 35-yr-old larch trees (Larix decidua) at the alpine treeline respond to changes in atmospheric CO(2) and climate? We evaluated the effects of previously elevated CO(2) concentrations (9 yr, 580 ppm, ended the previous season) and ongoing soil warming (4 yr, + 4°C). Larch branches were pulse labeled (50 at% (13)CO(2)) in July 2010 to trace fresh assimilates through tissues (buds, needles, bark and wood) and non-structural carbon compounds (NCC; starch, lipids, individual sugars) using compound-specific isotope analysis. Nine years of elevated CO(2) did not lead to increased NCC concentrations, nor did soil warming increase NCC transfer velocities. By contrast, we found slower transfer velocities and higher NCC concentrations than reported in the literature for lowland larch. As a result of low dilution with older carbon, sucrose and glucose showed the highest maximum (13)C labels, whereas labels were lower for starch, lipids and pinitol. Label residence times in needles were shorter for sucrose and starch (c. 2 d) than for glucose (c. 6 d). Although our treatments showed no persistent effect on larch carbon relations, low temperature at high altitudes clearly induced a limitation of sink activities (growth, respiration, root exudation), expressed in slower carbon transfer and higher NCC concentrations. © 2012 The Authors. New Phytologist © 2012 New Phytologist Trust.

Tracing fetal and childhood exposure to lead using isotope analysis of deciduous teeth

Energy Technology Data Exchange (ETDEWEB)

Shepherd, Thomas J. [Centre for Oral Health Research, School of Dental Sciences, Newcastle University, Newcastle upon Tyne (United Kingdom); British Geological Survey, Keyworth, Nottingham (United Kingdom); Dirks, Wendy [Department of Anthropology, Durham University, Durham (United Kingdom); Roberts, Nick M.W. [NERC Isotope Geosciences Laboratory, British Geological Survey, Nottingham (United Kingdom); Patel, Jaiminkumar G. [Leeds Dental Institute, University Leeds, Leeds (United Kingdom); Hodgson, Susan [MRC-PHE Centre for Environment and Health, Department of Epidemiology and Biostatistics, Imperial College London (United Kingdom); Pless-Mulloli, Tanja [Institute of Health and Society, Newcastle University, Newcastle upon Tyne (United Kingdom); Walton, Pamela [Centre for Oral Health Research, School of Dental Sciences, Newcastle University, Newcastle upon Tyne (United Kingdom); Parrish, Randall R. [British Geological Survey, Keyworth, Nottingham (United Kingdom)

2016-04-15

We report progress in using the isotopic composition and concentration of Pb in the dentine and enamel of deciduous teeth to provide a high resolution time frame of exposure to Pb during fetal development and early childhood. Isotope measurements (total Pb and {sup 208}Pb/{sup 206}Pb, {sup 207}Pb/{sup 206}Pb ratios) were acquired by laser ablation inductively coupled mass spectrometry at contiguous 100 micron intervals across thin sections of the teeth; from the outer enamel surface to the pulp cavity. Teeth samples (n=10) were selected from two cohorts of children, aged 5–8 years, living in NE England. By integrating the isotope data with histological analysis of the teeth, using the daily incremental lines in dentine, we were able to assign true estimated ages to each ablation point (first 2–3 years for molars, first 1–2 years for incisors+pre-natal growth). Significant differences were observed in the isotope composition and concentration of Pb between children, reflecting differences in the timing and sources of exposure during early childhood. Those born in 2000, after the withdrawal of leaded petrol in 1999, have the lowest dentine Pb levels (<0.2 µg Pb/g) with {sup 208}Pb/{sup 206}Pb (mean ±2σ: 2.126–2.079) {sup 208}Pb/{sup 206}Pb (mean ±2σ: 0.879–0.856) ratios that correlate very closely with modern day Western European industrial aerosols (PM{sub 10}, PM{sub 2.5}) suggesting that diffuse airborne pollution was probably the primary source and exposure pathway. Legacy lead, if present, is insignificant. For those born in 1997, dentine lead levels are typically higher (>0.4 µgPb/g) with {sup 208}Pb/{sup 206}Pb (mean ±2σ: 2.145–2.117) {sup 208}Pb/{sup 206}Pb (mean ±2σ: 0.898–0.882) ratios that can be modelled as a binary mix between industrial aerosols and leaded petrol emissions. Short duration, high intensity exposure events (1–2 months) were readily identified, together with evidence that dentine provides a good proxy for childhood

Isotopic methods in hydrogeology and their application to the Underground Research Laboratory, Manitoba

Energy Technology Data Exchange (ETDEWEB)

Gascoyne, M [Atomic Energy of Canada Ltd., Pinawa, MB (Canada). Whiteshell Labs.; Kotzer, T

1995-09-01

This review examines isotopic methods used to determine groundwater sources, residence times and processes of geochemical evolution that have been published in the international literature, with specific reference to AECL`s experience in these methods and applications to groundwaters at the Underground Research Laboratory (URL), Manitoba. The program of groundwater sampling and analysis currently being planned for the URL area over the next several years will concentrate on specific isotopic measurements that may assist in understanding the groundwater flow system at the URL site. These results will add to the existing data for the URL area and indicate which isotopes are most useful when applied to the known groundwater flow system of the URL. This program of study is especially important because it not only uses standard geochemical and isotopic measurements (e.g., major ion, trace elements, {sup 2}H/{sup 18}O, {sup 14}C, {sup 34}S) of groundwaters, but will determine values of more exotic and unusual ratios, such as {sup 6}Li/{sup 7}Li, and B{sup 11}/B{sup 10}, whose potential for understanding groundwater geochemical evolution is largely unknown at present. In addition, the more established but equally complex methods of isotopic analysis, to determine {sup 3}He/{sup 4}He, {sup 36}Cl/Cl and {sup 129}I/I, will be used to assess their potential for adding to the hydrogeochemical understanding of flow paths in crystalline rock. (author). 182 refs., 11 tabs., 27 figs.

Stable-carbon isotope ratios for sourcing the nerve-agent precursor methylphosphonic dichloride and its products.

Science.gov (United States)

Moran, James J; Fraga, Carlos G; Nims, Megan K

2018-08-15

The ability to connect a chemical threat agent to a specific batch of a synthetic precursor can provide a fingerprint to contribute to effective forensic investigations. Stable isotope analysis can leverage intrinsic, natural isotopic variability within the molecules of a threat agent to unlock embedded chemical fingerprints in the material. Methylphosphonic dichloride (DC) is a chemical precursor to the nerve agent sarin. DC is converted to methylphosphonic difluoride (DF) as part of the sarin synthesis process. We used a suite of commercially available DC stocks to both evaluate the potential for δ 13 C analysis to be used as a fingerprinting tool in sarin-related investigations and to develop sample preparation techniques (using chemical hydrolysis) that can simplify isotopic analysis of DC and its synthetic products. We demonstrate that natural isotopic variability in DC results in at least three distinct, isotope-resolved clusters within the thirteen stocks we analyzed. Isotopic variability in the carbon feedstock (i.e., methanol) used for DC synthesis is likely inherited by the DC samples we measured. We demonstrate that the hydrolysis of DC and DF to methylphosphonic acid (MPA) can be used as a preparative step for isotopic analysis because the reaction does not impart a significant isotopic fractionation. MPA is more chemically stable, less toxic, and easier to handle than DC or DF. Further, the hydrolysis method we demonstrated can be applied to a suite of other precursors or to sarin itself, thereby providing a potentially valuable forensic tool. Copyright © 2018. Published by Elsevier B.V.

Isotopic analysis of uranium hexafluoride highly enriched in U-235

International Nuclear Information System (INIS)

Chaussy, L.; Boyer, R.

1968-01-01

Isotopic analysis of uranium in the form of the hexafluoride by mass-spectrometry gives gross results which are not very accurate. Using a linear interpolation method applied to two standards it is possible to correct for this inaccuracy as long as the isotopic concentrations are less than about 10 per cent in U-235. Above this level, the interpolations formula overestimates the results, especially if the enrichment of the analyzed samples is higher than 1.3 with respect to the standards. A formula is proposed for correcting the interpolation equation and for the extending its field of application to high values of the enrichment (≅2) and of the concentration. It is shown that by using this correction the results obtained have an accuracy which depends practically only on that of the standards, taking into account the dispersion in the measurements. (authors) [fr

Research on aerodynamic means of isotope enrichment

International Nuclear Information System (INIS)

Cattolica, R.J.; Gallagher, R.J.; Talbot, L.; Willis, D.R.; Hurlbut, F.C.; Fiszdon, W.; Anderson, J.B.

1978-03-01

The results of a research program directed toward the understanding of the fundamental gas dynamics involved in aerodynamic isotope enrichment are summarized. The specific aerodynamic isotope enrichment method which was examined in this research is based on a velocity slip phenomenon which occurs in the rarefied hypersonic expansion of a heavy molecular weight gas and a light carrier gas in a nozzle or free jet. This particular aerodynamic method was chosen for study because it contains the fundamental molecular physics of other more complex techniques within the context of a one-dimensional flow without boundary effects. From both an experimental and theoretical modeling perspective this provides an excellent basis for testing the experimental and numerical tools with which to investigate more complex aerodynamic isotope enrichment processes. This report consists of three separate parts. Part I contains a theoretical analysis of the velocity slip effect in free jet expansions of binary and ternary gas mixtures. The analysis, based on a source flow model and using moment equations is derived from the Boltzmann equation using the hypersonic approximation. Part II contains the experimental measurements of velocity slip. The numerical simulation of the slip process was carried out by using a Monte-Carlo numerical technique. In addition, comparisons between the theoretical analysis of Part I and the experiments are presented. Part III describes impact pressure measurements of free jet expansions from slot shaped two dimensional nozzles. At least two methods of aerodynamic isotope enrichment (opposed jet and velocity slip) would depend on the use of this type of two dimensional expansion. Flow surveys of single free jet and the interferene of crossed free jets are presented

Validation of chlorine and oxygen isotope ratio analysis to differentiate perchlorate sources and to document perchlorate biodegradation

Science.gov (United States)

Paul B. Hatzinger,; Böhlke, John Karl; Sturchio, Neil C.; Gu, Baohua

2013-01-01

Increased health concerns about perchlorate (ClO4-) during the past decade and subsequent regulatory considerations have generated appreciable interest in source identification. The key objective of the isotopic techniques described in this guidance manual is to provide evidence concerning the origin of ClO4- in soils and groundwater and, more specifically, whether that ClO4- is synthetic or natural. Chlorine and oxygen isotopic analyses of ClO4- provide the primary direct approach whereby different sources of ClO4- can be distinguished from each other. These techniques measure the relative abundances of the stable isotopes of chlorine (37Cl and 35Cl) and oxygen (18O, 17O, and 16O) in ClO4- using isotope-ratio mass spectrometry (IRMS). In addition, the relative abundance of the radioactive chlorine isotope 36Cl is measured using accelerator mass spectrometry (AMS). Taken together, these measurements provide four independent quantities that can be used to distinguish natural and synthetic ClO4- sources, to discriminate different types of natural ClO4-, and to detect ClO4- biodegradation in the environment. Other isotopic, chemical, and geochemical techniques that can be applied in conjunction with isotopic analyses of ClO4- to provide supporting data in forensic studies are also described.

Enhanced sensitivity of DNA- and rRNA-based stable isotope probing by fractionation and quantitative analysis of isopycnic centrifugation gradients.

Science.gov (United States)

Lueders, Tillmann; Manefield, Mike; Friedrich, Michael W

2004-01-01

Stable isotope probing (SIP) of nucleic acids allows the detection and identification of active members of natural microbial populations that are involved in the assimilation of an isotopically labelled compound into nucleic acids. SIP is based on the separation of isotopically labelled DNA or rRNA by isopycnic density gradient centrifugation. We have developed a highly sensitive protocol for the detection of 'light' and 'heavy' nucleic acids in fractions of centrifugation gradients. It involves the fluorometric quantification of total DNA or rRNA, and the quantification of either 16S rRNA genes or 16S rRNA in gradient fractions by real-time PCR with domain-specific primers. Using this approach, we found that fully 13C-labelled DNA or rRNA of Methylobacterium extorquens was quantitatively resolved from unlabelled DNA or rRNA of Methanosarcina barkeri by cesium chloride or cesium trifluoroacetate density gradient centrifugation respectively. However, a constant low background of unspecific nucleic acids was detected in all DNA or rRNA gradient fractions, which is important for the interpretation of environmental SIP results. Consequently, quantitative analysis of gradient fractions provides a higher precision and finer resolution for retrieval of isotopically enriched nucleic acids than possible using ethidium bromide or gradient fractionation combined with fingerprinting analyses. This is a prerequisite for the fine-scale tracing of microbial populations metabolizing 13C-labelled compounds in natural ecosystems.

Cl and C isotope analysis to assess the effectiveness of chlorinated ethene degradation by zero-valent iron: Evidence from dual element and product isotope values

International Nuclear Information System (INIS)

Audí-Miró, Carme; Cretnik, Stefan; Otero, Neus; Palau, Jordi; Shouakar-Stash, Orfan; Soler, Albert

2013-01-01

Highlights: ► TCE and cis-DCE Cl isotope fractionation was investigated for the first time with ZVI. ► A C–Cl bond is broken in the rate-limiting step during ethylene ZVI dechlorination. ► Dual C/Cl isotope plot is a promising tool to discriminate abiotic degradation. ► Product-related carbon isotopic fractionation gives evidence of abiotic degradation. ► Hydrogenolysis and β-dichloroelimination pathways occur simultaneously. - Abstract: This study investigated C and, for the first time, Cl isotope fractionation of trichloroethene (TCE) and cis-dichloroethene (cis-DCE) during reductive dechlorination by cast zero-valent iron (ZVI). Hydrogenolysis and β-dichloroelimination pathways occurred as parallel reactions, with ethene and ethane deriving from the β-dichloroelimination pathway. Carbon isotope fractionation of TCE and cis-DCE was consistent for different batches of Fe studied. Transformation of TCE and cis-DCE showed Cl isotopic enrichment factors (ε Cl ) of −2.6‰ ± 0.1‰ (TCE) and −6.2‰ ± 0.8‰ (cis-DCE), with Apparent Kinetic Isotope Effects (AKIE Cl ) for Cl of 1.008 ± 0.001 (TCE) and 1.013 ± 0.002 (cis-DCE). This indicates that a C–Cl bond breakage is rate-determining in TCE and cis-DCE transformation by ZVI. Two approaches were investigated to evaluate if isotope fractionation analysis can distinguish the effectiveness of transformation by ZVI as opposed to natural biodegradation. (i) Dual isotope plots. This study reports the first dual (C, Cl) element isotope plots for TCE and cis-DCE degradation by ZVI. The pattern for cis-DCE differs markedly from that reported for biodegradation of the same compound by KB-1, a commercially available Dehalococcoides-containing culture. The different trends suggest an expedient approach to distinguish abiotic and biotic transformation, but this needs to be confirmed in future studies. (ii) Product-related isotope fractionation. Carbon isotope ratios of the hydrogenolysis product cis

Use of alpha spectrometry for analysis of U-isotopes in some granite samples

International Nuclear Information System (INIS)

El-Galy, M.M.; Desouky, O.A.; Khattab, M.R.; Issa, F.A.

2011-01-01

The present study aims to use the α-spectrometry, at NMA. A radiochemical technique for analysis of U-isotopes was carried out for some granite samples from Gabal Gattar and El Missikat localities and also for some reference soil samples of IAEA. Several steps of sample preparation, radiochemical separation, and source preparation were performed before analysis. The concerned sample was leached by HNO 3 , HF and H 2 O 2 acids after ashing. The ashed sample was spiked with uranium tracer ( 232 U) for chemical yield and activity calculation. Then uranium was extracted from the matrix elements with trioctylphosphine oxide (TOPO) and stripped with 1 M NH 4 F/0.1 M HCl solution. The uranium fraction was purified by co-precipitation with LaF 3 to ensure complete removal of thorium and traces of resolution degrading elements. This was followed by a final clean-up step using an anion exchange. The pure uranium fraction was electrodeposited on a stainless steel disc from HCl/oxalate solution. The obtained results from the soil reference samples indicate general similarities between the techniques of α-spectrometers of NMA, EAEA and IAEA for analysis of U-isotopes. The U-isotopes in the granite samples of high radioactivity levels need more attempts after dilution process to be in the limit detection of α-spectrometry. (author)

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.

A method of uranium isotopes concentration analysis

International Nuclear Information System (INIS)

Lin Yuangen; Jiang Meng; Wu Changli; Duan Zhanyuan; Guo Chunying

2010-01-01

A basic method of uranium isotopes concentration is described in this paper. The iteration method is used to calculate the relative efficiency curve, by analyzing the characteristic γ energy spectrum of 235 U, 232 U and the daughter nuclide of 238 U, then the relative activity can be calculated, at last the uranium isotopes concentration can be worked out, and the result is validated by the experimentation. (authors)

Quantification and isotopic analysis of intracellular sulfur metabolites in the dissimilatory sulfate reduction pathway

Science.gov (United States)

Sim, Min Sub; Paris, Guillaume; Adkins, Jess F.; Orphan, Victoria J.; Sessions, Alex L.

2017-06-01

Microbial sulfate reduction exhibits a normal isotope effect, leaving unreacted sulfate enriched in 34S and producing sulfide that is depleted in 34S. However, the magnitude of sulfur isotope fractionation is quite variable. The resulting changes in sulfur isotope abundance have been used to trace microbial sulfate reduction in modern and ancient ecosystems, but the intracellular mechanism(s) underlying the wide range of fractionations remains unclear. Here we report the concentrations and isotopic ratios of sulfur metabolites in the dissimilatory sulfate reduction pathway of Desulfovibrio alaskensis. Intracellular sulfate and APS levels change depending on the growth phase, peaking at the end of exponential phase, while sulfite accumulates in the cell during stationary phase. During exponential growth, intracellular sulfate and APS are strongly enriched in 34S. The fractionation between internal and external sulfate is up to 49‰, while at the same time that between external sulfate and sulfide is just a few permil. We interpret this pattern to indicate that enzymatic fractionations remain large but the net fractionation between sulfate and sulfide is muted by the closed-system limitation of intracellular sulfate. This 'reservoir effect' diminishes upon cessation of exponential phase growth, allowing the expression of larger net sulfur isotope fractionations. Thus, the relative rates of sulfate exchange across the membrane versus intracellular sulfate reduction should govern the overall (net) fractionation that is expressed. A strong reservoir effect due to vigorous sulfate reduction might be responsible for the well-established inverse correlation between sulfur isotope fractionation and the cell-specific rate of sulfate reduction, while at the same time intraspecies differences in sulfate uptake and/or exchange rates could account for the significant scatter in this relationship. Our approach, together with ongoing investigations of the kinetic isotope

Calcium isotope effects in ion exchange electromigration and calcium isotope analysis by thermo-ionization mass spectrometry

International Nuclear Information System (INIS)

Fujii, Y.; Hoshi, J.; Iwamoto, H.; Okamoto, M.; Kakihana, H.

1985-01-01

Calcium ions were made to electromigrate along a cation exchange membrane. The abundance ratios of the calcium isotopes (Ca-40, 42, 43, 44, 48) in the migrated bands were measured by thermo-ionization mass spectrometry. The lighter isotopes were enriched in the front part of the migrated band. The increments in the isotope abundance ratios were found to be proportional to the mass difference of the isotopes. The observed epsilon-values per unit mass difference (epsilon/ΔM) were 1.26 x 10 -4 (at 20 0 C), 1.85 x 10 -4 (at 25 0 C) and 2.4 x 10 -4 (at 40 0 C). The mass spectrometry was improved by using a low temperature for the evaporation of CaI 2 . (orig.)

Isotopes in environmental research

International Nuclear Information System (INIS)

Bowen, G.; Rozanski, K.; Vose, P.

1990-01-01

Radioactive and stable isotopes have long been considered a very efficient tool for studying physical and biological aspects of how the global ecosystem functions. Their applications in environmental research are numerous, embracing research at all levels. This article looks at only a few of the approaches to environmental problems that involve the use of isotopes. Special attention is given to studies of the Amazon Basin. Environmental isotopes are very efficient tools in water cycle studies. Tritium, a radioactive tracer, is especially useful in studying dynamics of water movement in different compartments of the hydrosphere, both on the local and global scales. Heavy stable isotopes of hydrogen and oxygen (deuterium and oxygen-18) provide information about steady-state characteristics of the water cycle. Isotope methods, some relatively new, have a major role in site-specific studies. Some indicative examples include: Studying turnover of organic matter. Changes in the carbon-13/carbon-12 isotopic ratio of organic matter were used to determine the respective contributions of organic carbon derived from forest and pasture. Studying biological nitrogen fixation. One of the ways nitrogen levels in soil can be maintained for productivity is by biological nitrogen fixation. Studying nitrogen availability and losses. The experimental use of nitrogen-15 is invaluable for defining losses of soil nitrogen to the atmosphere and to groundwater. Studies can similarly be done with stable and radioactive sulphur isotopes. This article indicates some potential uses of isotopes in environmental research. While the major problem of global climate change has not been specifically addressed here, the clearing of the Amazon forest, one focus of the IAEA's environmental programme, may have serious consequences for the global climate. These include substantial reduction of the amount of latent heat transported to the regions outside the tropics and acceleration of the greenhouse

Free-drop analysis of the transport container for hydrogen isotopes

International Nuclear Information System (INIS)

Lee, M. S.; Hong, C. S.; Baek, S. W.; Ahn, D. H.; Kim, K. R.; Lee, S. H.; Lim, S. P.; Jung, H. S.

2002-01-01

The vessel used for the transport of radioactive materials, containing hydrogen isotopes is evaluated for hypothetical accident conditions according to national regulations. The computational analysis is a cost effective tool to minimize testing and streamline the regulatory procedures, and supports experimental programs to qualify the container for the safe transport of radioactive materials. The numerical analysis of 9m free-drop onto a flat unyielding, horizontal surface has been performed using the explicit finite element computer program ABAQUS. Especially free-drop simulations for 30.deg. C tilted condition is precisely estimated

Laser photochemical separation of hydrogen isotopes

International Nuclear Information System (INIS)

Fowler, M.C.

1979-01-01

A method of separating isotopes of hydrogen utilizing isotopically selective photodissociation of organic acid is disclosed. Specifically acetic or formic acid containing compounds of deuterated nd hydrogenated acid is irradiated by radiation having a wavelength in the infrared spectrum between 9.2 to 10.8 microns to produce deuterium hydroxide and deuterium hydride respectively. Maintaining the acid at an elevated temperature significantly improves the yield of isotope separation

Keratin decomposition by trogid beetles: evidence from a feeding experiment and stable isotope analysis

Science.gov (United States)

Sugiura, Shinji; Ikeda, Hiroshi

2014-03-01

The decomposition of vertebrate carcasses is an important ecosystem function. Soft tissues of dead vertebrates are rapidly decomposed by diverse animals. However, decomposition of hard tissues such as hairs and feathers is much slower because only a few animals can digest keratin, a protein that is concentrated in hairs and feathers. Although beetles of the family Trogidae are considered keratin feeders, their ecological function has rarely been explored. Here, we investigated the keratin-decomposition function of trogid beetles in heron-breeding colonies where keratin was frequently supplied as feathers. Three trogid species were collected from the colonies and observed feeding on heron feathers under laboratory conditions. We also measured the nitrogen (δ15N) and carbon (δ13C) stable isotope ratios of two trogid species that were maintained on a constant diet (feathers from one heron individual) during 70 days under laboratory conditions. We compared the isotopic signatures of the trogids with the feathers to investigate isotopic shifts from the feathers to the consumers for δ15N and δ13C. We used mixing models (MixSIR and SIAR) to estimate the main diets of individual field-collected trogid beetles. The analysis indicated that heron feathers were more important as food for trogid beetles than were soft tissues under field conditions. Together, the feeding experiment and stable isotope analysis provided strong evidence of keratin decomposition by trogid beetles.

Following Carbon Isotopes from Methane to Molecules

Science.gov (United States)

Freeman, K. H.

2017-12-01

Continuous-flow methods introduced by Hayes (Matthews and Hayes, 1978; Freeman et al., 1990; Hayes et al., 1990) for compound-specific isotope analyses (CSIA) transformed how we study the origins and fates of organic compounds. This analytical revolution launched several decades of research in which researchers connect individual molecular structures to diverse environmental and climate processes affecting their isotopic profiles. Among the first applications, and one of the more dramatic isotopically, was tracing the flow of natural methane into cellular carbon and cellular biochemical constituents. Microbial oxidation of methane can be tracked by strongly 13C-depleted organic carbon in early Earth sedimentary environments, in marine and lake-derived biomarkers in oils, and in modern organisms and their environments. These signatures constrain microbial carbon cycling and inform our understanding of ocean redox. The measurement of molecular isotopes has jumped forward once again, and it is now possible to determine isotope abundances at specific positions within increasingly complex organic structures. In addition, recent analytical developments have lowered sample sensitivity limits of CSIA to picomole levels. These new tools have opened new ways to measure methane carbon in the natural environment and within biochemical pathways. This talk will highlight how molecular isotope methods enable us to follow the fate of methane carbon in complex environments and along diverse metabolic pathways, from trace fluids to specific carbon positions within microbial biomarkers.

Discrimination factors of carbon and nitrogen stable isotopes in meerkat feces

Directory of Open Access Journals (Sweden)

Shaena Montanari

2017-06-01

Full Text Available Stable isotope analysis of feces can provide a non-invasive method for tracking the dietary habits of nearly any mammalian species. While fecal samples are often collected for macroscopic and genetic study, stable isotope analysis can also be applied to expand the knowledge of species-specific dietary ecology. It is somewhat unclear how digestion changes the isotope ratios of animals’ diets, so more controlled diet studies are needed. To date, most diet-to-feces controlled stable isotope experiments have been performed on herbivores, so in this study I analyzed the carbon and nitrogen stable isotope ratios in the diet and feces of the meerkat (Suricata suricatta, a small omnivorous mammal. The carbon trophic discrimination factor between diet and feces (Δ13Cfeces is calculated to be 0.1 ± 1.5‰, which is not significantly different from zero, and in turn, not different than the dietary input. On the other hand, the nitrogen trophic discrimination factor (Δ15Nfeces is 1.5 ± 1.1‰, which is significantly different from zero, meaning it is different than the average dietary input. Based on data generated in this experiment and a review of the published literature, carbon isotopes of feces characterize diet, while nitrogen isotope ratios of feces are consistently higher than dietary inputs, meaning a discrimination factor needs to be taken into account. The carbon and nitrogen stable isotope values of feces are an excellent snapshot of diet that can be used in concert with other analytical methods to better understand ecology, diets, and habitat use of mammals.

An application of nitrogen microwave-induced plasma mass spectrometry to isotope dilution analysis of selenium in marine organisms

Energy Technology Data Exchange (ETDEWEB)

Shirasaki, Toshihiro [Hitachi Instruments Engineering Co. Ltd., Hitachinaka, Ibaraki (Japan); Yoshinaga, Jun; Morita, Masatoshi; Okumoto, Toyoharu; Oishi, Konosuke

1996-01-01

Nitrogen microwave-induced plasma mass spectrometry was studied for its applicability to the isotope dilution analysis of selenium in biological samples. Spectroscopic interference by calcium, which is present in high concentrations in biological samples, was investigated. No detectable background spectrum was observed for the major selenium isotopes of {sup 78}Se and {sup 80}Se. No detectable interferences by sodium, potassium, calcium and phosphorus on the isotope ratio {sup 80}Se/{sup 78}Se were observed up to concentration of 200 mg/ml. The method was applied to the analysis of selenium in biological reference materials of marine organisms. The results showed good agreement between the certified and found values. (author).

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.

Individual economical value of plutonium isotopes and analysis of the reprocessing of irradiated fuel

International Nuclear Information System (INIS)

Gomes, I.C.; Rubini, L.A.; Barroso, D.E.G.

1983-01-01

An economical analysis of plutonium recycle in a PWR reactor, without any modification, is done, supposing an open market for the plutonium. The individual value of the plutonium isotopes is determined solving a system with four equations, which the unknow factors are the Pu-239, Pu-240, pu-241 and Pu-242 values. The equations are obtained equalizing the cost of plutonium fuel cycle of four different isotope mixture to the cost of the uranium fuel cycle. (E.G.) [pt

Isotope Dilution - Thermal Ionisation Mass Spectrometric Analysis for Tin in a Fly Ash Material

International Nuclear Information System (INIS)

Hernandez, C.; Fernandez, M.; Quejido, A. L.

2006-01-01

Isotope dilution-thermal ionisation mass spectrometry (ID-TIMS) analysis has been applied to the determination of tin in a fly ash sample supplied by the EC Joint Research Centre (Ispra, Italy). The proposed procedure includes the silica gel/phosphoric acid technique for tin thermal ionisation activation and a strict heating protocol for isotope ratio measurements. Instrumental mass discrimination factor has been previously determined measuring a natural tin standard solution. Spike solutions has been prepared from 112Sn-enriched metal and quantified by reverse isotope dilution analysis. Two sample aliquots were spiked and tin was extracted with 4,5 M HCI during 25 min ultrasound esposure time. Due to the complex matrix of this fly ash material, a two-steps purification stage using ion-exchange chromatography was required prior TIMS analysis. Obtained results for the two sample-spike blends (10,10 + - 0,55 y 10,50 + - 0,64 imolg-1) are comprarable, both value and uncertainty. Also a good reproducibility is observed between measurements. The proposed ID-TIMS procedure, as a primary method and due to the lack of fly ash reference material certified for tin content, can be used to validate more routine methodologies applied to tin determination in this kind of materials. (Author) 75 refs

Water-hydrogen isotope exchange process analysis

International Nuclear Information System (INIS)

Fedorchenko, O.; Alekseev, I.; Uborsky, V.

2008-01-01

The use of a numerical method is needed to find a solution to the equation system describing a general case of heterogeneous isotope exchange between gaseous hydrogen and liquid water in a column. A computer model of the column merely outputting the isotope compositions in the flows leaving the column, like the experimental column itself, is a 'black box' to a certain extent: the solution is not transparent and occasionally not fully comprehended. The approximate analytical solution was derived from the ZXY-diagram (McCabe-Thiele diagram), which illustrates the solution of the renewed computer model called 'EVIO-4.2' Several 'unusual' results and dependences have been analyzed and explained. (authors)

Isotopic analysis of a single Pb particle by using laser ablation TOF-MS

Energy Technology Data Exchange (ETDEWEB)

Choi, I. H.; Yoo, H. S. [Chungbuk National Univ., Cheongju (Korea, Republic of); Song, K. S. [KAERI, Daejeon (Korea, Republic of)

2008-11-15

A laser ablation can be applied to a direct isotopic analysis of solid samples due to the following advantages. Because a laser ablation is a very powerful ionization source, an additional ionization source is not required and an one step vaporization and ionization of samples is possible. Due to the small size of a laser beam, an analysis of a local trace can be applied. Also, the contamination or loss of samples is reduced because there is no need for a sample preparation process. In this study, Pb particles with a size of∼150μm were analyzed by LA TOF MS and a second harmonic of the Nd:YAG laser, 532nm, was used for the laser ablation. First, the ion signal of Pb was measured depending on the matrices. For loading a Pb particle, a silicon wafer, cotton textile, and Ta metal plate were used as a basic plate. As a result, the silicon wafer plate was identified to be the best matrix for the analysis of Pb with a good resolution and its measured isotopic ratios reasonably agree with the natural abundance within 5%. The figure shows a mass spectrum of Pb onto a silicon wafer. In applying the resonance laser ablation, the detection sensitivity was increased by more than 10 times. In the experiment regarding the cotton textile, the mass resolution of Pb was more than 500 which was enough to measure the isotopes, and it is applicable to real swipe samples in various fields such as environmental analysis, industry, and nuclear forensic.

A simple cleanup method for the isolation of nitrate from natural water samples for O isotopes analysis

International Nuclear Information System (INIS)

Haberhauer, G.; Blochberger, K.

1999-09-01

The analysis of O-isotopic composition of nitrate has many potential applications in studies of environmental processes. O-isotope nitrate analysis require sample free of other oxygen-containing compounds. More than 100 % of non-NO 3 - oxygen relative to NO 3 - oxygen can still be found in forest soil water samples after cleanup if improper cleanup strategies, e.g., adsorption onto activated carbon, are used. Such non-NO 3 - oxygen compounds will bias O-isotropic data. Therefore, an efficient cleanup method was developed to isolate nitrate from natural water samples. In a multistep cleanup procedure using adsorption onto water-insoluble poly(vinylpyrrolidone), removal of almost all other oxygen-containing compounds, such as fulvic acids, and isolation of nitrate was achieved. The method supplied samples free of non-NO 3 - oxygen which can be directly combusted to CO 2 for subsequent O-isotope analysis. (author)

Uranium isotope separation using styrene cation exchangers

International Nuclear Information System (INIS)

Kahovec, J.

1980-01-01

The separation of 235 U and 238 U isotopes is carried out either by simple isotope exchange in the system uranium-cation exchanger (sulphonated styrene divinylbenzene resin), or by combination of isotope exchange in a uranium-cation exchanger (Dowex 50, Amberlite IR-120) system and a chemical reaction. A review is presented of elution agents used, the degree of cation exchanger cross-linking, columns length, and 235 U enrichment. The results are described of the isotope effect study in a U(IV)-U(VI)-cation exchanger system conducted by Japanese and Romanian authors (isotope exchange kinetics, frontal analysis, reverse (indirect) frontal analysis). (H.S.)

Stable isotopes as tracers for radionuclides

International Nuclear Information System (INIS)

Giussani, A.; Bartolo, D. de; Cantone, M.C.; Zilker, T.; Greim, H.; Roth, P.; Werner, E.

2000-01-01

The assessment of internal dose after incorporation of radionuclides requires as input data the knowledge of the uptake into the systemic circulation, the distribution and retention in selected organs, the excretion pathways. Realistic biokinetic models are needed for reliable estimates, correct interpretation of bioassay measurements, appropriate decision-making in radiological emergencies. For many radionuclides, however, the biokinetic models currently recommended are often generic, with very few specific parameters, due to the lack of experimental human data. The use of stable isotopes as tracers enables to determine important biokinetic parameters such as the fractional uptake, the clearance from the transfer compartment, the excretion patterns under experimentally controlled conditions. The subjects investigated are not exposed to any radiation risk, so this technique enables to obtain biokinetic information also for sensitive groups of the population, such as children or pregnant women, and to determine age- and gender-specific model parameters. Sophisticated analytical method, able to discriminate and quantitate different isotopes of the same element in complex matrices such as biological fluids, have to be purposely developed and optimized. Activation analysis and mass spectrometry are the most proper techniques of choice. Experiments were conducted with molybdenum, tellurium, ruthenium and zirconium. Activation analysis with protons, thermal ionization mass spectrometry and inductively coupled mass spectrometry were employed for the determination of stable isotopes of these elements in blood plasma and urine samples. Several deviations from the predictions of the ICRP models were observed. For example, modifications to the current model for molybdenum have been suggested on the basis of these results. The dose coefficients to the target regions calculated with this proposed model are even of one order of magnitude different than the ICRP estimates

Methods in the use of GC/C/IRMS for the analysis of biochemical and pollutant isotope signatures of compounds

International Nuclear Information System (INIS)

Macko, S.A.; Engel, M.H.

2001-01-01

The potential for application of GC/C/IRMS analysis to any multitude of environmental, ecological or biochemical research areas is only beginning to be realized. Extension of compound-specific isotope analytical data derived from modern organisms and settings to yield interpretations of ancient depositional environments certainly appears possible. Further application of GC/C/IRMS approaches to understand the cycling of carbon and nitrogen, the identification and alteration of pollutants, or resolve metabolic relationships between compounds in living or extinct organisms are all within the scope of future research. (author)

Conditional CO2 flux analysis of a managed grassland with the aid of stable isotopes

Science.gov (United States)

Zeeman, M. J.; Tuzson, B.; Emmenegger, L.; Knohl, A.; Buchmann, N.; Eugster, W.

2009-04-01

Short statured managed ecosystems, such as agricultural grasslands, exhibit high temporal changes in carbon dioxide assimilation and respiration fluxes for which measurements of the net CO2 flux, e.g. by using the eddy covariance (EC) method, give only limited insight. We have therefore adopted a recently proposed concept for conditional EC flux analysis of forest to grasslands, in order to identify and quantify daytime sub-canopy respiration fluxes. To validate the concept, high frequency (≈5 Hz) stable carbon isotope analyis of CO2 was used. We made eddy covariance measurements of CO2 and its isotopologues during four days in August 2007, using a novel quantum cascade laser absorption spectrometer, capable of high time resolution stable isotope analysis. The effects of a grass cut during the measurement period could be detected and resulted in a sub-canopy source conditional flux classification, for which the isotope composition of the CO2 could be confirmed to be of a respiration source. However, the conditional flux method did not work for an undisturbed grassland canopy. We attribute this to the flux measurement height that was chosen well above the roughness sublayer, where the natural isotopic tracer (δ13C) of respiration was too well mixed with background air.

Development of Stable Isotope Analysis Technology for Epidemiological Study of Migratory Birds in Connection with Avian Influenza

International Nuclear Information System (INIS)

Kim, Jongyun; Park, Jongho; Han, Sunho; Song, Kyuseok; Ko, Yongkwon; Bae, Inae; Cho, Mihyun; Jung, Gahee; Yeom, Ina

2012-03-01

In order to clarify correlations between the spread of avian influenza and migratory routes of birds, various conventional methods including a ring method, gene analysis, geolocator and a satellite tracking method are being used together. We first report on the estimation of origin of migratory bird in the Korea based on the statistical method of stable isotope ratio analysis of feathers. It is expected that migratory birds in Junam reservoir were from the two different regions according to the stable isotope ration analysis. However, it is not easy to conclude the breeding ground of northern pintails based on the current data because the degree of precision or accuracy can be influenced by many factors. For this reason, this statistical analysis accuracy can be influenced by many factors. For this reason, this statistical analysis can have a scientific significance if the reliability of the whole measurement system is improved. Furthermore, databases are not enough to prepare base map of regional isotope ratios because database of stable isotope ratio in oxygen and hydrogen of rainwater in Korea should be constructed. Though the research has focused on the hydrogen and oxygen until now, investigation of other elements, such as carbon, sulfur, nitrogen and others that can describe metabolic process or regional characteristics, is also worthwhile subject. And it is believed that this research will improve a resolution of detection for the migratory pathway and habitat of birds

Development of Stable Isotope Analysis Technology for Epidemiological Study of Migratory Birds in Connection with Avian Influenza

Energy Technology Data Exchange (ETDEWEB)

Kim, Jongyun; Park, Jongho; Han, Sunho; Song, Kyuseok; Ko, Yongkwon; Bae, Inae; Cho, Mihyun; Jung, Gahee; Yeom, Ina

2012-03-15

In order to clarify correlations between the spread of avian influenza and migratory routes of birds, various conventional methods including a ring method, gene analysis, geolocator and a satellite tracking method are being used together. We first report on the estimation of origin of migratory bird in the Korea based on the statistical method of stable isotope ratio analysis of feathers. It is expected that migratory birds in Junam reservoir were from the two different regions according to the stable isotope ration analysis. However, it is not easy to conclude the breeding ground of northern pintails based on the current data because the degree of precision or accuracy can be influenced by many factors. For this reason, this statistical analysis accuracy can be influenced by many factors. For this reason, this statistical analysis can have a scientific significance if the reliability of the whole measurement system is improved. Furthermore, databases are not enough to prepare base map of regional isotope ratios because database of stable isotope ratio in oxygen and hydrogen of rainwater in Korea should be constructed. Though the research has focused on the hydrogen and oxygen until now, investigation of other elements, such as carbon, sulfur, nitrogen and others that can describe metabolic process or regional characteristics, is also worthwhile subject. And it is believed that this research will improve a resolution of detection for the migratory pathway and habitat of birds.

Redox substoichiometry in isotope dilution analysis Pt. 2

International Nuclear Information System (INIS)

Kambara, T.; Suzuki, J.; Yoshioka, H.; Nakajima, N.

1978-01-01

Isotope dilution analysis using the redox substoichiometric principle has been applied to the determination of antimony content in metallic zinc. As the substoichiometric reaction, the oxidation of trivalent to pentavalent antimony with potassium permanganate was used, followed by separation of these species by the BHPA extraction of trivalent antimony. Determination of antimony contents less than 0.5 μg was found to be possible with good accuracy, without separation of zinc ions. The antimony content in a metallic zinc sample was determined to be 19.7+-0.8 ppm, in good agreement with the results obtained by the other analytical methods. (author)

Reassessment of the NH4 NO3 thermal decomposition technique for calibration of the N2 O isotopic composition.

Science.gov (United States)

Mohn, Joachim; Gutjahr, Wilhelm; Toyoda, Sakae; Harris, Eliza; Ibraim, Erkan; Geilmann, Heike; Schleppi, Patrick; Kuhn, Thomas; Lehmann, Moritz F; Decock, Charlotte; Werner, Roland A; Yoshida, Naohiro; Brand, Willi A

2016-09-08

In the last few years, the study of N 2 O site-specific nitrogen isotope composition has been established as a powerful technique to disentangle N 2 O emission pathways. This trend has been accelerated by significant analytical progress in the field of isotope-ratio mass-spectrometry (IRMS) and more recently quantum cascade laser absorption spectroscopy (QCLAS). Methods The ammonium nitrate (NH 4 NO 3 ) decomposition technique provides a strategy to scale the 15 N site-specific (SP ≡ δ 15 N α - δ 15 N β ) and bulk (δ 15 N bulk  = (δ 15 N α  + δ 15 N β )/2) isotopic composition of N 2 O against the international standard for the 15 N/ 14 N isotope ratio (AIR-N 2 ). Within the current project 15 N fractionation effects during thermal decomposition of NH 4 NO 3 on the N 2 O site preference were studied using static and dynamic decomposition techniques. The validity of the NH 4 NO 3 decomposition technique to link NH 4 + and NO 3 - moiety-specific δ 15 N analysis by IRMS to the site-specific nitrogen isotopic composition of N 2 O was confirmed. However, the accuracy of this approach for the calibration of δ 15 N α and δ 15 N β values was found to be limited by non-quantitative NH 4 NO 3 decomposition in combination with substantially different isotope enrichment factors for the conversion of the NO 3 - or NH 4 + nitrogen atom into the α or β position of the N 2 O molecule. The study reveals that the completeness and reproducibility of the NH 4 NO 3 decomposition reaction currently confine the anchoring of N 2 O site-specific isotopic composition to the international isotope ratio scale AIR-N 2 . The authors suggest establishing a set of N 2 O isotope reference materials with appropriate site-specific isotopic composition, as community standards, to improve inter-laboratory compatibility. This article is protected by copyright. All rights reserved.

Preparation of Authigenic Pyrite from Methane-bearing Sediments for In Situ Sulfur Isotope Analysis Using SIMS.

Science.gov (United States)

Lin, Zhiyong; Sun, Xiaoming; Peckmann, Jörn; Lu, Yang; Strauss, Harald; Xu, Li; Lu, Hongfeng; Teichert, Barbara M A

2017-08-31

Different sulfur isotope compositions of authigenic pyrite typically result from the sulfate-driven anaerobic oxidation of methane (SO4-AOM) and organiclastic sulfate reduction (OSR) in marine sediments. However, unravelling the complex pyritization sequence is a challenge because of the coexistence of different sequentially formed pyrite phases. This manuscript describes a sample preparation procedure that enables the use of secondary ion mass spectroscopy (SIMS) to obtain in situ δ 34 S values of various pyrite generations. This allows researchers to constrain how SO4-AOM affects pyritization in methane-bearing sediments. SIMS analysis revealed an extreme range in δ 34 S values, spanning from -41.6 to +114.8‰, which is much wider than the range of δ 34 S values obtained by the traditional bulk sulfur isotope analysis of the same samples. Pyrite in the shallow sediment mainly consists of 34 S-depleted framboids, suggesting early diagenetic formation by OSR. Deeper in the sediment, more pyrite occurs as overgrowths and euhedral crystals, which display much higher SIMS δ 34 S values than the framboids. Such 34 S-enriched pyrite is related to enhanced SO4-AOM at the sulfate-methane transition zone, postdating OSR. High-resolution in situ SIMS sulfur isotope analyses allow for the reconstruction of the pyritization processes, which cannot be resolved by bulk sulfur isotope analysis.

Investigating the provenance of un-dyed spun cotton fibre using multi-isotope profiles and chemometric analysis.

Science.gov (United States)

Daéid, Niamh Nic; Meier-Augenstein, Wolfram; Kemp, Helen F

2011-07-15

The analysis of un-dyed spun cotton fibres can be challenging within a forensic science context where discrimination of one fibre from another is of importance. Conventional microscopic and chemical analysis of these fibres is generally unsuccessful because of their similar morphology. In this work we have explored the potential of isotope ratio mass spectrometry (IRMS) as a tool for spun cotton fibre analysis in an attempt to reveal any discriminatory information available. Seven different batches of un-dyed spun cotton fibre from four different countries were analysed. A combination of the hydrogen and oxygen isotopic data facilitated the correct association of the samples, demonstrating, for the first time, the applicability of IRMS to fibre analysis in this way. Copyright © 2011 John Wiley & Sons, Ltd.

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

Isotope ratio monitoring LC/MS (IRM-LC/MS): new applications

International Nuclear Information System (INIS)

Juchelka, D; Hilkert, A.; Krummen, M.

2005-01-01

With the introduction of compound specific isotope analysis by isotope ratio monitoring GC/ MS (IRM-GC/MS) the immediate demand for similar applications using HPLC was created. Many compounds of biological, medical, pharmaceutical and environmental interest are not volatile or too polar. Consequently, they cannot be directly analyzed by gas chromatography. In IRM-GC/MS the carrier is helium, which does not interfere with the essential combust ion step prior to isotope ratio mass spectrometry (IRMS). In opposite the LC mobile phase has inhibited a similar direct conversion up to now. All earlier IRM-LC/MS approaches were based on the removal of the liquid phase prior to combustion risking fractionation of the isotope ratios of the eluted compounds. To avoid such restrictions we developed a new continuous flow concept for the coupling of an HPLC system to the isotope ratio MS for 13 C/ 12C isotope ratio analysis. In the Finnigan LC IsoLink, the liquid phase is not removed from the sample prior to oxidation. The sample is oxidized still in the mobile phase followed by on-line separation of the CO 2 from the liquid phase and transfer into the isotope ratio MS. Therefore, this strategy is based on water and inorganic buffers as mobile phase. The new approach opens up a whole new world in the application of gas isotope ratio mass spectrometry. The 13 C/ 12 C ratio s of organic acids, amino acids, carbohydrates and nucleotides can now be measured. These components typically within a complex matrix are separated by liquid chromatography followed by on-line determination of the isotope ratios. The draw backs of using derivatization and off-line preparation procedures can now be over come. This new technique allow s studying biochemical cycles, running tracer experiments and determining the origin of components. Applications from different scientific areas such as biogeochemistry, molecular biology, and pharmacy as well as authenticity control o f foods will be presented