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.

High-precision measurement of variations in calcium isotope ratios in urine by multiple collector inductively coupled plasma mass spectrometry

Science.gov (United States)

Morgan, J.L.L.; Gordon, G.W.; Arrua, R.C.; Skulan, J.L.; Anbar, A.D.; Bullen, T.D.

2011-01-01

We describe a new chemical separation method to isolate Ca from other matrix elements in biological samples, developed with the long-term goal of making high-precision measurement of natural stable Ca isotope variations a clinically applicable tool to assess bone mineral balance. A new two-column procedure utilizing HBr achieves the purity required to accurately and precisely measure two Ca isotope ratios (44Ca/42Ca and 44Ca/43Ca) on a Neptune multiple collector inductively coupled plasma mass spectrometer (MC-ICPMS) in urine. Purification requirements for Sr, Ti, and K (Ca/Sr > 10000; Ca/Ti > 10000000; and Ca/K > 10) were determined by addition of these elements to Ca standards of known isotopic composition. Accuracy was determined by (1) comparing Ca isotope results for samples and standards to published data obtained using thermal ionization mass spectrometry (TIMS), (2) adding a Ca standard of known isotopic composition to a urine sample purified of Ca, and (3) analyzing mixtures of urine samples and standards in varying proportions. The accuracy and precision of δ44/42Ca measurements of purified samples containing 25 μg of Ca can be determined with typical errors less than ±0.2‰ (2σ).

High-precision measurement of phenylalanine δ15N values for environmental samples: a new approach coupling high-pressure liquid chromatography purification and elemental analyzer isotope ratio mass spectrometry.

Science.gov (United States)

Broek, Taylor A B; Walker, Brett D; Andreasen, Dyke H; McCarthy, Matthew D

2013-11-15

Compound-specific isotope analysis of individual amino acids (CSI-AA) is a powerful new tool for tracing nitrogen (N) source and transformation in biogeochemical cycles. Specifically, the δ(15)N value of phenylalanine (δ(15)N(Phe)) represents an increasingly used proxy for source δ(15)N signatures, with particular promise for paleoceanographic applications. However, current derivatization/gas chromatography methods require expensive and relatively uncommon instrumentation, and have relatively low precision, making many potential applications impractical. A new offline approach has been developed for high-precision δ(15)N measurements of amino acids (δ(15)N(AA)), optimized for δ(15)N(Phe) values. Amino acids (AAs) are first purified via high-pressure liquid chromatography (HPLC), using a mixed-phase column and automated fraction collection. The δ(15)N values are determined via offline elemental analyzer-isotope ratio mass spectrometry (EA-IRMS). The combined HPLC/EA-IRMS method separated most protein AAs with sufficient resolution to obtain accurate δ(15)N values, despite significant intra-peak isotopic fractionation. For δ(15)N(Phe) values, the precision was ±0.16‰ for standards, 4× better than gas chromatography/combustion/isotope ratio mass spectrometry (GC/C/IRMS; ±0.64‰). We also compared a δ(15)N(Phe) paleo-record from a deep-sea bamboo coral from Monterey Bay, CA, USA, using our method versus GC/C/IRMS. The two methods produced equivalent δ(15)N(Phe) values within error; however, the δ(15)N(Phe) values from HPLC/EA-IRMS had approximately twice the precision of GC/C/IRMS (average stdev of 0.27‰ ± 0.14‰ vs 0.60‰ ± 0.20‰, respectively). These results demonstrate that offline HPLC represents a viable alternative to traditional GC/C/IMRS for δ(15)N(AA) measurement. HPLC/EA-IRMS is more precise and widely available, and therefore useful in applications requiring increased precision for data interpretation (e.g. δ(15)N paleoproxies

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.

High-precision mass spectrometric analysis using stable isotopes in studies of children

NARCIS (Netherlands)

Schierbeek, Henk; van den Akker, Chris H. P.; Fay, Laurent B.; van Goudoever, Johannes B.

2012-01-01

The use of stable isotopes combined with mass spectrometry (MS) provides insight into metabolic processes within the body. Herein, an overview on the relevance of stable isotope methodology in pediatric research is presented. Applications for the use of stable isotopes with MS cover carbohydrate,

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.

High-precision γ -ray spectroscopy of the cardiac PET imaging isotope 82Rb and its impact on dosimetry

Science.gov (United States)

Nino, M. N.; McCutchan, E. A.; Smith, S. V.; Lister, C. J.; Greene, J. P.; Carpenter, M. P.; Muench, L.; Sonzogni, A. A.; Zhu, S.

2016-02-01

82Rb is a positron-emitting isotope used in cardiac positron emission tomography (PET) imaging which has been reported to deliver a significantly lower effective radiation dose than analogous imaging isotopes like 201Tl and 99 mTc sestamibi. High-quality β -decay data are essential to accurately appraise the total dose received by the patients. A source of 82Sr was produced at the Brookhaven Linac Isotope Producer (BLIP), transported to Argonne National Laboratory, and studied with the Gammasphere facility. Significant revisions have been made to the level scheme of 82Kr including 12 new levels, 50 new γ -ray transitions, and the determination of many new spin assignments through angular correlations. These new high-quality data allow a precise reappraisal of the β -decay strength function and thus the consequent dose received by patients.

Precision Mass Measurement of Argon Isotopes

CERN Multimedia

Lunney, D

2002-01-01

% IS388\\\\ \\\\ A precision mass measurement of the neutron-deficient isotopes $^{32,33,34}$Ar is proposed. Mass values of these isotopes are of importance for: a) a stringent test of the Isobaric-Multiplet- Mass-Equation, b) a verification of the correctness of calculated charge-dependent corrections as used in super-allowed $\\beta$- decay studies aiming at a test of the CVC hypothesis, and c) the determination of the kinematics in electron-neutrino correlation experiments searching for scalar currents in weak interaction. The measurements will be carried out with the ISOLTRAP Penning trap mass spectrometer.

Precision experiments with rare isotopes with LEBIT at MSU

Energy Technology Data Exchange (ETDEWEB)

Schury, P.; Bollen, G.; Ringle, R.; Sun, T. [National Superconducting Cyclotron Laboratory, East Lansing, MI (United States); Michigan State University, Department of Physics and Astronomy, East Lansing, MI (United States); Davies, D.A.; Morrissey, D.J. [National Superconducting Cyclotron Laboratory, East Lansing, MI (United States); Michigan State University, Department of Chemistry, East Lansing, MI (United States); Doemer, A.; Prinke, A. [Michigan State University, Department of Physics and Astronomy, East Lansing, MI (United States); Lawton, D.; Ottarson, J.; Schwarz, S.; Weissman, L. [National Superconducting Cyclotron Laboratory, East Lansing, MI (United States)

2005-09-01

The Low-Energy Beam and Ion Trap facility LEBIT at the NSCL is in the final phase of commissioning. Gas stopping of fast fragment beams and modern ion manipulation techniques are used to provide beams for high-precision mass measurements and other experiments. The status of the facility and the result of first test mass measurements on stable krypton isotopes are presented. (orig.)

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

International Nuclear Information System (INIS)

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

2013-01-01

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

High-precision gamma-ray spectroscopy of 61Cu, an emerging medical isotope used in positron emission tomography

Science.gov (United States)

Nelson, N.; Ellison, P.; Nickles, R.; McCutchan, E.; Sonzogni, A.; Smith, S.; Greene, J.; Carpenter, M.; Zhu, S.; Lister, C.; Moran, K.

2017-09-01

61Cu (t1 / 2 = 3.339h) is an important medical isotope used in positron emission tomography (PET) tumor hypoxia imaging scans; however, its beta-plus decay and the subsequent gamma decay of 61Ni has not been studied in over 30 years. Therefore, high quality decay data of 61Cu is desired to determine the overall dose delivered to a patient. In this study, 61Cu was produced at the University of Wisconsin - Madison cyclotron and then assayed using the Gammasphere array at Argonne National Laboratory. Consisting of 70 Compton-suppressed high-purity germanium (HPGe) detectors, Gammasphere provides precise decay data that exceeds that of previous 61Cu studies. γ-ray singles and coincident data were recorded and then analyzed using Radware gf3m software. Through γ- γ coincidence techniques, new γ-ray transitions were identified and high precision determination of γ-ray intensities were made. These modifications and additions to the current decay scheme will be presented, and their impact on the resulting does estimates will be discussed. DOE Isotope Program is acknowledged for funding ST5001030. Work supported by the U.S. DOE under Grant No. DE-FG02-94ER40848 and Contract Nos. DE-AC02-98CH10946 and DE-AC02-06CH11357 and by the Science Undergraduate Laboratory Internship Program (SULI).

The precise measurement of TL isotopic compositions by MC-ICPMS: Application to the analysis of geological materials and meteorites.

Science.gov (United States)

Rehkämper, Mark; Halliday, Alex N.

1999-07-01

The precision of Tl isotopic measurements by thermal ionization mass spectrometry (TIMS) is severely limited by the fact that Tl possesses only two naturally occurring isotopes, such that there is no invariant isotope ratio that can be used to correct for instrumental mass discrimination. In this paper we describe new chemical and mass spectrometric techniques for the determination of Tl isotopic compositions at a level of precision hitherto unattained. Thallium is first separated from the geological matrix using a two-stage anion-exchange procedure. Thallium isotopic compositions are then determined by multiple-collector inductively coupled plasma-mass spectrometry with correction for mass discrimination using the known isotopic composition of Pb that is admixed to the sample solutions. With these procedures we achieve a precision of 0.01-0.02% for Tl isotope ratio measurements in geological samples and this is a factor of ≥3-4 better than the best published results by TIMS. However, without adequate precautions, experimental artifacts can be generated that result in apparent Tl isotopic fractionations of up to one per mil. Analysis of five terrestrial samples indicate the existence of Tl isotopic variations related to natural fractionation processes on the Earth. Two of the three igneous rocks analyzed in this study display Tl isotopic compositions indistinguishable from our laboratory standard, the reference material NIST-997 Tl. A third sample, however, is characterized by ɛ Tl ≈ 2.5 ± 1.5, where ɛ Tl represents the deviation of the 205Tl/ 203Tl ratio of the sample relative to NIST-997 Tl in parts per 10 4. Even larger deviations were identified for two ferromanganese crusts from the Pacific Ocean, which display ɛ Tl-values of +5.0 ± 1.5 and +11.7 ± 1.3. We suggest that the large variability of Tl isotopic compositions in the latter samples are caused by low-temperature processes related to the formation of the Fe-Mn crusts by precipitation and

High Precision 142Nd/144Nd and 143Nd/144Nd Isotope Ratio Measurements in Rock Samples

Science.gov (United States)

Ali, A.; Srinivasan, G.

2009-05-01

The long-lived 147Sm-143Nd system with a half-life (T1/2) of 106 Gyr is generally used for geochronology. The short-lived 146Sm-142Nd system (T1/2= 103 Myr) is used as a geological tracer to track early (˜500 Ma) silicate differentiation [1] events in different planetary bodies. The isotope composition measurements by thermal ionization mass spectrometry (TIMS) require purification of Nd using chemical separation methods. This is important as an impure sample will give both a very poor ion yield and cause beam instability in the mass spectrometer, potentially resulting in a poor analysis [2]. The separation of Nd for 143Nd isotope measurement is, fairly straightforward because there is no isobaric interference of any other REE. While 142Nd isotope analysis needs chemically separated Nd fraction to be ˜100% Ce-free as latter is composed of a substantial amount of 142Ce isotope. A 4-steps technique, modified from Caro et al., [3], for the separation of Nd is established at the Cosmochemistry Laboratory of University of Toronto, Canada and applied to the measurement of Nd isotope ratios in geological reference sample BCR-2 (USGS, Columbia River basalt) using TIMS. Results of the isotopic ratios obtained for BCR-2 are in good agreement with published values [e.g., 4]. Analytical work on the samples discovered as the oldest rocks on Earth [5] from Nuvvuagittuq greenstone belt in Québec, Canada and various meteorites is in progress. An account of the procedures involved is briefly described here. All working solutions and acids were prepared using >18.2 MΩ.cm-1 H2O from a Milli-Q water system. Experiments were performed under Class 100 clean work bench with acid-cleaned apparatus and plastic-ware. The whole rock powders were weighed (20-30 mg) and dissolved in a mixture of HF and HNO3 using PFA vials and heated at 110°C. Further decomposition was done in Teflon bomb in the oven at 205°C. Later on contents of the Teflon bomb were transferred to vials and fluorides

Influence of sulfur-bearing polyatomic species on high precision measurements of Cu isotopic composition

Science.gov (United States)

Pribil, M.J.; Wanty, R.B.; Ridley, W.I.; Borrok, D.M.

2010-01-01

An increased interest in high precision Cu isotope ratio measurements using multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS) has developed recently for various natural geologic systems and environmental applications, these typically contain high concentrations of sulfur, particularly in the form of sulfate (SO42-) and sulfide (S). For example, Cu, Fe, and Zn concentrations in acid mine drainage (AMD) can range from 100??g/L to greater than 50mg/L with sulfur species concentrations reaching greater than 1000mg/L. Routine separation of Cu, Fe and Zn from AMD, Cu-sulfide minerals and other geological matrices usually incorporates single anion exchange resin column chromatography for metal separation. During chromatographic separation, variable breakthrough of SO42- during anion exchange resin column chromatography into the Cu fractions was observed as a function of the initial sulfur to Cu ratio, column properties, and the sample matrix. SO42- present in the Cu fraction can form a polyatomic 32S-14N-16O-1H species causing a direct mass interference with 63Cu and producing artificially light ??65Cu values. Here we report the extent of the mass interference caused by SO42- breakthrough when measuring ??65Cu on natural samples and NIST SRM 976 Cu isotope spiked with SO42- after both single anion column chromatography and double anion column chromatography. A set of five 100??g/L Cu SRM 976 samples spiked with 500mg/L SO42- resulted in an average ??65Cu of -3.50?????5.42??? following single anion column separation with variable SO42- breakthrough but an average concentration of 770??g/L. Following double anion column separation, the average SO42-concentration of 13??g/L resulted in better precision and accuracy for the measured ??65Cu value of 0.01?????0.02??? relative to the expected 0??? for SRM 976. We conclude that attention to SO42- breakthrough on sulfur-rich samples is necessary for accurate and precise measurements of ??65Cu and may require

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

Energy Technology Data Exchange (ETDEWEB)

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

2013-09-02

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

Development of precise analytical methods for strontium and lanthanide isotopic ratios using multiple collector inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Ohno, Takeshi; Takaku, Yuichi; Hisamatsu, Shun'ichi

2007-01-01

We have developed precise analytical methods for strontium and lanthanide isotopic ratios using multiple collector-ICP-mass spectrometry (MC-ICP-MS) for experimental and environmental studies of their behavior. In order to obtain precise isotopic data using MC-ICP-MS, the mass discrimination effect was corrected by an exponential law correction method. The resulting isotopic data demonstrated that highly precise isotopic analyses (better than 0.1 per mille as 2SD) could be achieved. We also adopted a de-solvating nebulizer system to improve the sensitivity. This system could minimize the water load into the plasma and provided about five times larger intensity of analyte than a conventional nebulizer system did. (author)

DeuteRater: a tool for quantifying peptide isotope precision and kinetic proteomics.

Science.gov (United States)

Naylor, Bradley C; Porter, Michael T; Wilson, Elise; Herring, Adam; Lofthouse, Spencer; Hannemann, Austin; Piccolo, Stephen R; Rockwood, Alan L; Price, John C

2017-05-15

Using mass spectrometry to measure the concentration and turnover of the individual proteins in a proteome, enables the calculation of individual synthesis and degradation rates for each protein. Software to analyze concentration is readily available, but software to analyze turnover is lacking. Data analysis workflows typically don't access the full breadth of information about instrument precision and accuracy that is present in each peptide isotopic envelope measurement. This method utilizes both isotope distribution and changes in neutromer spacing, which benefits the analysis of both concentration and turnover. We have developed a data analysis tool, DeuteRater, to measure protein turnover from metabolic D 2 O labeling. DeuteRater uses theoretical predictions for label-dependent change in isotope abundance and inter-peak (neutromer) spacing within the isotope envelope to calculate protein turnover rate. We have also used these metrics to evaluate the accuracy and precision of peptide measurements and thereby determined the optimal data acquisition parameters of different instruments, as well as the effect of data processing steps. We show that these combined measurements can be used to remove noise and increase confidence in the protein turnover measurement for each protein. Source code and ReadMe for Python 2 and 3 versions of DeuteRater are available at https://github.com/JC-Price/DeuteRater . Data is at https://chorusproject.org/pages/index.html project number 1147. Critical Intermediate calculation files provided as Tables S3 and S4. Software has only been tested on Windows machines. jcprice@chem.byu.edu. Supplementary data are available at Bioinformatics online. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please e-mail: journals.permissions@oup.com

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

Science.gov (United States)

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

2007-10-15

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

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)

Otolith oxygen isotopes measured by high-precision secondary ion mass spectrometry reflect life history of a yellowfin sole (Limanda aspera).

Science.gov (United States)

Matta, Mary Elizabeth; Orland, Ian J; Ushikubo, Takayuki; Helser, Thomas E; Black, Bryan A; Valley, John W

2013-03-30

The oxygen isotope ratio (δ(18)O value) of aragonite fish otoliths is dependent on the temperature and the δ(18)O value of the ambient water and can thus reflect the environmental history of a fish. Secondary ion mass spectrometry (SIMS) offers a spatial-resolution advantage over conventional acid-digestion techniques for stable isotope analysis of otoliths, especially given their compact nature. High-precision otolith δ(18)O analysis was conducted with an IMS-1280 ion microprobe to investigate the life history of a yellowfin sole (Limanda aspera), a Bering Sea species known to migrate ontogenetically. The otolith was cut transversely through its core and one half was roasted to eliminate organic contaminants. Values of δ(18)O were measured in 10-µm spots along three transects (two in the roasted half, one in the unroasted half) from the core toward the edge. Otolith annual growth zones were dated using the dendrochronology technique of crossdating. Measured values of δ(18)O ranged from 29.0 to 34.1‰ (relative to Vienna Standard Mean Ocean Water). Ontogenetic migration from shallow to deeper waters was reflected in generally increasing δ(18)O values from age-0 to approximately age-7 and subsequent stabilization after the expected onset of maturity at age-7. Cyclical variations of δ(18)O values within juvenile otolith growth zones, up to 3.9‰ in magnitude, were caused by a combination of seasonal changes in the temperature and the δ(18)O value of the ambient water. The ion microprobe produced a high-precision and high-resolution record of the relative environmental conditions experienced by a yellowfin sole that was consistent with population-level studies of ontogeny. Furthermore, this study represents the first time that crossdating has been used to ensure the dating accuracy of δ(18)O measurements in otoliths. Copyright © 2013 John Wiley & Sons, Ltd.

Automated gravimetric sample pretreatment using an industrial robot for the high-precision determination of plutonium by isotope dilution mass spectrometry

International Nuclear Information System (INIS)

Surugaya, Naoki; Hiyama, Toshiaki; Watahiki, Masaru

2008-01-01

A robotized sample-preparation method for the determination of Pu, which is recovered by extraction reprocessing of spent nuclear fuel, by isotope dilution mass spectrometry (IDMS) is described. The automated system uses a six-axis industrial robot, whose motility is very fast, accurate, and flexible, installed in a glove box. The automation of the weighing and dilution steps enables operator-unattended sample pretreatment for the high-precision analysis of Pu in aqueous solutions. Using the developed system, the Pu concentration in a HNO 3 medium was successfully determined using a set of subsequent mass spectrometric measurements. The relative uncertainty in determining the Pu concentration by IDMS using this system was estimated to be less than 0.1% (k=2), which is equal to that expected of a talented analysis. The operation time required was the same as that for a skilled operator. (author)

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‰.

Accurate and precise measurement of oxygen isotopic fractions and diffusion profiles by selective attenuation of secondary ions (SASI).

Science.gov (United States)

Téllez, Helena; Druce, John; Hong, Jong-Eun; Ishihara, Tatsumi; Kilner, John A

2015-03-03

The accuracy and precision of isotopic analysis in Time-of-Flight secondary ion mass spectrometry (ToF-SIMS) relies on the appropriate reduction of the dead-time and detector saturation effects, especially when analyzing species with high ion yields or present in high concentrations. Conventional approaches to avoid these problems are based on Poisson dead-time correction and/or an overall decrease of the total secondary ion intensity by reducing the target current. This ultimately leads to poor detection limits for the minor isotopes and high uncertainties of the measured isotopic ratios. An alternative strategy consists of the attenuation of those specific secondary ions that saturate the detector, providing an effective extension of the linear dynamic range. In this work, the selective attenuation of secondary ion signals (SASI) approach is applied to the study of oxygen transport properties in electroceramic materials by isotopic labeling with stable (18)O tracer and ToF-SIMS depth profiling. The better analytical performance in terms of accuracy and precision allowed a more reliable determination of the oxygen surface exchange and diffusion coefficients while maintaining good mass resolution and limits of detection for other minor secondary ion species. This improvement is especially relevant to understand the ionic transport mechanisms and properties of solid materials, such as the parallel diffusion pathways (e.g., oxygen diffusion through bulk, grain boundary, or dislocations) in electroceramic materials with relevant applications in energy storage and conversion devices.

Precise measurement of chromium isotopes by MC-ICPMS

DEFF Research Database (Denmark)

Schiller, Martin; Van Kooten, Elishevah; Holst, Jesper Christian

2014-01-01

We report novel analytical procedures allowing for the concurrent determination of the stable and mass-independent Cr isotopic composition of silicate materials by multiple collector inductively coupled mass spectrometry (MC-ICPMS). In particular, we focus on improved precision of the measurement...

High-precision determination of the isotopic composition of dissolved iron in iron depleted seawater by double spike multicollector-ICPMS.

Science.gov (United States)

Lacan, Francois; Radic, Amandine; Labatut, Marie; Jeandel, Catherine; Poitrasson, Franck; Sarthou, Geraldine; Pradoux, Catherine; Chmeleff, Jerome; Freydier, Remi

2010-09-01

This work demonstrates the feasibility of the measurement of the isotopic composition of dissolved iron in seawater for an iron concentration range, 0.05-1 nmol L(-1), allowing measurements in most oceanic waters, including Fe depleted waters of high nutrient low chlorophyll areas. It presents a detailed description of our previously published protocol, with significant improvements on detection limit and blank contribution. Iron is preconcentrated using a nitriloacetic acid superflow resin and purified using an AG 1-x4 anion exchange resin. The isotopic ratios are measured with a multicollector-inductively coupled plasma mass spectrometer (MC-ICPMS) Neptune, coupled with a desolvator (Aridus II or Apex-Q), using a (57)Fe-(58)Fe double spike mass bias correction. A Monte Carlo test shows that optimum precision is obtained for a double spike composed of approximately 50% (57)Fe and 50% (58)Fe and a sample to double spike quantity ratio of approximately 1. Total procedural yield is 91 +/- 25% (2SD, n = 55) for sample sizes from 20 to 2 L. The procedural blank ranges from 1.4 to 1.1 ng, for sample sizes ranging from 20 to 2 L, respectively, which, converted into Fe concentrations, corresponds to blank contributions of 0.001 and 0.010 nmol L(-1), respectively. Measurement precision determined from replicate measurements of seawater samples and standard solutions is 0.08 per thousand (delta(56)Fe, 2SD). The precision is sufficient to clearly detect and quantify isotopic variations in the oceans, which so far have been observed to span 2.5 per thousand and thus opens new perspectives to elucidate the oceanic iron cycle.

High precision measurements of carbon isotopic ratio of atmospheric methane using a continuous flow mass spectrometer

Directory of Open Access Journals (Sweden)

Shinji Morimoto

2009-03-01

Full Text Available A high-precision measurement system for the carbon isotope ratio of atmospheric CH4 (δ^(13CH_4 was developed using a pre-concentration device for CH4 and a gas chromatograph-combustion-isotope ratio mass spectrometer (GC-C-IRMS. The measurement system required 100 mlSTP of an atmospheric air sample, corresponding to approximately 0.18μlSTP of CH_4, to determine the δ^(13CH_4 value with a reproducibility of 0.07‰. Replicated analyses of a CH_4-in-air standard gas during the period from 2002 to 2008 indicated that the value of δ^(13CH_4 measured by this system was consistent within the measurement reproducibility. To evaluate the δ^(13CH_4 measurement system, thus developed, diurnal variations of the atmospheric CH_4 concentration and δ^(13CH_4 were observed in the northern part of the Tokyo metropolitan area. From the relationship between the CH_4 concentration and δ^(13CH_4, dominant sources of the observed CH4 fluctuations were identified.

High-precision ²⁷Al/²⁴Mg ratio determination using a modified isotope-dilution approach

DEFF Research Database (Denmark)

Paton, Chad; Schiller, Martin; Ulfbeck, David Garf

2012-01-01

saves time and minimises the risk of contamination of other samples with spike (which is added immediately prior to analysis). Repeat measurements of the BHVO-2, BCR-2, and BIR-1 international rock standards, as well as a gravimetrically prepared Al–Mg reference solution, indicate that our method......The precision of the 26Al–26Mg system—one of the most widely used chronometers for constraining the relative timing of events in the early solar system—is presently limited by methods for the determination of 27Al/24Mg ratios, which have seen little improvement in the last decade. We present...... a novel method for the measurement of 27Al/24Mg ratios in unpurified sample solutions by multiple-collector inductively coupled plasma mass spectrometry. Because Al is monoisotopic we use a modified isotope dilution approach that employs a mixed spike containing isotopically enriched 25Mg and natural 27Al...

High-resolution continuous flow analysis setup for water isotopic measurement from ice cores using laser spectroscopy

Science.gov (United States)

Emanuelsson, B. D.; Baisden, W. T.; Bertler, N. A. N.; Keller, E. D.; Gkinis, V.

2014-12-01

Here we present an experimental setup for water stable isotopes (δ18O and δD) continuous flow measurements. It is the first continuous flow laser spectroscopy system that is using Off-Axis Integrated Cavity Output Spectroscopy (OA-ICOS; analyzer manufactured by Los Gatos Research - LGR) in combination with an evaporation unit to continuously analyze sample from an ice core. A Water Vapor Isotopic Standard Source (WVISS) calibration unit, manufactured by LGR, was modified to: (1) increase the temporal resolution by reducing the response time (2) enable measurements on several water standards, and (3) to reduce the influence from memory effects. While this setup was designed for the Continuous Flow Analysis (CFA) of ice cores, it can also continuously analyze other liquid or vapor sources. The modified setup provides a shorter response time (~54 and 18 s for 2013 and 2014 setup, respectively) compared to the original WVISS unit (~62 s), which is an improvement in measurement resolution. Another improvement compared to the original WVISS is that the modified setup has a reduced memory effect. Stability tests comparing the modified WVISS and WVISS setups were performed and Allan deviations (σAllan) were calculated to determine precision at different averaging times. For the 2013 modified setup the precision after integration times of 103 s are 0.060 and 0.070‰ for δ18O and δD, respectively. For the WVISS setup the corresponding σAllan values are 0.030, 0.060 and 0.043‰ for δ18O, δD and δ17O, respectively. For the WVISS setup the precision is 0.035, 0.070 and 0.042‰ after 103 s for δ18O, δD and δ17O, respectively. Both the modified setups and WVISS setup are influenced by instrumental drift with δ18O being more drift sensitive than δD. The σAllan values for δ18O of 0.30 and 0.18‰ for the modified (2013) and WVISS setup, respectively after averaging times of 104 s (2.78 h). The Isotopic Water Analyzer (IWA)-modified WVISS setup used during the

Separation of Platinum from Palladium and Iridium in Iron Meteorites and Accurate High-Precision Determination of Platinum Isotopes by Multi-Collector ICP-MS.

Science.gov (United States)

Hunt, Alison C; Ek, Mattias; Schönbächler, Maria

2017-12-01

This study presents a new measurement procedure for the isolation of Pt from iron meteorite samples. The method also allows for the separation of Pd from the same sample aliquot. The separation entails a two-stage anion-exchange procedure. In the first stage, Pt and Pd are separated from each other and from major matrix constituents including Fe and Ni. In the second stage, Ir is reduced with ascorbic acid and eluted from the column before Pt collection. Platinum yields for the total procedure were typically 50-70%. After purification, high-precision Pt isotope determinations were performed by multi-collector ICP-MS. The precision of the new method was assessed using the IIAB iron meteorite North Chile. Replicate analyses of multiple digestions of this material yielded an intermediate precision for the measurement results of 0.73 for ε 192 Pt, 0.15 for ε 194 Pt and 0.09 for ε 196 Pt (2 standard deviations). The NIST SRM 3140 Pt solution reference material was passed through the measurement procedure and yielded an isotopic composition that is identical to the unprocessed Pt reference material. This indicates that the new technique is unbiased within the limit of the estimated uncertainties. Data for three iron meteorites support that Pt isotope variations in these samples are due to exposure to galactic cosmic rays in space.

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.

High-precision Pb isotopic measurements of teeth and environmental samples from Sofia (Bulgaria): insights for regional lead sources and possible pathways to the human body

Science.gov (United States)

Kamenov, George D.

2008-08-01

High-precision Pb isotopic measurements on teeth and possible sources in a given area can provide important insights for the lead (Pb) sources and pathways in the human body. Pb isotopic analyses on soils from the area of Sofia, Bulgaria show that Pb is contributed by three end-members represented by two natural sources and leaded gasoline. Sequential leaching experiments reveal that the alumosilicate fraction of the soils is mainly controlled by natural Pb derived from two mountain massifs bordering the city. Around 1/3 to a half of the Pb in the soil leachates, however, can be explained by contamination from leaded gasoline. Contemporary teeth from Sofia residents show very similar Pb isotopic compositions to the soil leachates, also indicating that around 1/3 to a half of the Pb can be explained by derivation from leaded gasoline. The remarkable isotopic similarities between the teeth and the most labile fractions of the local soils suggest that the lead can be derived from the latter. Pb incorporation in the human body via soil-plant-human or soil-plant-animal-human chains is unlikely due to the fact that no significant farming occurs in the city area. The isotopic compositions of the local soil labile fractions can be used as approximation of the bioaccessible lead for humans. Considering all possible scenarios it appears that soil and/or soil-born dust inhalation and/or ingestion is the most probable pathway for incorporation of local soil lead in the local population. The high-precision Pb isotope data presented in this work indicate that apparently the local soil is what plays major role in the human Pb exposure.

High-precision measurement of mercury isotope ratios in sediments using cold-vapor generation multi-collector inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Foucher, Delphine; Hintelmann, Holger

2006-01-01

An on-line Hg reduction technique using stannous chloride as the reductant was applied for accurate and precise mercury isotope ratio determinations by multi-collector (MC)-ICP/MS. Special attention has been paid to ensure optimal conditions (such as acquisition time and mercury concentration) allowing precision measurements good enough to be able to significantly detect the anticipated small differences in Hg isotope ratios in nature. Typically, internal precision was better than 0.002% (1 RSE) on all Hg ratios investigated as long as approximately 20 ng of Hg was measured with a 10-min acquisition time. Introducing higher amounts of mercury (50 ng Hg) improved the internal precision to 205 Tl/ 203 Tl correction coupled to a standard-sample bracketing approach. The large number of data acquired allowed us to validate the consistency of our measurements over a one-year period. On average, the short-term uncertainty determined by repeated runs of NIST SRM 1641d Hg standard during a single day was 202 Hg/ 198 Hg, 202 Hg/ 199 Hg, 202 Hg/ 200 Hg, and 202 Hg/ 201 Hg). The precision fell to 202 Hg/ 198 Hg expressed as δ values (per mil deviations relative to NIST SRM 1641d Hg standard solution) displayed differences from +0.74 to -4.00 permille. The magnitude of the Hg fractionation per amu was constant within one type of sample and did not exceed 1.00 permille. Considering all results (the reproducibility of Hg standard solutions, reference sediment samples, and the examination of natural samples), the analytical error of our δ values for the overall method was within ±0.28 permille (1 SD), which was an order of magnitude lower than the extent of fractionation (4.74 permille) observed in sediments. This study confirmed that analytical techniques have reached a level of long-term precision and accuracy that is sufficiently sensitive to detect even small differences in Hg isotope ratios that occur within one type of samples (e.g., between different sediments) and so

High-precision dual-inlet IRMS measurements of the stable isotopes of CO2 and the N2O / CO2 ratio from polar ice core samples

Directory of Open Access Journals (Sweden)

T. K. Bauska

2014-11-01

Full Text Available An important constraint on mechanisms of past carbon cycle variability is provided by the stable isotopic composition of carbon in atmospheric carbon dioxide (δ13C-CO2 trapped in polar ice cores, but obtaining very precise measurements has proven to be a significant analytical challenge. Here we describe a new technique to determine the δ13C of CO2 at very high precision, as well as measuring the CO2 and N2O mixing ratios. In this method, ancient air is extracted from relatively large ice samples (~400 g with a dry-extraction "ice grater" device. The liberated air is cryogenically purified to a CO2 and N2O mixture and analyzed with a microvolume-equipped dual-inlet IRMS (Thermo MAT 253. The reproducibility of the method, based on replicate analysis of ice core samples, is 0.02‰ for δ13C-CO2 and 2 ppm and 4 ppb for the CO2 and N2O mixing ratios, respectively (1σ pooled standard deviation. Our experiments show that minimizing water vapor pressure in the extraction vessel by housing the grating apparatus in a ultralow-temperature freezer (−60 °C improves the precision and decreases the experimental blank of the method to −0.07 ± 0.04‰. We describe techniques for accurate calibration of small samples and the application of a mass-spectrometric method based on source fragmentation for reconstructing the N2O history of the atmosphere. The oxygen isotopic composition of CO2 is also investigated, confirming previous observations of oxygen exchange between gaseous CO2 and solid H2O within the ice archive. These data offer a possible constraint on oxygen isotopic fractionation during H2O and CO2 exchange below the H2O bulk melting temperature.

Evaluation of precision in measurements of uranium isotope ratio by thermionic mass spectrometry

International Nuclear Information System (INIS)

Moraes, N.M.P. de; Rodrigues, C.

1977-01-01

The parameters which affect the precision and accuracy of uranium isotopic ratios measurements by thermionic mass spectrometry are discussed. A statistical designed program for the analysis of the internal and external variances are presented. It was done an application of this statistical methods, in order to get mass discrimination factor, and its standard mean deviation, by using some results already published for 235 U/ 238 U ratio in NBS uranium samples, and natural uranium [pt

Real-time analysis of δ13C- and δD-CH4 by high precision laser spectroscopy

Science.gov (United States)

Eyer, Simon; Emmenegger, Lukas; Tuzson, Béla; Fischer, Hubertus; Mohn, Joachim

2014-05-01

Methane (CH4) is the most important non-CO2 greenhouse gas (GHG) contributing 18% to total radiative forcing. Anthropogenic sources (e.g. ruminants, landfills) contribute 60% to total emissions and led to an increase in its atmospheric mixing ratio from 700 ppb in pre-industrial times to 1819 ± 1 ppb in 2012 [1]. Analysis of the most abundant methane isotopologues 12CH4, 13CH4 and 12CH3D can be used to disentangle the various source/sink processes [2] and to develop target oriented reduction strategies. High precision isotopic analysis of CH4 can be accomplished by isotope-ratio mass-spectrometry (IRMS) [2] and more recently by mid-infrared laser-based spectroscopic techniques. For high precision measurements in ambient air, however, both techniques rely on preconcentration of the target gas [3]. In an on-going project, we developed a fully-automated, field-deployable CH4 preconcentration unit coupled to a dual quantum cascade laser absorption spectrometer (QCLAS) for real-time analysis of CH4 isotopologues. The core part of the rack-mounted (19 inch) device is a highly-efficient adsorbent trap attached to a motorized linear drive system and enclosed in a vacuum chamber. Thereby, the adsorbent trap can be decoupled from the Stirling cooler during desorption for fast desorption and optimal heat management. A wide variety of adsorbents, including: HayeSep D, molecular sieves as well as the novel metal-organic frameworks and carbon nanotubes were characterized regarding their surface area, isosteric enthalpy of adsorption and selectivity for methane over nitrogen. The most promising candidates were tested on the preconcentration device and a preconcentration by a factor > 500 was obtained. Furthermore analytical interferants (e.g. N2O, CO2) are separated by step-wise desorption of trace gases. A QCL absorption spectrometer previously described by Tuzson et al. (2010) for CH4 flux measurements was modified to obtain a platform for high precision and simultaneous

High-Precision Half-Life Measurements for the Superallowed Fermi β+ Emitters 14O and 18Ne

Science.gov (United States)

Laffoley, A. T.; Andreoiu, C.; Austin, R. A. E.; Ball, G. C.; Bender, P. C.; Bidaman, H.; Bildstein, V.; Blank, B.; Bouzomita, H.; Cross, D. S.; Deng, G.; Diaz Varela, A.; Dunlop, M. R.; Dunlop, R.; Finlay, P.; Garnsworthy, A. B.; Garrett, P.; Giovinazzo, J.; Grinyer, G. F.; Grinyer, J.; Hadinia, B.; Jamieson, D. S.; Jigmeddorj, B.; Ketelhut, S.; Kisliuk, D.; Leach, K. G.; Leslie, J. R.; MacLean, A.; Miller, D.; Mills, B.; Moukaddam, M.; Radich, A. J.; Rajabali, M. M.; Rand, E. T.; Svensson, C. E.; Tardiff, E.; Thomas, J. C.; Turko, J.; Voss, P.; Unsworth, C.

High-precision half-life measurements, at the level of ±0.04%, for the superallowed Fermi emitters 14O and 18Ne have been performed at TRIUMF's Isotope Separator and Accelerator facility. Using 3 independent detector systems, a gas-proportional counter, a fast plastic scintillator, and a high-purity germanium array, a series of direct β and γ counting measurements were performed for each of the isotopes. In the case of 14O, these measurements were made to help resolve an existing discrepancy between detection methods, whereas for 18Ne the half-life precision has been improved in anticipation of forthcoming high-precision branching ratio measurements.

Calibrated high-precision 17O-excess measurements using cavity ring-down spectroscopy with laser-current-tuned cavity resonance

Directory of Open Access Journals (Sweden)

E. J. Steig

2014-08-01

Full Text Available High-precision analysis of the 17O / 16O isotope ratio in water and water vapor is of interest in hydrological, paleoclimate, and atmospheric science applications. Of specific interest is the parameter 17O excess (Δ17O, a measure of the deviation from a~linear relationship between 17O / 16O and 18O / 16O ratios. Conventional analyses of Δ17O of water are obtained by fluorination of H2O to O2 that is analyzed by dual-inlet isotope ratio mass spectrometry (IRMS. We describe a new laser spectroscopy instrument for high-precision Δ17O measurements. The new instrument uses cavity ring-down spectroscopy (CRDS with laser-current-tuned cavity resonance to achieve reduced measurement drift compared with previous-generation instruments. Liquid water and water-vapor samples can be analyzed with a better than 8 per meg precision for Δ17O using integration times of less than 30 min. Calibration with respect to accepted water standards demonstrates that both the precision and the accuracy of Δ17O are competitive with conventional IRMS methods. The new instrument also achieves simultaneous analysis of δ18O, Δ17O and δD with precision of < 0.03‰, < 0.02 and < 0.2‰, respectively, based on repeated calibrated measurements.

ICP magnetic sector multiple collector mass spectrometry and the precise measurement of isotopic compositions using nebulization of solutions and laser ablation of solids

International Nuclear Information System (INIS)

Halliday, A.N.; Lee, D-C.; Christensen, J.N.; Yi, W.; Hall, C.M.; Jones, C.E.; Teagle, D.A.H.; Freedman, P.A.

1996-01-01

Inductively-coupled plasma (ICP) sources offer considerable advantages over thermal sources because the high ionization efficiency facilitates measurements of relatively high sensitivity for elements such as Hf or Sn, which can be difficult to measure precisely with thermal ionization mass spectrometry (TIMS). The mass discrimination (bias) is larger than for TIMS, favours the heavier ions, and decreases in magnitude with increasing mass. However, in contrast to TIMS, this discrimination is largely independent of the chemical or physical properties of the element or the duration of the analysis. This has been demonstrated to high precision with a double focussing multiple collector magnetic sector mass spectrometer with an ICP source. The principle of this instrument is briefly described. The potential of the instrument for high precision isotopic measurements of a very broad range of elements, using solution aspiration or laser ablation, is indicated. 15 refs

Pb and Sr isotope measurements by inductively coupled plasma mass spectrometer: efficient time management for precision improvement

Science.gov (United States)

Monna, F.; Loizeau, J.-L.; Thomas, B. A.; Guéguen, C.; Favarger, P.-Y.

1998-08-01

One of the factors limiting the precision of inductively coupled plasma mass spectrometry is the counting statistics, which depend upon acquisition time and ion fluxes. In the present study, the precision of the isotopic measurements of Pb and Sr is examined. The time of measurement is optimally shared for each isotope, using a mathematical simulation, to provide the lowest theoretical analytical error. Different algorithms of mass bias correction are also taken into account and evaluated in term of improvement of overall precision. Several experiments allow a comparison of real conditions with theory. The present method significantly improves the precision, regardless of the instrument used. However, this benefit is more important for equipment which originally yields a precision close to that predicted by counting statistics. Additionally, the procedure is flexible enough to be easily adapted to other problems, such as isotopic dilution.

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

International Nuclear Information System (INIS)

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

2007-01-01

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

Numerical Simulation Analysis of High-precision Dispensing Needles for Solid-liquid Two-phase Grinding

Science.gov (United States)

Li, Junye; Hu, Jinglei; Wang, Binyu; Sheng, Liang; Zhang, Xinming

2018-03-01

In order to investigate the effect of abrasive flow polishing surface variable diameter pipe parts, with high precision dispensing needles as the research object, the numerical simulation of the process of polishing high precision dispensing needle was carried out. Analysis of different volume fraction conditions, the distribution of the dynamic pressure and the turbulence viscosity of the abrasive flow field in the high precision dispensing needle, through comparative analysis, the effectiveness of the abrasive grain polishing high precision dispensing needle was studied, controlling the volume fraction of silicon carbide can change the viscosity characteristics of the abrasive flow during the polishing process, so that the polishing quality of the abrasive grains can be controlled.

Can EC and UK national methane emission inventories be verified using high precision stable isotope data?

International Nuclear Information System (INIS)

Lowry, D.; Holmes, C.W.; Nisbet, E.G.; Rata, N.D.

2002-01-01

The main anthropogenic sources of methane in industrialised countries (landfill/waste treatment, gas storage and distribution, coal) are far easier to reduce than CO 2 sources and the implementation of reduction strategies is potentially profitable. Statistical databases of methane emissions need independent external verification and carbon isotope data provide one way of estimating the expected source mix for each country if the main source types have been characterised isotopically. Using this method each country participating in the CORINAIR 94 database has been assigned an expected isotopic value for its emissions. The averaged δ 13 C of methane emitted from the CORINAIR region of Europe, based on total emissions of each country is -55.4 per mille for 1994. This European source mix can be verified using trajectory analysis for air samples collected at background stations. Methane emissions from the UK, and particularly the London region, have undergone more detailed analysis using data collected at the Royal Holloway site on the western fringe of London. If the latest emissions inventory figures are correct then the modelled isotopic change in the UK source mix is from -48.4 per mille in 1990 to -50.7 per mille in 1997. This represents a reduction in emissions of 25% over a 7-year period, important in meeting proposed UK greenhouse gas reduction targets. These changes can be tested by the isotopic analysis of air samples at carefully selected coastal background and interior sites. Regular sampling and isotopic analysis coupled with back trajectory analysis from a range of sites could provide an important tool for monitoring and verification of EC and UK methane emissions in the run-up to 2010. (author)

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

Science.gov (United States)

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

2013-09-02

The study of Fe, Zn and Cd stable isotopes (δ(56)Fe, δ(66)Zn and δ(114)Cd) in seawater is a new field, which promises to elucidate the marine cycling of these bioactive trace metals. However, the analytical challenges posed by the low concentration of these metals in seawater has meant that previous studies have typically required large sample volumes, highly limiting data collection in the oceans. Here, we present the first simultaneous method for the determination of these three isotope systems in seawater, using Nobias PA-1 chelating resin to extract metals from seawater, purification by anion exchange chromatography, and analysis by double spike MC-ICPMS. This method is designed for use on only a single litre of seawater and has blanks of 0.3, 0.06 and <0.03 ng for Fe, Zn and Cd respectively, representing a 1-20 fold reduction in sample size and a 4-130 decrease in blank compared to previously reported methods. The procedure yields data with high precision for all three elements (typically 0.02-0.2‰; 1σ internal precision), allowing us to distinguish natural variability in the oceans, which spans 1-3‰ for all three isotope systems. Simultaneous extraction and purification of three metals makes this method ideal for high-resolution, large-scale endeavours such as the GEOTRACES program. Copyright © 2013 Elsevier B.V. All rights reserved.

A fast isotope switching system for high energy ions

International Nuclear Information System (INIS)

Niklaus, T.R.; Sie, S.H.; Suter, G.F.

1998-01-01

A fast bouncing system for the high energy end of an Accelerator Mass Spectrometry system has been devised for the AUSTRALIS at the CSIRO HIAF laboratory. Based on a method designed for excitation function measurements, it has been adapted as an isotope sequencer for AMS at the high energy side. In this scheme, different isotopes of the same energy are deflected off axis in the orbit plane by varying amounts at the entrance to the magnet and returned to the main axis at the exit by another deflection of the same magnitude in the same plane. Synchronised with the low energy side bouncer, the system will enable isotope ratios measurements with high precision by overcoming drifts in the source, beam transport and the accelerator itself

A continuous flow isotope ratio mass spectrometry method for high precision determination of dissolved gas ratios and isotopic composition

DEFF Research Database (Denmark)

Charoenpong, C. N.; Bristow, L. A.; Altabet, M. A.

2014-01-01

ratio mass spectrometer (IRMS). A continuous flow of He carrier gas completely degasses the sample, and passes through the preparation and purification system before entering the IRMS for analysis. The use of this continuous He carrier permits short analysis times (less than 8 min per sample......) as compared with current high-precision methods. In addition to reference gases, calibration is achieved using air-equilibrated water standards of known temperature and salinity. Assessment of reference gas injections, air equilibrated standards, as well as samples collected in the field shows the accuracy...

Uranium Isotopic Analysis with the FRAM Isotopic Analysis Code

International Nuclear Information System (INIS)

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

1999-01-01

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

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

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

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

International Nuclear Information System (INIS)

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

1981-09-01

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

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.

Stable oxygen and hydrogen isotopes of brines - comparing isotope ratio mass spectrometry and isotope ratio infrared spectroscopy

Science.gov (United States)

Ahrens, Christian; Koeniger, Paul; van Geldern, Robert; Stadler, Susanne

2013-04-01

Today's standard analytical methods for high precision stable isotope analysis of fluids are gas-water equilibration and high temperature pyrolysis coupled to isotope ratio mass spectrometers (IRMS). In recent years, relatively new laser-based analytical instruments entered the market that are said to allow high isotope precision data on nearly every media. This optical technique is referred to as isotope ratio infrared spectroscopy (IRIS). The objective of this study is to evaluate the capability of this new instrument type for highly saline solutions and a comparison of the analytical results with traditional IRMS analysis. It has been shown for the equilibration method that the presence of salts influences the measured isotope values depending on the salt concentration (see Lécuyer et al, 2009; Martineau, 2012). This so-called 'isotope salt effect' depends on the salt type and salt concentration. These factors change the activity in the fluid and therefore shift the isotope ratios measured by the equilibration method. Consequently, correction factors have to be applied to these analytical data. Direct conversion techniques like pyrolysis or the new laser instruments allow the measurement of the water molecule from the sample directly and should therefore not suffer from the salt effect, i.e. no corrections of raw values are necessary. However, due to high salt concentrations this might cause technical problems with the analytical hardware and may require labor-intensive sample preparation (e.g. vacuum distillation). This study evaluates the salt isotope effect for the IRMS equilibration technique (Thermo Gasbench II coupled to Delta Plus XP) and the laser-based IRIS instruments with liquid injection (Picarro L2120-i). Synthetic salt solutions (NaCl, KCl, CaCl2, MgCl2, MgSO4, CaSO4) and natural brines collected from the Stassfurt Salt Anticline (Germany; Stadler et al., 2012) were analysed with both techniques. Salt concentrations ranged from seawater salinity

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

Precise isotope ratio and multielement determination in prehistoric and historic human skeletal remains by HR-ICPMS - a novel application to shed light onto anthropological and archaeological questions

International Nuclear Information System (INIS)

Watkins, M.

2000-12-01

The primary aim of the presented work was the analytical setup for fast (including high sample throughput for statistical evaluation), precise and accurate measurement of strontium isotope ratios using HR-ICPMS (high-resolution inductively coupled plasma mass spectrometry) and their application to ancient human skeletal remains from different localities for the reconstruction of migration processes. Soils and plants are in isotopic equilibrium with local source rock and show therefore the same isotopic ratios for strontium (87Sr/86Sr). Dietary strontium incorporation varies for different body materials (teeth, muscle, bone, etc.) and repository periods depend on the different strontium turnover rates. Accordingly, strontium isotope analysis can provide important data for studying human or animal migration and mobility. An important issue will be addressed: the problem of strontium isotope ratio measurement reliability and the problem of post-mortem alterations. Thus a basic part of this interdisciplinary project is dealing with the systematic evaluation of diagenetic changes of the microstructure in human bone samples - including sample uptake and preparation. Different invasive histological techniques will be applied for further clarification. Newly developed chemical methods give us the opportunity to obtain details on ancient population mobility also in skeletal series of extreme fragmentary character, which usually restricts the macro-morphological approach. Since it is evident that strontium in teeth is only incorporated during childhood whereas strontium uptake in bones is constant, an intra-individual comparison of bone and teeth samples will answer the question whether teeth are indeed 'archives of the childhood'. The introduction of an analytical system allowing online matrix separation by High Performance Ion Chromatography (HPIC) and subsequent measurement of strontium isotope ratios by means of HR-ICPMS is presented, optimized and established as method

Precise Isotope ratio and multielement determination in prehistoric and historic human skeletal remains by HR-ICPMS - a novel application to shed light onto anthropological and archaeological questions

International Nuclear Information System (INIS)

Watkins, M.

2000-12-01

The primary aim of the presented work was the analytical setup for fast (including high sample throughput for statistical evaluation), precise and accurate measurement of strontium isotope ratios using HR-ICPMS (high-resolution inductively coupled plasma mass spectrometry) and their application to ancient human skeletal remains from different localities for the reconstruction of migration processes. Soils and plants are in isotopic equilibrium with local source rock and show therefore the same isotopic ratios for strontium (87Sr/86Sr). Dietary strontium incorporation varies for different body materials (teeth, muscle, bone, etc.) and repository periods depend on the different strontium turnover rates. Accordingly, strontium isotope analysis can provide important data for studying human or animal migration and mobility. An important issue will be addressed: the problem of strontium isotope ratio measurement reliability and the problem of post-mortem alterations. Thus a basic part of this interdisciplinary project is dealing with the systematic evaluation of diagenetic changes of the microstructure in human bone samples - including sample uptake and preparation. Different invasive histological techniques will be applied for further clarification. Newly developed chemical methods give us the opportunity to obtain details on ancient population mobility also in skeletal series of extreme fragmentary character, which usually restricts the macro-morphological approach. Since it is evident that strontium in teeth is only incorporated during childhood whereas strontium uptake in bones is constant, an intra-individual comparison of bone and teeth samples will answer the question whether teeth are indeed 'archives of the childhood'. The introduction of an analytical system allowing online matrix separation by High Performance Ion Chromatography (HPIC) and subsequent measurement of strontium isotope ratios by means of HR-ICPMS is presented, optimized and established as method

Fully automatic and precise data analysis developed for time-of-flight mass spectrometry.

Science.gov (United States)

Meyer, Stefan; Riedo, Andreas; Neuland, Maike B; Tulej, Marek; Wurz, Peter

2017-09-01

Scientific objectives of current and future space missions are focused on the investigation of the origin and evolution of the solar system with the particular emphasis on habitability and signatures of past and present life. For in situ measurements of the chemical composition of solid samples on planetary surfaces, the neutral atmospheric gas and the thermal plasma of planetary atmospheres, the application of mass spectrometers making use of time-of-flight mass analysers is a technique widely used. However, such investigations imply measurements with good statistics and, thus, a large amount of data to be analysed. Therefore, faster and especially robust automated data analysis with enhanced accuracy is required. In this contribution, an automatic data analysis software, which allows fast and precise quantitative data analysis of time-of-flight mass spectrometric data, is presented and discussed in detail. A crucial part of this software is a robust and fast peak finding algorithm with a consecutive numerical integration method allowing precise data analysis. We tested our analysis software with data from different time-of-flight mass spectrometers and different measurement campaigns thereof. The quantitative analysis of isotopes, using automatic data analysis, yields results with an accuracy of isotope ratios up to 100 ppm for a signal-to-noise ratio (SNR) of 10 4 . We show that the accuracy of isotope ratios is in fact proportional to SNR -1 . Furthermore, we observe that the accuracy of isotope ratios is inversely proportional to the mass resolution. Additionally, we show that the accuracy of isotope ratios is depending on the sample width T s by T s 0.5 . Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

High-precision lead isotope ratio measurement by inductively coupled plasma multiple collector mass spectrometry

International Nuclear Information System (INIS)

Walder, A.J.; Furuta, Naoki.

1993-01-01

An inductively coupled plasma (ICP) ion source coupled to a magnetic sector mass analyser equipped with seven Faraday detectors has been used to measure the lead isotope ratios in solutions of Sanshiro Pond sediment collected at the University of Tokyo, airborne particulates collected at Shinjuku in Tokyo and Merck multielement standard product number 97279494. A thallium correction technique was utilized to allow a simultaneous correction for mass bias. This work followed an earlier interlaboratory comparison study of the above-mentioned solutions using ICP quadrupole mass spectrometry, and has demonstrated a considerable improvement in analytical precision. The following isotope ratio measurements were recorded. Pond sediment solution containing 82 ng ml -1 lead: 206 Pb/ 204 Pb=17.762±0.014; 206 Pb/ 207 Pb=1.1424±0.0009; 208 Pb/ 204 Pb=37.678±0.034. Airborne particulate solution containing 45 ng ml -1 lead: 206 Pb/ 204 Pb=17.969±0.006; 206 Pb/ 207 Pb=1.1528±0.0003; 208 Pb/ 204 Pb=37.915±0.021. Merck multielement standard solution containing 100 ng ml -1 lead: 206 Pb/ 204 Pb=19.255±0.015; 206 Pb/ 207 Pb=1.2238±0.0004; 208 Pb/ 204 Pb=38.476±0.021 (All errors are given as ±2 standard deviations). (author)

Precision Isotope Shift Measurements in Calcium Ions Using Quantum Logic Detection Schemes.

Science.gov (United States)

Gebert, Florian; Wan, Yong; Wolf, Fabian; Angstmann, Christopher N; Berengut, Julian C; Schmidt, Piet O

2015-07-31

We demonstrate an efficient high-precision optical spectroscopy technique for single trapped ions with nonclosed transitions. In a double-shelving technique, the absorption of a single photon is first amplified to several phonons of a normal motional mode shared with a cotrapped cooling ion of a different species, before being further amplified to thousands of fluorescence photons emitted by the cooling ion using the standard electron shelving technique. We employ this extension of the photon recoil spectroscopy technique to perform the first high precision absolute frequency measurement of the 2D(3/2)→2P(1/2) transition in calcium, resulting in a transition frequency of f=346 000 234 867(96)  kHz. Furthermore, we determine the isotope shift of this transition and the 2S(1/2)→2P(1/2) transition for 42Ca+, 44Ca+, and 48Ca+ ions relative to 40Ca+ with an accuracy below 100 kHz. Improved field and mass shift constants of these transitions as well as changes in mean square nuclear charge radii are extracted from this high resolution data.

Precision mass measurements of neutron-rich Co isotopes beyond N =40

Science.gov (United States)

Izzo, C.; Bollen, G.; Brodeur, M.; Eibach, M.; Gulyuz, K.; Holt, J. D.; Kelly, J. M.; Redshaw, M.; Ringle, R.; Sandler, R.; Schwarz, S.; Stroberg, S. R.; Sumithrarachchi, C. S.; Valverde, A. A.; Villari, A. C. C.

2018-01-01

The region near Z =28 and N =40 is a subject of great interest for nuclear structure studies due to spectroscopic signatures in 68Ni suggesting a subshell closure at N =40 . Trends in nuclear masses and their derivatives provide a complementary approach to shell structure investigations via separation energies. Penning trap mass spectrometry has provided precise measurements for a number of nuclei in this region; however, a complete picture of the mass surfaces has so far been limited by the large uncertainty remaining for nuclei with N >40 along the iron (Z =26 ) and cobalt (Z =27 ) chains because these species are not available from traditional isotope separator online rare isotope facilities. The Low-Energy Beam and Ion Trap Facility at the National Superconducting Cyclotron Laboratory is the first and only Penning trap mass spectrometer coupled to a fragmentation facility and therefore presents the unique opportunity to perform precise mass measurements of these elusive isotopes. Here we present the first Penning trap measurements of Co,6968, carried out at this facility. Some ambiguity remains as to whether the measured values are ground-state or isomeric-state masses. A detailed discussion is presented to evaluate this question and to motivate future work. In addition, we perform ab initio calculations of ground-state and two-neutron separation energies of cobalt isotopes with the valence-space in-medium similarity renormalization group approach based on a particular set of two- and three-nucleon forces that predict saturation in infinite matter. We discuss the importance of these measurements and calculations for understanding the evolution of nuclear structure near 68Ni.

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.

High precision measurement by mass spectrometry of isotopic ratios δ13C and δ18O of carbon dioxide

International Nuclear Information System (INIS)

Bourg, Chr.; Ciais, Ph.

1998-02-01

Carbon dioxide (CO 2 ) is the second natural greenhouse gas in the Earth's atmosphere, after vapor water. Its concentration levels have been increasing by 25% due to human activities over the past 200 years, thus increasing the radiative forcing at the surface and potentially including major climate change for the next centuries. It is of primary importance to better quantify the role of carbon contained into the oceans and the land biota in moderating the anthropic perturbation. To do so, 13 C and 18 O isotopes are unique tools which allow to estimate indirectly the terrestrial CO 2 fluxes based on atmospheric measurements. The present reports describes the experimental set-up used at the CFR-LMCE laboratory to measure the 13 C and 18 O natural abundance in atmospheric carbon dioxide. This technique requires high levels of both precision and accuracy because the geochemical signal nevertheless consists of very small changes in isotopic composition (on the order of 0.01 permits). Also, given the large number of samples to analyses routinely, it must be run in an automatic mode. Our experiment design consists of 'extraction line' where CO 2 is separated cryogenically from the air, which is coupled to a (Finnigan MAT 252) mass spectrometer. (authors)

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

BEAMGAA. A chance for high precision analysis of big samples

International Nuclear Information System (INIS)

Goerner, W.; Berger, A.; Haase, O.; Segebade, Chr.; Alber, D.; Monse, G.

2005-01-01

In activation analysis of traces in small samples, the non-equivalence of the activating radiation doses of sample and calibration material gives rise to sometimes tolerable systematic errors. Conversely, analysis of major components usually demands high trueness and precision. To meet this, beam geometry activation analysis (BEAMGAA) procedures have been developed for instrumental photon (IPAA) and neutron activation analysis (INAA) in which the activating neutron/photon beam exhibits broad, flat-topped characteristics. This results in a very low lateral activating flux gradient compared to known radiation facilities, however, at significantly lower flux density. The axial flux gradient can be accounted for by a monitor-sample-monitor assembly. As a first approach, major components were determined in high purity substances as well as selenium in a cattle fodder additive. (author)

Precision mass measurements of very short-lived, neutron-rich Na isotopes using a radiofrequency spectrometer

CERN Document Server

Lunney, M D; Doubre, H; Henry, S; Monsanglant, C; De Saint-Simon, M; Thibault, C; Toader, C F; Borcea, C; Bollen, G

2001-01-01

Mass measurements of high precision have been performed on sodium isotopes out to $^{30}$Na using a new technique of radiofrequency excitation of ion trajectories in a homogeneous magnetic field. This method, especially suited to very short-lived nuclides, has allowed us to significantly reduce the uncertainty in mass of the most exotic Na isotopes: a relative error of 5x10$^{-7}$ was achieved for $^{28}$Na having a half-life of only 30.5 ms and 9x10$^{-7}$ for the weakly produced $^{30}$Na. Verifying and minimizing binding energy uncertainties in this region of the nuclear chart is important for clarification of a long standing problem concerning the strength of the $N$=20 magic shell closure. These results are the fruit of the commissioning of the new experimental program Mistral.

Further development of IDGS: Isotope dilution gamma-ray spectrometry

International Nuclear Information System (INIS)

Li, T.K.; Parker, J.L.; Kuno, Y.; Sato, S.; Kamata, M.; Akiyama, T.

1991-01-01

The isotope dilution gamma-ray spectrometry (IDGS) technique for determining the plutonium concentration and isotopic composition of highly radioactive spent-fuel dissolver solutions has been further developed. Both the sample preparation and the analysis have been improved. The plutonium isotopic analysis is based on high-resolution, low-energy gamma-ray spectrometry. The plutonium concentration in the dissolver solutions then is calculated from the measured isotopic differences among the spike, the dissolver solution, and the spiked dissolver solution. Plutonium concentrations and isotopic compositions of dissolver solutions analyzed from this study agree well with those obtained by traditional isotope dilution mass spectrometry (IDMS) and are consistent with the first IDGS experimental result. With the current detector efficiency, sample size, and a 100-min count time, the estimated precision is ∼0.5% for 239 Pu and 240 Pu isotopic analyses and ∼1% for the plutonium concentration analysis. 5 refs., 2 figs., 7 tabs

Potassium Stable Isotopic Compositions Measured by High-Resolution MC-ICP-MS

Science.gov (United States)

Morgan, Leah E.; Lloyd, Nicholas S.; Ellam, Robert M.; Simon, Justin I.

2012-01-01

Potassium isotopic (K-41/K-39) compositions are notoriously difficult to measure. TIMS measurements are hindered by variable fractionation patterns throughout individual runs and too few isotopes to apply an internal spike method for instrumental mass fractionation corrections. Internal fractionation corrections via the K-40/K-39 ratio can provide precise values but assume identical K-40/K-39 ratios (e.g. 0.05% (1sigma) in [1]); this is appropriate in some cases (e.g. identifying excess K-41) but not others (e.g., determining mass fractionation effects and metrologically traceable isotopic abundances). SIMS analyses have yielded measurements with 0.25% precisions (1sigma) [2]. ICP-MS analyses are significantly affected by interferences from molecular species such as Ar-38H(+) and Ar-40H(+) and instrument mass bias. Single collector ICP-MS instruments in "cold plasma" mode have yielded uncertainties as low as 2% (1sigma, e.g. [3]). Although these precisions may be acceptable for some concentration determinations, they do not resolve isotopic variation in terrestrial materials. Here we present data from a series of measurements made on the Thermo Scientific NEPTUNE Plus multi-collector ICP-MS that demonstrate the ability to make K-41/K-39 ratio measurements with 0.07% precisions (1sigma). These data, collected on NIST K standards, indicate the potential for MC-ICP-MS measurements to look for K isotopic variations at the sub-permil level. The NEPTUNE Plus can sufficiently resolve 39K and 41K from the interfering 38ArH+ and 40ArH+ peaks in wet cold plasma and high-resolution mode. Measurements were made on small but flat, interference-free, plateaus (ca. 50 ppm by mass width for K-41). Although ICP-MS does not yield accurate K-41/K-39 values due to significant instrumental mass fractionation (ca. 6%), this bias can be sufficiently stable over the time required for several measurements so that relative K-41/K-39 values can be precisely determined via sample

High-precision 41K/39K measurements by MC-ICP-MS indicate terrestrial variability of δ41K

Science.gov (United States)

Morgan, Leah; Santiago Ramos, Danielle P.; Davidheiser-Kroll, Brett; Faithfull, John; Lloyd, Nicholas S.; Ellam, Rob M.; Higgins, John A.

2018-01-01

Potassium is a major component in continental crust, the fourth-most abundant cation in seawater, and a key element in biological processes. Until recently, difficulties with existing analytical techniques hindered our ability to identify natural isotopic variability of potassium isotopes in terrestrial materials. However, measurement precision has greatly improved and a range of K isotopic compositions has now been demonstrated in natural samples. In this study, we present a new technique for high-precision measurement of K isotopic ratios using high-resolution, cold plasma multi-collector mass spectrometry. We apply this technique to demonstrate natural variability in the ratio of 41K to 39K in a diverse group of geological and biological samples, including silicate and evaporite minerals, seawater, and plant and animal tissues. The total range in 41K/39K ratios is ca. 2.6‰, with a long-term external reproducibility of 0.17‰ (2, N=108). Seawater and seawater-derived evaporite minerals are systematically enriched in 41K compared to silicate minerals by ca. 0.6‰, a result consistent with recent findings1, 2. Although our average bulk-silicate Earth value (-0.54‰) is indistinguishable from previously published values, we find systematic δ41K variability in some high-temperature sample suites, particularly those with evidence for the presence of fluids. The δ41K values of biological samples span a range of ca. 1.2‰ between terrestrial mammals, plants, and marine organisms. Implications of terrestrial K isotope variability for the atomic weight of K and K-based geochronology are discussed. Our results indicate that high-precision measurements of stable K isotopes, made using commercially available mass spectrometers, can provide unique insights into the chemistry of potassium in geological and biological systems. 

Automated Sample Preparation for Radiogenic and Non-Traditional Metal Isotopes: Removing an Analytical Barrier for High Sample Throughput

Science.gov (United States)

Field, M. Paul; Romaniello, Stephen; Gordon, Gwyneth W.; Anbar, Ariel D.; Herrmann, Achim; Martinez-Boti, Miguel A.; Anagnostou, Eleni; Foster, Gavin L.

2014-05-01

MC-ICP-MS has dramatically improved the analytical throughput for high-precision radiogenic and non-traditional isotope ratio measurements, compared to TIMS. The generation of large data sets, however, remains hampered by tedious manual drip chromatography required for sample purification. A new, automated chromatography system reduces the laboratory bottle neck and expands the utility of high-precision isotope analyses in applications where large data sets are required: geochemistry, forensic anthropology, nuclear forensics, medical research and food authentication. We have developed protocols to automate ion exchange purification for several isotopic systems (B, Ca, Fe, Cu, Zn, Sr, Cd, Pb and U) using the new prepFAST-MC™ (ESI, Nebraska, Omaha). The system is not only inert (all-flouropolymer flow paths), but is also very flexible and can easily facilitate different resins, samples, and reagent types. When programmed, precise and accurate user defined volumes and flow rates are implemented to automatically load samples, wash the column, condition the column and elute fractions. Unattended, the automated, low-pressure ion exchange chromatography system can process up to 60 samples overnight. Excellent reproducibility, reliability, recovery, with low blank and carry over for samples in a variety of different matrices, have been demonstrated to give accurate and precise isotopic ratios within analytical error for several isotopic systems (B, Ca, Fe, Cu, Zn, Sr, Cd, Pb and U). This illustrates the potential of the new prepFAST-MC™ (ESI, Nebraska, Omaha) as a powerful tool in radiogenic and non-traditional isotope research.

A simplified method for obtaining high-purity perchlorate from groundwater for isotope analyses.

Energy Technology Data Exchange (ETDEWEB)

vonKiparski, G; Hillegonds, D

2011-04-04

Investigations into the occurrence and origin of perchlorate (ClO{sub 4}{sup -}) found in groundwater from across North America have been sparse until recent years, and there is mounting evidence that natural formation mechanisms are important. New opportunities for identifying groundwater perchlorate and its origin have arisen with the utilization of improved detection methods and sampling techniques. Additionally, application of the forensic potential of isotopic measurements has begun to elucidate sources, potential formation mechanisms and natural attenuation processes. Procedures developed appear to be amenable to enable high precision stable isotopic analyses, as well as lower precision AMS analyses of {sup 36}Cl. Immediate work is in analyzing perchlorate isotope standards and developing full analytical accuracy and uncertainty expectations. Field samples have also been collected, and will be analyzed when final qa/qc samples are deemed acceptable.

High-Precision Direct Mass Determination of Unstable Isotopes

CERN Multimedia

2002-01-01

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

High-precision measurements of uranium and thorium isotopic ratios by multi-collector inductively coupled plasma mass spectrometry (MC-ICPMS)

Science.gov (United States)

Wang, Lisheng; Ma, Zhibang; Duan, Wuhui

2015-04-01

Isotopic compositions of U-Th and 230Th dating have been widely used in earth sciences, such as chronology, geochemistry, oceanography and hydrology. In this study, five ages of different carbonate samples were measured using 230Th dating technique with U-Th high-precision isotopic measurements by multi-collector inductively coupled plasma mass spectrometry, in Uranium-series Chronology Laboratory, Institute of Geology and Geophysics, Chinese Academy of Sciences.In this study, the precision and accuracy of uranium isotopic composition were estimated by measuring the uranium ratios of NBS-CRM 112A, NBS-CRM U500 and HU-1. The mean measured ratios, 234U/238U = 52.86 (±0.04) × 10-6 and δ234U = -38.36 (±0.77) × 10-3 for NBS-CRM 112A, 234U/238U = 10.4184 (±0.0001) × 10-3, 236U/238U = 15.43 (±0.01) × 10-4 and 238U/235U = 1.00021 (±0.00002) for NBS-CRM U500, 234U/238U = 54.911 (±0.007) and δ234U = -1.04 (±0.13) × 10-3 for HU-1 (95% confidence levels). The U isotope data for standard reference materials are in excellent agreement with previous studies, further highlighting the reliability and analytical capabilities of our technique. We measured the thorium isotopic ratios of three different thorium standards by MC-ICPMS. The three standards (Th-1, Th-2 and Th-3) were mixed by HU-1 and NBS 232Th standard, with the 230Th/232Th ratios from 10-4 to 10-6. The mean measured atomic ratios, 230Th/232Th = 2.1227 (±0.0024) × 10-6, 2.7246 (±0.0026) × 10-5, and 2.8358 (±0.0007) × 10-4 for Th-1, Th-2 and Th-3 (95% confidence levels), respectively. Using this technique, the following standard samples were dated by MC-ICPMS. Sample RKM-4, collected from Babardos Kendal Hill terrace, was used during the first stage of the Uranium-Series Intercomparison Project (USIP-I). Samples 76001, RKM-5 and RKM-6 were studied during the second stage of the USIP program (USIP-II). Sample 76001 is a laminated flowstone, collected from Sumidero Terejapa, Chiapas, Mexico, and samples

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

High-Precision In Situ 87Sr/86Sr Analyses through Microsampling on Solid Samples: Applications to Earth and Life Sciences

Directory of Open Access Journals (Sweden)

Sara Di Salvo

2018-01-01

Full Text Available An analytical protocol for high-precision, in situ microscale isotopic investigations is presented here, which combines the use of a high-performing mechanical microsampling device and high-precision TIMS measurements on micro-Sr samples, allowing for excellent results both in accuracy and precision. The present paper is a detailed methodological description of the whole analytical procedure from sampling to elemental purification and Sr-isotope measurements. The method offers the potential to attain isotope data at the microscale on a wide range of solid materials with the use of minimally invasive sampling. In addition, we present three significant case studies for geological and life sciences, as examples of the various applications of microscale 87Sr/86Sr isotope ratios, concerning (i the pre-eruptive mechanisms triggering recent eruptions at Nisyros volcano (Greece, (ii the dynamics involved with the initial magma ascent during Eyjafjallajökull volcano’s (Iceland 2010 eruption, which are usually related to the precursory signals of the eruption, and (iii the environmental context of a MIS 3 cave bear, Ursus spelaeus. The studied cases show the robustness of the methods, which can be also be applied in other areas, such as cultural heritage, archaeology, petrology, and forensic sciences.

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)

Diode laser based resonance ionization mass spectrometry for spectroscopy and trace analysis of uranium isotopes

International Nuclear Information System (INIS)

Hakimi, Amin

2013-01-01

In this doctoral thesis, the upgrade and optimization of a diode laser system for high-resolution resonance ionization mass spectrometry is described. A frequency-control system, based on a double-interferometric approach, allowing for absolute stabilization down to 1 MHz as well as frequency detunings of several GHz within a second for up to three lasers in parallel was optimized. This laser system was used for spectroscopic studies on uranium isotopes, yielding precise and unambiguous level energies, total angular momenta, hyperfine constants and isotope shifts. Furthermore, an efficient excitation scheme which can be operated with commercial diode lasers was developed. The performance of the complete laser mass spectrometer was optimized and characterized for the ultra-trace analysis of the uranium isotope 236 U, which serves as a neutron flux dosimeter and tracer for radioactive anthropogenic contaminations in the environment. Using synthetic samples, an isotope selectivity of ( 236 U)/( 238 U) = 4.5(1.5) . 10 -9 was demonstrated.

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

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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.

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

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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

Uranium isotopic ratio measurements ({sup 235}U/{sup 238}U) by laser ablation high resolution inductively coupled plasma mass spectrometry for environmental radioactivity monitoring - {sup 235}U/{sup 238}U isotope ratio analysis by LA-ICP-MS-HR for environmental radioactivity monitoring

Energy Technology Data Exchange (ETDEWEB)

David, K.; Mokili, M.B.; Rousseau, G.; Deniau, I.; Landesman, C. [SUBATECH, Ecole des Mines de Nantes, Universite de Nantes, CNRS/IN2P3, 4 rue Alfred Kastler, 44307 Nantes cedex 3 (France)

2014-07-01

The protection of the aquatic and terrestrial environments from a broad range of contaminants spread by nuclear activities (nuclear plants, weapon tests or mining) require continuous monitoring of long-lives radionuclides that were released into the environment. The precise determination of uranium isotope ratios in both natural and potential contaminated samples is of primary concern for the nuclear safeguards and the control of environmental contamination. As an example, analysis of environmental samples around nuclear plants are carried out to detect the traces in the environment originating from nuclear technology activities. This study deals with the direct analysis of {sup 235}U/{sup 238}U isotope ratios in real environmental solid samples performed with laser ablation (LA)-HR-ICP-MS. A similar technique has already been reported for the analysis of biological samples or uranium oxide particles [1,2] but to our knowledge, this was never applied on real environmental samples. The high sensitivity, rapid acquisition time and low detection limits are the main advantages of high resolution ICP-MS for accurate and precise isotope ratio measurements of uranium at trace and ultra-trace levels. In addition, the use of laser ablation allows the analysis of solid samples with minimal preparation. A a consequence, this technique is very attractive for conducting rapid direct {sup 235}U/{sup 238}U isotope ratio analysis on a large set of various matrix samples likely to be encountered in environmental monitoring such as corals, soils, sands, sediments, terrestrial and marine bio-indicators. For the present study, LA-ICP-MS-HR analyses are performed using a New Wave UP213 nano-second Nd:YAG laser coupled to a Thermo Element-XR high resolution mass spectrometer. Powdered samples are compacted with an hydraulic press (5 tons) in order to obtain disk-shaped pellet (10-13 mm in diameter and 2 mm in thickness). The NIST612 reference glass is used for LA-ICP-MS-HR tuning and as

High-Precision Computation and Mathematical Physics

International Nuclear Information System (INIS)

Bailey, David H.; Borwein, Jonathan M.

2008-01-01

At the present time, IEEE 64-bit floating-point arithmetic is sufficiently accurate for most scientific applications. However, for a rapidly growing body of important scientific computing applications, a higher level of numeric precision is required. Such calculations are facilitated by high-precision software packages that include high-level language translation modules to minimize the conversion effort. This paper presents a survey of recent applications of these techniques and provides some analysis of their numerical requirements. These applications include supernova simulations, climate modeling, planetary orbit calculations, Coulomb n-body atomic systems, scattering amplitudes of quarks, gluons and bosons, nonlinear oscillator theory, Ising theory, quantum field theory and experimental mathematics. We conclude that high-precision arithmetic facilities are now an indispensable component of a modern large-scale scientific computing environment.

Recent developments for high-precision mass measurements of the heaviest elements at SHIPTRAP

International Nuclear Information System (INIS)

Minaya Ramirez, E.; Ackermann, D.; Blaum, K.; Block, M.; Droese, C.; Düllmann, Ch. E.; Eibach, M.; Eliseev, S.; Haettner, E.; Herfurth, F.; Heßberger, F.P.

2013-01-01

Highlights: • Direct high-precision mass measurements of No and Lr isotopes performed. • High-precision mass measurements with a count rate of 1 ion/hour demonstrated. • The results provide anchor points for a large region connected by alpha-decay chains. • The binding energies determine the strength of the deformed shell closure N = 152. • Technical developments and new techniques will pave the way towards heavier elements. -- Abstract: Atomic nuclei far from stability continue to challenge our understanding. For example, theoretical models have predicted an “island of stability” in the region of the superheavy elements due to the closure of spherical proton and neutron shells. Depending on the model, these are expected at Z = 114, 120 or even 126 and N = 172 or 184. Valuable information on the road to the island of stability is derived from high-precision mass measurements, which give direct access to binding energies of short-lived trans-uranium nuclei. Recently, direct mass measurements at SHIPTRAP have been extended to nobelium and lawrencium isotopes around the deformed shell gap N = 152. In order to further extend mass measurements to the region of superheavy elements, new technical developments are required to increase the performance of our setup. The sensitivity will increase through the implementation of a new detection method, where observation of one single ion is sufficient. Together with the use of a more efficient gas stopping cell, this will us allow to significantly enhance the overall efficiency of SHIPTRAP

High-resolution stratigraphy with strontium isotopes.

Science.gov (United States)

Depaolo, D J; Ingram, B L

1985-02-22

The isotopic ratio of strontium-87 to strontium-86 shows no detectable variation in present-day ocean water but changes slowly over millions of years. The strontium contained in carbonate shells of marine organisms records the ratio of strontium-87 to strontium-86 of the oceans at the time that the shells form. Sedimentary rocks composed of accumulated fossil carbonate shells can be dated and correlated with the use of high precision measurements of the ratio of strontium-87 to strontium-86 with a resolution that is similar to that of other techniques used in age correlation. This method may prove valuable for many geological, paleontological, paleooceanographic, and geochemical problems.

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

Thorium spectrophotometric analysis with high precision

International Nuclear Information System (INIS)

Palmieri, H.E.L.

1983-06-01

An accurate and precise determination of thorium is proposed. Precision of about 0,1% is required for the determination of macroquantities of thorium processed. After an extensive literature search concerning this subject, spectrophotometric titration has been chosen, using disodium ethylenediaminetetraacetate (EDTA) solution and alizarin S as indicator. In order to obtain such a precision, an amount of 0,025 M EDTA solution precisely measured has been added and the titration was completed with less than 5 ml of 0,0025 M EDTA solution. It is usual to locate the end-point graphically, by plotting added titrant versus absorbance. The non-linear minimum square fit, using the Fletcher e Powell's minimization process and a computer program. (author)

Origins and evolution of rhyolitic magmas in the central Snake River Plain: insights from coupled high-precision geochronology, oxygen isotope, and hafnium isotope analyses of zircon

Science.gov (United States)

Colón, Dylan P.; Bindeman, Ilya N.; Wotzlaw, Jörn-Frederik; Christiansen, Eric H.; Stern, Richard A.

2018-02-01

We present new high-precision CA-ID-TIMS and in situ U-Pb ages together with Hf and O isotopic analyses (analyses performed all on the same grains) from four tuffs from the 15-10 Ma Bruneau-Jarbidge center of the Snake River Plain and from three rhyolitic units from the Kimberly borehole in the neighboring 10-6 Ma Twin Falls volcanic center. We find significant intrasample diversity in zircon ages (ranges of up to 3 Myr) and in δ18O (ranges of up to 6‰) and ɛHf (ranges of up to 24 ɛ units) values. Zircon rims are also more homogeneous than the associated cores, and we show that zircon rim growth occurs faster than the resolution of in situ dating techniques. CA-ID-TIMS dating of a subset of zircon grains from the Twin Falls samples reveals complex crystallization histories spanning 104-106 years prior to some eruptions, suggesting that magma genesis was characterized by the cyclic remelting of buried volcanic rocks and intrusions associated with previous magmatic episodes. Age-dependent trends in zircon isotopic compositions show that rhyolite production in the Yellowstone hotspot track is driven by the mixing of mantle-derived melts (normal δ18O and ɛHf) and a combination of Precambrian basement rock (normal δ18O and ɛHf down to - 60) and shallow Mesozoic and Cenozoic age rocks, some of which are hydrothermally altered (to low δ18O values) by earlier stages of Snake River Plain magmatism. These crustal melts hybridize with juvenile basalts and rhyolites to produce the erupted rhyolites. We also observe that the Precambrian basement rock is only an important component in the erupted magmas in the first eruption at each caldera center, suggesting that the accumulation of new intrusions quickly builds an upper crustal intrusive body which is isolated from the Precambrian basement and evolves towards more isotopically juvenile and lower-δ18O compositions over time.

Quantitation of stable isotopic tracers of calcium by fast atom bombardment mass spectrometry

International Nuclear Information System (INIS)

Jiang, X.; Smith, D.L.

1987-01-01

Instrumentation and methodology developed for quantitation of stable isotopic traces in urine are described. Calcium is isolated from urine as the insoluble oxalate salt which is subsequently dissolved in hydrochloric acid. The isotopic content of the acid solution is determined by use of a conventional mass spectrometer equipped with a fast atom bombardment ion source. Calcium ions are desorbed from the sample surface by a beam of high-energy xenon atoms and detected with a high-resolution mass spectrometer. A data acquisition system has been developed to control the mass spectrometer and record the ion signals. Detailed analysis of potential sources of error indicates that the precision of the method is presently limited primarily by an isotope effect that occurs during ion desorption. Results presented here demonstrate that the relative abundances of calcium isotopes in urine can be determined with high precision (coefficient of variation < 0.2%) and that the method is a viable alternative to conventional thermal ionization mass spectrometry. The method is especially attractive because it uses a conventional high-resolution mass spectrometer which is routinely used for analysis of organic substances

High precision time calibration of the Permo-Triassic boundary mass extinction by U-Pb geochronology

Science.gov (United States)

Baresel, Björn; Bucher, Hugo; Brosse, Morgane; Schaltegger, Urs

2014-05-01

U-Pb dating using Chemical Abrasion, Isotope Dilution Thermal Ionization Mass Spectrometry (CA-ID-TIMS) is the analytical method of choice for geochronologists, who are seeking highest temporal resolution and a high degree of accuracy for single grains of zircon. The use of double-isotope tracer solutions, cross-calibrated and assessed in different EARTHTIME labs, coinciding with the reassessment of the uranium decay constants and further improvements in ion counting technology led to unprecedented precision better than 0.1% for single grain, and 0.05% for population ages, respectively. These analytical innovations now allow calibrating magmatic and biological timescales at resolution adequate for both groups of processes. To construct a revised and high resolution calibrated time scale for the Permian-Triassic boundary (PTB) we use (i) high-precision U-Pb zircon age determinations of a unique succession of volcanic ash beds interbedded with shallow to deep water fossiliferous sediments in the Nanpanjiang Basin (South China) combined with (ii) accurate quantitative biochronology based on ammonoids and conodonts and (iii) carbon isotope excursions across the PTB. Using these alignments allows (i) positioning the PTB in different depositional environments and (ii) solving age/stratigraphic contradictions generated by the index, water depth-controlled conodont Hindeodus parvus, whose diachronous first occurrences are arbitrarily used for placing the base of the Triassic. This new age framework provides the basis for a combined calibration of chemostratigraphic records with high-resolution biochronozones of the Late Permian and Early Triassic. Besides the general improvement of the radio-isotopic calibration of the PTB at the ±100 ka level, this will also lead to a better understanding of cause and effect relations involved in this mass extinction.

Optically continuous silcrete quartz cements of the St. Peter Sandstone: High precision oxygen isotope analysis by ion microprobe

Science.gov (United States)

Kelly, Jacque L.; Fu, Bin; Kita, Noriko T.; Valley, John W.

2007-08-01

A detailed oxygen isotope study of detrital quartz and authigenic quartz overgrowths from shallowly buried (ratio by laser fluorination, resulting in an average δ 18O of 10.0 ± 0.2‰ (1SD, n = 109). Twelve thin sections were analyzed by CAMECA-1280 ion microprobe (6-10 μm spot size, analytical precision better than ±0.2‰, 1SD). Detrital quartz grains have an average δ 18O of 10.0 ± 1.4‰ (1SD, n = 91) identical to the data obtained by laser fluorination. The ion microprobe data reveal true variability that is otherwise lost by homogenization of powdered samples necessary for laser fluorination. Laser fluorination uses samples that are one million times larger than the ion microprobe. Whole rock (WR) samples from the 53 rocks were analyzed by laser fluorination, giving δ 18O between 9.8‰ and 16.7‰ ( n = 110). Quartz overgrowths in thin sections from 10 rocks were analyzed by ion microprobe and average δ 18O = 29.3 ± 1.0‰ (1SD, n = 161). Given the similarity, on average, of δ 18O for all detrital quartz grains and for all quartz overgrowths, samples with higher δ 18O(WR) values can be shown to have more cement. The quartz cement in the 53 rocks, calculated by mass balance, varies from outlier at 33 vol.% cement. Eolian samples have an average of 11% cement compared to marine samples, which average 4% cement. Two models for quartz cementation have been investigated: high temperature (50-110 °C) formation from ore-forming brines related to Mississippi Valley Type (MVT) mineralization and formation as silcretes at low temperature (10-30 °C). The homogeneity of δ 18O for quartz overgrowths determined by ion microprobe rules out a systematic regional variation of temperature as predicted for MVT brines and there are no other known heating events in these sediments that were never buried to depths >1 km. The data in this study suggest that quartz overgrowths formed as silcretes in the St. Peter Sandstone from meteoric water with δ 18O values of -10

MATS and LaSpec: High-precision experiments using ion traps and lasers at FAIR

Science.gov (United States)

Rodríguez, D.; Blaum, K.; Nörtershäuser, W.; Ahammed, M.; Algora, A.; Audi, G.; Äystö, J.; Beck, D.; Bender, M.; Billowes, J.; Block, M.; Böhm, C.; Bollen, G.; Brodeur, M.; Brunner, T.; Bushaw, B. A.; Cakirli, R. B.; Campbell, P.; Cano-Ott, D.; Cortés, G.; Crespo López-Urrutia, J. R.; Das, P.; Dax, A.; de, A.; Delheij, P.; Dickel, T.; Dilling, J.; Eberhardt, K.; Eliseev, S.; Ettenauer, S.; Flanagan, K. T.; Ferrer, R.; García-Ramos, J.-E.; Gartzke, E.; Geissel, H.; George, S.; Geppert, C.; Gómez-Hornillos, M. B.; Gusev, Y.; Habs, D.; Heenen, P.-H.; Heinz, S.; Herfurth, F.; Herlert, A.; Hobein, M.; Huber, G.; Huyse, M.; Jesch, C.; Jokinen, A.; Kester, O.; Ketelaer, J.; Kolhinen, V.; Koudriavtsev, I.; Kowalska, M.; Krämer, J.; Kreim, S.; Krieger, A.; Kühl, T.; Lallena, A. M.; Lapierre, A.; Le Blanc, F.; Litvinov, Y. A.; Lunney, D.; Martínez, T.; Marx, G.; Matos, M.; Minaya-Ramirez, E.; Moore, I.; Nagy, S.; Naimi, S.; Neidherr, D.; Nesterenko, D.; Neyens, G.; Novikov, Y. N.; Petrick, M.; Plaß, W. R.; Popov, A.; Quint, W.; Ray, A.; Reinhard, P.-G.; Repp, J.; Roux, C.; Rubio, B.; Sánchez, R.; Schabinger, B.; Scheidenberger, C.; Schneider, D.; Schuch, R.; Schwarz, S.; Schweikhard, L.; Seliverstov, M.; Solders, A.; Suhonen, M.; Szerypo, J.; Taín, J. L.; Thirolf, P. G.; Ullrich, J.; van Duppen, P.; Vasiliev, A.; Vorobjev, G.; Weber, C.; Wendt, K.; Winkler, M.; Yordanov, D.; Ziegler, F.

2010-05-01

Nuclear ground state properties including mass, charge radii, spins and moments can be determined by applying atomic physics techniques such as Penning-trap based mass spectrometry and laser spectroscopy. The MATS and LaSpec setups at the low-energy beamline at FAIR will allow us to extend the knowledge of these properties further into the region far from stability. The mass and its inherent connection with the nuclear binding energy is a fundamental property of a nuclide, a unique “fingerprint”. Thus, precise mass values are important for a variety of applications, ranging from nuclear-structure studies like the investigation of shell closures and the onset of deformation, tests of nuclear mass models and mass formulas, to tests of the weak interaction and of the Standard Model. The required relative accuracy ranges from 10-5 to below 10-8 for radionuclides, which most often have half-lives well below 1 s. Substantial progress in Penning trap mass spectrometry has made this method a prime choice for precision measurements on rare isotopes. The technique has the potential to provide high accuracy and sensitivity even for very short-lived nuclides. Furthermore, ion traps can be used for precision decay studies and offer advantages over existing methods. With MATS (Precision Measurements of very short-lived nuclei using an A_dvanced Trapping System for highly-charged ions) at FAIR we aim to apply several techniques to very short-lived radionuclides: High-accuracy mass measurements, in-trap conversion electron and alpha spectroscopy, and trap-assisted spectroscopy. The experimental setup of MATS is a unique combination of an electron beam ion trap for charge breeding, ion traps for beam preparation, and a high-precision Penning trap system for mass measurements and decay studies. For the mass measurements, MATS offers both a high accuracy and a high sensitivity. A relative mass uncertainty of 10-9 can be reached by employing highly-charged ions and a non

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.

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)

An improved method for high precision measurement of chromium isotopes using double spike MC-ICP-MS

Science.gov (United States)

Zhu, J.; Wu, G. L.; Wang, X.; Zhang, L. X.; Han, G.

2017-12-01

Chormium(Cr) isotopes have been used to trace pollution processes and reconstruct paleo-redox conditions. However, the precise determination of Cr isotopes has still been challenged due to difficulties in purifying Cr from samples with low Cr content and complex matrices. Here we report an improved four-step column chromatographic procedure to separate Cr from matrix elements. Firstly, Cr in sample solution was mixed with 50Cr-54Cr double spike (the optimized 54Crspike/52Crsample = 0.4 and (50Cr/54Cr)spike = 1.3:1) was completely converted into Cr (III) in 8.5mol/L HCl and loaded onto 2ml of AG50W-X8(200-400m) resin conditioned with 11 mol/L HCl. The 2.65ml of eluent was adjusted to 4.5ml of 6mol/L HCl and immediately loaded onto a Bio-Rad column filled with 2ml of AG1-X8 anion resin (100-200m). These two steps can remove at least 99% of Ca, Fe and most matrix elements. Secondly, the 7.5ml of eluent was dried down and dissolved in 0.1ml of 0.5mol/L HNO3.before adding 2ml 4mol/L HF, which was then loaded onto 1ml of AG1-X8 anion resin (100-200m) to remove Ti and V. Finally, sample was dissolved in 0.1ml of 0.5 mol/L HNO3 and oxidized by 0.5mL 0.2 mol/L (NH4)2S2O8 and 4.4mL H2O, which was then centrifuged to remove Mn oxide, and supernatant was loaded onto AG1-X8 resin to remove SO42-, Ni, Al, Na and some Mg using 8ml H2O and 3ml 2mol/L HCl. Cr was eluted by 2 mol/L HNO3 containing 5% H2O2 and the dried Cr was dissolved in 3% HNO3for isotopic analysis. The total yield to Cr is great than 80% even for samples with low Cr content. Chromium isotopes was measured on a Neptune plus MC-ICP-MS in China University of Geosciences(Beijing). Using our improved method, the δ53/52CrSRM979 values of USGS reference materials BHVO-2, BCR-2 and SGR-1b are -0.12±0.06‰(n=15), -0.09±0.06‰ (n=5), and 0.30±0.06‰ (n=12), respectively, which agree well with previously reported values. The δ53/52CrSRM979 of carbonaceous shale CP0-1 and CP0-12 collected from Hubei, China are 2.05�

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

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)

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)

High precision spectrophotometric analysis of thorium

International Nuclear Information System (INIS)

Palmieri, H.E.L.

1984-01-01

An accurate and precise determination of thorium is proposed. Precision of about 0,1% is required for the determination of macroquantities of thorium when processed. After an extensive literature search concerning this subject, spectrophotometric titration has been chosen, using dissodium ethylenediaminetetraacetate (EDTA) solution and alizarin-S as indicator. In order to obtain such a precision, an amount of 0,025 M EDTA solution precisely measured has been added and the titration was completed with less than 5 ml of 0,0025 M EDTA solution. It is usual to locate the end-point graphically, by plotting added titrant versus absorbance. The non-linear minimum square fit, using the Fletcher e Powell's minimization process and a computer programme. Besides the equivalence point, other parameters of titration were determined: the indicator concentration, the absorbance of the metal-indicator complex, and the stability constants of the metal-indicator and the metal-EDTA complexes. (Author) [pt

pH-dependent equilibrium isotope fractionation associated with the compound specific nitrogen and carbon isotope analysis of substituted anilines by SPME-GC/IRMS.

Science.gov (United States)

Skarpeli-Liati, Marita; Turgeon, Aurora; Garr, Ashley N; Arnold, William A; Cramer, Christopher J; Hofstetter, Thomas B

2011-03-01

Solid-phase microextraction (SPME) coupled to gas chromatography/isotope ratio mass spectrometry (GC/IRMS) was used to elucidate the effects of N-atom protonation on the analysis of N and C isotope signatures of selected aromatic amines. Precise and accurate isotope ratios were measured using polydimethylsiloxane/divinylbenzene (PDMS/DVB) as the SPME fiber material at solution pH-values that exceeded the pK(a) of the substituted aniline's conjugate acid by two pH-units. Deviations of δ(15)N and δ(13)C-values from reference measurements by elemental analyzer IRMS were small (IRMS. Under these conditions, the detection limits for accurate isotope ratio measurements were between 0.64 and 2.1 mg L(-1) for δ(15)N and between 0.13 and 0.54 mg L(-1) for δ(13)C, respectively. Substantial inverse N isotope fractionation was observed by SPME-GC/IRMS as the fraction of protonated species increased with decreasing pH leading to deviations of -20‰ while the corresponding δ(13)C-values were largely invariant. From isotope ratio analysis at different solution pHs and theoretical calculations by density functional theory, we derived equilibrium isotope effects, EIEs, pertinent to aromatic amine protonation of 0.980 and 1.001 for N and C, respectively, which were very similar for all compounds investigated. Our work shows that N-atom protonation can compromise accurate compound-specific N isotope analysis of aromatic amines.

High-precision determination of 18O/16O ratios of silver phosphate by EA-pyrolysis-IRMS continuous flow technique.

Science.gov (United States)

Lécuyer, Christophe; Fourel, François; Martineau, François; Amiot, Romain; Bernard, Aurélien; Daux, Valérie; Escarguel, Gilles; Morrison, John

2007-01-01

A high-precision, and rapid on-line method for oxygen isotope analysis of silver phosphate is presented. The technique uses high-temperature elemental analyzer (EA)-pyrolysis interfaced in continuous flow (CF) mode to an isotopic ratio mass spectrometer (IRMS). Calibration curves were generated by synthesizing silver phosphate with a 13 per thousand spread in delta(18)O values. Calibration materials were obtained by reacting dissolved potassium dihydrogen phosphate (KH(2)PO(4)) with water samples of various oxygen isotope compositions at 373 K. Validity of the method was tested by comparing the on-line results with those obtained by classical off-line sample preparation and dual inlet isotope measurement. In addition, silver phosphate precipitates were prepared from a collection of biogenic apatites with known delta(18)O values ranging from 12.8 to 29.9 per thousand (V-SMOW). Reproducibility of +/- 0.2 per thousand was obtained by the EA-Py-CF-IRMS method for sample sizes in the range 400-500 microg. Both natural and synthetic samples are remarkably well correlated with conventional (18)O/(16)O determinations. Silver phosphate is a very stable material and easy to degas and, thus, could be considered as a good candidate to become a reference material for the determination of (18)O/(16)O ratios of phosphate by high-temperature pyrolysis. Copyright 2006 John Wiley & Sons, Ltd.

Precision mass measurements on neutron-rich Zn isotopes and their consequences on the astrophysical r-process

International Nuclear Information System (INIS)

Baruah, Sudarshan

2008-07-01

The rapid neutron-capture or the r-process is responsible for the origin of about half of the neutron-rich atomic nuclei in the universe heavier than iron. For the calculation of the abundances of those nuclei, atomic masses are required as one of the input parameters with very high precision. In the present work, the masses of the neutron rich Zn isotopes (A=71 to 81) lying in the r-process path have been measured in the ISOLTRAP experiment at ISOLDE/CERN. The mass of 81 Zn has been measured directly for the rst time. The half-lives of the nuclides ranged from 46.5 h ( 72 Zn) down to 290 ms ( 81 Zn). In case of all the nuclides, the relative mass uncertainty (Δm=m) achieved was in the order of 10 -8 corresponding to a 100-fold improvement in precision over previous measurements. (orig.)

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

High-precision branching ratio measurement for the superallowed β+ emitter Ga62

Science.gov (United States)

Finlay, P.; Ball, G. C.; Leslie, J. R.; Svensson, C. E.; Towner, I. S.; Austin, R. A. E.; Bandyopadhyay, D.; Chaffey, A.; Chakrawarthy, R. S.; Garrett, P. E.; Grinyer, G. F.; Hackman, G.; Hyland, B.; Kanungo, R.; Leach, K. G.; Mattoon, C. M.; Morton, A. C.; Pearson, C. J.; Phillips, A. A.; Ressler, J. J.; Sarazin, F.; Savajols, H.; Schumaker, M. A.; Wong, J.

2008-08-01

A high-precision branching ratio measurement for the superallowed β+ decay of Ga62 was performed at the Isotope Separator and Accelerator (ISAC) radioactive ion beam facility. The 8π spectrometer, an array of 20 high-purity germanium detectors, was employed to detect the γ rays emitted following Gamow-Teller and nonanalog Fermi β+ decays of Ga62, and the SCEPTAR plastic scintillator array was used to detect the emitted β particles. Thirty γ rays were identified following Ga62 decay, establishing the superallowed branching ratio to be 99.858(8)%. Combined with the world-average half-life and a recent high-precision Q-value measurement for Ga62, this branching ratio yields an ft value of 3074.3±1.1 s, making Ga62 among the most precisely determined superallowed ft values. Comparison between the superallowed ft value determined in this work and the world-average corrected F tmacr value allows the large nuclear-structure-dependent correction for Ga62 decay to be experimentally determined from the CVC hypothesis to better than 7% of its own value, the most precise experimental determination for any superallowed emitter. These results provide a benchmark for the refinement of the theoretical description of isospin-symmetry breaking in A⩾62 superallowed decays.

Evaluation of the performance of high temperature conversion reactors for compound-specific oxygen stable isotope analysis.

Science.gov (United States)

Hitzfeld, Kristina L; Gehre, Matthias; Richnow, Hans-Hermann

2017-05-01

In this study conversion conditions for oxygen gas chromatography high temperature conversion (HTC) isotope ratio mass spectrometry (IRMS) are characterised using qualitative mass spectrometry (IonTrap). It is shown that physical and chemical properties of a given reactor design impact HTC and thus the ability to accurately measure oxygen isotope ratios. Commercially available and custom-built tube-in-tube reactors were used to elucidate (i) by-product formation (carbon dioxide, water, small organic molecules), (ii) 2nd sources of oxygen (leakage, metal oxides, ceramic material), and (iii) required reactor conditions (conditioning, reduction, stability). The suitability of the available HTC approach for compound-specific isotope analysis of oxygen in volatile organic molecules like methyl tert-butyl ether is assessed. Main problems impeding accurate analysis are non-quantitative HTC and significant carbon dioxide by-product formation. An evaluation strategy combining mass spectrometric analysis of HTC products and IRMS 18 O/ 16 O monitoring for future method development is proposed.

High-precision Al-Mg isotopic systematics in USNM 3898 - The benchmark "ALL" for initial 87Sr/86Sr in the earliest Solar System

Science.gov (United States)

MacPherson, G. J.; Defouilloy, C.; Kita, N. T.

2018-06-01

The Allende CAI USNM 3898 is the basis for "ALL", the lowest measured initial 87Sr/86Sr value in any solar system material including other CAIs (Gray et al., 1973). If the value ALL is correct (debated), then USNM 3898 must be 1-2 million years older than other CAIs (Podosek et al., 1991). This would require in turn that it have a much higher initial 26Al/27Al value than other CAIs, on the order of 4 × 10-4. Podosek et al. (1991) showed that this is not the case, with initial 26Al/27Al = (4.5 ± 0.7) × 10-5, but their Mg-isotopic data had large error bars and there was clear isotopic disturbance in the data having the highest 27Al/24Mg. Without the latter data, the slope of their isochron is higher (5.10 ± 1.19) × 10-5) and within (large) error of being supracanonical. We used high-precision SIMS to re-determine the initial 26Al/27Al in this CAI and obtained a value of (5.013 ± 0.099) × 10-5, with an intercept δ26Mg* = - 0.008 ± 0.048 and MSWD = 1.3. This value is indistinguishable from that measured in many other CAIs and conclusively shows that USNM 3898 is not uniquely ancient. We also confirmed evidence of later isotopic disturbance, similar to what Podosek et al. found, indicating a re-melting and evaporation event some 200,000 years after initial CAI solidification.

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

Californium-252 neutron activation analysis of high-level processed nuclear tank waste

International Nuclear Information System (INIS)

Troyer, G.L.; Purcell, M.A.

2000-01-01

The basis for production assessment of the vitrification of Hanford nuclear fuel reprocessing wastes will be high-precision measurements of the elemental sodium content. However, the chemical analysis of both radioactive and nonradioactive components in nuclear waste can be challenged by high radiation dose rates. The dose rates compromise many analytical techniques as well as pose personnel dosimetry risks. In many cases, reduction of dose rates through dilution compromises the precision and sensitivity for certain key components. The use of neutron activation analysis (NAA) provides a method of analysis that avoids the need for dilutions or extensive sample preparation. These waste materials also contain trace quantities of fissionable isotopes, which, through neutron activation, can be estimated by delayed neutron counting of fissioned fragments

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

Oxygen isotope analysis of shark teeth phosphates from Bartonian (Eocene) deposits in Mangyshlak peninsula, Kazakhstan

Science.gov (United States)

Pelc, Andrzej; Hałas, Stanisław; Niedźwiedzki, Robert

2011-01-01

We report the results of high-precision (±0.05‰) oxygen isotope analysis of phosphates in 6 teeth of fossil sharks from the Mangyshlak peninsula. This precision was achieved by the offline preparation of CO2 which was then analyzed on a dual-inlet and triple-collector IRMS. The teeth samples were separated from Middle- and Late Bartonian sediments cropping out in two locations, Usak and Kuilus. Seawater temperatures calculated from the δ18O data vary from 23-41°C. However, these temperatures are probably overestimated due to freshwater inflow. The data point at higher temperature in the Late Bartonian than in the Middle Bartonian and suggest differences in the depth habitats of the shark species studied.

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.

Overview of the JYFLTRAP mass measurements and high-precision ...

Indian Academy of Sciences (India)

nuclei, the mass difference can be determined with much higher precision than would normally be possible since for the mass doublets the systematic uncertainties become ..... The two-neutron separation energies in N = 60 indicate the. 338 ... Masses of zinc isotopes (Z = 30) were measured up to 80Zn, providing valuable.

Novel double-isotope technique for enzymatic assay of catecholamines, permitting high precision, sensitivity and plasma sample capacity

International Nuclear Information System (INIS)

Brown, M.J.; Jenner, D.A.

1981-01-01

A novel use of a double-isotope method is described which allows radioenzymatic assays to combine precision and sensitivity. In the catechol O-methyltransferase assay separate portions of each plasma sample are incubated with either S-[ 3 H]- or S-[ 14 C]-adenosyl-L-methionine. Standards of noradrenaline and adrenaline are added to the latter portions and are thus converted into standards of [ 14 C]metadrenalines. These are added to the 3 H-labelled portions after the incubation, where they function as tracers. The final recovery of 14 C radioactivity corrects for (a) the efficiency of methylation in the plasma sample concerned and (b) the recovery of metadrenalines during the extraction procedures. The 3 H/ 14 C ratio is constant in each assay for a given catecholamine concentration and is determined for samples to which standards of noradrenaline and adrenaline are added to the 3 H- (as well as the 14 C-) labelled portions before the initial incubation. The sensitivity of the assay is increased by using high specific radioactivity S-[ 3 H]adenosyl-L-methionine, and low backgrounds are maintained by catecholamine depletion in vivo in the rats used for enzyme preparation. Both catecholamines (1.5 pg/ml; 10 pmol/l) may be detected; the coefficients of variation are 3.0 and 3.2% for noradrenaline and adrenaline respectively (intra-assay) and 4.6 and 5.0% (inter-assay). (author)

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

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

Stable isotope investigations from tree rings (Betula pubescens) in Northern Iceland

International Nuclear Information System (INIS)

Bertler, N.A.N.; Rose, J.J.; Mattey, D.P.; Brownlees, M.; Stoetter, J.E.

1999-01-01

Stable isotope investigations from recent trees (Betual pubescens) from two different locations in Northern Iceland have been carried out to examine applicability for paleoclimatic research. The aim was to correlate oxygen and carbon isotope data of annual and three year resolution derived from individual rings with meteorological data, in order to establish a calibration function for fossil wood samples. A precise dendrochronological record has been established for all cores to permit a direct comparison between different data sets. The material used for the isotopic analysis is pure α-cellulose. The oxygen and carbon ratios were measured using a new technique, employing CO with continuous flow mass spectrometry. As this method does not allow a simultaneous measurements of the carbon ratios, the δ 13 C values have been analysed separately, using CO 2 . Both methods demonstrated their reliability through high precision and accuracy in the values for the measured standards. However there is little confidence in the sample data, as they suffer from poor precision and non-consistency

Improved accuracy and precision in δ15 NAIR measurements of explosives, urea, and inorganic nitrates by elemental analyzer/isotope ratio mass spectrometry using thermal decomposition.

Science.gov (United States)

Lott, Michael J; Howa, John D; Chesson, Lesley A; Ehleringer, James R

2015-08-15

Elemental analyzer systems generate N(2) and CO(2) for elemental composition and isotope ratio measurements. As quantitative conversion of nitrogen in some materials (i.e., nitrate salts and nitro-organic compounds) is difficult, this study tests a recently published method - thermal decomposition without the addition of O(2) - for the analysis of these materials. Elemental analyzer/isotope ratio mass spectrometry (EA/IRMS) was used to compare the traditional combustion method (CM) and the thermal decomposition method (TDM), where additional O(2) is eliminated from the reaction. The comparisons used organic and inorganic materials with oxidized and/or reduced nitrogen and included ureas, nitrate salts, ammonium sulfate, nitro esters, and nitramines. Previous TDM applications were limited to nitrate salts and ammonium sulfate. The measurement precision and accuracy were compared to determine the effectiveness of converting materials containing different fractions of oxidized nitrogen into N(2). The δ(13) C(VPDB) values were not meaningfully different when measured via CM or TDM, allowing for the analysis of multiple elements in one sample. For materials containing oxidized nitrogen, (15) N measurements made using thermal decomposition were more precise than those made using combustion. The precision was similar between the methods for materials containing reduced nitrogen. The %N values were closer to theoretical when measured by TDM than by CM. The δ(15) N(AIR) values of purchased nitrate salts and ureas were nearer to the known values when analyzed using thermal decomposition than using combustion. The thermal decomposition method addresses insufficient recovery of nitrogen during elemental analysis in a variety of organic and inorganic materials. Its implementation requires relatively few changes to the elemental analyzer. Using TDM, it is possible to directly calibrate certain organic materials to international nitrate isotope reference materials without off

Precision mass measurements on neutron-rich Zn isotopes and their consequences on the astrophysical r-process

Energy Technology Data Exchange (ETDEWEB)

Baruah, Sudarshan

2008-07-15

The rapid neutron-capture or the r-process is responsible for the origin of about half of the neutron-rich atomic nuclei in the universe heavier than iron. For the calculation of the abundances of those nuclei, atomic masses are required as one of the input parameters with very high precision. In the present work, the masses of the neutron rich Zn isotopes (A=71 to 81) lying in the r-process path have been measured in the ISOLTRAP experiment at ISOLDE/CERN. The mass of {sup 81}Zn has been measured directly for the rst time. The half-lives of the nuclides ranged from 46.5 h ({sup 72}Zn) down to 290 ms ({sup 81}Zn). In case of all the nuclides, the relative mass uncertainty ({delta}m=m) achieved was in the order of 10{sup -8} corresponding to a 100-fold improvement in precision over previous measurements. (orig.)

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.

Selection of mode for the measurement of lead isotope ratios by inductively coupled plasma mass spectrometry and its application to milk powder analysis

International Nuclear Information System (INIS)

Dean, J.R.; Ebdon, L.; Massey, R.

1987-01-01

An investigation into the selection of the optimum mode for the measurement of isotope ratios in inductively coupled plasma mass spectrometry (ICP-MS) is reported, with particular reference to lead isotope ratios. Variation in the accuracy and precision achievable using the measurement modes of scanning and peak jumping are discussed. It is concluded that if sufficient sample and time are available, scanning gives best accuracy and precision. Isotope dilution analysis (IDA) has been applied to the measurement of the lead content of two dried milk powders of Australian and European origin introduced as slurries into ICP-MS. Differences in the lead isotope ratios in the two milk powders were investigated and the total lead content determined by IDA. Isotope dilution analysis permitted accurate data to be obtained with an RSD of 4.2% or milk powder containing less than 30 ng g -1 of lead. The ICP-MS technique is confirmed as a useful tool for IDA. (author)

Isotope analysis of uranium by optical spectroscopy; Analyse isotopique de I'uranium par spectroscopie optique

Energy Technology Data Exchange (ETDEWEB)

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

1958-07-01

Isotope analysis of uranium is made by means of hollow cathode lamp and Fabry-Perot photoelectric spectrometer. When using the line U I 5027 A, this method allows to determine isotopic concentrations in {sup 235}U down to 0,1 per cent. The relative precision is about 2 per cent for amounts of {sup 235}U over 1 per cent. For weaker amounts this line would allow relative measurements of better precision when using standard mixtures. (author) [French] L'analyse isotopique de l'uranium est effectuee a l'aide d'une lampe a cathode creuse et du spectrometre Fabry-Perot photo-electrique. On utilise la raie U I 5027 A. Cette methode permet de doser des melanges isotopiques dont la teneur en {sup 235}U, peut descendre jusqu'a 0,1 pour cent. La precision relative est de l'ordre de 2 pour cent pour des teneurs en {sup 235}U superieures a 1 pour cent. Pour des teneurs plus faibles cette raie {lambda} = 5027 A permettrait des mesures relatives de meilleure precision, en utilisant des melanges prealablement doses. (auteur)

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

High-precision masses of 29-33Mg and the N=20 shell ''closure''

International Nuclear Information System (INIS)

Lunney, D.; Audi, G.; Gaulard, C.; Saint Simon, M. de; Thibault, C.; Vieira, N.

2006-01-01

High-precision mass measurements have been performed on the exotic magnesium isotopes 29-33 Mg using the MISTRAL radiofrequency spectrometer, especially suited for very short-lived nuclides. This method, combined with the powerful tool of resonant laser ionization at ISOLDE, has provided a significant reduction of uncertainty for the masses of the most exotic Mg isotopes: a relative error of 7 x 10 -7 was achieved for the weakly produced 33 Mg that has a half-life of only 90 ms. Moreover, the mass of 33 Mg is found to change by over 250 keV. Verifying and minimizing binding energy uncertainties in this region of the nuclear chart is important for understanding the lack of binding energy that is normally associated with magic numbers. (orig.)

Stepwise fluorination - a useful approach for the isotopic analysis of hydrous minerals

Energy Technology Data Exchange (ETDEWEB)

Haimson, M; Knauth, L P [Arizona State Univ., Tempe (USA). Dept. of Geology

1983-09-01

Analytical uncertainties in oxygen isotopic studies of hydrous silica have been investigated using a partial fluorination procedure in which fractional oxygen yields are achieved by reducing the amount of fluorine. Stepwise reaction of opaline silica results in a set of sequential oxygen fractions which show a wide range of delta/sup 18/O values due to variable amounts of water, organic matter, and other impurities. Delta-values for successive fractions in non-biogenic opal systematically increase as water is reacted away and then remain constant to within +- 0.2 per thousand as the remaining silica reacts. Delta-values in biogenic silica increase similarly but then decrease when low /sup 18/O oxide impurities begin to react. The troublesome water component in opal is readily removed by stepwise fluorination. This technique allows more precise oxygen isotope analysis of non-biogenic opal-A, and may improve the analytical precision for biogenic silica and any silicate mineral containing a significant water component.

Calcium-aluminum-rich inclusions with fractionation and unidentified nuclear effects (FUN CAIs): II. Heterogeneities of magnesium isotopes and 26Al in the early Solar System inferred from in situ high-precision magnesium-isotope measurements

Science.gov (United States)

Park, Changkun; Nagashima, Kazuhide; Krot, Alexander N.; Huss, Gary R.; Davis, Andrew M.; Bizzarro, Martin

2017-03-01

Calcium-aluminum-rich inclusions with isotopic mass fractionation effects and unidentified nuclear isotopic anomalies (FUN CAIs) have been studied for more than 40 years, but their origins remain enigmatic. Here we report in situ high precision measurements of aluminum-magnesium isotope systematics of FUN CAIs by secondary ion mass spectrometry (SIMS). Individual minerals were analyzed in six FUN CAIs from the oxidized CV3 carbonaceous chondrites Axtell (compact Type A CAI Axtell 2271) and Allende (Type B CAIs C1 and EK1-4-1, and forsterite-bearing Type B CAIs BG82DH8, CG-14, and TE). Most of these CAIs show evidence for excess 26Mg due to the decay of 26Al. The inferred initial 26Al/27Al ratios [(26Al/27Al)0] and the initial magnesium isotopic compositions (δ26Mg0) calculated using an exponential law with an exponent β of 0.5128 are (3.1 ± 1.6) × 10-6 and 0.60 ± 0.10‰ (Axtell 2271), (3.7 ± 1.5) × 10-6 and -0.20 ± 0.05‰ (BG82DH8), (2.2 ± 1.1) × 10-6 and -0.18 ± 0.05‰ (C1), (2.3 ± 2.4) × 10-5 and -2.23 ± 0.37‰ (EK1-4-1), (1.5 ± 1.1) × 10-5 and -0.42 ± 0.08‰ (CG-14), and (5.3 ± 0.9) × 10-5 and -0.05 ± 0.08‰ (TE) with 2σ uncertainties. We infer that FUN CAIs recorded heterogeneities of magnesium isotopes and 26Al in the CAI-forming region(s). Comparison of 26Al-26Mg systematics, stable isotope (oxygen, magnesium, calcium, and titanium) and trace element studies of FUN and non-FUN igneous CAIs indicates that there is a continuum among these CAI types. Based on these observations and evaporation experiments on CAI-like melts, we propose a generic scenario for the origin of igneous (FUN and non-FUN) CAIs: (i) condensation of isotopically normal solids in an 16O-rich gas of approximately solar composition; (ii) formation of CAI precursors by aggregation of these solids together with variable abundances of isotopically anomalous grains-possible carriers of unidentified nuclear (UN) effects; and (iii) melt evaporation of these precursors

Ion sources for solids isotopic analysis

Energy Technology Data Exchange (ETDEWEB)

Tyrrell, A. C. [Ministry of Defence, Foulness (UK). Atomic Weapons Research Establishment

1978-12-15

Of the dozen or so methods of producing ions from solid samples only the surface or thermal ionisation method has found general application for precise measurement of isotopic ratios. The author discusses the principal variables affecting the performance of the thermal source; sample preparation, loading onto the filament, sample pre-treatment, filament material.

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 measurements of 26Naβ- decay

Science.gov (United States)

Grinyer, G. F.; Svensson, C. E.; Andreoiu, C.; Andreyev, A. N.; Austin, R. A.; Ball, G. C.; Chakrawarthy, R. S.; Finlay, P.; Garrett, P. E.; Hackman, G.; Hardy, J. C.; Hyland, B.; Iacob, V. E.; Koopmans, K. A.; Kulp, W. D.; Leslie, J. R.; MacDonald, J. A.; Morton, A. C.; Ormand, W. E.; Osborne, C. J.; Pearson, C. J.; Phillips, A. A.; Sarazin, F.; Schumaker, M. A.; Scraggs, H. C.; Schwarzenberg, J.; Smith, M. B.; Valiente-Dobón, J. J.; Waddington, J. C.; Wood, J. L.; Zganjar, E. F.

2005-04-01

High-precision measurements of the half-life and β-branching ratios for the β- decay of 26Na to 26Mg have been measured in β-counting and γ-decay experiments, respectively. A 4π proportional counter and fast tape transport system were employed for the half-life measurement, whereas the γ rays emitted by the daughter nucleus 26Mg were detected with the 8π γ-ray spectrometer, both located at TRIUMF's isotope separator and accelerator radioactive beam facility. The half-life of 26Na was determined to be T1/2=1.07128±0.00013±0.00021s, where the first error is statistical and the second systematic. The logft values derived from these experiments are compared with theoretical values from a full sd-shell model calculation.

Mats and LaSpec: High-precision experiments using ion traps and lasers at Fair

Energy Technology Data Exchange (ETDEWEB)

Rodriguez, D.; Lallena, A.M.; Blaum, K.; Bohm, C.; Cakirli, R.B.; Crespo Lopez-Urrutia, J.R.; Eliseev, S.; Ketelaer, J.; Kreim, M.S.; Kowalska, M.; Litvinov, Y.A.; Nagy, S.; Neidherr, D.; Repp, J.; Roux, C.; Schabinger, B.; Ullrich, J.; Nortershauser, W.; Eberhardt, K.; Geppert, C.; Kramer, J.; Krieger, A.; Sanchez, R.; Ahammed, M.; Das, P.; Ray, A.; Algora, A.; Rubio, B.; Tain, J.L.; Audi, G.; Lunney, D.; Naimi, S.; Aysto, J.; Jokinen, A.; Kolhinen, V.; Moore, I.; Beck, D.; Block, M.; Geissel, H.; Heinz, S.; Herfurth, F.; Litvinov, Y.A.; Minaya-Ramirez, E.; Plab, W.R.; Quint, W.; Scheidenberger, C.; Winkler, M.; Bender, M.; Billowes, J.; Campbell, P.; Flanagan, K.T.; Schwarz, S.; Bollen, G.; Ferrer, R.; George, S.; Kester, O.; Brodeur, M.; Brunner, T.; Delheij, P.; Dilling, J.; Ettenauer, S.; Lapierre, A.; Bushaw, B.A.; Cano-Ott, D.; Martinez, T.; Cortes, G.; Gomez-Hornillos, M.B.; Dax, A.; Herlert, A.; Yordanov, D.; De, A.; Dickel, T.; Geissel, H.; Jesch, C.; Kuhl, T.; Petrick, M.; PlaB, W.R.; Scheidenberger, C.; Garcia-Ramos, J.E.; Gartzke, E.; Habs, D.; Szerypo, J.; Thirolf, P.G.; Weber, C.; Gusev, Y.; Nesterenko, D.; Novikov, Y.N.; Popov, A.; Seliverstov, M.; Vasiliev, A.; Vorobjev, G.; Heenen, P.H.; Marx, G.; Schweikhard, L.; Ziegler, F.; Hobein, M.; Schuch, R.; Solders, A.; Suhonen, M.; Huber, G.; Wendt, K.; Huyse, M.; Koudriavtsev, I.; Neyens, G.; Van Duppen, P.; Le Blanc, F.; Matos, M.; Reinhard, P.G.; Schneider, D.

2010-05-15

Nuclear ground state properties including mass, charge radii, spins and moments can be determined by applying atomic physics techniques such as Penning-trap based mass spectrometry and laser spectroscopy. The MATS and LaSpec setups at the low-energy beamline at FAIR will allow us to extend the knowledge of these properties further into the region far from stability. With MATS (Precision Measurements of very short-lived nuclei using an Advanced Trapping System for highly-charged ions) at FAIR we aim to apply several techniques to very short-lived radionuclides: High-accuracy mass measurements, in-trap conversion electron and alpha spectroscopy, and trap-assisted spectroscopy. The experimental setup of MATS is a unique combination of an electron beam ion trap for charge breeding, ion traps for beam preparation, and a high-precision Penning trap system for mass measurements and decay studies. For the mass measurements, MATS offers both a high accuracy and a high sensitivity. A relative mass uncertainty of 10{sup -9} can be reached by employing highly-charged ions and a non-destructive Fourier-Transform Ion-Cyclotron-Resonance (FT-ICR) detection technique on single stored ions. Decay studies in ion traps will become possible with MATS. Laser spectroscopy of radioactive isotopes and isomers is an efficient and model-independent approach for the determination of nuclear ground and isomeric state properties. Hyperfine structures and isotope shifts in electronic transitions exhibit readily accessible information on the nuclear spin, magnetic dipole and electric quadrupole moments as well as root-mean-square charge radii. The accuracy of laser-spectroscopic-determined nuclear properties is very high while requirements concerning production rates are moderate. This Technical Design Report describes a new Penning trap mass spectrometry setup as well as a number of complementary experimental devices for laser spectroscopy. Since MATS and LaSpec require high-quality low

Mats and LaSpec: High-precision experiments using ion traps and lasers at Fair

International Nuclear Information System (INIS)

Rodriguez, D.; Lallena, A.M.; Blaum, K.; Bohm, C.; Cakirli, R.B.; Crespo Lopez-Urrutia, J.R.; Eliseev, S.; Ketelaer, J.; Kreim, M.S.; Kowalska, M.; Litvinov, Y.A.; Nagy, S.; Neidherr, D.; Repp, J.; Roux, C.; Schabinger, B.; Ullrich, J.; Nortershauser, W.; Eberhardt, K.; Geppert, C.; Kramer, J.; Krieger, A.; Sanchez, R.; Ahammed, M.; Das, P.; Ray, A.; Algora, A.; Rubio, B.; Tain, J.L.; Audi, G.; Lunney, D.; Naimi, S.; Aysto, J.; Jokinen, A.; Kolhinen, V.; Moore, I.; Beck, D.; Block, M.; Geissel, H.; Heinz, S.; Herfurth, F.; Litvinov, Y.A.; Minaya-Ramirez, E.; Plab, W.R.; Quint, W.; Scheidenberger, C.; Winkler, M.; Bender, M.; Billowes, J.; Campbell, P.; Flanagan, K.T.; Schwarz, S.; Bollen, G.; Ferrer, R.; George, S.; Kester, O.; Brodeur, M.; Brunner, T.; Delheij, P.; Dilling, J.; Ettenauer, S.; Lapierre, A.; Bushaw, B.A.; Cano-Ott, D.; Martinez, T.; Cortes, G.; Gomez-Hornillos, M.B.; Dax, A.; Herlert, A.; Yordanov, D.; De, A.; Dickel, T.; Geissel, H.; Jesch, C.; Kuhl, T.; Petrick, M.; PlaB, W.R.; Scheidenberger, C.; Garcia-Ramos, J.E.; Gartzke, E.; Habs, D.; Szerypo, J.; Thirolf, P.G.; Weber, C.; Gusev, Y.; Nesterenko, D.; Novikov, Y.N.; Popov, A.; Seliverstov, M.; Vasiliev, A.; Vorobjev, G.; Heenen, P.H.; Marx, G.; Schweikhard, L.; Ziegler, F.; Hobein, M.; Schuch, R.; Solders, A.; Suhonen, M.; Huber, G.; Wendt, K.; Huyse, M.; Koudriavtsev, I.; Neyens, G.; Van Duppen, P.; Le Blanc, F.; Matos, M.; Reinhard, P.G.; Schneider, D.

2010-01-01

Nuclear ground state properties including mass, charge radii, spins and moments can be determined by applying atomic physics techniques such as Penning-trap based mass spectrometry and laser spectroscopy. The MATS and LaSpec setups at the low-energy beamline at FAIR will allow us to extend the knowledge of these properties further into the region far from stability. With MATS (Precision Measurements of very short-lived nuclei using an Advanced Trapping System for highly-charged ions) at FAIR we aim to apply several techniques to very short-lived radionuclides: High-accuracy mass measurements, in-trap conversion electron and alpha spectroscopy, and trap-assisted spectroscopy. The experimental setup of MATS is a unique combination of an electron beam ion trap for charge breeding, ion traps for beam preparation, and a high-precision Penning trap system for mass measurements and decay studies. For the mass measurements, MATS offers both a high accuracy and a high sensitivity. A relative mass uncertainty of 10 -9 can be reached by employing highly-charged ions and a non-destructive Fourier-Transform Ion-Cyclotron-Resonance (FT-ICR) detection technique on single stored ions. Decay studies in ion traps will become possible with MATS. Laser spectroscopy of radioactive isotopes and isomers is an efficient and model-independent approach for the determination of nuclear ground and isomeric state properties. Hyperfine structures and isotope shifts in electronic transitions exhibit readily accessible information on the nuclear spin, magnetic dipole and electric quadrupole moments as well as root-mean-square charge radii. The accuracy of laser-spectroscopic-determined nuclear properties is very high while requirements concerning production rates are moderate. This Technical Design Report describes a new Penning trap mass spectrometry setup as well as a number of complementary experimental devices for laser spectroscopy. Since MATS and LaSpec require high-quality low-energy beams

Ion sources for solids isotopic analysis

International Nuclear Information System (INIS)

Tyrrell, A.C.

Of the dozen or so methods of producing ions from solid samples only the surface or thermal ionisation method has found general application for precise measurement of isotopic ratios. The author discusses the principal variables affecting the performance of the thermal source; sample preparation, loading onto the filament, sample pre-treatment, filament material. (Auth.)

High-resolution continuous-flow analysis setup for water isotopic measurement from ice cores using laser spectroscopy

Science.gov (United States)

Emanuelsson, B. D.; Baisden, W. T.; Bertler, N. A. N.; Keller, E. D.; Gkinis, V.

2015-07-01

Here we present an experimental setup for water stable isotope (δ18O and δD) continuous-flow measurements and provide metrics defining the performance of the setup during a major ice core measurement campaign (Roosevelt Island Climate Evolution; RICE). We also use the metrics to compare alternate systems. Our setup is the first continuous-flow laser spectroscopy system that is using off-axis integrated cavity output spectroscopy (OA-ICOS; analyzer manufactured by Los Gatos Research, LGR) in combination with an evaporation unit to continuously analyze water samples from an ice core. A Water Vapor Isotope Standard Source (WVISS) calibration unit, manufactured by LGR, was modified to (1) enable measurements on several water standards, (2) increase the temporal resolution by reducing the response time and (3) reduce the influence from memory effects. While this setup was designed for the continuous-flow analysis (CFA) of ice cores, it can also continuously analyze other liquid or vapor sources. The custom setups provide a shorter response time (~ 54 and 18 s for 2013 and 2014 setup, respectively) compared to the original WVISS unit (~ 62 s), which is an improvement in measurement resolution. Another improvement compared to the original WVISS is that the custom setups have a reduced memory effect. Stability tests comparing the custom and WVISS setups were performed and Allan deviations (σAllan) were calculated to determine precision at different averaging times. For the custom 2013 setup the precision after integration times of 103 s is 0.060 and 0.070 ‰ for δ18O and δD, respectively. The corresponding σAllan values for the custom 2014 setup are 0.030, 0.060 and 0.043 ‰ for δ18O, δD and δ17O, respectively. For the WVISS setup the precision is 0.035, 0.070 and 0.042 ‰ after 103 s for δ18O, δD and δ17O, respectively. Both the custom setups and WVISS setup are influenced by instrumental drift with δ18O being more drift sensitive than δD. The �

Computer automated mass spectrometer for isotope analysis on gas samples

International Nuclear Information System (INIS)

Pamula, A.; Kaucsar, M.; Fatu, C.; Ursu, D.; Vonica, D.; Bendea, D.; Muntean, F.

1998-01-01

A low resolution, high precision instrument was designed and realized in the mass spectrometry laboratory of the Institute of Isotopic and Molecular Technology, Cluj-Napoca. The paper presents the vacuum system, the sample inlet system, the ion source, the magnetic analyzer and the ion collector. The instrument is almost completely automated. There are described the analog-to-digital conversion circuits, the local control microcomputer, the automation systems and the performance checking. (authors)

Reference and intercomparison materials for stable isotopes of light elements. Proceedings of a consultants meeting held in Vienna, 1-3 December 1993

International Nuclear Information System (INIS)

1995-09-01

The stable isotope composition of elements varies in natural compounds as a consequence of the slightly different physico-chemical behaviour of isotopes. The possibility of measuring the stable isotope relative variations with high precision, using mass spectrometry, promoted the rise of new fields of research in geochemistry and hydrology and, more recently, in environmental studies. The steady growth of these investigations and of their practical applications has emphasized the need for high quality isotopic standards and intercomparison samples, with well determined isotopic composition, for the intercalibration of analytical techniques and results among laboratories. The organization of the Consultants Meeting on Stable Isotope Standards and Intercomparison Materials held in Vienna from 1 to 3 December 1993, the fifth of this type (the previous meetings took place in 1966, 1976, 1983 and 1985), called for a review and a discussion of the characteristics, quality and availability of the existing standards and intercalibration materials, and for an assessment of needs for new materials, in view of recent developments and applications. A large part of the discussions was devoted to the new materials prepared for sulphur isotope analysis and the analytical requirements for highly precise isotopic analysis of CO 2 . The papers presented at the meeting are assembled in this volume. Refs, figs and tabs

Reference and intercomparison materials for stable isotopes of light elements. Proceedings of a consultants meeting held in Vienna, 1-3 December 1993

Energy Technology Data Exchange (ETDEWEB)

NONE

1995-09-01

The stable isotope composition of elements varies in natural compounds as a consequence of the slightly different physico-chemical behaviour of isotopes. The possibility of measuring the stable isotope relative variations with high precision, using mass spectrometry, promoted the rise of new fields of research in geochemistry and hydrology and, more recently, in environmental studies. The steady growth of these investigations and of their practical applications has emphasized the need for high quality isotopic standards and intercomparison samples, with well determined isotopic composition, for the intercalibration of analytical techniques and results among laboratories. The organization of the Consultants Meeting on Stable Isotope Standards and Intercomparison Materials held in Vienna from 1 to 3 December 1993, the fifth of this type (the previous meetings took place in 1966, 1976, 1983 and 1985), called for a review and a discussion of the characteristics, quality and availability of the existing standards and intercalibration materials, and for an assessment of needs for new materials, in view of recent developments and applications. A large part of the discussions was devoted to the new materials prepared for sulphur isotope analysis and the analytical requirements for highly precise isotopic analysis of CO{sub 2}. The papers presented at the meeting are assembled in this volume. Refs, figs and tabs.

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

Weak gravitational lensing towards high-precision cosmology

International Nuclear Information System (INIS)

Berge, Joel

2007-01-01

This thesis aims at studying weak gravitational lensing as a tool for high-precision cosmology. We first present the development and validation of a precise and accurate tool for measuring gravitational shear, based on the shapelets formalism. We then use shapelets on real images for the first time, we analyze CFHTLS images, and combine them with XMM-LSS data. We measure the normalisation of the density fluctuations power spectrum σ 8 , and the one of the mass-temperature relation for galaxy clusters. The analysis of the Hubble space telescope COSMOS field confirms our σ 8 measurement and introduces tomography. Finally, aiming at optimizing future surveys, we compare the individual and combined merits of cluster counts and power spectrum tomography. Our results demonstrate that next generation surveys will allow weak lensing to yield its full potential in the high-precision cosmology era. (author) [fr

Chemical and isotopic fingerprinting of ancient Chinese porcelains

International Nuclear Information System (INIS)

Zhao, J.-X.; Li, B.-P.; Greig, A.; Collerson, K.D.; Feng, Y.-X.

2005-01-01

We have obtained unequivocal fingerprinting for many Chinese porcelains of utmost significance, based on high-precision multi-element and isotopic analysis by inductively-coupled mass spectrometry (ICP-MS) and thermal ionization mass spectrometry (TIMS) in our laboratory. As most ancient Chinese kilns used raw materials mined from local areas, differences in the geochemistry and mineralogy of these raw materials are expected to be preserved as distinctive geochemical and isotopic signatures in finished products and this may be useful for identifying their sources. Production techniques, such as purifying and mixing of different raw materials, may also vary from kiln to kiln, or may even change over time. All of that could also potentially leave a characteristic chemical and isotopic signature in a kiln's finished products. Using a tiny amount (often a few tens milligrams) of porcelain material, more than 40 element concentrations and Sr-Nd isotopic compositions can be rapidly and precisely determined on the ICP-MS and TIMS, respectively. The analytical results show that visibly similar Chinese porcelains made in different places and/or dynasties are strikingly distinctive. The data also allow modern fakes to be readily distinguished from antique porcelains. (author). 4 refs., 7 figs

Ultra-High Precision Half-Life Measurement for the Superallowed &+circ; Emitter ^26Al^m

Science.gov (United States)

Finlay, P.; Demand, G.; Garrett, P. E.; Leach, K. G.; Phillips, A. A.; Sumithrarachchi, C. S.; Svensson, C. E.; Triambak, S.; Grinyer, G. F.; Leslie, J. R.; Andreoiu, C.; Cross, D.; Austin, R. A. E.; Ball, G. C.; Bandyopadhyay, D.; Djongolov, M.; Ettenauer, S.; Hackman, G.; Pearson, C. J.; Williams, S. J.

2009-10-01

The calculated nuclear structure dependent correction for ^26Al^m (δC-δNS= 0.305(27)% [1]) is smaller by nearly a factor of two than the other twelve precision superallowed cases, making it an ideal case to pursue a reduction in the experimental errors contributing to the Ft value. An ultra-high precision half-life measurement for the superallowed &+circ; emitter ^26Al^m has been made at the Isotope Separator and Accelerator (ISAC) facility at TRIUMF in Vancouver, Canada. A beam of ˜10^5 ^26Al^m/s was delivered in October 2007 and its decay was observed using a 4π continuous gas flow proportional counter as part of an ongoing experimental program in superallowed Fermi β decay studies. With a statistical precision of ˜0.008%, the present work represents the single most precise measurement of any superallowed half-life to date. [4pt] [1] I.S. Towner and J.C. Hardy, Phys. Rev. C 79, 055502 (2009).

Rapid and precise measurement of serum branched-chain and aromatic amino acids by isotope dilution liquid chromatography tandem mass spectrometry.

Directory of Open Access Journals (Sweden)

Ruiyue Yang

Full Text Available BACKGROUND: Serum branched-chain and aromatic amino acids (BCAAs and AAAs have emerged as predictors for the future development of diabetes and may aid in diabetes risk assessment. However, the current methods for the analysis of such amino acids in biological samples are time consuming. METHODS: An isotope dilution liquid chromatography tandem mass spectrometry (ID-LC/MS/MS method for serum BCAAs and AAAs was developed. The serum was mixed with isotope-labeled BCAA and AAA internal standards and the amino acids were extracted with acetonitrile, followed by analysis using LC/MS/MS. The LC separation was performed on a reversed-phase C18 column, and the MS/MS detection was performed via the positive electronic spray ionization in multiple reaction monitoring mode. RESULTS: Specific analysis of the amino acids was achieved within 2 min. Intra-run and total CVs for the amino acids were less than 2% and 4%, respectively, and the analytical recoveries ranged from 99.6 to 103.6%. CONCLUSION: A rapid and precise method for the measurement of serum BCAAs and AAAs was developed and may serve as a quick tool for screening serum BCAAs and AAAs in studies assessing diabetes risk.

UV-laser microdissection system - A novel approach for the preparation of high-resolution stable isotope records (δ13C/δ18O) from tree rings

Science.gov (United States)

Schollaen, Karina; Helle, Gerhard

2013-04-01

Intra-annual stable isotope (δ13C and δ18O) studies of tree rings at various incremental resolutions have been attempting to extract valuable seasonal climatic and environmental information or assessing plant ecophysiological processes. For preparing high-resolution isotope samples normally wood segments or cores are mechanically divided in radial direction or cut in tangential direction. After mechanical dissection, wood samples are ground to a fine powder and either cellulose is extracted or bulk wood samples are analyzed. Here, we present a novel approach for the preparation of high-resolution stable isotope records from tree rings using an UV-laser microdissection system. Firstly, tree-ring cellulose is directly extracted from wholewood cross-sections largely leaving the wood anatomical structure intact and saving time as compared to the classical procedure. Secondly, micro-samples from cellulose cross-sections are dissected with an UV-Laser dissection microscope. Tissues of interest from cellulose cross-sections are identified and marked precisely with a screen-pen and dissected via an UV-laser beam. Dissected cellulose segments were automatically collected in capsules and are prepared for stable isotope (δ13C and δ18O) analysis. The new techniques facilitate inter- and intra-annual isotope analysis on tree-ring and open various possibilities for comparisons with wood anatomy in plant eco-physiological studies. We describe the design and the handling of this novel methodology and discuss advantages and constraints given by the example of intra-annual oxygen isotope analysis on tropical trees.

Tests of a Fast Plastic Scintillator for High-Precision Half-Life Measurements

Science.gov (United States)

Laffoley, A. T.; Dunlop, R.; Finlay, P.; Leach, K. G.; Michetti-Wilson, J.; Rand, E. T.; Svensson, C. E.; Grinyer, G. F.; Thomas, J. C.; Ball, G.; Garnsworthy, A. B.; Hackman, G.; Orce, J. N.; Triambak, S.; Williams, S. J.; Andreoiu, C.; Cross, D.

2013-03-01

A fast plastic scintillator detector is evaluated for possible use in an ongoing program of high-precision half-life measurements of short lived β emitters. Using data taken at TRI-UMF's Isotope Separator and Accelerator Facility with a radioactive 26Na beam, a detailed investigation of potential systematic effects with this new detector setup is being performed. The technique will then be applied to other β-decay half-life measurements including the superallowed Fermi β emitters 10C, 14O, and T = 1/2 decay of 15O.

High-precision 13C and 18O measurements by continuous flow-isotope ratio mass spectrometry (CF-IRMS) in Romanian wines characterization

International Nuclear Information System (INIS)

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

2008-01-01

Wines characterization is an important problem to which isotopic analysis by continuous flow- IRMS has made a significant contribution. 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. There is a strong need for reliable and validated methods to ensure compliance with such regulation and to protect the interests of the consumer. The right to producing wines with an appellation of origin is guaranteed by the Ministry of Agriculture, based on proposals made by the National Office of Vine and Wine (starting with the 1993 vintage year). The Ministry of Agriculture, the National Office for Vine and Wine, and the National Research Institute grants the authentication of the wines with appellation of origin. The present paper emphasize the isotopic analysis for 18 O/ 16 O and 13 C/ 12 C from wines, using a new generation Isotope Ratio MS, CF-IRMS Delta V Plus, coupled with three flexible continuous flow preparation devices (GasBench II and TC Elemental Analyser). (authors)

High Precision Continuous and Real-Time Measurement of Atmospheric Oxygen Using Cavity Ring-Down Spectroscopy.

Science.gov (United States)

Kim-Hak, D.; Hoffnagle, J.; Rella, C.; Sun, M.

2016-12-01

Oxygen is a major and vital component of the Earth atmosphere representing about 21% of its composition. It is consumed or produced through biochemical processes such as combustion, respiration, and photosynthesis. Although atmospheric oxygen is not a greenhouse gas, it can be used as a top-down constraint on the carbon cycle. The variation observations of oxygen in the atmosphere are very small, in the order of the few ppm's. This presents the main technical challenge for measurement as a very high level of precision is required and only few methods including mass spectrometry, fuel cell, and paramagnetic are capable of overcoming it. Here we present new developments of a high-precision gas analyzer that utilizes the technique of Cavity Ring-Down Spectroscopy to measure oxygen concentration and oxygen isotope. Its compact and ruggedness design combined with high precision and long-term stability allows the user to deploy the instrument in the field for continuous monitoring of atmospheric oxygen level. Measurements have a 1-σ 5-minute averaging precision of 1-2 ppm for O2 over a dynamic range of 0-20%. We will present supplemental data acquired from our 10m tower measurements in Santa Clara, CA.

PRECISE - pregabalin in addition to usual care: Statistical analysis plan

NARCIS (Netherlands)

S. Mathieson (Stephanie); L. Billot (Laurent); C. Maher (Chris); A.J. McLachlan (Andrew J.); J. Latimer (Jane); B.W. Koes (Bart); M.J. Hancock (Mark J.); I. Harris (Ian); R.O. Day (Richard O.); J. Pik (Justin); S. Jan (Stephen); C.-W.C. Lin (Chung-Wei Christine)

2016-01-01

textabstractBackground: Sciatica is a severe, disabling condition that lacks high quality evidence for effective treatment strategies. This a priori statistical analysis plan describes the methodology of analysis for the PRECISE study. Methods/design: PRECISE is a prospectively registered, double

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

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

Use of azeotropic distillation for isotopic analysis of deuterium in soil water and saturate saline solution

International Nuclear Information System (INIS)

Santos, Antonio Vieira dos.

1995-05-01

The azeotropic distillation technique was adapted to extract soil water and saturate saline solution, which is similar to the sea water for the Isotopic Determination of Deuterium (D). A soil test was used to determine the precision and the nature of the methodology to extract soil water for stable isotopic analysis, using the azeotropic distillation and comparing with traditional methodology of heating under vacuum. This methodology has been very useful for several kinds of soil or saturate saline solution. The apparatus does not have a memory effect, and the chemical reagents do not affect the isotopic composition of soil water. (author). 43 refs., 10 figs., 12 tabs

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.

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

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.

Measurement of isotopic composition of lanthanides in reprocessing process solutions by high-performance liquid chromatography with inductively coupled plasma mass spectrometry (HPLC/ICP-MS)

International Nuclear Information System (INIS)

Okano, Masanori; Jitsukata, Shu; Kuno, Takehiko; Yamada, Keiji

2011-01-01

Isotopic compositions of fission products in process solutions and wastes in a reprocessing plant are valuable to proceed safety study of the solutions and research/development concerning treatment/disposal of the wastes. The amount of neodymium-148 is a reliable indication to evaluate irradiation history. The isotopic compositions of samarium and gadolinium in high radioactive wastes are referred to as essential data to evaluate environmental impact in geological repositories. However, pretreatment of analysis must be done with complicated chemical separation such as solvent extraction and ion exchange. The actual measurement data of isotopic compositions of lanthanides comparable to the one of actinides in spent fuel reprocessing process has not been obtained enough. Rapid and high sensitive analytical technique based on high-performance liquid chromatography (HPLC) with an inductively coupled plasma mass spectrometry (ICP-MS) has been developed for the measurement of isotopic compositions of lanthanides in spent fuel reprocessing solutions. HPLC/ICP-MS measurement system was customized for a glove-box to be applied to the radioactive solutions. The cation exchange chromatographic columns (Shim-pack IC-C1) and injection valve (20μL) were located inside of the glove-box except the chromatographic pump. The elements of lanthanide group were separated by a gradient program of HPLC with α-hydroxyisobutyric acid. Isotopic compositions of lanthanides in eluate was sequentially analyzed by a quadruple ICP-MS. Optimization of parameter of HPLC and ICP-MS measurement system was examined with standard solutions containing 14 lanthanide elements. The elements of lanthanides were separated by HPLC and detected by ICP-MS within 25 minutes. The detection limits of Nd-146, Sm-147 and Gd-157 were 0.37 μg L -1 , 0.69 μg L -1 and 0.47 μg L -1 , respectively. The analytical precision of the above three isotopes was better than 10% for standard solutions of 100 μg L -1 with

High-Precision Plutonium Isotopic Compositions Measured on Los Alamos National Laboratory’s General’s Tanks Samples: Bearing on Model Ages, Reactor Modelling, and Sources of Material. Further Discussion of Chronometry

Energy Technology Data Exchange (ETDEWEB)

Spencer, Khalil J. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Rim, Jung Ho [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Porterfield, Donivan R. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Roback, Robert Clifford [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Boukhalfa, Hakim [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Stanley, Floyd E. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

2015-06-29

In this study, we re-analyzed late-1940’s, Manhattan Project era Plutonium-rich sludge samples recovered from the ''General’s Tanks'' located within the nation’s oldest Plutonium processing facility, Technical Area 21. These samples were initially characterized by lower accuracy, and lower precision mass spectrometric techniques. We report here information that was previously not discernable: the two tanks contain isotopically distinct Pu not only for the major (i.e., ²⁴⁰Pu, ²³⁹Pu) but trace (²³⁸Pu ,²⁴¹Pu, ²⁴²Pu) isotopes. Revised isotopics slightly changed the calculated ²⁴¹Am-²⁴¹Pu model ages and interpretations.

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.

Laser Spectroscopic Analysis of Liquid Water Samples for Stable Hydrogen and Oxygen Isotopes

International Nuclear Information System (INIS)

2009-01-01

Stable isotope ratios of hydrogen and oxygen are tracers of choice for water cycle processes in hydrological, atmospheric and ecological studies. The use of isotopes has been limited to some extent because of the relatively high cost of isotope ratio mass spectrometers and the need for specialized operational skills. Here, the results of performance testing of a recently developed laser spectroscopic instrument for measuring stable hydrogen and oxygen isotope ratios of water samples are described, along with a procedure for instrument installation and operation. Over the last four years, the IAEA Water Resources Programme conducted prototype and production model testing of these instruments and this publication is the outcome of those efforts. One of the main missions of the IAEA is to promote the use of peaceful applications of isotope and nuclear methods in Member States and this publication is intended to facilitate the use of laser absorption based instruments for hydrogen and oxygen stable isotope analyses of liquid water samples for hydrological and other studies. The instrument uses off-axis integrated cavity output spectroscopy to measure absolute abundances of 2 HHO, HH 18 O, and HHO via laser absorption. Test results using a number of natural and synthetic water standards and samples with a large range of isotope values demonstrate adequate precision and accuracy (e.g. precisions of 1 per mille for δ 2 H and 0.2 per mille for δ 18 O). The laser instrument has much lower initial and maintenance costs than mass spectrometers and is substantially easier to operate. Thus, these instruments have the potential to bring about a paradigm shift in isotope applications by enabling researchers in all fields to measure isotope ratios by themselves. The appendix contains a detailed procedure for the installation and operation of the instrument. Using the procedure, new users should be able to install the instrument in less than two hours. It also provides step

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

NARCIS (Netherlands)

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

2008-01-01

On-line gas chromatography-combustion-isotope ratio mass spectrometry (GC-C-IRMS) is commonly used to measure isotopic ratios at natural abundance as well as for tracer studies in nutritional and medical research. However, high-precision (13)C isotopic enrichment can also be measured by liquid

High spatial resolution and high brightness ion beam probe for in-situ elemental and isotopic analysis

Science.gov (United States)

Long, Tao; Clement, Stephen W. J.; Bao, Zemin; Wang, Peizhi; Tian, Di; Liu, Dunyi

2018-03-01

A high spatial resolution and high brightness ion beam from a cold cathode duoplasmatron source and primary ion optics are presented and applied to in-situ analysis of micro-scale geological material with complex structural and chemical features. The magnetic field in the source as well as the influence of relative permeability of magnetic materials on source performance was simulated using COMSOL to confirm the magnetic field strength of the source. Based on SIMION simulation, a high brightness and high spatial resolution negative ion optical system has been developed to achieve Critical (Gaussian) illumination mode. The ion source and primary column are installed on a new Time-of-Flight secondary ion mass spectrometer for analysis of geological samples. The diameter of the ion beam was measured by the knife-edge method and a scanning electron microscope (SEM). Results show that an O2- beam of ca. 5 μm diameter with a beam intensity of ∼5 nA and an O- beam of ca. 5 μm diameter with a beam intensity of ∼50 nA were obtained, respectively. This design will open new possibilities for in-situ elemental and isotopic analysis in geological studies.

Job/task analysis for I ampersand C [Instrumentation and Controls] instrument technicians at the High Flux Isotope Reactor

International Nuclear Information System (INIS)

Duke, L.L.

1989-09-01

To comply with Department of Energy Order 5480.XX (Draft), a job/task analysis was initiated by the Maintenance Management Department at Oak Ridge National Laboratory (ORNL). The analysis was applicable to instrument technicians working at the ORNL High Flux Isotope Reactor (HFIR). This document presents the procedures and results of that analysis. 2 refs., 2 figs

Analysis of Precision of Activation Analysis Method

DEFF Research Database (Denmark)

Heydorn, Kaj; Nørgaard, K.

1973-01-01

The precision of an activation-analysis method prescribes the estimation of the precision of a single analytical result. The adequacy of these estimates to account for the observed variation between duplicate results from the analysis of different samples and materials, is tested by the statistic T...

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

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

Paradigms in isotope dilution mass spectrometry for elemental speciation analysis

International Nuclear Information System (INIS)

Meija, Juris; Mester, Zoltan

2008-01-01

Isotope dilution mass spectrometry currently stands out as the method providing results with unchallenged precision and accuracy in elemental speciation. However, recent history of isotope dilution mass spectrometry has shown that the extent to which this primary ratio measurement method can deliver accurate results is still subject of active research. In this review, we will summarize the fundamental prerequisites behind isotope dilution mass spectrometry and discuss their practical limits of validity and effects on the accuracy of the obtained results. This review is not to be viewed as a critique of isotope dilution; rather its purpose is to highlight the lesser studied aspects that will ensure and elevate current supremacy of the results obtained from this method

High-precision mass measurements of neutron-deficient Tl isotopes at ISOLTRAP and the development of an ultra-stable voltage source for the PENTATRAP experiment

Energy Technology Data Exchange (ETDEWEB)

Boehm, Christine

2015-01-14

Atomic masses and hence binding energies of nuclides are of great importance for studies of nuclear structure since they reflect all effective interactions in a nucleus. Within this thesis the masses of seven nuclides, namely {sup 194}Au, {sup 194}Hg, {sup 190,193,198}Tl and {sup 202,208}Pb, were determined at the Penning-trap mass spectrometer ISOLTRAP at ISOLDE/CERN. The thallium region in the chart of isotopes is of special interest due to the occurrence of nuclear structure effects like low-lying isomers, level inversion, shape coexistence and deformations. These effects are investigated by applying finite-difference mass formulas, such as the two-neutron separation energies or the so-called empirical pairing gaps. The second topic addressed within the present thesis is an ultra-stable voltage source, called StaReP (Stable Reference for Penning Trap Experiments), which was developed at the Max-Planck-Institut fuer Kernphysik. It is one of the key components of the high-precision mass spectrometer PENTATRAP, containing a tower of five Penning traps. A 25-channel voltage source with a relative stability of few 10{sup -8} over a period of 10 minutes in the range of 0 to -100V is mandatory for PENTATRAP aiming for mass measurements with relative mass uncertainties of ≤ 10{sup -11}. Mass values with such a high precision allow for stringent tests of quantum electrodynamics in strong electric fields, testing Einstein's mass-energy relation E = mc{sup 2} as well as measurements of decay energies (Q-values) with applications in neutrino physics.

High resolution conductometry for isotopic assay of deuterium in mixtures of heavy water and light water

International Nuclear Information System (INIS)

Ananthanarayanan, R.; Sahoo, P.; Murali, N.

2014-01-01

A PC based high resolution conductivity monitoring technique has been deployed for determination of isotopic purity of heavy water in samples containing heavy water and light water mixtures using pulsating sensor based conductivity monitoring instrument. The technique involves accurate determination of conductivities of a series of specially treated heavy water and light water mixtures of various compositions at a constant solution temperature. The shift in conductivity (Δκ), which is the difference between conductivities of composite mixture after and before the formation of a typical complex compound (boric acid–mannitol complex in this case), shows a smooth and reproducible decreasing trend with increase in percentage composition of heavy water. This relation, which is obtained by appropriate calibration, is used in the software program for direct display of isotopic purity of heavy water. The technique is examined for determination of percentage composition of heavy water in the entire range of concentration (0-100 %) with reasonable precision (relative standard deviation, RSD ≤1.5 %). About 1 mL of sample is required for each analysis and analysis is completed within a couple of minutes after pretreatment of sample. The accuracy in measurement is ≤1.75 %. (author)

Mass spectrometric analysis of lithium

International Nuclear Information System (INIS)

Chitambar, S.A.; Kavimandan, V.D.; Aggarwal, S.K.; Ramasubramanian, P.A.; Shah, P.M.; Almoula, A.I.; Acharya, S.N.; Parab, A.R.; Jain, H.C.; Mathews, C.K.; Ramaniah, M.V.

1978-01-01

The details of investigations carried out on the isotopic analysis of lithium using surface ionisation mass spectrometry are presented. Various parameters affecting the precision in isotopic analysis of lithium are discussed. A precision of 1% is achieved in the relative isotope abundance measurement. (author)

Status and outlook of CHIP-TRAP: The Central Michigan University high precision Penning trap

Science.gov (United States)

Redshaw, M.; Bryce, R. A.; Hawks, P.; Gamage, N. D.; Hunt, C.; Kandegedara, R. M. E. B.; Ratnayake, I. S.; Sharp, L.

2016-06-01

At Central Michigan University we are developing a high-precision Penning trap mass spectrometer (CHIP-TRAP) that will focus on measurements with long-lived radioactive isotopes. CHIP-TRAP will consist of a pair of hyperbolic precision-measurement Penning traps, and a cylindrical capture/filter trap in a 12 T magnetic field. Ions will be produced by external ion sources, including a laser ablation source, and transported to the capture trap at low energies enabling ions of a given m / q ratio to be selected via their time-of-flight. In the capture trap, contaminant ions will be removed with a mass-selective rf dipole excitation and the ion of interest will be transported to the measurement traps. A phase-sensitive image charge detection technique will be used for simultaneous cyclotron frequency measurements on single ions in the two precision traps, resulting in a reduction in statistical uncertainty due to magnetic field fluctuations.

a High-Precision Branching-Ratio Measurement for the Superallowed β+ Emitter 74Rb

Science.gov (United States)

Dunlop, R.; Chagnon-Lessard, S.; Finlay, P.; Garrett, P. E.; Hadinia, B.; Leach, K. G.; Svensson, C. E.; Wong, J.; Ball, G.; Garnsworthy, A. B.; Glister, J.; Hackman, G.; Tardiff, E. R.; Triambak, S.; Williams, S. J.; Leslie, J. R.; Andreoiu, C.; Chester, A.; Cross, D.; Starosta, K.; Yates, S. W.; Zganjar, E. F.

2013-03-01

Precision measurements of superallowed Fermi beta decay allow for tests of the Cabibbo-Kobayashi-Maskawa matrix (CKM) unitarity, the conserved vector current hypothesis, and the magnitude of isospin-symmetry-breaking effects in nuclei. A high-precision measurement of the branching ratio for the β+ decay of 74Rb has been performed at the Isotope Separator and ACcelerator (ISAC) facility at TRIUMF. The 8π spectrometer, an array of 20 close-packed HPGe detectors, was used to detect gamma rays emitted following the decay of 74Rb. PACES, an array of 5 Si(Li) detectors, was used to detect emitted conversion electrons, while SCEPTAR, an array of plastic scintillators, was used to detect emitted beta particles. A total of 51γ rays have been identified following the decay of 21 excited states in the daughter nucleus 74Kr.

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

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

Mars Atmospheric Escape Recorded by H, C and O Isotope Ratios in Carbon Dioxide and Water Measured by the Sam Tunable Laser Spectrometer on the Curiosity Rover

Science.gov (United States)

Webster, C. R.; Mahaffy, P. R.; Leshin, L. A.; Atreya, S. K.; Flesch, G. J.; Stern, J.; Christensen, L. E.; Vasavada, A. R.; Owen, T.; Niles, P. B.;

Temperature and void reactivity coefficient calculations for the high flux isotope reactor safety analysis report

International Nuclear Information System (INIS)

Engle, W.W. Jr.; Williams, L.R.

1994-07-01

This report provides documentation of a series of calculations performed in 1991 in order to provide input for the High Flux Isotope Reactor Safety Analysis Report. In particular, temperature and void reactivity coefficients were calculated for beginning-of-life, end-of-life, and xenon equilibrium (29 h) conditions. Much of the data used to prepare the computer models for these calculations was derived from the original HFIR nuclear design study

Analysis of dissolved organic carbon concentration and 13C isotopic signature by TOC-IRMS - assessment of analytical performance

Science.gov (United States)

Kirkels, Frédérique; Cerli, Chiara; Federherr, Eugen; Kalbitz, Karsten

2013-04-01

Stable carbon isotopes provide a powerful tool to assess carbon pools and their dynamics. Dissolved organic carbon (DOC) has been recognized to play an important role in ecosystem functioning and carbon cycling and has therefore gained increased research interest. However, direct measurement of 13C isotopic signature of carbon in the dissolved phase is technically challenging particularly using high temperature combustion. Until recently, mainly custom-made systems existed which were modified for coupling of TOC instruments with IRMS for simultaneous assessment of C content and isotopic signature. The variety of coupled systems showed differences in their analytical performances. For analysis of DOC high temperature combustion is recognized as best performing method, owing to its high efficiency of conversion to CO2 also for highly refractory components (e.g. humic, fulvic acids) present in DOC and soil extracts. Therefore, we tested high temperature combustion TOC coupled to IRMS (developed by Elementar Group) for bulk measurements of DOC concentration and 13C signature. The instruments are coupled via an Interface to exchange the carrier gas from O2 to He and to concentrate the derived CO2 for the isotope measurement. Analytical performance of the system was assessed for a variety of organic compounds characterized by different stability and complexity, including humic acid and DOM. We tested injection volumes between 0.2-3 ml, thereby enabling measurement of broad concentration ranges. With an injection volume of 0.5 ml (n=3, preceded by 1 discarded injection), DOC and 13C signatures for concentrations between 5-150 mg C/L were analyzed with high precision (standard deviation (SD) predominantly TOC-IRMS in comparison with other systems capable of determining C concentration and isotopic signatures. We recognize the advantages of this system providing: - High sample throughput, short measurement time (15 minutes), flexible sample volume - Easy maintenance

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.

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

Isotope analysis in the transmission electron microscope.

Science.gov (United States)

Susi, Toma; Hofer, Christoph; Argentero, Giacomo; Leuthner, Gregor T; Pennycook, Timothy J; Mangler, Clemens; Meyer, Jannik C; Kotakoski, Jani

2016-10-10

The Ångström-sized probe of the scanning transmission electron microscope can visualize and collect spectra from single atoms. This can unambiguously resolve the chemical structure of materials, but not their isotopic composition. Here we differentiate between two isotopes of the same element by quantifying how likely the energetic imaging electrons are to eject atoms. First, we measure the displacement probability in graphene grown from either 12 C or 13 C and describe the process using a quantum mechanical model of lattice vibrations coupled with density functional theory simulations. We then test our spatial resolution in a mixed sample by ejecting individual atoms from nanoscale areas spanning an interface region that is far from atomically sharp, mapping the isotope concentration with a precision better than 20%. Although we use a scanning instrument, our method may be applicable to any atomic resolution transmission electron microscope and to other low-dimensional materials.

Determination of boron isotope ratios by high-resolution continuum source molecular absorption spectrometry using graphite furnace vaporizers

Science.gov (United States)

Abad, Carlos; Florek, Stefan; Becker-Ross, Helmut; Huang, Mao-Dong; Heinrich, Hans-Joachim; Recknagel, Sebastian; Vogl, Jochen; Jakubowski, Norbert; Panne, Ulrich

2017-10-01

Boron isotope amount ratios n(10B)/n(11B) have been determined by monitoring the absorption spectrum of boron monohydride (BH) in a graphite furnace using high-resolution continuum source molecular absorption spectrometry (HR-CS-MAS). Bands (0 → 0) and (1 → 1) for the electronic transition X1Σ+ → A1Π were evaluated around wavelengths 433.1 nm and 437.1 nm respectively. Clean and free of memory effect molecular spectra of BH were recorded. In order to eliminate the memory effect of boron, a combination of 2% (v/v) hydrogen gas in argon and 1% trifluoromethane in argon, an acid solution of calcium chloride and mannitol as chemical modifiers was used. Partial least square regression (PLS) for analysis of samples and reference materials were applied. For this, a spectral library with different isotopes ratios for PLS regression was built. Results obtained around the 433.1 nm and 437.1 nm spectral regions are metrologically compatible with those reported by mass spectrometric methods. Moreover, for the evaluated region of 437 nm, an accuracy of 0.15‰ is obtained as the average deviation from the isotope reference materials. Expanded uncertainties with a coverage factor of k = 2 range between 0.15 and 0.44‰. This accuracy and precision are compatible with those obtained by mass spectrometry for boron isotope ratio measurements.

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)

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

High precision time calibration of the Permian-Triassic boundary mass extinction event in a deep marine context

Science.gov (United States)

Baresel, Björn; Bucher, Hugo; Brosse, Morgane; Bagherpour, Borhan; Schaltegger, Urs

2015-04-01

To construct a revised and high resolution calibrated time scale for the Permian-Triassic boundary (PTB) we use (1) high-precision U-Pb zircon age determinations of a unique succession of volcanic ash layers interbedded with deep water fossiliferous sediments in the Nanpanjiang Basin (South China) combined with (2) accurate quantitative biochronology based on ammonoids, conodonts, radiolarians, and foraminifera and (3) tracers of marine bioproductivity (carbon isotopes) across the PTB. The unprecedented precision of the single grain chemical abrasion isotope-dilution thermal ionization mass spectrometry (CA-ID-TIMS) dating technique at sub-per mil level (radio-isotopic calibration of the PTB at the groups of processes. Using these alignments allows (1) positioning the PTB in different depositional setting and (2) solving the age contradictions generated by the misleading use of the first occurrence (FO) of the conodont Hindeodus parvus, whose diachronous first occurrences are arbitrarily used for placing the base of the Triassic. This new age framework provides the basis for a combined calibration of chemostratigraphic records with high-resolution biochronozones of the Late Permian and Early Triassic. Here, we present new single grain U-Pb zircon data of volcanic ash layers from two deep marine sections (Dongpan and Penglaitan) revealing stratigraphic consistent dates over several volcanic ash layers bracketing the PTB. These analyses define weighted mean 206Pb/238U ages of 251.956±0.033 Ma (Dongpan) and 252.062±0.043 Ma (Penglaitan) for the last Permian ash bed. By calibration with detailed litho- and biostratigraphy new U-Pb ages of 251.953±0.038 Ma (Dongpan) and 251.907±0.033 Ma (Penglaitan) are established for the onset of the Triassic.

From Crustal Anatexis to Pluton Emplacement: High-Precision Zircon Geochronology Reveals the Thermal History of the Larderello-Travale Geothermal System (Italy)

Science.gov (United States)

Farina, F.; Dini, A.; Ovtcharova, M.; Davies, J.; Bouvier, A. S.; Baumgartner, L. P.; Caricchi, L.; Schaltegger, U.

2017-12-01

Late Miocene to recent post-collisional extension in Tuscany (Italy) led to the emplacement of shallow-level granitic plutons and to the eruption of small rhyolitic bodies. The intrusion of peraluminous two-mica and tourmaline-bearing granites triggered the formation of the steam-dominated Larderello-Travale geothermal system. In this study, zircon crystals from granite samples obtained from drill holes at 3.0-4.5 km depth were investigated by combining in-situ oxygen isotopes analysis and high-precision CA-ID-TIMS U-Pb age determinations to gain insight into the nature of the magmatic heat source fuelling the geothermal field. Magmatic zircon crystals display δ18O values ranging from 8.6 to 13.5‰ and crystals from individual samples exhibit inter- and intra-grain oxygen isotope variability exceeding 3‰. The geochronological data indicates the existence of three magmatic pulses with ages between 3.637 ± 0.008 and 1.671 ± 0.004 Ma. More importantly, zircon crystals from individual samples exhibit an age spread as large as 200-400 ky. This age dispersion, which is more than one order of magnitude greater than the uncertainty on a single date, suggest that most of the zircon did not crystallize at the emplacement level, but within isolated and isotopically distinct magma batches before large-scale homogenization in a magmatic reservoir at depth. The rate of assembly and final volume of this reservoir is estimated using the distribution of precise U-Pb zircon dates following the approach of Caricchi et al. (2014). Thermal modelling indicates that the heat flow at the surface in the geothermal field cannot be sustained by the inferred reservoir or by heat advection from the mantle. Our data suggest the existence of a younger shallow-level intrusion, whose occurrence also accounts for the existence of confined magmatic fluids at the top of the Larderello-Travale intrusion. We conclude that a multi-disciplinary approach, integrating high-precision zircon dating, in

High-precision analysis on annual variations of heavy metals, lead isotopes and rare earth elements in mangrove tree rings by inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Yu Kefu; Kamber, Balz S.; Lawrence, Michael G.; Greig, Alan; Zhao Jianxin

2007-01-01

Annual variations from 1982 to 1999 of a wide range of trace elements and reconnaissance Pb isotopes ( 207 Pb/ 206 Pb and 208 Pb/ 206 Pb) were analyzed by solution ICP-MS on digested ash from mangrove Rhizophora apiculata, obtained from Leizhou Peninsula, along northern coast of South China Sea. The concentrations of the majority of elements show a weak declining trend with growth from 1982 to 1999, punctuated by several high concentration spikes. The declining trends are positively correlated with ring width and negatively correlated with inferred water-use efficiency, suggesting a physiological control over metal-uptake in this species. The episodic metal concentration-peaks cannot be interpreted with lateral movement or growth activities and appear to be related to environmental pollution events. Pb isotope ratios for most samples plot along the 'Chinese Pb line' and clearly document the importance of gasoline Pb as a source of contaminant. Shale-normalised REE + Y patterns are relatively flat and consistent across the growth period, with all patterns showing a positive Ce anomaly and elevated Y/Ho ratio. The positive Ce anomaly is observed regardless of the choice of normaliser, in contrast to previously reported REE patterns for terrestrial and marine plants. This pilot study of trace element, REE + Y and Pb isotope distribution in mangrove tree rings indicates the potential use of mangroves as monitors of historical environmental change

Isotopic Ratios of Samarium by TIMS for Nuclear Forensic Application

Energy Technology Data Exchange (ETDEWEB)

Louis Jean, James [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Inglis, Jeremy David [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

2017-08-08

The isotopic ratio of Nd, Sm, and Gd can provide important information regarding fissile material (nuclear devices, reactors), neutron environment, and device yield. These studies require precise measurement of Sm isotope ratios, by either TIMS or MC-ICP-MS. There has been an increasing trend to measure smaller and smaller quantities of Sm bearing samples. In nuclear forensics 10-100 ng of Sm are needed for precise measurement. To measure sub-ng Sm samples using TIMS for nuclear forensic analysis.

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

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.

Continuous-flow isotope ratio mass spectrometry method for carbon and hydrogen isotope measurements on atmospheric methane

Directory of Open Access Journals (Sweden)

M. Brass

2010-12-01

Full Text Available We describe a continuous-flow isotope ratio mass spectrometry (CF-IRMS technique for high-precision δD and δ¹³C measurements of atmospheric methane on 40 mL air samples. CH₄ is separated from other air components by utilizing purely physical processes based on temperature, time and mechanical valve switching. Chemical agents are avoided. Trace amounts of interfering compounds can be separated by gas chromatography after pre-concentration of the CH₄ sample. The purified sample is then either combusted to CO₂ or pyrolyzed to H₂ for stable isotope measurement. Apart from connecting samples and refilling liquid nitrogen as coolant the system is fully automated and allows an unobserved, continuous analysis of samples. The analytical system has been used for analysis of air samples with CH₄ mixing ratios between ~100 and ~10 000 ppb, for higher mixing ratios samples usually have to be diluted.

Isotope Ratio Monitoring Gas Chromatography Mass Spectrometry (IRM-GCMS)

International Nuclear Information System (INIS)

Freeman, K.H.; Ricci, S.A.; Studley, A.; Hayes, J.M.

1989-01-01

On Earth, the C-13 content of organic compounds is depleted by roughly 13 to 23 permil from atmospheric carbon dioxide. This difference is largely due to isotope effects associated with the fixation of inorganic carbon by photosynthetic organisms. If life once existed on Mars, then it is reasonable to expect to observe a similar fractionation. Although the strongly oxidizing conditions on the surface of Mars make preservation of ancient organic material unlikely, carbon-isotope evidence for the existence of life on Mars may still be preserved. Carbon depleted in C-13 could be preserved either in organic compounds within buried sediments, or in carbonate minerals produced by the oxidation of organic material. A technique is introduced for rapid and precise measurement of the C-13 contents of individual organic compounds. A gas chromatograph is coupled to an isotope-ratio mass spectrometer through a combustion interface, enabling on-line isotopic analysis of isolated compounds. The isotope ratios are determined by integration of ion currents over the course of each chromatographic peak. Software incorporates automatic peak determination, corrections for background, and deconvolution of overlapped peaks. Overall performance of the instrument was evaluated by the analysis of a mixture of high purity n-alkanes of know isotopic composition. Isotopic values measured via IRM-GCMS averaged withing 0.55 permil of their conventionally measured values

The status of applying stable isotope in the studies of environmental science

International Nuclear Information System (INIS)

Bai Zhipeng; Zhang Liwen; Zhu Tan; Feng Yinchang

2007-01-01

The stable isotope composition is characteristic in the pollution source, and it is relatively fixed in the process of transferring and reaction. At present the precise analysis result of stable isotope ratio can be obtained easily. So the stable isotopes can be applied to the pollution affair arbitration and source study. The concept and analytical method of stable isotopes are introduced. The research status of the stable isotopes in the field of environmental science and the isotope fractionation is reviewed. (authors)

Method of high precision interval measurement in pulse laser ranging system

Science.gov (United States)

Wang, Zhen; Lv, Xin-yuan; Mao, Jin-jin; Liu, Wei; Yang, Dong

2013-09-01

Laser ranging is suitable for laser system, for it has the advantage of high measuring precision, fast measuring speed,no cooperative targets and strong resistance to electromagnetic interference,the measuremen of laser ranging is the key paremeters affecting the performance of the whole system.The precision of the pulsed laser ranging system was decided by the precision of the time interval measurement, the principle structure of laser ranging system was introduced, and a method of high precision time interval measurement in pulse laser ranging system was established in this paper.Based on the analysis of the factors which affected the precision of range measure,the pulse rising edges discriminator was adopted to produce timing mark for the start-stop time discrimination,and the TDC-GP2 high precision interval measurement system based on TMS320F2812 DSP was designed to improve the measurement precision.Experimental results indicate that the time interval measurement method in this paper can obtain higher range accuracy. Compared with the traditional time interval measurement system,the method simplifies the system design and reduce the influence of bad weather conditions,furthermore,it satisfies the requirements of low costs and miniaturization.

High sensitivity isotope analysis with a 252Cf--235U fueled subcritical multiplier and low background photon detector systems

International Nuclear Information System (INIS)

Wogman, N.A.; Rieck, H.G. Jr.; Laul, J.C.; MacMurdo, K.W.

1976-09-01

A 252 Cf activation analysis facility has been developed for routine multielement analysis of a wide variety of solid and liquid samples. The facility contains six sources of 252 Cf totaling slightly over 100 mg. These sources are placed in a 93 percent 235 U-enriched uranium core which is subcritical with a K effective of 0.985 (multiplication factor of 66). The system produces a thermal flux on the order of 10 +1 neutrons per square centimeter per second. A pneumatic rabbit system permits automatic irradiation, decay, and counting regimes to be performed unattended on the samples. The activated isotopes are analyzed through their photon emissions with state-of-the-art intrinsic Ge detectors, Ge(Li) detectors, and NaI(Tl) multidimensional gamma ray spectrometers. High efficiency (25 percent), low background, anticoincidence shielded Ge(Li) gamma ray detector systems have been constructed to provide the lowest possible background, yet maintain a peak to Compton ratio of greater than 1000 to 1. The multidimensional gamma ray spectrometer systems are composed of 23 cm diameter x 20 cm thick NaI(Tl) crystals surrounded by NaI(Tl) anticoincidence shields. The detection limits for over 65 elements have been determined for this system. Over 40 elements are detectable at the 1 part per million level at a precision of +-10 percent

An evaluation of a single-step extraction chromatography separation method for Sm-Nd isotope analysis of micro-samples of silicate rocks by high-sensitivity thermal ionization mass spectrometry

International Nuclear Information System (INIS)

Li Chaofeng; Li Xianhua; Li Qiuli; Guo Jinghui; Li Xianghui; Liu Tao

2011-01-01

Graphical abstract: Distribution curve of all eluting fractions for a BCR-2 (1-2-3.5-7 mg) on LN column using HCl and HF as eluting reagent. Highlights: → This analytical protocol affords a simple and rapid analysis for Sm and Nd isotope in minor rock samples. → The single-step separation method exhibits satisfactory separation effect for complex silicate samples. → Corrected 143 Nd/ 144 Nd data show excellent accuracy even if the 140 Ce 16 O + / 144 Nd 16 O + ratio reached to 0.03. - Abstract: A single-step separation scheme is presented for Sm-Nd radiogenic isotope system on very small samples (1-3 mg) of silicate rock. This method is based on Eichrom LN Spec chromatographic material and affords a straightforward separation of Sm-Nd from complex matrix with good purity and satisfactory blank levels, suitable for thermal ionization mass spectrometry (TIMS). This technique, characterized by high efficiency (single-step Sm-Nd separation) and high sensitivity (TIMS on NdO + ion beam), is able to process rapidly (3-4 h), with low procedure blanks ( 143 Nd/ 144 Nd ratios and Sm-Nd concentrations are presented for eleven international silicate rock reference materials, spanning a wide range of Sm-Nd contents and bulk compositions. The analytical results show a good agreement with recommended values within ±0.004% for the 143 Nd/ 144 Nd isotopic ratio and ±2% for Sm-Nd quantification at the 95% confidence level. It is noted that the uncertainty of this method is about 3 times larger than typical precision achievable with two-stage full separation followed by state-of-the-art conventional TIMS using Nd + ion beams which require much larger amounts of Nd. Hence, our single-step separation followed by NdO + ion beam technique is preferred to the analysis for microsamples.

High-precision half-life and branching-ratio measurements for superallowed Fermi β+ emitters at TRIUMF - ISAC

Science.gov (United States)

Laffoley, A. T.; Dunlop, R.; Finlay, P.; Grinyer, G. F.; Andreoiu, C.; Austin, R. A. E.; Ball, G. C.; Bandyopadhyay, D.; Blank, B.; Bouzomita, H.; Chagnon-Lessard, S.; Chester, A.; Cross, D. S.; Demand, G.; Diaz Varela, A.; Djongolov, M.; Ettenauer, S.; Garnsworthy, A. B.; Garrett, P. E.; Giovinazzo, J.; Glister, J.; Green, K. L.; Hackman, G.; Hadinia, B.; Jamieson, D. S.; Ketelhut, S.; Leach, K. G.; Leslie, J. R.; Pearson, C. J.; Phillips, A. A.; Rand, E. T.; Starosta, K.; Sumithrarachchi, C. S.; Svensson, C. E.; Tardiff, E. R.; Thomas, J. C.; Towner, I. S.; Triambak, S.; Unsworth, C.; Williams, S. J.; Wong, J.; Yates, S. W.; Zganjar, E. F.

2014-03-01

A program of high-precision half-life and branching-ratio measurements for superallowed Fermi β emitters is being carried out at TRIUMF's Isotope Separator and Accelerator (ISAC) radioactive ion beam facility. Recent half-life measurements for the superallowed decays of 14O, 18Ne, and 26Alm, as well as branching-ratio measurements for 26Alm and 74Rb are reported. These results provide demanding tests of the Standard Model and the theoretical isospin symmetry breaking (ISB) corrections in superallowed Fermi β decays.

High-Precision U-Pb Geochronology and Correlation: An example Using the Neoproterozic-Cambrian Transition

Science.gov (United States)

Bowring, S. A.; Grotzinger, J. P.; Amthor, J.; Martin, M. E.

2001-05-01

The precise, global correlation of Precambrian and Paleozoic sedimentary rocks can be achieved using temporally calibrated chemostratigraphic records. This approach is essential for determining rates and causes of environmental and faunal change, including mass extinctions. For example, The Neoproterozoic is marked by major environmental change, including periods of global glaciation, large fluctuations in the sequestration of carbon and major tectonic reorganization followed by the explosive diversification of animals in the earliest Cambrian. The extreme climatic change associated with these glaciations have been implicated as a possible trigger for the Cambrian explosion. The recognition of thin zircon-bearing air-fall ash in Neoproterozoic and Cambrian rocks has allowed the establishment of a high-precision temporal framework for animal evolution and is helping to untangle the history of glaciations. In some cases analytical uncertainties translate to age uncertainties of less than 1 Ma and when integrated with chemostratigraphy, the potential for global correlations at even higher resolution. Progress in the global correlation of Neoproterozoic strata has been achieved through the use of C and Sr isotope chemostratigraphy although it has been hampered by a lack of precise geochronological and faunal control. For example, the period from ca 800-580 Ma is characterized by at least two and perhaps as many as four glacial events that are interpreted by many to be global glaciations on a "Snowball Earth". A lack of precise chronological constraints on the number and duration of glaciations, multiple large excursions in the carbon isotopic record, and an absence of detailed biostratigraphy have complicated global correlation and hindered our understanding of this important period of Earth history. However, the ongoing integration of chemostratigraphic and geochronological data are improving temporal resolution and detailed correlations. These data are critical for

Oxygen Isotopes in Chondritic Interplanetary Dust: Parent-Bodies and Nebular Oxygen Reservoirs

International Nuclear Information System (INIS)

Aleon, J; McKeegan, K D; Leshin, L

2006-01-01

Planetary objects have preserved various amounts of oxygen issued from isotopically different oxygen reservoirs reflecting their origin and physico-chemical history. An 16 O-rich component is preserved in refractory inclusions (CAIs) whereas meteorites matrices are enriched in an 16 O-poor component. The origin of these components is still unclear. The most recent models are based on isotope selective photodissociation of CO in a 16 O-rich nebula/presolr cloud resulting in a 16 O-poor gas in the outer part of the nebula. However because most meteorite components are thought to be formed in the inner 3AU of the solar nebula, the precise isotopic composition of outer solar system components is yet unknown. In that respect, the oxygen isotopic composition of cometary dust is a key to understand the origin of the solar system. The Stardust mission will bring back to the Earth dust samples from comet Wild2, a short period comet from the Jupiter family. A precise determination of the oxygen isotope composition of Wild2 dust grains is essential to decipher the oxygen reservoirs of the outer solar system. However, Stardust samples may be extremely fragmented upon impact in the collector. In addition, interplanetary dust particles (IDPs) collected in the stratosphere are likely to contain comet samples. Therefore, they started to investigate the oxygen isotopic composition of a suite of chondritic interplanetary dust particles that includes IDPs of potential cometary origin using a refined procedure to increase the lateral resolution for the analysis of Stardust grains or IDP subcomponents down to ∼ 3 (micro)m. High precision data for 4 IDPs were previously reported, here they have measured 6 additional IDPs

High Precision Edge Detection Algorithm for Mechanical Parts

Science.gov (United States)

Duan, Zhenyun; Wang, Ning; Fu, Jingshun; Zhao, Wenhui; Duan, Boqiang; Zhao, Jungui

2018-04-01

High precision and high efficiency measurement is becoming an imperative requirement for a lot of mechanical parts. So in this study, a subpixel-level edge detection algorithm based on the Gaussian integral model is proposed. For this purpose, the step edge normal section line Gaussian integral model of the backlight image is constructed, combined with the point spread function and the single step model. Then gray value of discrete points on the normal section line of pixel edge is calculated by surface interpolation, and the coordinate as well as gray information affected by noise is fitted in accordance with the Gaussian integral model. Therefore, a precise location of a subpixel edge was determined by searching the mean point. Finally, a gear tooth was measured by M&M3525 gear measurement center to verify the proposed algorithm. The theoretical analysis and experimental results show that the local edge fluctuation is reduced effectively by the proposed method in comparison with the existing subpixel edge detection algorithms. The subpixel edge location accuracy and computation speed are improved. And the maximum error of gear tooth profile total deviation is 1.9 μm compared with measurement result with gear measurement center. It indicates that the method has high reliability to meet the requirement of high precision measurement.

Optimization of on-line hydrogen stable isotope ratio measurements of halogen- and sulfur-bearing organic compounds using elemental analyzer-chromium/high-temperature conversion isotope ratio mass spectrometry (EA-Cr/HTC-IRMS).

Science.gov (United States)

Gehre, Matthias; Renpenning, Julian; Geilmann, Heike; Qi, Haiping; Coplen, Tyler B; Kümmel, Steffen; Ivdra, Natalija; Brand, Willi A; Schimmelmann, Arndt

2017-03-30

Accurate hydrogen isotopic analysis of halogen- and sulfur-bearing organics has not been possible with traditional high-temperature conversion (HTC) because the formation of hydrogen-bearing reaction products other than molecular hydrogen (H 2 ) is responsible for non-quantitative H 2 yields and possible hydrogen isotopic fractionation. Our previously introduced, new chromium-based EA-Cr/HTC-IRMS (Elemental Analyzer-Chromium/High-Temperature Conversion Isotope Ratio Mass Spectrometry) technique focused primarily on nitrogen-bearing compounds. Several technical and analytical issues concerning halogen- and sulfur-bearing samples, however, remained unresolved and required further refinement of the reactor systems. The EA-Cr/HTC reactor was substantially modified for the conversion of halogen- and sulfur-bearing samples. The performance of the novel conversion setup for solid and liquid samples was monitored and optimized using a simultaneously operating dual-detection system of IRMS and ion trap MS. The method with several variants in the reactor, including the addition of manganese metal chips, was evaluated in three laboratories using EA-Cr/HTC-IRMS (on-line method) and compared with traditional uranium-reduction-based conversion combined with manual dual-inlet IRMS analysis (off-line method) in one laboratory. The modified EA-Cr/HTC reactor setup showed an overall H 2 -recovery of more than 96% for all halogen- and sulfur-bearing organic compounds. All results were successfully normalized via two-point calibration with VSMOW-SLAP reference waters. Precise and accurate hydrogen isotopic analysis was achieved for a variety of organics containing F-, Cl-, Br-, I-, and S-bearing heteroelements. The robust nature of the on-line EA-Cr/HTC technique was demonstrated by a series of 196 consecutive measurements with a single reactor filling. The optimized EA-Cr/HTC reactor design can be implemented in existing analytical equipment using commercially available material and

High-speed precision motion control

CERN Document Server

Yamaguchi, Takashi; Pang, Chee Khiang

2011-01-01

Written for researchers and postgraduate students in Control Engineering, as well as professionals in the Hard Disk Drive industry, this book discusses high-precision and fast servo controls in Hard Disk Drives (HDDs). The editors present a number of control algorithms that enable fast seeking and high precision positioning, and propose problems from commercial products, making the book valuable to researchers in HDDs. Each chapter is self contained, and progresses from concept to technique, present application examples that can be used within automotive, aerospace, aeronautical, and manufactu

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

Science.gov (United States)

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

2008-10-01

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

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.

High - speed steel for precise cased tools

International Nuclear Information System (INIS)

Karwiarz, J.; Mazur, A.

2001-01-01

The test results of high-vanadium high - speed steel (SWV9) for precise casted tools are presented. The face -milling cutters of NFCa80A type have been tested in industrial operating conditions. An average life - time of SWV9 steel tools was 3-10 times longer compare to the conventional high - speed milling cutters. Metallography of SWB9 precise casted steel revealed beneficial for tool properties distribution of primary vanadium carbides in the steel matrix. Presented results should be a good argument for wide application of high - vanadium high - speed steel for precise casted tools. (author)

High-precision gamma-ray spectroscopy of 82Rb and 72As, two important medical isotopes used in positron emission tomography

Science.gov (United States)

Nino, Michael; McCutchan, E.; Smith, S.; Sonzogni, A.; Muench, L.; Greene, J.; Carpenter, M.; Zhu, S.; Lister, C.

2015-10-01

Both 82Rb and 72As are very important medical isotopes used in imaging procedures, yet their full decay schemes were last studied decades ago using low-sensitivity detection systems; high quality decay data is necessary to determine the total dose received by the patient, the background in imaging technologies, and shielding requirements in production facilities. To improve the decay data of these two isotopes, sources were produced at the Brookhaven Linac Isotope Producer (BLIP) and then the Gammasphere array, consisting of 89 Compton-suppressed HPGe detectors, at Argonne National Laboratory was used to analyze the gamma-ray emissions from the daughter nuclei 82 Kr and 72 Ge. Gamma-ray singles and coincidence information were recorded and analyzed using Radware Gf3m software. Significant revisions were made to the level schemes including the observation of many new transitions and levels as well as a reduction in uncertainty on measured γ-ray intensities and deduced β-feedings. The new decay schemes as well as their impact on dose calculations will be presented. DOE Isotope Program is acknowledged for funding ST5001030. Work supported by the U.S. DOE under Grant No. DE-FG02-94ER40848 and Contract Nos. DE-AC02-98CH10946 and DE-AC02-06CH11357 and by the Science Undergraduate Laboratory Internships Program (SULI).

Development of High Precision Tsunami Runup Calculation Method Coupled with Structure Analysis

Science.gov (United States)

Arikawa, Taro; Seki, Katsumi; Chida, Yu; Takagawa, Tomohiro; Shimosako, Kenichiro

2017-04-01

The 2011 Great East Japan Earthquake (GEJE) has shown that tsunami disasters are not limited to inundation damage in a specified region, but may destroy a wide area, causing a major disaster. Evaluating standing land structures and damage to them requires highly precise evaluation of three-dimensional fluid motion - an expensive process. Our research goals were thus to develop a coupling STOC-CADMAS (Arikawa and Tomita, 2016) coupling with the structure analysis (Arikawa et. al., 2009) to efficiently calculate all stages from tsunami source to runup including the deformation of structures and to verify their applicability. We also investigated the stability of breakwaters at Kamaishi Bay. Fig. 1 shows the whole of this calculation system. The STOC-ML simulator approximates pressure by hydrostatic pressure and calculates the wave profiles based on an equation of continuity, thereby lowering calculation cost, primarily calculating from a e epi center to the shallow region. As a simulator, STOC-IC solves pressure based on a Poisson equation to account for a shallower, more complex topography, but reduces computation cost slightly to calculate the area near a port by setting the water surface based on an equation of continuity. CS3D also solves a Navier-Stokes equation and sets the water surface by VOF to deal with the runup area, with its complex surfaces of overflows and bores. STR solves the structure analysis including the geo analysis based on the Biot's formula. By coupling these, it efficiently calculates the tsunami profile from the propagation to the inundation. The numerical results compared with the physical experiments done by Arikawa et. al.,2012. It was good agreement with the experimental ones. Finally, the system applied to the local situation at Kamaishi bay. The almost breakwaters were washed away, whose situation was similar to the damage at Kamaishi bay. REFERENCES T. Arikawa and T. Tomita (2016): "Development of High Precision Tsunami Runup

Precise isotope analysis. Application of accelerator mass spectrometry to human sample

International Nuclear Information System (INIS)

Tokanai, Fuyuki

2016-01-01

Isotope 14 C is a radioisotope with a half-life of 5,730 years, and the measurement of its concentration makes it possible to calculate 'carbon 14 age.' This paper introduces up-to-date accelerator mass spectrometry (AMS), which is used in 14 C concentration measurement, and outlines its applied researches in pharmaceutical and medical fields. AMS technique has been applied in Europe and the United States to microdose clinical tests. In Japan, implementation foundation has been ready through the guidelines of the Ministry of Health, Labour and Welfare, five years behind Europe and the United States. Although conventional AMS measurement of 14 C required an acceleration voltage of 3 million volts or more, technological development has enabled a high accuracy of 14 C concentration measurement with the low acceleration voltage of about 400,000 volts. A sample for AMS method is graphitized, transformed to carbon ions ( 12 C-, 13 C-, and 14 C-) through negative ionization with cesium irradiation, accelerated under 450 kV, bombarded with argon gas, charge-converted to 12 C+, 13 C+, and 14 C+, and measured. Biological samples for microdose study are plasma, urine, feces, and biological tissue. Model tests showed a very good linearity between the concentrations of 14 C-containing compounds and 14 C concentrations. Applied research on microdose clinical tests is expected to increase its usability in the future, as an effective means of drug development. (A.O.)

Development of a highly precise ID-ICP-SFMS method for analysis of low concentrations of lead in rice flour reference materials.

Science.gov (United States)

Zhu, Yanbei; Inagaki, Kazumi; Yarita, Takashi; Chiba, Koichi

2008-07-01

Microwave digestion and isotope dilution inductively coupled plasma mass spectrometry (ID-ICP-SFMS) has been applied to the determination of Pb in rice flour. In order to achieve highly precise determination of low concentrations of Pb, the digestion blank for Pb was reduced to 0.21 ng g(-1) after optimization of the digestion conditions, in which 20 mL analysis solution was obtained after digestion of 0.5 g rice flour. The observed value of Pb in a non-fat milk powder certified reference material (CRM), NIST SRM 1549, was 16.8 +/- 0.8 ng g(-1) (mean +/- expanded uncertainty, k = 2; n = 5), which agreed with the certified value of 19 +/- 3 ng g(-1) and indicated the effectiveness of the method. Analytical results for Pb in three brown rice flour CRMs, NIST SRM 1568a, NIES CRM 10-a, and NIES CRM 10-b, were 7.32 +/- 0.24 ng g(-1) (n = 5), 1010 +/- 10 ng g(-1) (n = 5), and 1250 +/- 20 ng g(-1) (n = 5), respectively. The concentration of Pb in a candidate white rice flour reference material (RM) sample prepared by the National Metrology Institute of Japan (NMIJ) was observed to be 4.36 +/- 0.28 ng g(-1) (n = 10 bottles).

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

Science.gov (United States)

Koehler, Geoff; Wassenaar, Leonard I

2012-04-17

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

Nuclear material safeguards surveillance and accountancy by isotope correlation techniques

International Nuclear Information System (INIS)

Persiani, P.J.; Goleb, J.A.

1981-01-01

This paper presents the initial phase of the US study program and involves the computation of isotopic correlations for the LMFBR fuel cycle. The LWR fuel cycle phase of the study is currently in progress. The selection of the more safeguards effective functionals will depend not only on the level of reliability of isotope correlation technique (ICT) for verification, but also on the capability and difficulty of developing measurement methods. Performance characteristics of existing and proposed isotopic measurement techniques cover the general areas including assay and isotopic wet chemistry and NDA: (1) simultaneous multicomponent analysis techniques, (2) mass spectrometry, (3) x-ray fluorescence or densitometry with high flux monochromatic x-ray sources and high dispersion spectrometers, (4) passive and active neutron interrogation, (5) high level gamma-ray spectroscopy, (6) coulometry, and (7) potentiometry. The measurement capabilities and inherent limitations of these systems are to be evaluated in terms of total systems, operational mode, sample preparation requirements and consequent effect on dissolver solution representation, accuracy and precision estimates (if available), development status of the technique, and development requirements. The isotopic correlation technique shows considerable promise for use in verifying the initial isotopic composition and burnup of discharged assemblies based on the measured ratios of several key isotopes, obtained probably at the dissolver stage in reprocessing. This technique should, for example, easily be capable of indicating the exchange of a blanket assembly for a fuel assembly

Precision mechatronics based on high-precision measuring and positioning systems and machines

Science.gov (United States)

Jäger, Gerd; Manske, Eberhard; Hausotte, Tino; Mastylo, Rostyslav; Dorozhovets, Natalja; Hofmann, Norbert

2007-06-01

Precision mechatronics is defined in the paper as the science and engineering of a new generation of high precision systems and machines. Nanomeasuring and nanopositioning engineering represents important fields of precision mechatronics. The nanometrology is described as the today's limit of the precision engineering. The problem, how to design nanopositioning machines with uncertainties as small as possible will be discussed. The integration of several optical and tactile nanoprobes makes the 3D-nanopositioning machine suitable for various tasks, such as long range scanning probe microscopy, mask and wafer inspection, nanotribology, nanoindentation, free form surface measurement as well as measurement of microoptics, precision molds, microgears, ring gauges and small holes.

High Precision Edge Detection Algorithm for Mechanical Parts

Directory of Open Access Journals (Sweden)

Duan Zhenyun

2018-04-01

Full Text Available High precision and high efficiency measurement is becoming an imperative requirement for a lot of mechanical parts. So in this study, a subpixel-level edge detection algorithm based on the Gaussian integral model is proposed. For this purpose, the step edge normal section line Gaussian integral model of the backlight image is constructed, combined with the point spread function and the single step model. Then gray value of discrete points on the normal section line of pixel edge is calculated by surface interpolation, and the coordinate as well as gray information affected by noise is fitted in accordance with the Gaussian integral model. Therefore, a precise location of a subpixel edge was determined by searching the mean point. Finally, a gear tooth was measured by M&M3525 gear measurement center to verify the proposed algorithm. The theoretical analysis and experimental results show that the local edge fluctuation is reduced effectively by the proposed method in comparison with the existing subpixel edge detection algorithms. The subpixel edge location accuracy and computation speed are improved. And the maximum error of gear tooth profile total deviation is 1.9 μm compared with measurement result with gear measurement center. It indicates that the method has high reliability to meet the requirement of high precision measurement.

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.

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

Development of Exact Matrix-Matching Inductively Coupled Plasma-Optical Emission Spectroscopy for the Analysis of Cu and K in Infant Formula

Energy Technology Data Exchange (ETDEWEB)

Lee, Ye-Ji; Yim, Yong-Hyeon [University of Science and Technology, Daejeon (Korea, Republic of); Heo, Sung Woo; Han, Myung-Sub; Lim, Youngran [Korea Research Institute of Standards and Science, Daejeon (Korea, Republic of)

2016-08-15

In the present study, we have developed an exact matrix-matching inductively coupled plasma-optical emission spectroscopy (ICP-OES) as a low-cost alternative to the isotope dilution inductively coupled plasma mass spectrometry (ICP-MS) method for accurate and precise measurements of nutrient elements K and Cu in infant formula. In spite of its high precision and accuracy, ICP-OES analysis of complex samples was not reliable due to biases originating from various matrix effects. The elaborated exact matrix-matching approach tested here demonstrated its potential to minimize biases due to matrix mismatch. The exact matrix-matching ICP-OES method was successfully validated by comparing the results with those from an isotope dilution ICP-M S method. Because the model provides reliable results without significant loss of precision, it will be an excellent choice for major element analysis in a complex sample, especially when isotope dilution is not applicable due to the l ck of alternative isotopes or the high cost of enriched isotopes.

Isotopic analysis of plutonium by optical spectroscopy; Analyse isotopique du plutonium par spectroscopie optique

Energy Technology Data Exchange (ETDEWEB)

Artaud, J; Chaput, M; Gerstenkorn, S [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

1961-07-01

Isotopic analysis of mixtures of plutonium 239 and 240 has been carried out by means of the photo-electric spectrometer Fabry-Perot, the source being a hollow cathode cooled by liquid nitrogen. This first research has been concerned with finding among the spectral lines given by the hollow cathode, those suitable for use in analysis. Actually, the relative precision is of the order of 2 per cent (for samples containing 3 per cent of {sup 240}Pu). The study of the reproducibility of the measurements should make it possible to increase the precision; the relative precision which can be expected from this method should be 1 per cent for mixtures containing 1 per cent of {sup 240}Pu. (author) [French] L'analyse isotopique des melanges de plutonium 239 et 240 a ete effectuee a l'aide du spectrometre photoelectrique Fabry-Perot, la source etant une cathode creuse refroidie a l'azote liquide. Ce premier travail a eu pour but de discerner parmi les raies spectrales emises par la cathode creuse, celles susceptibles de servir de raies d'analyse. Actuellement, la precision relative est de l'ordre de 2 pour cent (pour des echantillons contenant 3 pour cent de {sup 240}Pu). L'etude de la reproductibilite des mesures devrait permettre d'ameliorer la precision; la precision relative que l'on pourrait atteindre par cette methode serait de 1 pour cent pour des melanges contenant 1 pour cent de {sup 240}Pu. (auteur)

37Cl/35Cl isotope ratio analysis in perchlorate by ion chromatography/multi collector -ICPMS: Analytical performance and implication for biodegradation studies.

Science.gov (United States)

Zakon, Yevgeni; Ronen, Zeev; Halicz, Ludwik; Gelman, Faina

2017-10-01

In the present study we propose a new analytical method for 37 Cl/ 35 Cl analysis in perchlorate by Ion Chromatography(IC) coupled to Multicollector Inductively Coupled Plasma Mass Spectrometry (MC-ICPMS). The accuracy of the analytical method was validated by analysis of international perchlorate standard materials USGS-37 and USGS -38; analytical precision better than ±0.4‰ was achieved. 37 Cl/ 35 Cl isotope ratio analysis in perchlorate during laboratory biodegradation experiment with microbial cultures enriched from the contaminated soil in Israel resulted in isotope enrichment factor ε 37 Cl = -13.3 ± 1‰, which falls in the range reported previously for perchlorate biodegradation by pure microbial cultures. The proposed analytical method may significantly simplify the procedure for isotope analysis of perchlorate which is currently applied in environmental studies. Copyright © 2017. Published by Elsevier Ltd.

Quantitative imaging of subcellular metabolism with stable isotopes and multi-isotope imaging mass spectrometry

Science.gov (United States)

Steinhauser, Matthew L.; Lechene, Claude P.

2014-01-01

Multi-isotope imaging mass spectrometry (MIMS) is the quantitative imaging of stable isotope labels in cells with a new type of secondary ion mass spectrometer (NanoSIMS). The power of the methodology is attributable to (i) the immense advantage of using non-toxic stable isotope labels, (ii) high resolution imaging that approaches the resolution of usual transmission electron microscopy and (iii) the precise quantification of label down to 1 part-per-million and spanning several orders of magnitude. Here we review the basic elements of MIMS and describe new applications of MIMS to the quantitative study of metabolic processes including protein and nucleic acid synthesis in model organisms ranging from microbes to humans. PMID:23660233

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.

Are Polyatomic Interferences, Cross Contamination, Mixing-Effect, etc., Obstacles for the Use of Laser Ablation-ICP-MS Coupling as an Operational Technique for Uranium Isotope Ratio Particle Analysis?

International Nuclear Information System (INIS)

Donard, A.; Pointurier, F.; Pecheyran, C.

2015-01-01

Analysis of ''environmental samples'', which consists in dust collected with cotton clothes wiped by inspectors on surfaces inside declared nuclear facilities, is a key tool for safeguards. Although two methods (fission tracks-TIMS and SIMS) are already used routinely to determine the isotopic composition of uranium particles, the laser ablationinductively coupled plasma mass spectrometry (LA-ICP-MS) coupling has been proven to be an interesting option thanks to its rapidity, high sensitivity and high signal/noise ratio. At CEA and UPPA, feasibility of particle analysis using a nanosecond LA device and a quadrupole ICP-MS has been demonstrated. However, despite the obvious potential of LA-ICP-MS for particle analysis, the effect of many phenomena which may bias isotope ratio measurements or lead to false detections must be investigated. Actually, environmental samples contain many types of non-uranium particles (organic debris, iron oxides, etc.) that can form molecular interferences and induce the risk of isotopic measurement bias, especially for minor isotopes (234U, 236U). The influence of these polyatomic interferences on the measurements will be discussed. Moreover, different uranium isotopic compositions can be found in the same sample. Therefore, risks of memory effect and of particle-toparticle cross-contamination by the deposition of ablation debris around the crater have also been investigated. This study has been conducted by using a femtosecond laser ablation device coupled to a high sensitivity sector field ICP-MS. Particles were fixed onto the discs with collodion and were located thanks to their fission tracks so that micrometric particles can be analyzed separately. All uranium isotope ratios were measured. Results are compared with the ones obtained with the fission tracks-TIMS technique on other deposition discs from the same sample. Performance of the method in terms of accuracy, precision, and detection limits are estimated

A routine high-precision method for Lu-Hf isotope geochemistry and chronology

Science.gov (United States)

Patchett, P.J.; Tatsumoto, M.

1981-01-01

A method for chemical separation of Lu and Hf from rock, meteorite and mineral samples is described, together with a much improved mass spectrometric running technique for Hf. This allows (i) geo- and cosmochronology using the176Lu???176Hf+??- decay scheme, and (ii) geochemical studies of planetary processes in the earth and moon. Chemical yields for the three-stage ion-exchange column procedure average 90% for Hf. Chemical blanks are international mass spectrometric standard; suitable aliquots, prepared from a single batch of JMC 475, are available from Denver. Lu-Hf analyses of the standard rocks BCR-1 and JB-1 are given. The potential of the Lu-Hf method in isotope geochemistry is assessed. ?? 1980 Springer-Verlag.

Determination of Trace Iron in Red Wine by Isotope Dilution Mass Spectrometry Using Multiple-Collector Inductively Coupled Plasma Mass Spectrometry

International Nuclear Information System (INIS)

Zhou Tao; Wang Jun; Lu Hai; Zhou Yuanjing; Li Haifeng

2009-01-01

This paper introduces determination of trace iron in red wine certified reference material by isotope dilution mass spectrometry (IDMS) method using a multiplecollector inductively coupled plasma mass spectrometry, equipped with a hexapole collision cell. The measurement procedure of iron isotopic abundance ratios was deeply researched. Reduced polyatomic ion interferences to iron isotopes ion by collision reaction using Ar and H 2 gas, high precise isotopic abundance ratios were achieved. Two relative measurement methods (ICP-MS and ICP-OES) were used to analyze trace iron in red wine. The results are compared with IDMS results, which indicate that they are accordant. The uncertainty analyses include each uncertainty factor in whole experiment and the uncertainty of used certified reference material and it shows that the procedure blank is not neglectable to detect limit and precision of the method. The establishment of IDMS method for analysis of trace iron in red wine supports the certification of certified reference materials. (authors)

Concerns about Quadrupole ICP-MS Lead Isotopic Data and Interpretations in the Environment and Health Fields

Directory of Open Access Journals (Sweden)

Brian Gulson

2018-04-01

Full Text Available There has been a massive increase in recent years of the use of lead (Pb isotopes in attempts to better understand sources and pathways of Pb in the environment and in man or experimental animals. Unfortunately, there have been many cases where the quality of the isotopic data, especially that obtained by quadrupole inductively coupled plasma mass spectrometry (Q-ICP-MS, are questionable, resulting in questionable identification of potential sources, which, in turn, impacts study interpretation and conclusions. We present several cases where the isotopic data have compromised interpretation because of the use of only the major isotopes 208Pb/206Pb and 207Pb/206Pb, or their graphing in other combinations. We also present some examples comparing high precision data from thermal ionization (TIMS or multi-collector plasma mass spectrometry (MC-ICP-MS to illustrate the deficiency in the Q-ICP-MS data. In addition, we present cases where Pb isotopic ratios measured on Q-ICP-MS are virtually impossible for terrestrial samples. We also evaluate the Pb isotopic data for rat studies, which had concluded that Pb isotopic fractionation occurs between different organs and suggest that this notion of biological fractionation of Pb as an explanation for isotopic differences is not valid. Overall, the brief review of these case studies shows that Q-ICP-MS as commonly practiced is not a suitable technique for precise and accurate Pb isotopic analysis in the environment and health fields.

Concerns about Quadrupole ICP-MS Lead Isotopic Data and Interpretations in the Environment and Health Fields.

Science.gov (United States)

Gulson, Brian; Kamenov, George D; Manton, William; Rabinowitz, Michael

2018-04-11

There has been a massive increase in recent years of the use of lead (Pb) isotopes in attempts to better understand sources and pathways of Pb in the environment and in man or experimental animals. Unfortunately, there have been many cases where the quality of the isotopic data, especially that obtained by quadrupole inductively coupled plasma mass spectrometry (Q-ICP-MS), are questionable, resulting in questionable identification of potential sources, which, in turn, impacts study interpretation and conclusions. We present several cases where the isotopic data have compromised interpretation because of the use of only the major isotopes 208 Pb/ 206 Pb and 207 Pb/ 206 Pb, or their graphing in other combinations. We also present some examples comparing high precision data from thermal ionization (TIMS) or multi-collector plasma mass spectrometry (MC-ICP-MS) to illustrate the deficiency in the Q-ICP-MS data. In addition, we present cases where Pb isotopic ratios measured on Q-ICP-MS are virtually impossible for terrestrial samples. We also evaluate the Pb isotopic data for rat studies, which had concluded that Pb isotopic fractionation occurs between different organs and suggest that this notion of biological fractionation of Pb as an explanation for isotopic differences is not valid. Overall, the brief review of these case studies shows that Q-ICP-MS as commonly practiced is not a suitable technique for precise and accurate Pb isotopic analysis in the environment and health fields.

Accurate and precise 40Ar/39Ar dating by high-resolution, multi-collection, mass spectrometry

DEFF Research Database (Denmark)

Storey, Michael; Rivera, Tiffany; Flude, Stephanie

New generation, high resolution, multi-collector noble gas mass spectrometers equipped with ion-counting electron multipliers provide opportunities for improved accuracy and precision in 40Ar/39Ar dating. Here we report analytical protocols and age cross-calibration studies using a NU-Instruments......New generation, high resolution, multi-collector noble gas mass spectrometers equipped with ion-counting electron multipliers provide opportunities for improved accuracy and precision in 40Ar/39Ar dating. Here we report analytical protocols and age cross-calibration studies using a NU......-Instruments multi-collector Noblesse noble gas mass spectrometer configured with a faraday detector and three ion-counting electron multipliers. The instrument has the capability to measure several noble gas isotopes simultaneously and to change measurement configurations instantaneously by the use of QUAD lenses...... (zoom optics). The Noblesse offer several advantages over previous generation noble gas mass spectrometers and is particularly suited for single crystal 40Ar/39Ar dating because of: (i) improved source sensitivity (ii) ion-counting electron multipliers, which have much lower signal to noise ratios than...

A novel methylation derivatization method for δ(18)O analysis of individual carbohydrates by gas chromatography/pyrolysis-isotope ratio mass spectrometry.

Science.gov (United States)

Lehmann, Marco M; Fischer, Maria; Blees, Jan; Zech, Michael; Siegwolf, Rolf T W; Saurer, Matthias

2016-01-15

The oxygen isotope ratio (δ(18)O) of carbohydrates derived from animals, plants, sediments, and soils provides important information about biochemical and physiological processes, past environmental conditions, and geographical origins, which are otherwise not available. Nowadays, δ(18)O analyses are often performed on carbohydrate bulk material, while compound-specific δ(18)O analyses remain challenging and methods for a wide range of individual carbohydrates are rare. To improve the δ(18)O analysis of individual carbohydrates by gas chromatography/pyrolysis-isotope ratio mass spectrometry (GC/Pyr-IRMS) we developed a new methylation derivatization method. Carbohydrates were fully methylated within 24 h in an easy-to-handle one-pot reaction in acetonitrile, using silver oxide as proton acceptor, methyl iodide as methyl group carrier, and dimethyl sulfide as catalyst. The precision of the method ranged between 0.12 and 1.09‰ for the δ(18)O values of various individual carbohydrates of different classes (mono-, di-, and trisaccharides, alditols), with an accuracy of a similar order of magnitude, despite high variation in peak areas. Based on the δ(18)O values of the main isomers, important monosaccharides such as glucose and fructose could also be precisely analyzed for the first time. We tested the method on standard mixtures, honey samples, and leaf carbohydrates extracted from Pinus sylvestris, showing that the method is also applicable to different carbohydrate mixtures. The new methylation method shows unrivalled accuracy and precision for δ(18)O analysis of various individual carbohydrates; it is fast and easy-to-handle, and may therefore find wide-spread application. Copyright © 2015 John Wiley & Sons, Ltd.

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.

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

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

Science.gov (United States)

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

2015-01-06

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

Sample preparation techniques of biological material for isotope analysis

International Nuclear Information System (INIS)

Axmann, H.; Sebastianelli, A.; Arrillaga, J.L.

1990-01-01

Sample preparation is an essential step in all isotope-aided experiments but often it is not given enough attention. The methods of sample preparation are very important to obtain reliable and precise analytical data and for further interpretation of results. The size of a sample required for chemical analysis is usually very small (10mg-1500mg). On the other hand the amount of harvested plant material from plots in a field experiment is often bulky (several kilograms) and the entire sample is too large for processing. In addition, while approaching maturity many crops show not only differences in physical consistency but also a non-uniformity in 15 N content among plant parts, requiring a plant fractionation or separation into parts (vegetative and reproductive) e.g. shoots and spikes, in case of small grain cereals, shoots and pods in case of grain legumes and tops and roots or beets (including crown) in case of sugar beet, etc. In any case the ultimate goal of these procedures is to obtain representative subsample harvested from greenhouse or field experiments for chemical analysis. Before harvesting an isotopic-aided experiment the method of sampling has to be selected. It should be based on the type of information required in relation to the objectives of the research and the availability of resources (staff, sample preparation equipment, analytical facilities, chemicals and supplies, etc.). 10 refs, 3 figs, 3 tabs

High Precision Stable Isotope Measurements of Caribic Aircraft CO{sub 2} Samples: Global Distribution and Exchange with the Biosphere

Energy Technology Data Exchange (ETDEWEB)

Assonov, S. S. [Max Planck Institute for Chemistry, Mainz (Germany); Joint Research Centre, Institute for Reference Materials and Measurements (JRC-IRMM), European Commission, Geel (Belgium); Brenninkmeijer, C. A.M.; Schuck, T. J. [Max Planck Institute for Chemistry, Mainz (Germany); Taylor, P. [Joint Research Centre, Institute for Reference Materials and Measurements (JRC-IRMM), European Commission, Geel (Belgium)

2013-07-15

In 2007-2009 JRC-IRMM, in collaboration with the project CARIBIC (Civil Aircraft for Regular Investigation of the atmosphere Based on an Instrument Container, www.caribicatmospheric. com), conducted systematic measurements aimed to study the global distribution of CO{sub 2} isotopic composition. A large data set for the upper troposphere-lowermost stratosphere and free troposphere was obtained. For the first time it is demonstrated how CO{sub 2} isotope signals reflect global scale variability in air mass origin. Tight correlations observed arise either from stratosphere/troposphere mixing or from mixing of background air and air masses affected by CO{sub 2} sources and sinks, over long distances and throughout the seasons. The high quality {delta}{sup 18}O(CO{sub 2}) data prove to be a useful tracer reflecting long range CO{sub 2} transport and also CO{sub 2} exchange with land biosphere and soils. The data provide a benchmark for future comparisons and are available for modelling studies. (author)

Rapid Analysis of U isotopic ratios in Food Stuff samples using Fusion and ICP-MS measurement: For radiation monitoring program in the vicinity of nuclear facilities

Energy Technology Data Exchange (ETDEWEB)

Lim, Jong Myoung; Park, Ji Young; Jung, Yoon Hee; Kim, Hyun Cheol; Kim, Won Young; Chung, Gun Ho; Kang, Mun Ja [KAERI, Daejeon (Korea, Republic of)

2016-05-15

In this study, a rapid digestion and separation method for U isotopes was developed in food stuff matrix such as cabbage and rice. As an attempt to reduce social costs and apprehension arising from the radioactivity in food, an accurate and rapid assessment of radioactivity is highly desirable. Hence, it is very important to develop a series of evaluation of rapid procedures for efficient radioactivity management in food. Contrary to the α-spectrometry method, a measurement technique using ICP-MS with an advanced sample introduction and mass counting system allows radioactivity in many samples to be measured with a short time period with a high degree of accuracy and precision. In order to satisfy the method detectable activity (MDA) for the regulation of radioactivity monitoring program the analysis of U isotopes always require the extremely large sample amount. These procedures make usually the food stuff sample to carbonize during dry ashing process. The ashed residues have been especially complicated into a liquid phase because of their carbonization. This process are very time consuming and not fully recovered target isotopes.

Isotope ratio measurements with multiple collection inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Platzner, I.T.; Segal, I.; Halicz, L.

2003-01-01

In the studies summarized in this review, it has been shown that IRM of lead in silicates can be carried out without lead separation and purification. Because of time independent mass discrimination and lack of chemical interaction at high plasma temperatures, simple interference corrections are feasible. This data further support the observation that MC-ICP-MS provides data with superior precision comparing to TIMS. Furthermore, it should be noted that the multi collection instrumental configuration exhibits the capability to perform a single IRM with excellent precision and high accuracy for elements with a large number of isotopes. Four of the discussed elements have six (Er) and seven (Dy, Yb, Os) isotopes

Quantifying the Contribution of Grape Hexoses to Wine Volatiles by High-Precision [U13C]-Glucose Tracer Studies

Science.gov (United States)

Nisbet, Mark A.; Tobias, Herbert J.; Brenna, J. Thomas; Sacks, Gavin L.; Mansfield, Anna Katharine

2016-01-01

Many fermentation volatiles important to wine aroma potentially arise from yeast metabolism of hexose sugars, but assessing the relative importance of these pathways is challenging due to high endogenous hexose substrate concentrations. To overcome this problem, gas chromatography combustion isotope ratio mass spectrometry (GC-C-IRMS) was used to measure high-precision 13C/12C isotope ratios of volatiles in wines produced from juices spiked with tracer levels (0.01–1 APE) of uniformly labeled [U-13C]-glucose. The contribution of hexose to individual volatiles was determined from the degree of 13C enrichment. As expected, straight-chain fatty acids and their corresponding ethyl esters were derived almost exclusively from hexoses. Most fusel alcohols and their acetate esters were also majority hexose-derived, indicating the importance of anabolic pathways for their formation. Only two compounds were not derived primarily from hexoses (hexanol and isobutyric acid). This approach can be extended to other food systems or substrates for studying precursor–product relationships. PMID:24960193

Quantifying the contribution of grape hexoses to wine volatiles by high-precision [U¹³C]-glucose tracer studies.

Science.gov (United States)

Nisbet, Mark A; Tobias, Herbert J; Brenna, J Thomas; Sacks, Gavin L; Mansfield, Anna Katharine

2014-07-16

Many fermentation volatiles important to wine aroma potentially arise from yeast metabolism of hexose sugars, but assessing the relative importance of these pathways is challenging due to high endogenous hexose substrate concentrations. To overcome this problem, gas chromatography combustion isotope ratio mass spectrometry (GC-C-IRMS) was used to measure high-precision (13)C/(12)C isotope ratios of volatiles in wines produced from juices spiked with tracer levels (0.01-1 APE) of uniformly labeled [U-(13)C]-glucose. The contribution of hexose to individual volatiles was determined from the degree of (13)C enrichment. As expected, straight-chain fatty acids and their corresponding ethyl esters were derived almost exclusively from hexoses. Most fusel alcohols and their acetate esters were also majority hexose-derived, indicating the importance of anabolic pathways for their formation. Only two compounds were not derived primarily from hexoses (hexanol and isobutyric acid). This approach can be extended to other food systems or substrates for studying precursor-product relationships.

Isotopic composition of neon in the galactic cosmic rays: a high resolution measurement

International Nuclear Information System (INIS)

Greiner, D.E.; Wiedenbeck, M.E.; Bieser, F.S.; Crawford, H.J.; Heckman, H.H.; Lindstrom, P.J.

1979-06-01

A measurement of the isotopic composition of galactic cosmic ray neon in the energy range 70 to 260 MeV/amu has been made using the U.C. Berkeley HKH instrument aboard ISEE-3. A combination of high resolution and good statistical accuracy makes possible a precise determination of the local interplanetary neon composition. We find 22 Ne/ 20 Ne = 0.64 +- 0.07 and 21 Ne/ 20 Ne < 0.30 in local interplanetary space. These ratios, when interpreted in using standard galactic propagation and solar modulation models, yield cosmic ray source abundances which are inconsistent with a solar-like source composition

Comparison between isotope dilution and activation analysis as a method for determining the macro content of mercury

International Nuclear Information System (INIS)

Soedyartomo; Sunoko, S.R.

1975-01-01

It is true that the mercury content in the environment should be measured accurately because of its toxicity even at levels of microgram order. The assessment of hazards due to environmental contamination with mercury is based on the results of the metal analysis in a number of different samples. Consequently, the study of the character of analytical methods used, i.e. their accuracy, precision, sensitivity, etc. is essential. A brief description on the microanalysis methods of mercury as given. The discussion of the results obtained from analysing some sludge and water by means of isotope dilution and destructive thermal neutron activation analysis is also presented. It is found that both methods are suitable for routine work. It can be concluded that the isotope dilution method has some advantages. It is more simple, more sensitive, more rapid, and has lower radiation hazard. (author)

Routine lead isotope determinations using a lead-207-lead-204 double spike: a long-term assessment of analytical precision and accuracy

International Nuclear Information System (INIS)

Woodhead, J.D.; McCulloch, M.T.; Volker, F.

1995-01-01

Lead-isotope data obtained on a multicollector mass spectrometer over a four year period using a 207 Pb- 204 Pb double spike to correct for the effects of mass discrimination, are reported. Considerable improvements in both precision and accuracy over conventional correction procedures were noted, without recourse to rigorous loading or run conditions. An external precision in 206 Pb/ 204 Pb, 207 Pb/ 204 Pb and 208 Pb/ 204 Pb ratios ± 0.003, 0.003 and 0.01 (2 x standard deviation), respectively, is routinely obtainable independent of minor variations in loading and run parameters. (author)

Hf isotope evidence for a hidden mantle reservoir

DEFF Research Database (Denmark)

Bizzarro, Martin; Simonetti, A.; Stevenson, R.K.

2002-01-01

High-precision Hf isotopic analyses and U-Pb ages of carbonatites and kimberlites from Greenland and eastern North America, including Earth's oldest known carbonatite (3 Ga), indicate derivation from an enriched mantle source. This previously unidentified mantle reservoir-marked by an unradiogenic...... Hf isotopic composition and preserved in the deep mantle for at least 3 b.y.-may account for the mass imbalance in Earth's Hf-Nd budget. The Hf isotopic data presented here support a common mantle source region and genetic link between carbonatite and some oceanic-island basalt volcanoes....

Recent development in isotope ratio mass spectrometry

International Nuclear Information System (INIS)

Platzner, I.

1992-01-01

Within the limited of this review the following topics will be briefly discussed: a) Accuracy, precision, internal relative standard deviation (RISD) and external relative standard deviation (RESD) of isotope ratio measurements. With advanced instrumentation and use of standard reference materials, high accuracy and RESD = 0.002% (or better) may be achieved; b) The advantages of modern automatic isotope ratio mass spectrometer are briefly described. Computer controlled operation and data acquisition, and multiple ion collection are the recent important improvement; c) The isotopic fractionation during the course of isotope ratio measurement is considered as a major source of errors in thermal ionization of metallic elements. The phenomenon in strontium, neodymium, uranium, lead and calcium and methods to correct the measured data are discussed; d) Applications of isotope ratio mass spectrometry in atomic weight determinations, the isotope dilution technique, isotope geology, and isotope effects in biological systems are described together with specific applications in various research and technology area. (author)

Dual Si and O Isotope Measurement of Lunar Samples Using IRMS

Science.gov (United States)

Banerjee, N.; Hill, P. J. A.; Osinski, G. R.

2016-12-01

The use of isotopic systems and their associated theoretical models have become an increasingly sophisticated tool for investigating the origin of planetary bodies in the solar system. It was originally hypothesized that evidence for the impact origin of Moon would manifest itself as an isotopic heterogeneity between lunar and terrestrial samples; however, most isotope systems show no difference between the bulk Earth and Moon. The stable isotopes of both silicon (Si) and oxygen (O) have been essential in further understanding planetary processes including core formation. Historically the analysis of the Si and O isotope ratios in terrestrial and extraterrestrial material has primarily been measured independent of each other through three main techniques: isotope ratio mass spectrometry (IRMS), secondary ion mass spectrometry (SIMS), and multi-collector inductively coupled plasma mass-spectrometry (MC-ICPMS). Each technique has its own strength and weakness in regards to resolution and precision; however, one of the main limiting factors in all three of these techniques rests on the requirement of multiple aliquots. As most literature focuses on the measurement of oxygen or silicon isotopes, this unique line allows for the precise analysis of Si and O isotopes from the same aliquot of bulk sample, which cannot be done with SIMS or ICP-MS analysis. To deal with this problem a unique laser line system has been developed in the Laboratory for Stable Isotope Science at Western University, Canada, that simultaneously extracts SiF4 and O2 from the same 1-2 mg aliquot. We present the application of analyzing both isotopic systems from the sample aliquot to Apollo, meteoritic, and terrestrial samples and its implication for the formation of the Moon. Preliminary results from this line suggest that although the O isotopes ratios are consistent with a homogenous Moon-Earth system, a difference is observed in Si isotopes between Apollo and terrestrial samples compared to

NiftyPET: a High-throughput Software Platform for High Quantitative Accuracy and Precision PET Imaging and Analysis.

Science.gov (United States)

Markiewicz, Pawel J; Ehrhardt, Matthias J; Erlandsson, Kjell; Noonan, Philip J; Barnes, Anna; Schott, Jonathan M; Atkinson, David; Arridge, Simon R; Hutton, Brian F; Ourselin, Sebastien

2018-01-01

We present a standalone, scalable and high-throughput software platform for PET image reconstruction and analysis. We focus on high fidelity modelling of the acquisition processes to provide high accuracy and precision quantitative imaging, especially for large axial field of view scanners. All the core routines are implemented using parallel computing available from within the Python package NiftyPET, enabling easy access, manipulation and visualisation of data at any processing stage. The pipeline of the platform starts from MR and raw PET input data and is divided into the following processing stages: (1) list-mode data processing; (2) accurate attenuation coefficient map generation; (3) detector normalisation; (4) exact forward and back projection between sinogram and image space; (5) estimation of reduced-variance random events; (6) high accuracy fully 3D estimation of scatter events; (7) voxel-based partial volume correction; (8) region- and voxel-level image analysis. We demonstrate the advantages of this platform using an amyloid brain scan where all the processing is executed from a single and uniform computational environment in Python. The high accuracy acquisition modelling is achieved through span-1 (no axial compression) ray tracing for true, random and scatter events. Furthermore, the platform offers uncertainty estimation of any image derived statistic to facilitate robust tracking of subtle physiological changes in longitudinal studies. The platform also supports the development of new reconstruction and analysis algorithms through restricting the axial field of view to any set of rings covering a region of interest and thus performing fully 3D reconstruction and corrections using real data significantly faster. All the software is available as open source with the accompanying wiki-page and test data.

High-precision branching ratio measurement for the superallowed β+ emitter 62Ga

International Nuclear Information System (INIS)

Finlay, P.E.J.

2007-01-01

A high-precision branching ratio measurement for the superallowed β + decay of 62 Ga was performed at the Isotope Separator and Accelerator radioactive ion beam facility. An array of 20 high-purity germanium detectors known as the 8π spectrometer was employed to detect the rays emitted following the Gamow-Teller and non-analog Fermi decays of 62 Ga, while the plastic scintillator array known as SCEPTAR was used to detect the emitted particles. A total of 32 γ rays were identified, establishing the superallowed branching ratio to be 99:859(8)%. Combined with the most recent half-life and Q-value measurements for 62 Ga, this branching ratio yields an ft-value of 3074.3 ± 1.1 s. Comparisons between the superallowed ft-value determined in this work and the world average Ft-bar are made, providing a benchmark for the refinement of theoretical models used to describe isospin-symmetry breaking in A ≥ 62 nuclei. (author)

In situ observations of the isotopic composition of methane at the Cabauw tall tower site

Directory of Open Access Journals (Sweden)

T. Röckmann

2016-08-01

Full Text Available High-precision analyses of the isotopic composition of methane in ambient air can potentially be used to discriminate between different source categories. Due to the complexity of isotope ratio measurements, such analyses have generally been performed in the laboratory on air samples collected in the field. This poses a limitation on the temporal resolution at which the isotopic composition can be monitored with reasonable logistical effort. Here we present the performance of a dual isotope ratio mass spectrometric system (IRMS and a quantum cascade laser absorption spectroscopy (QCLAS-based technique for in situ analysis of the isotopic composition of methane under field conditions. Both systems were deployed at the Cabauw Experimental Site for Atmospheric Research (CESAR in the Netherlands and performed in situ, high-frequency (approx. hourly measurements for a period of more than 5 months. The IRMS and QCLAS instruments were in excellent agreement with a slight systematic offset of (+0.25 ± 0.04 ‰ for δ13C and (−4.3 ± 0.4 ‰ for δD. This was corrected for, yielding a combined dataset with more than 2500 measurements of both δ13C and δD. The high-precision and high-temporal-resolution dataset not only reveals the overwhelming contribution of isotopically depleted agricultural CH4 emissions from ruminants at the Cabauw site but also allows the identification of specific events with elevated contributions from more enriched sources such as natural gas and landfills. The final dataset was compared to model calculations using the global model TM5 and the mesoscale model FLEXPART-COSMO. The results of both models agree better with the measurements when the TNO-MACC emission inventory is used in the models than when the EDGAR inventory is used. This suggests that high-resolution isotope measurements have the potential to further constrain the methane budget when they are performed at multiple sites that are representative for

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

Cu isotopic signature in blood serum of liver transplant patients: a follow-up study

Science.gov (United States)

Lauwens, Sara; Costas-Rodríguez, Marta; van Vlierberghe, Hans; Vanhaecke, Frank

2016-07-01

End-stage liver disease (ESLD) is life-threatening and liver transplantation (LTx) is the definitive treatment with good outcomes. Given the essential role of hepatocytes in Cu homeostasis, the potential of the serum Cu isotopic composition for monitoring a patient’s condition post-LTx was evaluated. For this purpose, high-precision Cu isotopic analysis of blood serum of ESLD patients pre- and post-LTx was accomplished via multi-collector ICP-mass spectrometry (MC-ICP-MS). The Cu isotopic composition of the ESLD patients was fractionated in favour of the lighter isotope (by about -0.50‰). Post-LTx, a generalized normalization of the Cu isotopic composition was observed for the patients with normal liver function, while it remained light when this condition was not reached. A strong decrease in the δ65Cu value a longer term post-LTx seems to indicate the recurrence of liver failure or cancer. The observed trend in favour of the heavier Cu isotopic composition post-LTx seems to be related with the restored biosynthetic capacity of the liver, the restored hepatic metabolism and/or the restored biliary secretion pathways. Thus, Cu isotopic analysis could be a valuable tool for the follow-up of liver transplant patients and for establishing the potential recurrence of liver failure.

Preferential flow pathways revealed by field based stable isotope analysis of CO2 by mid-infrared laser spectroscopy

Science.gov (United States)

van Geldern, Robert; Nowak, Martin; Zimmer, Martin; Szizybalski, Alexandra; Myrttinen, Anssi; Barth, Johannes A. C.; Jost, Hj

2016-04-01

A newly developed and commercially available isotope ratio laser spectrometer for CO2 analyses has been tested during a 10-day field monitoring campaign at the Ketzin pilot site for CO2 storage in northern Germany. The laser instrument is based on tunable laser direct absorption in the mid-infrared. The instrument recorded a continuous 10-day carbon stable isotope data set with 30 minutes resolution directly on-site in a field-based laboratory container during a tracer experiment. To test the instruments performance and accuracy the monitoring campaign was accompanied by daily CO2 sampling for laboratory analyses with isotope ratio mass spectrometry (IRMS). The carbon stable isotope ratios measured by conventional IRMS technique and by the new mid-infrared laser spectrometer agree remarkably well within 2σ analytical precision (<0.3 ‰). This proves the capability of the new mid-infrared direct absorption technique to measure high precision and accurate real-time table isotope data directly in the field. The injected CO2 tracer had a distinct δ13C value that was largely different from the reservoir background value. The laser spectroscopy data revealed a prior to this study unknown, intensive dynamic with fast changing δ13C values. The arrival pattern of the tracer suggest that the observed fluctuations were probably caused by migration along separate and distinct preferential flow paths between injection well and observation well. The new technique might contribute to a better tracing of the migration of the underground CO2 plume and help to ensure the long-term integrity of the reservoir.

Simultaneous stable carbon isotopic analysis of wine glycerol and ethanol by liquid chromatography coupled to isotope ratio mass spectrometry.

Science.gov (United States)

Cabañero, Ana I; Recio, Jose L; Rupérez, Mercedes

2010-01-27

A novel procedure was established for the simultaneous characterization of wine glycerol and ethanol (13)C/(12)C isotope ratio, using liquid chromatography/isotope ratio mass spectrometry (LC-IRMS). Several parameters influencing separation of glycerol and ethanol from wine matrix were optimized. Results obtained for 35 Spanish samples exposed no significant differences and very strong correlations (r = 0.99) between the glycerol (13)C/(12)C ratios obtained by an alternative method (gas chromatography/isotope ratio mass spectrometry) and the proposed new methodology, and between the ethanol (13)C/(12)C ratios obtained by the official method (elemental analyzer/isotope ratio mass spectrometry) and the proposed new methodology. The accuracy of the proposed method varied from 0.01 to 0.19 per thousand, and the analytical precision was better than 0.25 per thousand. The new developed LC-IRMS method it is the first isotopic method that allows (13)C/(12)C determination of both analytes in the same run directly from a liquid sample with no previous glycerol or ethanol isolation, overcoming technical difficulties associated with complex sample treatment and improving in terms of simplicity and speed.

Measurement Model and Precision Analysis of Accelerometers for Maglev Vibration Isolation Platforms.

Science.gov (United States)

Wu, Qianqian; Yue, Honghao; Liu, Rongqiang; Zhang, Xiaoyou; Ding, Liang; Liang, Tian; Deng, Zongquan

2015-08-14

High precision measurement of acceleration levels is required to allow active control for vibration isolation platforms. It is necessary to propose an accelerometer configuration measurement model that yields such a high measuring precision. In this paper, an accelerometer configuration to improve measurement accuracy is proposed. The corresponding calculation formulas of the angular acceleration were derived through theoretical analysis. A method is presented to minimize angular acceleration noise based on analysis of the root mean square noise of the angular acceleration. Moreover, the influence of installation position errors and accelerometer orientation errors on the calculation precision of the angular acceleration is studied. Comparisons of the output differences between the proposed configuration and the previous planar triangle configuration under the same installation errors are conducted by simulation. The simulation results show that installation errors have a relatively small impact on the calculation accuracy of the proposed configuration. To further verify the high calculation precision of the proposed configuration, experiments are carried out for both the proposed configuration and the planar triangle configuration. On the basis of the results of simulations and experiments, it can be concluded that the proposed configuration has higher angular acceleration calculation precision and can be applied to different platforms.

Measurement Model and Precision Analysis of Accelerometers for Maglev Vibration Isolation Platforms

Directory of Open Access Journals (Sweden)

Qianqian Wu

2015-08-01

Full Text Available High precision measurement of acceleration levels is required to allow active control for vibration isolation platforms. It is necessary to propose an accelerometer configuration measurement model that yields such a high measuring precision. In this paper, an accelerometer configuration to improve measurement accuracy is proposed. The corresponding calculation formulas of the angular acceleration were derived through theoretical analysis. A method is presented to minimize angular acceleration noise based on analysis of the root mean square noise of the angular acceleration. Moreover, the influence of installation position errors and accelerometer orientation errors on the calculation precision of the angular acceleration is studied. Comparisons of the output differences between the proposed configuration and the previous planar triangle configuration under the same installation errors are conducted by simulation. The simulation results show that installation errors have a relatively small impact on the calculation accuracy of the proposed configuration. To further verify the high calculation precision of the proposed configuration, experiments are carried out for both the proposed configuration and the planar triangle configuration. On the basis of the results of simulations and experiments, it can be concluded that the proposed configuration has higher angular acceleration calculation precision and can be applied to different platforms.

In situ sulfur isotopes (δ{sup 34}S and δ{sup 33}S) analyses in sulfides and elemental sulfur using high sensitivity cones combined with the addition of nitrogen by laser ablation MC-ICP-MS

Energy Technology Data Exchange (ETDEWEB)

Fu, Jiali [State Key Laboratory of Geological Processes and Mineral Resources, China University of Geosciences, Wuhan 430074 (China); Hu, Zhaochu, E-mail: zchu@vip.sina.com [State Key Laboratory of Geological Processes and Mineral Resources, China University of Geosciences, Wuhan 430074 (China); The Beijing SHRIMP Center, Institute of Geology, Chinese Academy of Geological Sciences, Beijing 102206 (China); Zhang, Wen [State Key Laboratory of Geological Processes and Mineral Resources, China University of Geosciences, Wuhan 430074 (China); Yang, Lu [State Key Laboratory of Geological Processes and Mineral Resources, China University of Geosciences, Wuhan 430074 (China); National Research Council Canada, 1200 Montreal Rd., Ottawa, Ontario K1A 0R6 (Canada); Liu, Yongsheng; Li, Ming; Zong, Keqing; Gao, Shan; Hu, Shenghong [State Key Laboratory of Geological Processes and Mineral Resources, China University of Geosciences, Wuhan 430074 (China)

2016-03-10

The sulfur isotope is an important geochemical tracer in diverse fields of geosciences. In this study, the effects of three different cone combinations with the addition of N{sub 2} on the performance of in situ S isotope analyses were investigated in detail. The signal intensities of S isotopes were improved by a factor of 2.3 and 3.6 using the X skimmer cone combined with the standard sample cone or the Jet sample cone, respectively, compared with the standard arrangement (H skimmer cone combined with the standard sample cone). This signal enhancement is important for the improvement of the precision and accuracy of in situ S isotope analysis at high spatial resolution. Different cone combinations have a significant effect on the mass bias and mass bias stability for S isotopes. Poor precisions of S isotope ratios were obtained using the Jet and X cones combination at their corresponding optimum makeup gas flow when using Ar plasma only. The addition of 4–8 ml min{sup −1} nitrogen to the central gas flow in laser ablation MC-ICP-MS was found to significantly enlarge the mass bias stability zone at their corresponding optimum makeup gas flow in these three different cone combinations. The polyatomic interferences of OO, SH, OOH were also significantly reduced, and the interference free plateaus of sulfur isotopes became broader and flatter in the nitrogen mode (N{sub 2} = 4 ml min{sup −1}). However, the signal intensity of S was not increased by the addition of nitrogen in this study. The laser fluence and ablation mode had significant effects on sulfur isotope fractionation during the analysis of sulfides and elemental sulfur by laser ablation MC-ICP-MS. The matrix effect among different sulfides and elemental sulfur was observed, but could be significantly reduced by line scan ablation in preference to single spot ablation under the optimized fluence. It is recommended that the d{sub 90} values of the particles in pressed powder pellets for accurate

Laser ablation molecular isotopic spectrometry of water for {sub 1}D{sup 2}/{sub 1}H{sup 1} ratio analysis

Energy Technology Data Exchange (ETDEWEB)

Sarkar, Arnab [Lawrence Berkeley National Laboratory, University of California, Berkeley, CA 94720 (United States); Fuel Chemistry Division, Bhabha Atomic Research Centre, Mumbai 400085 (India); Mao, Xianglei; Chan, George C.-Y. [Lawrence Berkeley National Laboratory, University of California, Berkeley, CA 94720 (United States); Russo, Richard E., E-mail: rerusso@lbl.gov [Lawrence Berkeley National Laboratory, University of California, Berkeley, CA 94720 (United States)

2013-10-01

Laser Ablation Molecular Isotopic Spectrometry (LAMIS) has been investigated for optical isotopic analysis of the deuterium to protium ratio in enriched water samples in ambient air at atmospheric pressure. Multivariate PLSR (Partial Least Squares Regression) based calibrations were carried out and validated using multiple statistical parameters. Comparisons of results are reported using two spectrometers having two orders of magnitude difference in spectral resolution. The accuracy and precision of isotopic analysis depends on the spectral resolution and the inherent isotope shift of the elements. The requirements for spectral resolution of the measurement system can be significantly relaxed when the isotopic abundance ratio is determined using chemometric processing of the spectra. Large isotopic shifts in the individual rotational branches of OH/OD molecular emission spectra were measured. Optimized temporal conditions for LAMIS measurements were established. Several sub-regions of spectra were used for PLSR calibration and the results demonstrate that both the emission intensity and degree of spectral differentiation affect the quality of the PLSR calibration. LAMIS results also were compared with traditional LIBS results obtained using PLSR and a spectral deconvolution method, demonstrating the advantages of LAMIS over LIBS with respect to isotopic composition determination. - Highlights: • D/H isotopic ratio in water over a large dynamic range was measured by LAMIS. • PLSR based multivariate calibration was used for construction of calibrations. • Region of interest significantly affects the analytical results of isotopic ratio. • LAMIS has improved results over LIBS irrespective of the spectrometer resolution. • The superiority is more prominent in the case using low resolution spectrometer.

Isotope analysis of diamond-surface passivation effect of high-temperature H{sub 2}O-grown atomic layer deposition-Al{sub 2}O{sub 3} films

Energy Technology Data Exchange (ETDEWEB)

Hiraiwa, Atsushi, E-mail: hiraiwa@aoni.waseda.jp, E-mail: qs4a-hriw@asahi-net.or.jp [Institute for Nanoscience and Nanotechnology, Waseda University, 513 Waseda-tsurumaki, Shinjuku, Tokyo 162-0041 (Japan); Saito, Tatsuya; Matsumura, Daisuke; Kawarada, Hiroshi, E-mail: kawarada@waseda.jp [Faculty of Science and Engineering, Waseda University, 3-4-1 Okubo, Shinjuku, Tokyo 169-8555 (Japan)

2015-06-07

The Al{sub 2}O{sub 3} film formed using an atomic layer deposition (ALD) method with trimethylaluminum as Al precursor and H{sub 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{sub 2}O instead of H{sub 2}O in the ALD and found that the Al{sub 2}O{sub 3} film formed at a conventional temperature (100 °C) incorporates 50 times more CH{sub 3} groups than the high-temperature film. This CH{sub 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{sub 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{sub 2}O. Additionally, we not only observed the kinetic isotope effect in the form of reduced growth rate of D{sub 2}O-oxidant ALD but found that the mass density and dielectric constant of D{sub 2}O-grown Al{sub 2}O{sub 3} films are smaller than those of H{sub 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{sub 2}O{sub 3} films as a passivation and/or gate-insulation layer of high-temperature-operation diamond SC devices, and the knowledge of

High-precision half-life determination for the superallowed β+ emitter Ga62

Science.gov (United States)

Grinyer, G. F.; Finlay, P.; Svensson, C. E.; Ball, G. C.; Leslie, J. R.; Austin, R. A. E.; Bandyopadhyay, D.; Chaffey, A.; Chakrawarthy, R. S.; Garrett, P. E.; Hackman, G.; Hyland, B.; Kanungo, R.; Leach, K. G.; Mattoon, C. M.; Morton, A. C.; Pearson, C. J.; Phillips, A. A.; Ressler, J. J.; Sarazin, F.; Savajols, H.; Schumaker, M. A.; Wong, J.

2008-01-01

The half-life of the superallowed β+ emitter Ga62 has been measured at TRIUMF's Isotope Separator and Accelerator facility using a fast-tape-transport system and 4π continuous-flow gas proportional counter to detect the positrons from the decay of Ga62 to the daughter Zn62. The result, T1/2=116.100±0.025 ms, represents the most precise measurement to date (0.022%) for any superallowed β-decay half-life. When combined with six previous measurements of the Ga62 half-life, a new world average of T1/2=116.121±0.021 ms is obtained. This new half-life measurement results in a 20% improvement in the precision of the Ga62 superallowed ft value while reducing its mean by 0.9σ to ft=3074.3(12) s. The impact of this half-life measurement on precision tests of the CVC hypothesis and isospin symmetry breaking corrections for A⩾62 superallowed decays is discussed.

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.

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.

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.

Measurement of zinc stable isotope ratios in biogeochemical matrices by double-spike MC-ICPMS and determination of the isotope ratio pool available for plants from soil.

Science.gov (United States)

Arnold, Tim; Schönbächler, Maria; Rehkämper, Mark; Dong, Schuofei; Zhao, Fang-Jie; Kirk, Guy J D; Coles, Barry J; Weiss, Dominik J

2010-12-01

Analysis of naturally occurring isotopic variations is a promising tool for investigating Zn transport and cycling in geological and biological settings. Here, we present the recently installed double-spike (DS) technique at the MAGIC laboratories at Imperial College London. The procedure improves on previous published DS methods in terms of ease of measurement and precisions obtained. The analytical method involves addition of a (64)Zn-(67)Zn double-spike to the samples prior to digestion, separation of Zn from the sample matrix by ion exchange chromatography, and isotopic analysis by multiple-collector inductively coupled plasma mass spectrometry. The accuracy and reproducibility of the method were validated by analyses of several in-house and international elemental reference materials. Multiple analyses of pure Zn standard solutions consistently yielded a reproducibility of about ±0.05‰ (2 SD) for δ(66)Zn, and comparable precisions were obtained for analyses of geological and biological materials. Highly fractionated Zn standards analyzed by DS and standard sample bracketing yield slightly varying results, which probably originate from repetitive fractionation events during manufacture of the standards. However, the δ(66)Zn values (all reported relative to JMC Lyon Zn) for two less fractionated in-house Zn standard solutions, Imperial Zn (0.10 ± 0.08‰: 2 SD) and London Zn (0.08 ± 0.04‰), are within uncertainties to data reported with different mass spectrometric techniques and instruments. Two standard reference materials, blend ore BCR 027 and ryegrass BCR 281, were also measured, and the δ(66)Zn were found to be 0.25 ± 0.06‰ (2 SD) and 0.40 ± 0.09‰, respectively. Taken together, these standard measurements ascertain that the double-spike methodology is suitable for accurate and precise Zn isotope analyses of a wide range of natural samples. The newly installed technique was consequently applied to soil samples and soil leachates to

Direct lead isotope analysis in Hg-rich sulfides by LA-MC-ICP-MS with a gas exchange device and matrix-matched calibration

Energy Technology Data Exchange (ETDEWEB)

Zhang, Wen [State Key Laboratory of Geological Processes and Mineral Resources, Faculty of Earth Sciences, China University of Geosciences, Wuhan, 430074 (China); Hu, Zhaochu, E-mail: zchu@vip.sina.com [State Key Laboratory of Geological Processes and Mineral Resources, Faculty of Earth Sciences, China University of Geosciences, Wuhan, 430074 (China); Günther, Detlef, E-mail: guenther@inorg.chem.ethz.ch [ETH Zurich, Laboratory for Inorganic Chemistry, CH-8093, Zurich (Switzerland); Liu, Yongsheng; Ling, Wenli; Zong, Keqing; Chen, Haihong; Gao, Shan [State Key Laboratory of Geological Processes and Mineral Resources, Faculty of Earth Sciences, China University of Geosciences, Wuhan, 430074 (China)

2016-12-15

In situ Pb isotope data of sulfide samples measured by LA-MC-ICP-MS provide valuable geochemical information for studies of the origin and evolution of ore deposits. However, the severe isobaric interference of {sup 204}Hg on {sup 204}Pb and the lack of matrix-matched sulfide reference materials limit the precision of Pb isotopic analyses for Hg-rich sulfides. In this study, we observe that Hg forms vapor and can be completely removed from sample aerosol particles produced by laser ablation using a gas exchange device. Additionally, this device does not influence the signal intensities of Pb isotopes. The within-run precision, the external reproducibility and the analytical accuracy are significantly improved for the Hg-rich sulfide samples using this mercury-vapor-removing device. Matrix effects are observed when using silicate glass reference materials as the external standards to assess the relationship of mass fractionation factors between Tl and Pb in sulfide samples, resulting in a maximum deviation of ∼0.20% for {sup 20x}Pb/{sup 204}Pb. Matrix-matched reference materials are therefore required for the highly precise and accurate Pb isotope analyses of sulfide samples. We investigated two sulfide samples, MASS-1 (the Unites States Geological Survey reference materials) and Sph-HYLM (a natural sphalerite), as potential candidates. Repeated analyses of the two proposed sulfide reference materials by LA-MC-ICP-MS yield good external reproducibility of <0.04% (RSD, k = 2) for {sup 20x}Pb/{sup 206}Pb and <0.06% (RSD, k = 2) for {sup 20x}Pb/{sup 204}Pb with the exception of {sup 20x}Pb/{sup 204}Pb in MASS-1, which provided an external reproducibility of 0.24% (RSD, k = 2). Because the concentration of Pb in MASS-1 (76 μg g{sup −1}) is ∼5.2 times lower than that in Sph-HYLM (394 ± 264 μg g{sup −1}). The in situ analytical results of MASS-1 and Sph-HYLM are consistent with the values obtained by solution MC-ICP-MS, demonstrating the reliability

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.

Frequency Comb Driven Raman Transitions in the THz Range: High Precision Isotope Shift Measurements in Ca+

DEFF Research Database (Denmark)

Meyer, Steffen

2017-01-01

and frequency resolved optical gating (FROG) are used, and the two frequency comb systems used for the experiments are thoroughly characterized, a Coherent Mira Ti:sapph oscillator and a MenloSystems fiber based frequency comb system. The potential of frequency comb driven Raman transitions is shown...... transition frequencies typically are on the order of a few THz. High precision measurements on these ions have many intriguing applications, for example the test of time-variations of fundamental constants, ultracold chemistry on the quantum level, and quantum information and computing, to name just a few...

Plutonium determination by isotope dilution

International Nuclear Information System (INIS)

Lucas, M.

1980-01-01

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

Isotopic analysis of uranium hexafluoride highly enriched in U-235; Analyse isotopique de l'hexafluorure d'uranium fortement enrichi en U 235

Energy Technology Data Exchange (ETDEWEB)

Chaussy, L; Boyer, R [Commissariat a l' Energie Atomique, Pierrelatte (France). Centre d' Etudes Nucleaires

1968-07-01

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 ({approx_equal}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) [French] L'analyse isotopique de l'uranium sous forme d'hexafluorure, par spectrometrie de masse, fournit des resultats bruts entaches d'inexactitude. Une methode d'interpolation lineaire entre deux etalons permet de corriger cette inexactitude, tant que les concentrations isotopiques sont inferieures a 10 pour cent en U-235 environ. Au-dessus de cette valeur, la formule d'interpolation surestime les resultats, notamment si l'enrichissement des echantillons analyses par rapport aux etalons est superieur a 1,3. On propose une formule de correction de l'equation d'interpolation qui etend son domaine d'application jusqu'a des valeurs elevees d'enrichissement ({approx_equal}2) et de concentration. On montre experimentalement que par cette correction, les resultats atteignent, a la precision des mesures, une exactitude qui ne depend pratiquement plus que de celles des etalons. (auteurs)

Precision and reproducibility in AMS radiocarbon measurements.

Energy Technology Data Exchange (ETDEWEB)

Hotchkis, M.A.; Fink, D.; Hua, Q.; Jacobsen, G.E.; Lawson, E. M.; Smith, A.M.; Tuniz, C. [Australian Nuclear Science and Technology Organisation, Lucas Heights, NSW (Australia)

1996-12-31

Accelerator Mass Spectrometry (AMS) is a technique by which rare radioisotopes such as {sup 14}C can be measured at environmental levels with high efficiency. Instead of detecting radioactivity, which is very weak for long-lived environmental radioisotopes, atoms are counted directly. The sample is placed in an ion source, from which a negative ion beam of the atoms of interest is extracted, mass analysed, and injected into a tandem accelerator. After stripping to positive charge states in the accelerator HV terminal, the ions are further accelerated, analysed with magnetic and electrostatic devices and counted in a detector. An isotopic ratio is derived from the number of radioisotope atoms counted in a given time and the beam current of a stable isotope of the same element, measured after the accelerator. For radiocarbon, {sup 14}C/{sup 13}C ratios are usually measured, and the ratio of an unknown sample is compared to that of a standard. The achievable precision for such ratio measurements is limited primarily by {sup 14}C counting statistics and also by a variety of factors related to accelerator and ion source stability. At the ANTARES AMS facility at Lucas Heights Research Laboratories we are currently able to measure {sup 14}C with 0.5% precision. In the two years since becoming operational, more than 1000 {sup 14}C samples have been measured. Recent improvements in precision for {sup 14}C have been achieved with the commissioning of a 59 sample ion source. The measurement system, from sample changing to data acquisition, is under common computer control. These developments have allowed a new regime of automated multi-sample processing which has impacted both on the system throughput and the measurement precision. We have developed data evaluation methods at ANTARES which cross-check the self-consistency of the statistical analysis of our data. Rigorous data evaluation is invaluable in assessing the true reproducibility of the measurement system and aids in

Precision and reproducibility in AMS radiocarbon measurements.

Energy Technology Data Exchange (ETDEWEB)

Hotchkis, M A; Fink, D; Hua, Q; Jacobsen, G E; Lawson, E M; Smith, A M; Tuniz, C [Australian Nuclear Science and Technology Organisation, Lucas Heights, NSW (Australia)

1997-12-31

Accelerator Mass Spectrometry (AMS) is a technique by which rare radioisotopes such as {sup 14}C can be measured at environmental levels with high efficiency. Instead of detecting radioactivity, which is very weak for long-lived environmental radioisotopes, atoms are counted directly. The sample is placed in an ion source, from which a negative ion beam of the atoms of interest is extracted, mass analysed, and injected into a tandem accelerator. After stripping to positive charge states in the accelerator HV terminal, the ions are further accelerated, analysed with magnetic and electrostatic devices and counted in a detector. An isotopic ratio is derived from the number of radioisotope atoms counted in a given time and the beam current of a stable isotope of the same element, measured after the accelerator. For radiocarbon, {sup 14}C/{sup 13}C ratios are usually measured, and the ratio of an unknown sample is compared to that of a standard. The achievable precision for such ratio measurements is limited primarily by {sup 14}C counting statistics and also by a variety of factors related to accelerator and ion source stability. At the ANTARES AMS facility at Lucas Heights Research Laboratories we are currently able to measure {sup 14}C with 0.5% precision. In the two years since becoming operational, more than 1000 {sup 14}C samples have been measured. Recent improvements in precision for {sup 14}C have been achieved with the commissioning of a 59 sample ion source. The measurement system, from sample changing to data acquisition, is under common computer control. These developments have allowed a new regime of automated multi-sample processing which has impacted both on the system throughput and the measurement precision. We have developed data evaluation methods at ANTARES which cross-check the self-consistency of the statistical analysis of our data. Rigorous data evaluation is invaluable in assessing the true reproducibility of the measurement system and aids in

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.

Observing exoplanet populations with high-precision astrometry

Science.gov (United States)

Sahlmann, Johannes

2012-06-01

This thesis deals with the application of the astrometry technique, consisting in measuring the position of a star in the plane of the sky, for the discovery and characterisation of extra-solar planets. It is feasible only with a very high measurement precision, which motivates the use of space observatories, the development of new ground-based astronomical instrumentation and of innovative data analysis methods: The study of Sun-like stars with substellar companions using CORALIE radial velocities and HIPPARCOS astrometry leads to the determination of the frequency of close brown dwarf companions and to the discovery of a dividing line between massive planets and brown dwarf companions; An observation campaign employing optical imaging with a very large telescope demonstrates sufficient astrometric precision to detect planets around ultra-cool dwarf stars and the first results of the survey are presented; Finally, the design and initial astrometric performance of PRIMA, ! a new dual-feed near-infrared interferometric observing facility for relative astrometry is presented.

A solvent extraction technique for the isotopic measurement of dissolved copper in seawater

Energy Technology Data Exchange (ETDEWEB)

Thompson, Claire M., E-mail: claire.thompson@anu.edu.au; Ellwood, Michael J., E-mail: michael.ellwood@anu.edu.au; Wille, Martin, E-mail: martin.wille@uni-tuebingen.de

2013-05-02

Graphical abstract: -- Highlights: •A new sample preparation method for seawater copper isotopic analysis (δ{sup 65}Cu). •Solvent-extraction was used to pre-concentrate metals from seawater samples. •Anion-exchange was used to purify copper from the metal-rich extract. •δ{sup 65}Cu was measured in the north Tasman Sea. •Seawater δ{sup 65}Cu may be linked to marine biological activity. -- Abstract: Stable copper (Cu) isotope geochemistry provides a new perspective for investigating and understanding Cu speciation and biogeochemical Cu cycling in seawater. In this work, sample preparation for isotopic analysis employed solvent-extraction with amino pyrollidine dithiocarbamate/diethyl dithiocarbamate (APDC/DDC), coupled with a nitric acid back-extraction, to concentrate Cu from seawater. This was followed by Cu-purification using anion-exchange. This straightforward technique is high yielding and fractionation free for Cu and allows precise measurement of the seawater Cu isotopic composition using multi-collector inductively coupled plasma mass-spectrometry. A deep-sea profile measured in the oligotrophic north Tasman Sea shows fractionation in the Cu isotopic signature in the photic zone but is relatively homogenised at depth. A minima in the Cu isotopic profile correlates with the chlorophyll a maximum at the site. These results indicate that a range of processes are likely to fractionate stable Cu isotopes in seawater.

Application of Stable Isotope-Assisted Metabolomics for Cell Metabolism Studies

Science.gov (United States)

You, Le; Zhang, Baichen; Tang, Yinjie J.

2014-01-01

The applications of stable isotopes in metabolomics have facilitated the study of cell metabolisms. Stable isotope-assisted metabolomics requires: (1) properly designed tracer experiments; (2) stringent sampling and quenching protocols to minimize isotopic alternations; (3) efficient metabolite separations; (4) high resolution mass spectrometry to resolve overlapping peaks and background noises; and (5) data analysis methods and databases to decipher isotopic clusters over a broad m/z range (mass-to-charge ratio). This paper overviews mass spectrometry based techniques for precise determination of metabolites and their isotopologues. It also discusses applications of isotopic approaches to track substrate utilization, identify unknown metabolites and their chemical formulas, measure metabolite concentrations, determine putative metabolic pathways, and investigate microbial community populations and their carbon assimilation patterns. In addition, 13C-metabolite fingerprinting and metabolic models can be integrated to quantify carbon fluxes (enzyme reaction rates). The fluxome, in combination with other “omics” analyses, may give systems-level insights into regulatory mechanisms underlying gene functions. More importantly, 13C-tracer experiments significantly improve the potential of low-resolution gas chromatography-mass spectrometry (GC-MS) for broad-scope metabolism studies. We foresee the isotope-assisted metabolomics to be an indispensable tool in industrial biotechnology, environmental microbiology, and medical research. PMID:24957020

Efficacy of passive sampler collection for atmospheric NO2 isotopes under simulated environmental conditions.

Science.gov (United States)

Coughlin, Justin G; Yu, Zhongjie; Elliott, Emily M

2017-07-30

Nitrogen oxides or NO x (NO x = NO + NO 2 ) play an important role in air quality, atmospheric chemistry, and climate. The isotopic compositions of anthropogenic and natural NO 2 sources are wide-ranging, and they can be used to constrain sources of ambient NO 2 and associated atmospheric deposition of nitrogen compounds. While passive sample collection of NO 2 isotopes has been used in field studies to determine NO x source influences on atmospheric deposition, this approach has not been evaluated for accuracy or precision under different environmental conditions. The efficacy of NO 2 passive sampler collection for NO 2 isotopes was evaluated under varied temperature and relative humidity (RH) conditions in a dynamic flux chamber. The precision and accuracy of the filter NO 2 collection as nitrite (NO 2 - ) for isotopic analysis were determined using a reference NO 2 gas tank and through inter-calibration with a modified EPA Method 7. The bacterial denitrifer method was used to convert 20 μM of collected NO 2 - or nitrate (NO 3 - ) into N 2 O and was carried out on an Isoprime continuous flow isotope ratio mass spectrometer. δ 15 N-NO 2 values determined from passive NO 2 collection, in conditions of 11-34 °C, 1-78% RH, have an overall accuracy and precision of ±2.1 ‰, and individual run precision of ±0.6 ‰. δ 18 O-NO 2 values obtained from passive NO 2 sampler collection, under the same conditions, have an overall precision of ± 1.3 ‰. Suitable conditions for passive sampler collection of NO 2 isotopes are in environments ranging from 11 to 34 °C and 1 to 78% RH. The passive NO 2 isotope measurement technique provides an accurate method to determine variations in atmospheric δ 15 N-NO 2 values and a precise method for determining atmospheric δ 18 O-NO 2 values. The ability to measure NO 2 isotopes over spatial gradients at the same temporal resolution provides a unique perspective on the extent and seasonality of fluctuations in atmospheric NO 2

Gas chromatography/isotope ratio mass spectrometry: analysis of methanol, ethanol and acetic acid by direct injection of aqueous alcoholic and acetic acid samples.

Science.gov (United States)

Ai, Guomin; Sun, Tong; Dong, Xiuzhu

2014-08-15

Methanol, ethanol, and acetic acid are not easily extracted from aqueous samples and are susceptible to isotope fractionation in gas chromatography/isotope ratio mass spectrometry (GC/IRMS) analysis. Developing a direct dilution GC/IRMS method for aqueous samples, by adjusting the sample concentrations in common solvents to be similar to each other and using a fixed GC split ratio, is very convenient and important because any linearity effects caused by amount-dependent isotope fractionation can be avoided. The suitability of acetonitrile and acetone solvents for the GC/IRMS analysis of pure methanol, ethanol and acetic acid, and commercial liquor and vinegar samples was evaluated using n-hexane and water as control solvents. All the solvents including water were separated from the analyte on a HP-INNOWAX column and were diverted away from the combustion interface. The influence of liquor matrix on the ethanol GC/IRMS analyses was evaluated by adding pure ethanol to liquor samples. Acetonitrile and acetone gave similar δ(13) C values for pure ethanol and pure acetic acid to those obtained in water and n-hexane, and also gave similar δ(13) C values of ethanol in liquor and acetic acid in white vinegar to that obtained in water. For methanol analysis, acetonitrile and refined acetone gave similar δ(13) C values to that obtained in water, but n-hexane was not a suitable solvent. In addition, isotopic fractionation caused by solvent and solute interactions was observed. We recommend using acetonitrile for the GC/IRMS analysis of aqueous alcoholic samples, and acetone for the analysis of aqueous acetic acid samples. This direct dilution method can provide high accurate and precise GC/IRMS analysis of the relative changes in δ(13) C values of methanol, ethanol, and acetic acid. Copyright © 2014 John Wiley & Sons, Ltd.

High Precision Fast Projective Synchronization for Chaotic Systems with Unknown Parameters

Science.gov (United States)

Nian, Fuzhong; Wang, Xingyuan; Lin, Da; Niu, Yujun

2013-08-01

A high precision fast projective synchronization method for chaotic systems with unknown parameters was proposed by introducing optimal matrix. Numerical simulations indicate that the precision be improved about three orders compared with other common methods under the same condition of software and hardware. Moreover, when average error is less than 10-3, the synchronization speed is 6500 times than common methods, the iteration needs only 4 times. The unknown parameters also were identified rapidly. The theoretical analysis and proof also were given.

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...

High Precision Zinc Stable Isotope Measurement of Certified Biological Reference Materials Using the Double Spike Technique and Multiple Collector-ICP-MS.

Science.gov (United States)

Moore, Rebekah E T; Larner, Fiona; Coles, Barry J; Rehkämper, Mark

2017-04-01

Biological reference materials with well-characterised stable isotope compositions are lacking in the field of 'isotope biochemistry', which seeks to understand bodily processes that rely on essential metals by determining metal stable isotope ratios. Here, we present Zn stable isotope data for six biological reference materials with certified trace metal concentrations: fish muscle, bovine muscle, pig kidney, human hair, human blood serum and human urine. Replicate analyses of multiple aliquots of each material achieved reproducibilities (2sd) of 0.04-0.13‰ for δ 66/64 Zn (which denotes the deviation of the 66 Zn/ 64 Zn ratio of a sample from a pure Zn reference material in parts per 1000). This implies only very minor isotopic heterogeneities within the samples, rendering them suitable as quality control materials for Zn isotope analyses. This endorsement is reinforced by (i) the close agreement of our Zn isotope data for two of the samples (bovine muscle and human blood serum) to previously published results for different batches of the same material and (ii) the similarity of the isotopic data for the samples (δ 66/64 Zn ≈ -0.8 to 0.0‰) to previously published Zn isotope results for similar biological materials. Further tests revealed that the applied Zn separation procedure is sufficiently effective to enable accurate data acquisition even at low mass resolving power (M/ΔM ≈ 400), as measurements and analyses conducted at much higher mass resolution (M/ΔM ≈ 8500) delivered essentially identical results.

Calibration and correction of LA-ICP-MS and LA-MC-ICP-MS analyses for element contents and isotopic ratios

Directory of Open Access Journals (Sweden)

Jie Lin

2016-06-01

Full Text Available LA-ICP-MS and LA-MC-ICP-MS have been the techniques of choice for achieving accurate and precise element content and isotopic ratio, the state-of-the-art technique combines the advantages of low detection limits with high spatial resolution, however, the analysis accuracy and precision are restricted by many factors, such as sensitivity drift, elemental/isotopic fractionation, matrix effects, interferences and the lack of sufficiently matrix-matched reference materials. Thus, rigorous and suitable calibration and correction methods are needed to obtain quantitative data. This review systematically summarized and evaluated the interference correction, quantitative calculation and sensitivity correction strategies in order to provide the analysts with suitable calibration and correction strategies according to the sample types and the analyzed elements. The functions and features of data reduction software ICPMSDataCal were also outlined, which can provide real-time and on-line data reduction of element content and isotopic ratios analyzed by LA-ICP-MS and LA-MC-ICP-MS.

Redox substoichiometric isotope dilution analysis of metallic arsenic for antimony

International Nuclear Information System (INIS)

Kambara, Tomihisa; Yoshioka, Hiroe; Suzuki, Junsuke; Shibata, Yasue.

1979-01-01

In 1 M HCl solution Sb(III) reacts with N-benzoyl-N-phenylhydroxylamine (BPHA) to form a complex extractable into chloroform while the extraction of Sb(V) is negligible. The redox substoichiometric isotope dilution analysis based on this reaction was applied to the determination of antimony in metallic arsenic. After the dissolution of metallic arsenic, Sb(V) was separated from As(V) by a tribenzylamine extraction from 8 M HCl solution and the extracted Sb(V) was stripped into 0.5 M NaOH solution. Thereafter, all the Sb(V) were completely reduced to Sb(III) by bubbling SO 2 gas through 3 M HCl solution. As the substoichiometric reaction, the oxidation of Sb(III) to Sb(V) by a substoichiometric amount of potassium dichromate was used, followed by separation of these species by the BPHA extraction of Sb(III). The substoichiometric oxidation of Sb(III) was found to be quantitative over HCl concentration range from 0.8 to 1.2 M. The amount of antimony was determined by isotope dilution analysis using the method of carrier amount variation. By the present method the determination of as small as 0.36 μg antimony was accomplished with a good accuracy (relative error; 5.6%) and also the method was successfully applied to the determination of antimony in arsenic samples containing known amounts of Sb(III) and in metallic arsenic. The present method gives reliable results with the good accuracy and precision. (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.

Long-term field performance of a tunable diode laser absorption spectrometer for analysis of carbon isotopes of CO2 in forest air

Directory of Open Access Journals (Sweden)

D. R. Bowling

2008-09-01

Full Text Available Tunable diode laser absorption spectrometry (TDLAS is gaining in popularity for measuring the mole fraction [CO2] and stable isotopic composition (δ13C of carbon dioxide (CO2 in air in studies of biosphere-atmosphere gas exchange. Here we present a detailed examination of the performance of a commercially-available TDLAS located in a high-altitude subalpine coniferous forest (the Niwot Ridge AmeriFlux site, providing the first multi-year analysis of TDLAS instrument performance for measuring CO2 isotopes in the field. Air was sampled from five to nine vertical locations in and above the forest canopy every ten minutes for 2.4 years. A variety of methods were used to assess instrument performance. Measurement of two compressed air cylinders that were in place over the entire study establish the long-term field precision of 0.2 μmol mol−1 for [CO2] and 0.35‰ for δ13C, but after fixing several problems the isotope precision improved to 0.2permil (over the last several months. The TDLAS provided detail on variability of δ13C of atmospheric CO2 that was not represented in weekly flask samples, as well as information regarding the influence of large-scale (regional seasonal cycle and local forest processes on [CO2] and δ13C of CO2. There were also clear growing season and winter differences in the relative contributions of photosynthesis and respiration on the [CO2] and δ13C of forest air.

Pb isotope analysis of ng size samples by TIMS equipped with a 1013 Ω resistor using a 207Pb-204Pb double spike

NARCIS (Netherlands)

Klaver, M.; Smeets, R.J.; Koornneef, J.M.; Davies, G.R.; Vroon, P.Z.

2016-01-01

The use of the double spike technique to correct for instrumental mass fractionation has yielded high precision results for lead isotope measurements by thermal ionisation mass spectrometry (TIMS), but the applicability to ng size Pb samples is hampered by the small size of the

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

Upgrade of the SPIRAL identification station for high-precision measurements of nuclear β decay

Science.gov (United States)

Grinyer, G. F.; Thomas, J. C.; Blank, B.; Bouzomita, H.; Austin, R. A. E.; Ball, G. C.; Bucaille, F.; Delahaye, P.; Finlay, P.; Frémont, G.; Gibelin, J.; Giovinazzo, J.; Grinyer, J.; Kurtukian-Nieto, T.; Laffoley, A. T.; Leach, K. G.; Lefèvre, A.; Legruel, F.; Lescalié, G.; Perez-Loureiro, D.

2014-03-01

The low-energy identification station at SPIRAL (Système de Production d'Ions Radioactifs Accélérés en Ligne) has been upgraded for studying the β decays of short-lived radioactive isotopes and to perform high-precision half-life and branching-ratio measurements for superallowed Fermi and isospin T=1/2 mirror β decays. These new capabilities, combined with an existing Paul trap setup for measurements of β-ν angular-correlation coefficients, provide a powerful facility for investigating fundamental properties of the electroweak interaction through nuclear β decays. A detailed description of the design study, construction, and first results obtained from an in-beam commissioning experiment on the β+ decays 14 O and 17F are presented.

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

H/D isotope effects in high temperature proton conductors

DEFF Research Database (Denmark)

Bonanos, Nikolaos; Huijser, A.; Poulsen, Finn Willy

2015-01-01

The atomic mass ratio of ca. 2 between deuterium and hydrogen is the highest for any pair of stable isotopes and results in significant and measurable H/D isotope effects in high temperature proton conductors containing these species. This paper discusses H/D isotope effects manifested in O-H/O-D...

Oxygen isotope systematics of chondrules in the Allende CV3 chondrite: High precision ion microprobe studies

Digital Repository Service at National Institute of Oceanography (India)

Rudraswami, N.G.; Ushikubo, T.; Nakashima, D.; Kita, N.T.

grains and some of them were derived from precursors related to refractory inclusions. However, most relict olivine grains show oxygen isotope ratios that overlap with those in homogeneous chondrules. The delta sup(17)O values of four barred olivine...

Solution Method and Precision Analysis of Double-difference Dynamic Precise Orbit Determination of BeiDou Navigation Satellite System

Directory of Open Access Journals (Sweden)

LIU Weiping

2016-02-01

Full Text Available To resolve the high relativity between the transverse element of GEO orbit and double-difference ambiguity, the classical double-difference dynamic method is improved and the method, which is to determine precise BeiDou satellite orbit using carrier phase and pseudo-range smoothed by phase, is proposed. The feasibility of the method is discussed and the influence of the method about ambiguity fixing is analyzed. Considering the characteristic of BeiDou, the method, which is to fix double-difference ambiguity of BeiDou satellites by QIF, is derived. The real data analysis shows that the new method, which can reduce the relativity and assure the precision, is better than the classical double-difference dynamic method. The result of ambiguity fixing is well by QIF, but the ambiguity fixing success rate is not high on the whole. So the precision of BeiDou orbit can't be improved clearly after ambiguity fixing.

Isotopic measurement of uranium using NP-type chelate resin beads

International Nuclear Information System (INIS)

Wu Lanbi; Chen Wenpo; Wang Shijun

1994-08-01

NP-type chelate resin beads is used as a carrier of samples in the isotopic measurements of uranium by mass spectrometry. The results show that its absorption efficiency for uranium can be greater than 50%. It is one order magnitude higher than that strong basic anion resin, however, the ionization efficiencies of both are almost the same. Therefore, the amount of uranium required for isotopic analysis can be reduced one order of magnitude. This method has been used for isotopic analysis of uranium in NP-type chelate resin beads contained 10 -9 ∼ 10 -7 g uranium. For standard sample UTB-500, the external precision of measurements are within +-0.2%, for natural uranium samples are within +- 0.5%. The application of NP-type chelate resin beads in the isotopic measurement of uranium is a new creative achievement. It has been used in the depletion test of uranium-atomic vapor laser isotope separation

Dynamics of High-Speed Precision Geared Rotor Systems

Directory of Open Access Journals (Sweden)

Lim Teik C.

2014-07-01

Full Text Available Gears are one of the most widely applied precision machine elements in power transmission systems employed in automotive, aerospace, marine, rail and industrial applications because of their reliability, precision, efficiency and versatility. Fundamentally, gears provide a very practical mechanism to transmit motion and mechanical power between two rotating shafts. However, their performance and accuracy are often hampered by tooth failure, vibrations and whine noise. This is most acute in high-speed, high power density geared rotor systems, which is the primary scope of this paper. The present study focuses on the development of a gear pair mathematical model for use to analyze the dynamics of power transmission systems. The theory includes the gear mesh representation derived from results of the quasi-static tooth contact analysis. This proposed gear mesh theory comprising of transmission error, mesh point, mesh stiffness and line-of-action nonlinear, time-varying parameters can be easily incorporated into a variety of transmission system models ranging from the lumped parameter type to detailed finite element representation. The gear dynamic analysis performed led to the discovery of the out-of-phase gear pair torsion modes that are responsible for much of the mechanical problems seen in gearing applications. The paper concludes with a discussion on effectual design approaches to minimize the influence of gear dynamics and to mitigate gear failure in practical power transmission systems.

High mass isotope separation arrangement

International Nuclear Information System (INIS)

Eerkens, J.W.

1976-01-01

An isotope separation arrangement for separating a preselected isotope from a mixture of chemically-identical but isotopically-different molecules by either photon-induced pure revibrational or vibronic selective excitation of the molecules containing the atoms of the isotope to be separated from a lower to a higher energy state, and a chemical reaction of the higher energy state molecules with a chemically-reactive agent to form a chemical compound containing primarily the atoms of the isotope to be separated in a physicochemical state different from the physicochemical state of the mixture of chemically-identical but isotopically-different molecules. The chemical compound containing the atoms of the isotope to be separated may be subsequently processed to obtain the isotope. The laser configuration used to generate the photon beam is fully described

Isotopic analysis using optical spectroscopy (1963); Analyse isotopique par spectroscopie optique (1963)

Energy Technology Data Exchange (ETDEWEB)

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

1963-07-01

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) [French] Le deplacement isotopique dans les raies atomiques de certains elements (H, He, Li, Ne, Sr, Hg, Pb, U, Pu) est utilise pour effectuer le dosage isotopique de ces elements. L'utilisation du spectrometre interferentiel Fabry-Perot photoelectrique se revele particulierement adapte a ce genre de probleme: dans chaque cas, nous donnons d'une part l'essentiel des resultats obtenus avec cet appareil, et d'autre part, les resultats obtenus anterieurement a l'aide de l'appareillage classique (reseau, plaque photographique). L'ensemble de ces informations donne une idee des possibilites offertes par la spectroscopie optique: dans le meilleur des cas, la precision que l'on peut esperer est de l'ordre de 1 a 2 pour cent pour des isotopes dont la concentration est de l'ordre de 1 pour cent. (auteur)

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.

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

Analysis of 14C and 13C in teeth provides precise birth dating and clues to geographical origin.

Science.gov (United States)

Alkass, K; Buchholz, B A; Druid, H; Spalding, K L

2011-06-15

The identification of human bodies in situations when there are no clues as to the person's identity from circumstantial data, poses a difficult problem to the investigators. The determination of age and sex of the body can be crucial in order to limit the search to individuals that are a possible match. We analyzed the proportion of bomb pulse derived carbon-14 ((14)C) incorporated in the enamel of teeth from individuals from different geographical locations. The 'bomb pulse' refers to a significant increase in (14)C levels in the atmosphere caused by above ground test detonations of nuclear weapons during the cold war (1955-1963). By comparing (14)C levels in enamel with (14)C atmospheric levels systematically recorded over time, high precision birth dating of modern biological material is possible. Above ground nuclear bomb testing was largely restricted to a couple of locations in the northern hemisphere, producing differences in atmospheric (14)C levels at various geographical regions, particularly in the early phase. Therefore, we examined the precision of (14)C birth dating of enamel as a function of time of formation and geographical location. We also investigated the use of the stable isotope (13)C as an indicator of geographical origin of an individual. Dental enamel was isolated from 95 teeth extracted from 84 individuals to study the precision of the (14)C method along the bomb spike. For teeth formed before 1955 (N=17), all but one tooth showed negative Δ(14)C values. Analysis of enamel from teeth formed during the rising part of the bomb-spike (1955-1963, N=12) and after the peak (>1963, N=66) resulted in an average absolute date of birth estimation error of 1.9±1.4 and 1.3±1.0 years, respectively. Geographical location of an individual had no adverse effect on the precision of year of birth estimation using radiocarbon dating. In 46 teeth, measurement of (13)C was also performed. Scandinavian teeth showed a substantially greater depression in

Using a laser-based CO2 carbon isotope analyser to investigate gas transfer in geological media

International Nuclear Information System (INIS)

Guillon, S.; Pili, E.; Agrinier, P.

2012-01-01

CO 2 stable carbon isotopes are very attractive in environmental research to investigate both natural and anthropogenic carbon sources. Laser-based CO 2 carbon isotope analysis provides continuous measurement at high temporal resolution and is a promising alternative to isotope ratio mass spectrometry (IRMS). We performed a thorough assessment of a commercially available CO 2 Carbon Isotope Analyser (CCIA DLT-100, Los Gatos Research) that allows in situ measurement of C-13 in CO 2 . Using a set of reference gases of known CO 2 concentration and carbon isotopic composition, we evaluated the precision, long-term stability, temperature sensitivity and concentration dependence of the analyser. Despite good precision calculated from Allan variance (5.0 ppm for CO 2 concentration, and 0.05 per thousand for δC-13 at 60 s averaging), real performances are altered by two main sources of error: temperature sensitivity and dependence of C-13 on CO 2 concentration. Data processing is required to correct for these errors. Following application of these corrections, we achieve an accuracy of 8.7 ppm for CO 2 concentration and 1.3 per thousand for δC-13, which is worse compared to mass spectrometry performance, but still allowing field applications. With this portable analyser we measured CO 2 flux degassed from rock in an underground tunnel. The obtained carbon isotopic composition agrees with IRMS measurement, and can be used to identify the carbon source. (authors)

Increasing Precision and Accuracy of Laser Isotope Analyser Data

International Nuclear Information System (INIS)

Chen, Janet; Mayr, Leopold; Resch, Christian; Dercon, Gerd

2017-01-01

Isotope analysis with laser spectroscopy is an emerging technology that is growing in scientific demand. Because this technology allows for real-time, in situ measurements of carbon-13 ("1"3C) and nitrogen-15 ("1"5N) of CO_2, CH_4 and N_2O, it is increasingly being used to monitor fluxes of these greenhouse gases. However, despite its potential to provide robust data to researchers, methods of calibration and data correction are still being developed and refined. Furthermore, standard reference gases are currently not available and researchers must make their own gases to ensure proper calibration and data correction. To improve quality of data and allow for comparison of data between studies, it is essential that standard CO_2, CH_4 and N_2O gases are accessible to researchers.

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

International Nuclear Information System (INIS)

Patterson, K.Y.; Veillon, Claude

1992-01-01

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

An improved data acquisition system for isotopic ratio mass spectrometers

International Nuclear Information System (INIS)

Saha, T.K.; Reddy, B.; Nazare, C.K.; Handu, V.K.

1999-01-01

Isotopic ratio mass spectrometers designed and fabricated to measure the isotopic ratios with a precision of better than 0.05%. In order to achieve this precision, the measurement system consisting of ion signal to voltage converters, analog to digital converters, and data acquisition electronics should be at least one order better than the overall precision of measurement. Using state of the art components and techniques, a data acquisition system, which is an improved version of the earlier system, has been designed and developed for use with multi-collector isotopic ratio mass spectrometers

Trace analysis of U, Th and other heavy metals in high purity aluminium with isotope dilution mass spectrometry

International Nuclear Information System (INIS)

Beer, B.; Heumann, K.G.

1992-01-01

A method for the determination of very low concentrations of U, Th, Fe, Zn, Tl, Cd, Cu and Ag in high purity aluminium with isotope dilution mass spectrometry (IDMS) is developed using a compact and cost-efficient thermal ionization quadrupole mass spectrometer. The detection limits obtained are (in ng/g):U=0.018, Th=0.06, Fe=82, Zn=86, Tl=0.2, Cd=4, Cu=1, Ag=2.6. By this method it is possible to determine the α-emitters U and Th in aluminium down to the sub-ng/g level with good precision of 0.4-10% and 0.5-5%, respectively. The results should also be accurate because IDMS is a reliable analytical method. The dissolution of aluminium is carried out by aqua regia followed by the trace/matrix separation and the isolation of the trace elements by anion exchange chromatography (U, Th, Zn, Tl, Cd), electrodeposition (Cu, Ag) and extraction (Fe). Different aluminium samples are analysed by IDMS and the results are compared with those of other methods. (orig.)

Use of isotopes for increasing biological nitrogen fixation and yield of pastures

International Nuclear Information System (INIS)

Yao Yunyin

1992-05-01

The N-15 natural abundance and N-15 isotope dilution (ID) methods for measuring dinitrogen fixation and nitrogen transfer in alfalfa and alfalfa intercropped with meadow fescue were compared in three experiments. Although both methods gave essentially the same estimates the precision of the values obtained differed, and values obtained by the isotope dilution method were more precise. Similarly, the N-15 natural abundance method was not very suitable for detecting N transfer from legume to non-legume. Greater amounts of N transfer were detected by the ID method, and with a greater precision. Mixed cropping sometimes gave slight to high increases in % nitrogen fixation compared to alfalfa cropped alone. On the whole alfalfa was found to be a high nitrogen fixer, with fixation values from the second harvest onwards almost always greater than 80% and often close to 100%. 23 refs, 30 tabs

Near-Continuous Isotopic Characterization of Soil N2O Fluxes from Maize Production

Science.gov (United States)

Anex, R. P.; Francis Clar, J.

2015-12-01

Isotopomer ratios of N2O and especially intramolecular 15N site preference (SP) have been proposed as indicators of the sources of N2O and for providing insight into the contributions of different microbial processes. Current knowledge, however, is mainly based on pure culture studies and laboratory flask studies using mass spectrometric analysis. Recent development of laser spectroscopic methods has made possible high-precision, in situ measurements. We present results from a maize production field in Columbia County, Wisconsin, USA. Data were collected from the fertilized maize phase of a maize-soybean rotation. N2O mole fractions and isotopic composition were determined using an automatic gas flux measurement system comprising a set of custom-designed automatic chambers, circulating gas paths and an OA-ICOS N2O Isotope Analyzer (Los Gatos Research, Inc., Model 914-0027). The instrument system allows for up to 15 user programmable soil gas chambers. Wide dynamic range and parts-per-billion precision of OA-ICOS laser absorption instrument allows for extremely rapid estimation of N2O fluxes. Current operational settings provide measurements of N2O and its isotopes every 20 seconds with a precision of 0.1 ± 0.050 PPB. Comparison of measurements from four chambers (two between row and two in-row) show very different aggregate N2O flux, but SP values suggest similar sources from nitrifier denitrification and incomplete bacterial denitrification. SP values reported are being measured throughout the current growing season. To date, the majority of values are consistent with an origin from bacterial denitrification and coincide with periods of high water filled pore space.

A novel high-temperature combustion based system for stable isotope analysis of dissolved organic carbon in aqueous samples. : I development and validation

NARCIS (Netherlands)

Federherr, E.; Cerli, C.; Kirkels, F. M. S. A.; Kalbitz, K.; Kupka, H. J.; Dunsbach, R.; Lange, L.; Schmidt, T. C.

2014-01-01

RATIONALE: Traditionally, dissolved organic carbon (DOC) stable isotope analysis (SIA) is performed using either offline sample preparation followed by elemental analyzer/isotope ratiomass spectrometry (EA/IRMS) or a wet chemical oxidation (WCO)-based device coupled to an isotope ratio mass

High precision timing in a FLASH

Energy Technology Data Exchange (ETDEWEB)

Hoek, Matthias; Cardinali, Matteo; Dickescheid, Michael; Schlimme, Soeren; Sfienti, Concettina; Spruck, Bjoern; Thiel, Michaela [Institut fuer Kernphysik, Johannes Gutenberg-Universitaet Mainz (Germany)

2016-07-01

A segmented highly precise start counter (FLASH) was designed and constructed at the Institute for Nuclear Physics in Mainz. Besides determining a precise reference time, a Time-of-Flight measurement can be performed with two identical FLASH units. Thus, particle identification can be provided for mixed hadron beam environments. The detector design is based on the detection of Cherenkov light produced in fused silica radiator bars with fast multi-anode MCP-PMTs. The segmentation of the radiator improves the timing resolution while allowing a coarse position resolution along one direction. Both, the arrival time and the Time-over-Threshold are determined by the readout electronics, which enables walk correction of the arrival time. The performance of two FLASH units was investigated in test experiments at the Mainz Microton (MAMI) using an electron beam with an energy of 855 MeV and at CERN's PS T9 beam line with a mixed hadron beam with momenta between 3-8 GeV/c. Effective Time-walk correction methods based on Time-over-Threshold were developed for the data analysis. The achieved Time-Of-Flight resolution after applying all corrections was found to be 70 ps. Furthermore, the PID and position resolution capabilities are discussed in this contribution.

High-Precision Computation: Mathematical Physics and Dynamics

International Nuclear Information System (INIS)

Bailey, D.H.; Barrio, R.; Borwein, J.M.

2010-01-01

At the present time, IEEE 64-bit oating-point arithmetic is suficiently accurate for most scientic applications. However, for a rapidly growing body of important scientic computing applications, a higher level of numeric precision is required. Such calculations are facilitated by high-precision software packages that include high-level language translation modules to minimize the conversion e ort. This pa- per presents a survey of recent applications of these techniques and provides someanalysis of their numerical requirements. These applications include supernova simulations, climate modeling, planetary orbit calculations, Coulomb n-body atomic systems, studies of the one structure constant, scattering amplitudes of quarks, glu- ons and bosons, nonlinear oscillator theory, experimental mathematics, evaluation of orthogonal polynomials, numerical integration of ODEs, computation of periodic orbits, studies of the splitting of separatrices, detection of strange nonchaotic at- tractors, Ising theory, quantum held theory, and discrete dynamical systems. We conclude that high-precision arithmetic facilities are now an indispensable compo- nent of a modern large-scale scientic computing environment.

High-Precision Computation: Mathematical Physics and Dynamics

Energy Technology Data Exchange (ETDEWEB)

Bailey, D. H.; Barrio, R.; Borwein, J. M.

2010-04-01

At the present time, IEEE 64-bit oating-point arithmetic is suficiently accurate for most scientic applications. However, for a rapidly growing body of important scientic computing applications, a higher level of numeric precision is required. Such calculations are facilitated by high-precision software packages that include high-level language translation modules to minimize the conversion e ort. This pa- per presents a survey of recent applications of these techniques and provides someanalysis of their numerical requirements. These applications include supernova simulations, climate modeling, planetary orbit calculations, Coulomb n-body atomic systems, studies of the one structure constant, scattering amplitudes of quarks, glu- ons and bosons, nonlinear oscillator theory, experimental mathematics, evaluation of orthogonal polynomials, numerical integration of ODEs, computation of periodic orbits, studies of the splitting of separatrices, detection of strange nonchaotic at- tractors, Ising theory, quantum held theory, and discrete dynamical systems. We conclude that high-precision arithmetic facilities are now an indispensable compo- nent of a modern large-scale scientic computing environment.

A Portable, Field-Deployable Analyzer for Isotopic Water Measurements

Science.gov (United States)

Berman, E. S.; Gupta, M.; Huang, Y. W.; Lacelle, D.; McKay, C. P.; Fortson, S.

2015-12-01

Water stable isotopes have for many years been used to study the hydrological cycle, catchment hydrology, and polar climate among other applications. Typically, discrete water samples are collected and transported to a laboratory for isotope analysis. Due to the expense and labor associated with such sampling, isotope studies have generally been limited in scope and time-resolution. Field sampling of water isotopes has been shown in recent years to provide dense data sets with the increased time resolution illuminating substantially greater short term variability than is generally observed during discrete sampling. A truly portable instrument also opens the possibility to utilize the instrument as a tool for identifying which water samples would be particularly interesting for further laboratory investigation. To make possible such field measurements of liquid water isotopes, Los Gatos Research has developed a miniaturized, field-deployable liquid water isotope analyzer. The prototype miniature liquid water isotope analyzer (mini-LWIA) uses LGR's patented Off-Axis ICOS (Integrated Cavity Output Spectroscopy) technology in a rugged, Pelican case housing for easy transport and field operations. The analyzer simultaneously measures both δ2H and δ18O from liquid water, with both manual and automatic water introduction options. The laboratory precision for δ2H is 0.6 ‰, and for δ18O is 0.3 ‰. The mini-LWIA was deployed in the high Arctic during the summer of 2015 at Inuvik in the Canadian Northwest Territories. Samples were collected from Sachs Harbor, on the southwest coast of Banks Island, including buried basal ice from the Lurentide Ice Sheet, some ice wedges, and other types of ground ice. Methodology and water analysis results from this extreme field deployment will be presented.

High mass isotope separation arrangement

International Nuclear Information System (INIS)

Eerkens, J.W.

1980-01-01

This invention relates to the isotope separation art and, more particularly, to a selectively photon-induced energy level transition of an isotopic molecule containing the isotope to be separated and a chemical reaction with a chemically reactive agent to provide a chemical compound containing atoms of the isotope desired. In particular a description is given of a method of laser isotope separation applied to the separation of 235 UF 6 from 238 UF 6 . (U.K.)

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.

Rigorous high-precision enclosures of fixed points and their invariant manifolds

Science.gov (United States)

Wittig, Alexander N.

The well established concept of Taylor Models is introduced, which offer highly accurate C0 enclosures of functional dependencies, combining high-order polynomial approximation of functions and rigorous estimates of the truncation error, performed using verified arithmetic. The focus of this work is on the application of Taylor Models in algorithms for strongly non-linear dynamical systems. A method is proposed to extend the existing implementation of Taylor Models in COSY INFINITY from double precision coefficients to arbitrary precision coefficients. Great care is taken to maintain the highest efficiency possible by adaptively adjusting the precision of higher order coefficients in the polynomial expansion. High precision operations are based on clever combinations of elementary floating point operations yielding exact values for round-off errors. An experimental high precision interval data type is developed and implemented. Algorithms for the verified computation of intrinsic functions based on the High Precision Interval datatype are developed and described in detail. The application of these operations in the implementation of High Precision Taylor Models is discussed. An application of Taylor Model methods to the verification of fixed points is presented by verifying the existence of a period 15 fixed point in a near standard Henon map. Verification is performed using different verified methods such as double precision Taylor Models, High Precision intervals and High Precision Taylor Models. Results and performance of each method are compared. An automated rigorous fixed point finder is implemented, allowing the fully automated search for all fixed points of a function within a given domain. It returns a list of verified enclosures of each fixed point, optionally verifying uniqueness within these enclosures. An application of the fixed point finder to the rigorous analysis of beam transfer maps in accelerator physics is presented. Previous work done by

Ubiquitous isotopic anomalies in Ti from normal Allende inclusions

International Nuclear Information System (INIS)

Niemeyer, S.; Lugmair, G.W.

1981-01-01

A newly developed technique for high-precision isotopic analyses of titanium was applied to terrestrial rocks and course- and fine-grained Allende inclusions. Repeated analyses of three terrestrial rocks gave excellent agreement (usually less than 2 x 10 -4 deviations) with a Ti metal standard. All seven Allende inclusions studied here were previously determined to contain isotopically normal Nd and/or Sm, indicating that none belongs to a small group of peculiar inclusions, dubbed as FUN inclusions. (orig./ME)

High precision target center determination from a point cloud

Directory of Open Access Journals (Sweden)

K. Kregar

2013-10-01

Full Text Available Many applications of terrestrial laser scanners (TLS require the determination of a specific point from a point cloud. In this paper procedure of high precision planar target center acquisition from point cloud is presented. The process is based on an image matching algorithm but before we can deal with raster image to fit a target on it, we need to properly determine the best fitting plane and project points on it. The main emphasis of this paper is in the precision estimation and propagation through the whole procedure which allows us to obtain precision assessment of final results (target center coordinates. Theoretic precision estimations – obtained through the procedure were rather high so we compared them with the empiric precision estimations obtained as standard deviations of results of 60 independently scanned targets. An χ2-test confirmed that theoretic precisions are overestimated. The problem most probably lies in the overestimated precisions of the plane parameters due to vast redundancy of points. However, empirical precisions also confirmed that the proposed procedure can ensure a submillimeter precision level. The algorithm can automatically detect grossly erroneous results to some extent. It can operate when the incidence angles of a laser beam are as high as 80°, which is desirable property if one is going to use planar targets as tie points in scan registration. The proposed algorithm will also contribute to improve TLS calibration procedures.

A new set-up for simultaneous high-precision measurements of CO2, δ13C-CO2 and δ18O-CO2 on small ice core samples

Science.gov (United States)

Jenk, Theo Manuel; Rubino, Mauro; Etheridge, David; Ciobanu, Viorela Gabriela; Blunier, Thomas

2016-08-01

Palaeoatmospheric records of carbon dioxide and its stable carbon isotope composition (δ13C) obtained from polar ice cores provide important constraints on the natural variability of the carbon cycle. However, the measurements are both analytically challenging and time-consuming; thus only data exist from a limited number of sampling sites and time periods. Additional analytical resources with high analytical precision and throughput are thus desirable to extend the existing datasets. Moreover, consistent measurements derived by independent laboratories and a variety of analytical systems help to further increase confidence in the global CO2 palaeo-reconstructions. Here, we describe our new set-up for simultaneous measurements of atmospheric CO2 mixing ratios and atmospheric δ13C and δ18O-CO2 in air extracted from ice core samples. The centrepiece of the system is a newly designed needle cracker for the mechanical release of air entrapped in ice core samples of 8-13 g operated at -45 °C. The small sample size allows for high resolution and replicate sampling schemes. In our method, CO2 is cryogenically and chromatographically separated from the bulk air and its isotopic composition subsequently determined by continuous flow isotope ratio mass spectrometry (IRMS). In combination with thermal conductivity measurement of the bulk air, the CO2 mixing ratio is calculated. The analytical precision determined from standard air sample measurements over ice is ±1.9 ppm for CO2 and ±0.09 ‰ for δ13C. In a laboratory intercomparison study with CSIRO (Aspendale, Australia), good agreement between CO2 and δ13C results is found for Law Dome ice core samples. Replicate analysis of these samples resulted in a pooled standard deviation of 2.0 ppm for CO2 and 0.11 ‰ for δ13C. These numbers are good, though they are rather conservative estimates of the overall analytical precision achieved for single ice sample measurements. Facilitated by the small sample requirement

Sensitive determination of thiols in wine samples by a stable isotope-coded derivatization reagent d0/d4-acridone-10-ethyl-N-maleimide coupled with high-performance liquid chromatography-electrospray ionization-tandem mass spectrometry analysis.

Science.gov (United States)

Lv, Zhengxian; You, Jinmao; Lu, Shuaimin; Sun, Weidi; Ji, Zhongyin; Sun, Zhiwei; Song, Cuihua; Chen, Guang; Li, Guoliang; Hu, Na; Zhou, Wu; Suo, Yourui

2017-03-31

As the key aroma compounds, varietal thiols are the crucial odorants responsible for the flavor of wines. Quantitative analysis of thiols can provide crucial information for the aroma profiles of different wine styles. In this study, a rapid and sensitive method for the simultaneous determination of six thiols in wine using d 0 /d 4 -acridone-10-ethyl-N-maleimide (d 0 /d 4 -AENM) as stable isotope-coded derivatization reagent (SICD) by high performance liquid chromatography-electrospray ionization-tandem mass spectrometry (HPLC-ESI-MS/MS) has been developed. Quantification of thiols was performed by using d 4 -AENM labeled thiols as the internal standards (IS), followed by stable isotope dilution HPLC-ESI-MS/MS analysis. The AENM derivatization combined with multiple reactions monitoring (MRM) not only allowed trace analysis of thiols due to the extremely high sensitivity, but also efficiently corrected the matrix effects during HPLC-MS/MS and the fluctuation in MS/MS signal intensity due to instrument. The obtained internal standard calibration curves for six thiols were linear over the range of 25-10,000pmol/L (R 2 ≥0.9961). Detection limits (LODs) for most of analytes were below 6.3pmol/L. The proposed method was successfully applied for the simultaneous determination of six kinds of thiols in wine samples with precisions ≤3.5% and recoveries ≥78.1%. In conclusion, the developed method is expected to be a promising tool for detection of trace thiols in wine and also in other complex matrix. Copyright © 2017 Elsevier B.V. All rights reserved.

Emergency diesel generator reliability analysis high flux isotope reactor

International Nuclear Information System (INIS)

Merryman, L.; Christie, B.

1993-01-01

A program to apply some of the techniques of reliability engineering to the High Flux Isotope Reactor (HFIR) was started on August 8, 1992. Part of the program was to track the conditional probabilities of the emergency diesel generators responding to a valid demand. This was done to determine if the performance of the emergency diesel generators (which are more than 25 years old) has deteriorated. The conditional probabilities of the diesel generators were computed and trended for the period from May 1990 to December 1992. The calculations indicate that the performance of the emergency diesel generators has not deteriorated in recent years, i.e., the conditional probabilities of the emergency diesel generators have been fairly stable over the last few years. This information will be one factor than may be considered in the decision to replace the emergency diesel generators

DNA-, RNA-, and Protein-Based Stable-Isotope Probing for High-Throughput Biomarker Analysis of Active Microorganisms.

Science.gov (United States)

Jameson, Eleanor; Taubert, Martin; Coyotzi, Sara; Chen, Yin; Eyice, Özge; Schäfer, Hendrik; Murrell, J Colin; Neufeld, Josh D; Dumont, Marc G

2017-01-01

Stable-isotope probing (SIP) enables researchers to target active populations within complex microbial communities, which is achieved by providing growth substrates enriched in heavy isotopes, usually in the form of 13 C, 18 O, or 15 N. After growth on the substrate and subsequent extraction of microbial biomarkers, typically nucleic acids or proteins, the SIP technique is used for the recovery and analysis of isotope-labeled biomarkers from active microbial populations. In the years following the initial development of DNA- and RNA-based SIP, it was common practice to characterize labeled populations by targeted gene analysis. Such approaches usually involved fingerprint-based analyses or sequencing of clone libraries containing 16S rRNA genes or functional marker gene amplicons. Although molecular fingerprinting remains a valuable approach for rapid confirmation of isotope labeling, recent advances in sequencing technology mean that it is possible to obtain affordable and comprehensive amplicon profiles, metagenomes, or metatranscriptomes from SIP experiments. Not only can the abundance of microbial groups be inferred from metagenomes, but researchers can bin, assemble, and explore individual genomes to build hypotheses about the metabolic capabilities of labeled microorganisms. Analysis of labeled mRNA is a more recent advance that can provide independent metatranscriptome-based analysis of active microorganisms. The power of metatranscriptomics is that mRNA abundance often correlates closely with the corresponding activity of encoded enzymes, thus providing insight into microbial metabolism at the time of sampling. Together, these advances have improved the sensitivity of SIP methods and allow the use of labeled substrates at ecologically relevant concentrations. Particularly as methods improve and costs continue to drop, we expect that the integration of SIP with multiple omics-based methods will become prevalent components of microbial ecology studies

Precision Measurement of the Energies and Line Shapes of Antiprotonic Lyman and Balmer Transitions From Hydrogen and Helium Isotopes

CERN Multimedia

2002-01-01

% PS207 \\\\ \\\\ For the study of the antiproton-proton and antiproton-nuclear spin-spin and spin-orbital interaction at threshold a high resolution measurement is proposed of the line shapes and energy shifts of antiprotonic K$\\alpha$ and L$\\alpha$ transitions of hydrogen and helium isotopes. The intense LEAR beam, stopped in the cyclotron trap at low gas pressure, provides a unique~X-ray~source with sufficient brightness. Charge coupled devices with their excellent background rejection and energy resolution allow a precise determination of the strong shifts and widths of the 1s hyperfine states of protonium, in addition the detection of the $\\bar{p}$D K$\\alpha$ transition should be possible. A focussing crystal spectrometer with a resolution $\\Delta$E/E of about l0$ ^- ^{4} $, which is superior in the accuracy of the energy determination by two orders of magnitude as compared to the present detection methods, will be used to measure the energies of the L$\\alpha$ transitions. This permits a first direct measure...

PALOMA : an isotope analyzer using static mass spectrometry, coupled with cryogenic and chemical trapping, for the MSL mission to Mars

Science.gov (United States)

Chassefiere, E.; Jambon, A.; Berthelier, J.-J.; Goulpeau, G.; Leblanc, F.; Montmessin, F.; Sarda, P.; Agrinier, P.; Fouchet, T.; Waite, H.

The technique of GCMS analysis has to be completed by static mass spectrometry for precise in-situ measurements of the isotopic composition of planetary atmospheres (noble gases, stable isotopes), and volatile outgassed products from solid sample pyrolysis. Static mass spectrometry, coupled with gas separation by cryo-separation and gettering, is commonly used in the laboratory to study volatiles extracted from terrestrial and meteoritic samples. Such an instrument (PALOMA) is presently developed in our laboratories, and it will be coupled with a Pyr-GCMS analyzer (MACE), built by a US consortium of science laboratories and industrials (University of Michigan, Southwest Research Institute, JPL, Ball Aerospace). The MACE/PALOMA experiment will be proposed on the NASA Mars Science Laboratory mission, planned to be launched in 2009. The scientific objectives of PALOMA, coupled with MACE, may be listed as follows : (i) search for isotopic signatures of past life in atmosphere, rock, dust and ice samples, with emphasis on carbon, nitrogen and hydrogen; (ii) accurately measure isotopic composition of atmospheric noble gases, and stable isotopes, in order to better constrain past escape, surface interaction, outgassing history and climate evolution; (iii) precisely measure diurnal/ seasonal variations of isotopic ratios of H2O, CO2, and N2, for improving our understanding of present and past climate, and of the role of water cycle. Main measurement objectives are : (i) C, H, O, N isotopic composition in both organic evolved samples (provided by MACE pyrolysis system) and atmosphere with high accuracy (a few per mil at 1-s level); (ii) noble gas (He, Ne, Ar, Kr, Xe) and stable (C, H, O, N) isotope composition in atmosphere with high accuracy (a few per mil at 1-s level); (iii) molecular and isotopic composition of inorganic evolved samples (salts, hydrates, nitrates, {ldots}), including ices; (iv) diurnal and seasonal monitoring of D/H in water vapor, and water ice.

Layered compression for high-precision depth data.

Science.gov (United States)

Miao, Dan; Fu, Jingjing; Lu, Yan; Li, Shipeng; Chen, Chang Wen

2015-12-01

With the development of depth data acquisition technologies, access to high-precision depth with more than 8-b depths has become much easier and determining how to efficiently represent and compress high-precision depth is essential for practical depth storage and transmission systems. In this paper, we propose a layered high-precision depth compression framework based on an 8-b image/video encoder to achieve efficient compression with low complexity. Within this framework, considering the characteristics of the high-precision depth, a depth map is partitioned into two layers: 1) the most significant bits (MSBs) layer and 2) the least significant bits (LSBs) layer. The MSBs layer provides rough depth value distribution, while the LSBs layer records the details of the depth value variation. For the MSBs layer, an error-controllable pixel domain encoding scheme is proposed to exploit the data correlation of the general depth information with sharp edges and to guarantee the data format of LSBs layer is 8 b after taking the quantization error from MSBs layer. For the LSBs layer, standard 8-b image/video codec is leveraged to perform the compression. The experimental results demonstrate that the proposed coding scheme can achieve real-time depth compression with satisfactory reconstruction quality. Moreover, the compressed depth data generated from this scheme can achieve better performance in view synthesis and gesture recognition applications compared with the conventional coding schemes because of the error control algorithm.

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

International Nuclear Information System (INIS)

Tagami, Keiko; Uchida, Shigeo

2008-01-01

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

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

High-precision efficiency calibration of a high-purity co-axial germanium detector

Energy Technology Data Exchange (ETDEWEB)

Blank, B., E-mail: blank@cenbg.in2p3.fr [Centre d' Etudes Nucléaires de Bordeaux Gradignan, UMR 5797, CNRS/IN2P3, Université de Bordeaux, Chemin du Solarium, BP 120, 33175 Gradignan Cedex (France); Souin, J.; Ascher, P.; Audirac, L.; Canchel, G.; Gerbaux, M.; Grévy, S.; Giovinazzo, J.; Guérin, H.; Nieto, T. Kurtukian; Matea, I. [Centre d' Etudes Nucléaires de Bordeaux Gradignan, UMR 5797, CNRS/IN2P3, Université de Bordeaux, Chemin du Solarium, BP 120, 33175 Gradignan Cedex (France); Bouzomita, H.; Delahaye, P.; Grinyer, G.F.; Thomas, J.C. [Grand Accélérateur National d' Ions Lourds, CEA/DSM, CNRS/IN2P3, Bvd Henri Becquerel, BP 55027, F-14076 CAEN Cedex 5 (France)

2015-03-11

A high-purity co-axial germanium detector has been calibrated in efficiency to a precision of about 0.15% over a wide energy range. High-precision scans of the detector crystal and γ-ray source measurements have been compared to Monte-Carlo simulations to adjust the dimensions of a detector model. For this purpose, standard calibration sources and short-lived online sources have been used. The resulting efficiency calibration reaches the precision needed e.g. for branching ratio measurements of super-allowed β decays for tests of the weak-interaction standard model.

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.

Chromatographic measurement of hydrogen isotopic and permanent gas impurities in tritium

International Nuclear Information System (INIS)

Warner, D.K.; Kinard, C.; Bohl, D.C.

1976-01-01

This paper describes a gas chromatograph that was designed for dedicated analysis of hydrogen isotopic and permanent gas impurities in tritium and tritium-deuterium mixtures. The instrument that was developed substantially improved the accuracy and precision of hydrogen isotopic analysis in the 20 ppM to one mole percent range as compared with other analytical methods. Several unique design features of the instrument were required due to the radiation and isotopic exchange properties of the tritium in the samples; descriptions of these features are presented along with details of the complete chromatographic system. The experimental procedures used to calibrate the detector and statistically evaluate its performance are given, and the sources of analytical error are cited. The limitations of the present system are also discussed

SIMS chemical and isotopic analysis of impact features from LDEF experiments AO187-1 and AO187-2

Science.gov (United States)

Stadermann, Frank J.; Amari, Sachiko; Foote, John; Swan, Pat; Walker, Robert M.; Zinner, Ernst

1995-01-01

Previous secondary ion mass spectrometry (SIMS) studies of extended impact features from LDEF capture cell experiment AO187-2 showed that it is possible to distinguish natural and man-made particle impacts based on the chemical composition of projectile residues. The same measurement technique has now been applied to specially prepared gold target impacts from experiment AO187-1 in order to identify the origins of projectiles that left deposits too thin to be analyzed by conventional energy-dispersive x-ray (EDX) spectroscopy. The results indicate that SIMS may be the method of choice for the analysis of impact deposits on a variety of sample surfaces. SIMS was also used to determine the isotopic compositions of impact residues from several natural projectiles. Within the precision of the measurements all analyzed residues show isotopically normal compositions.

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....

Measurement of organic carbon stable isotope composition of different soil types by EA-IRMS system

International Nuclear Information System (INIS)

Qi Biao; Ding Lingling; Cui Jiehua; Wang Yanhong

2009-01-01

Element analyzer-isotope ratio mass spectrometers (EA-IRMS) is a rapid and precise method for measuring stable carbon isotope. Pure CO 2 reference gas was calibrated via international standard-Urea, and the δ 13 C us PDB value of pure CO 2 is (-29.523 ± 0.0181)%. Stability and linearity of the EA-IRMS system, precision of δ 13 C measurement for samples were tested through experimental comparison. Moreover, determination method of organic carbon stable isotope in soil was based on the system. The EA-IRMS system had well linearity when ion intensity ranged from 1.0 to 7.0V, and it excelled the total linearity when the ion intensity was from 1.5 to 5.0V, and the accurate result of δ 13 C for sample analysis could be obtained with precision of 0.015%. If carbon content in sample is more than 5μg, the requirement for analyzing accurate result of δ 13 C could be achieved. The organic carbon stable isotope was measured in 18 different types soil samples, the average natural abundance of 13 C was 1.082%, and the organic carbon stable isotope composition was significantly different among different type soils. (authors)

Contributions of isotopic bio-geochemistry to the analysis of water - soil - root interactions

International Nuclear Information System (INIS)

Cayet, S.

2001-07-01

The aim of this work is to study the origin of the isotopic signal of the water produced by plants transpiration. It stresses more particularly on the water movements between the soil and the plant in a context of heterogenous water availability for the root system. The use of water isotopes ( 18 O and 2 H) should allow to precise the water extraction depth of the roots and the plant strategy in front of a hydric stress of edaphic origin. The first chapter presents the place of water in the soil-plant-atmosphere continuum, the different potential sources of water accessible to the plant, the principles of water absorption and the hydric transfer in the plant in relation with the variations of water absorption and of the evaporative conditions. The isotopic method is introduced with the natural variability of the isotopic composition of the atmospheric and soil waters. Finally, the reaction of the plant in front of a hydric stress is described. The second chapter presents a series of experiments carried out in the natural environment and shows the problems encountered during the determination of water origin in heterogenous hydric availability conditions. The third chapter describes the experiments performed in controlled environment. One series of experiments is performed in homogenous hydric availability condition. The aim is to analyze the isotopic signal emitted by the plant and its significance with respect to the feeding water. The second series of experiments is performed in heterogenous hydric availability conditions and in stable or variable climatic conditions. In the last chapter, the different experiments performed in natural environment are presented, first in optimum hydric availability conditions, and second in variable hydric conditions. These experiments allow to reconstruct the isotopic signal of the soil water which is recorded by the plant and to precise the preferential areas of water extraction by the roots, and the competitive behaviour of

Spectroscopic measurement of 204Pb isotope shift and 205Pb nuclear spin

International Nuclear Information System (INIS)

Schonberger, P.

1984-01-01

The isotope shift of 204 Pb and the nuclear spin of 1.4 X 10 7 -y 205 Pb was determined from a high-resolution optical measurement of the 6p 23 P 0 -6p7s 3 P 1 0 283.3-nm resonance line. The value of the shift, relative to 208 Pb is -140.2(8) x 10 -3 cm -1 , the negative sign indicating a shift to lower wave numbers. The precision is 3-4 times greater than that of previous measurements. The spin of 205 Pb I = 5/2 was obtained from the measurement of the relative intensities of its three hyperfine components. This method of absorption spectroscopy determination of ground state nuclear spin is applicable to any stable or long-lived isotope. High resolution optical absorption spectra were obtained with a 25.4 cm diffraction grating in a 9.1 m focal length Czerny-Turner spectrometer. A signal-averaging scanning technique was used to record the spectra. Increased precision in the isotope shift measurement was attained by using separated isotope samples of 204 Pb and 207 Pb

Combined chemometric analysis of (1)H NMR, (13)C NMR and stable isotope data to differentiate organic and conventional milk.

Science.gov (United States)

Erich, Sarah; Schill, Sandra; Annweiler, Eva; Waiblinger, Hans-Ulrich; Kuballa, Thomas; Lachenmeier, Dirk W; Monakhova, Yulia B

2015-12-01

The increased sales of organically produced food create a strong need for analytical methods, which could authenticate organic and conventional products. Combined chemometric analysis of (1)H NMR-, (13)C NMR-spectroscopy data, stable-isotope data (IRMS) and α-linolenic acid content (gas chromatography) was used to differentiate organic and conventional milk. In total 85 raw, pasteurized and ultra-heat treated (UHT) milk samples (52 organic and 33 conventional) were collected between August 2013 and May 2014. The carbon isotope ratios of milk protein and milk fat as well as the α-linolenic acid content of these samples were determined. Additionally, the milk fat was analyzed by (1)H and (13)C NMR spectroscopy. The chemometric analysis of combined data (IRMS, GC, NMR) resulted in more precise authentication of German raw and retail milk with a considerably increased classification rate of 95% compared to 81% for NMR and 90% for IRMS using linear discriminate analysis. Copyright © 2015 Elsevier Ltd. All rights reserved.

Cyclotrons as Drivers for Precision Neutrino Measurements

International Nuclear Information System (INIS)

Alonso, J.; Barletta, W. A.; Winslow, L. A.; Shaevitz, M. H.; Spitz, J.; Conrad, J. M.; Toups, M.; Adelmann, A.

2014-01-01

As we enter the age of precision measurement in neutrino physics, improved flux sources are required. These must have a well defined flavor content with energies in ranges where backgrounds are low and cross-section knowledge is high. Very few sources of neutrinos can meet these requirements. However, pion/muon and isotope decay-at-rest sources qualify. The ideal drivers for decay-at-rest sources are cyclotron accelerators, which are compact and relatively inexpensive. This paper describes a scheme to produce decay-at-rest sources driven by such cyclotrons, developed within the DAEδALUS program. Examples of the value of the high precision beams for pursuing Beyond Standard Model interactions are reviewed. New results on a combined DAEδALUS—Hyper-K search for CP violation that achieve errors on the mixing matrix parameter of 4° to 12° are presented

Community-based Approaches to Improving Accuracy, Precision, and Reproducibility in U-Pb and U-Th Geochronology

Science.gov (United States)

McLean, N. M.; Condon, D. J.; Bowring, S. A.; Schoene, B.; Dutton, A.; Rubin, K. H.

2015-12-01

The last two decades have seen a grassroots effort by the international geochronology community to "calibrate Earth history through teamwork and cooperation," both as part of the EARTHTIME initiative and though several daughter projects with similar goals. Its mission originally challenged laboratories "to produce temporal constraints with uncertainties approaching 0.1% of the radioisotopic ages," but EARTHTIME has since exceeded its charge in many ways. Both the U-Pb and Ar-Ar chronometers first considered for high-precision timescale calibration now regularly produce dates at the sub-per mil level thanks to instrumentation, laboratory, and software advances. At the same time new isotope systems, including U-Th dating of carbonates, have developed comparable precision. But the larger, inter-related scientific challenges envisioned at EARTHTIME's inception remain - for instance, precisely calibrating the global geologic timescale, estimating rates of change around major climatic perturbations, and understanding evolutionary rates through time - and increasingly require that data from multiple geochronometers be combined. To solve these problems, the next two decades of uranium-daughter geochronology will require further advances in accuracy, precision, and reproducibility. The U-Th system has much in common with U-Pb, in that both parent and daughter isotopes are solids that can easily be weighed and dissolved in acid, and have well-characterized reference materials certified for isotopic composition and/or purity. For U-Pb, improving lab-to-lab reproducibility has entailed dissolving precisely weighed U and Pb metals of known purity and isotopic composition together to make gravimetric solutions, then using these to calibrate widely distributed tracers composed of artificial U and Pb isotopes. To mimic laboratory measurements, naturally occurring U and Pb isotopes were also mixed in proportions to mimic samples of three different ages, to be run as internal

Precision measurements with LPCTrap at GANIL

Energy Technology Data Exchange (ETDEWEB)

Liénard, E., E-mail: lienard@lpccaen.in2p3.fr; Ban, G. [LPC CAEN, ENSICAEN, Université de Caen, CNRS/IN2P3 (France); Couratin, C. [Instituut voor Kern- en Stralingsfysica, KU Leuven (Belgium); Delahaye, P. [GANIL, CEA/DSM-CNRS/IN2P3 (France); Durand, D.; Fabian, X. [LPC CAEN, ENSICAEN, Université de Caen, CNRS/IN2P3 (France); Fabre, B. [CELIA, Université Bordeaux, CNRS, CEA (France); Fléchard, X. [LPC CAEN, ENSICAEN, Université de Caen, CNRS/IN2P3 (France); Finlay, P. [Instituut voor Kern- en Stralingsfysica, KU Leuven (Belgium); Mauger, F. [LPC CAEN, ENSICAEN, Université de Caen, CNRS/IN2P3 (France); Méry, A. [CIMAP, CEA/CNRS/ENSICAEN, Université de Caen (France); Naviliat-Cuncic, O. [NSCL and Department of Physics and Astronomy, MSU (United States); Pons, B. [CELIA, Université Bordeaux, CNRS, CEA (France); Porobic, T. [Instituut voor Kern- en Stralingsfysica, KU Leuven (Belgium); Quéméner, G. [LPC CAEN, ENSICAEN, Université de Caen, CNRS/IN2P3 (France); Severijns, N. [Instituut voor Kern- en Stralingsfysica, KU Leuven (Belgium); Thomas, J. C. [GANIL, CEA/DSM-CNRS/IN2P3 (France); Velten, Ph. [Instituut voor Kern- en Stralingsfysica, KU Leuven (Belgium)

2015-11-15

The experimental achievements and the results obtained so far with the LPCTrap device installed at GANIL are presented. The apparatus is dedicated to the study of the weak interaction at low energy by means of precise measurements of the β − ν angular correlation parameter in nuclear β decays. So far, the data collected with three isotopes have enabled to determine, for the first time, the charge state distributions of the recoiling ions, induced by shakeoff process. The analysis is presently refined to deduce the correlation parameters, with the potential of improving both the constraint deduced at low energy on exotic tensor currents ({sup 6}He{sup 1+}) and the precision on the V{sub ud} element of the quark-mixing matrix ({sup 35}Ar{sup 1+} and {sup 19}Ne{sup 1+}) deduced from the mirror transitions dataset.

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

High precision detector robot arm system

Science.gov (United States)

Shu, Deming; Chu, Yong

2017-01-31

A method and high precision robot arm system are provided, for example, for X-ray nanodiffraction with an X-ray nanoprobe. The robot arm system includes duo-vertical-stages and a kinematic linkage system. A two-dimensional (2D) vertical plane ultra-precision robot arm supporting an X-ray detector provides positioning and manipulating of the X-ray detector. A vertical support for the 2D vertical plane robot arm includes spaced apart rails respectively engaging a first bearing structure and a second bearing structure carried by the 2D vertical plane robot arm.

Analysis of high burnup pressurized water reactor fuel using uranium, plutonium, neodymium, and cesium isotope correlations with burnup

International Nuclear Information System (INIS)

Kim, Jung Suk; Jeon, Young Shin; Park, Soon Dal; Ha, Yeong Keong; Song, Kyu Seok

2015-01-01

The correlation of the isotopic composition of uranium, plutonium, neodymium, and cesium with the burnup for high burnup pressurized water reactor fuels irradiated in nuclear power reactors has been experimentally investigated. The total burnup was determined by Nd-148 and the fractional 235 U burnup was determined by U and Pu mass spectrometric methods. The isotopic compositions of U, Pu, Nd, and Cs after their separation from the irradiated fuel samples were measured using thermal ionization mass spectrometry. The contents of these elements in the irradiated fuel were determined through an isotope dilution mass spectrometric method using 233 U, 242 Pu, 150 Nd, and 133 Cs as spikes. The activity ratios of Cs isotopes in the fuel samples were determined using gamma-ray spectrometry. The content of each element and its isotopic compositions in the irradiated fuel were expressed by their correlation with the total and fractional burnup, burnup parameters, and the isotopic compositions of different elements. The results obtained from the experimental methods were compared with those calculated using the ORIGEN-S code

Ultratrace Uranium Fingerprinting with Isotope Selective Laser Ionization Spectrometry

International Nuclear Information System (INIS)

Ziegler, Summer L.; Bushaw, Bruce A.

2008-01-01

Uranium isotope ratios can provide source information for tracking uranium contamination in a variety of fields, ranging from occupational bioassay to monitoring aftereffects of nuclear accidents. We describe the development of Isotope Selective Laser Ionization Spectrometry (ISLIS) for ultratrace measurement of the minor isotopes 234U, 235U, and 236U with respect to 238U. Optical isotopic selectivity in three-step excitation with single-mode continuous wave lasers is capable of measuring the minor isotopes at relative abundances below 1 ppm, and is not limited by isobaric interferences such as 235UH+ during measurement of 236U. This relative abundance limit approaches the threshold for measurement of uranium minor isotopes with conventional mass spectrometry, typically 10-7, but without mass spectrometric analysis of the laser-created ions. Uranyl nitrate standards from an international blind comparison were used to test analytical performance for different isotopic compositions and with quantities ranging from 11 ng to 10 (micro)g total uranium. Isotopic ratio determination was demonstrated over a linear dynamic range of 7 orders of magnitude with a few percent relative precision and detection limits below 500 fg for the minor isotopes

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)

Precision crystal alignment for high-resolution electron microscope imaging

International Nuclear Information System (INIS)

Wood, G.J.; Beeching, M.J.

1990-01-01

One of the more difficult tasks involved in obtaining quality high-resolution electron micrographs is the precise alignment of a specimen into the required zone. The current accepted procedure, which involves changing to diffraction mode and searching for symmetric point diffraction pattern, is insensitive to small amounts of misalignment and at best qualitative. On-line analysis of the fourier space representation of the image, both for determining and correcting crystal tilt, is investigated. 8 refs., 42 figs

Noble gases in Mars atmosphere: new precise analysis with Paloma

Science.gov (United States)

Sarda, Ph.; Paloma Team

2003-04-01

The Viking mission embarked a mass spectrometer designed by Alfred O. Nier that yielded the first determination of the elemental and isotopic composition of noble gases in Mars atmosphere. For example, the 40Ar/36Ar ratio in martian air is roughly 10 fold that in terrestrial air. This extraordinary accomplishment, however, has furnished only partial results with large analytical uncertainties. For example, we do not know the isotopic composition of helium, and only very poorly that of Ne, Kr and Xe. In planetary science, it is fundamental to have a good knowledge of the atmosphere because this serves as a reference for all further studies of volatiles. In addition, part of our present knowledge of Mars atmosphere is based on the SNC meteorites, and again points to important differences between the atmospheres of Earth and Mars. For example the 129Xe/132Xe ratio of martian atmosphere would be twice that of terrestrial air and the 36Ar/38Ar ratio strongly different from the terrestrial or solar value. There is a need for confirming that the atmospheric components found in SNC meteorites actually represents the atmosphere of Mars, or to determine how different they are. Paloma is an instrument designed to generate elemental and isotopic data for He, Ne, Ar, Kr and Xe (and other gases) using a mass spectrometer with a purification and separation line. Gas purification and separation did not exist on the Vicking instrument. Because Paloma includes purification and separation, we expect strong improvement in precision. Ne, Ar and Xe isotope ratios should be obtained with an accuracy of better than 1%. Determination of the presently unknown ^3He/^4He ratio is also awaited from this experiment. Knowledge of noble gas isotopes in Mars atmosphere will allow some insight into major planetary processes such as degassing (^3He/^4He, 40Ar/36Ar, 129Xe/130Xe, 136Xe/130Xe), gravitational escape to space (^3He/^4He, 20Ne/22Ne), hydrodynamic escape and/or impact erosion of the

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,

Spectroscopic Measurement of LEAD-204 Isotope Shift and LEAD-205 Nuclear Spin.

Science.gov (United States)

Schonberger, Peter

The isotope shift of ('204)Pb and the nuclear spin of 1.4 x 10('7)-y ('205)Pb was determined from a high -resolution optical measurement of the 6p('2) ('3)P(,o) -6p7s('3)P(,1)('o) 283.3-nm resonance line. The value of the shift, relative to ('208)Pb is -140.2(8) x 10('-3)cm(' -1), the negative sign indicating a shift to lower wave numbers. The precision is 3-4 times greater than that of previous measurements. The spin of ('205)Pb l = 5/2 was obtained from the measurement of the relative intensities of its three hyperfine components. This method of absorption spectroscopy determination of ground state nuclear spin is applicable to any stable or longlived isotope. High resolution optical absorption spectra were obtained with a 25.4cm diffraction grating in a 9.1m focal length Czerny-Turner spectrometer. A signal-averaging scanning technique was used to record the spectra. Increased precision in the isotope shift measurement was attained by using separated isotope samples of ('204)Pb and ('207)Pb. A controlled amount of the later was incorporated in the absorption cell to provide internal calibration by its 6p7s ('3)P(,1)('o) hfs separation. Absorption spectra were recorded for several optical thicknesses of the absorber. A single spin value of increased precision was derived from the entire set of combined data.

The influence of room temperature on Mg isotope measurements by MC-ICP-MS.

Science.gov (United States)

Zhang, Xing-Chao; Zhang, An-Yu; Zhang, Zhao-Feng; Huang, Fang; Yu, Hui-Min

2018-03-24

We observed that the accuracy and precision of magnesium (Mg) isotope analyses could be affected if the room temperature oscillated during measurements. To achieve high quality Mg isotopic data, it is critical to evaluate how the unstable room temperature affects Mg isotope measurements by multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS). We measured the Mg isotopes for the reference material DSM-3 using MC-ICP-MS under oscillating room temperatures in spring. For a comparison, we also measured the Mg isotopes under stable room temperatures, which was achieved by the installation of an improved temperature control system in the laboratory. The δ 26 Mg values measured under oscillating room temperatures have a larger deviation (δ 26 Mg from -0.09 to 0.08‰, with average δ 26 Mg = 0.00 ± 0.08 ‰) than those measured under a stable room temperature (δ 26 Mg from -0.03 to 0.03‰, with average δ 26 Mg = 0.00 ± 0.02 ‰) using the same MC-ICP-MS system. The room temperature variation can influence the stability of MC-ICP-MS. Therefore, it is critical to keep the room temperature stable to acquire high precise and accurate isotopic data when using MC-ICP-MS, especially when using the sample-standard bracketing (SSB) correction method. This article is protected by copyright. All rights reserved.

The Stanford-U.S. Geological Survey SHRIMP ion microprobe--a tool for micro-scale chemical and isotopic analysis

Science.gov (United States)

Bacon, Charles R.; Grove, Marty; Vazquez, Jorge A.; Coble, Matthew A.

2012-01-01

Answers to many questions in Earth science require chemical analysis of minute volumes of minerals, volcanic glass, or biological materials. Secondary Ion Mass Spectrometry (SIMS) is an extremely sensitive analytical method in which a 5–30 micrometer diameter "primary" beam of charged particles (ions) is focused on a region of a solid specimen to sputter secondary ions from 1–5 nanograms of the sample under high vacuum. The elemental abundances and isotopic ratios of these secondary ions are determined with a mass spectrometer. These results can be used for geochronology to determine the age of a region within a crystal thousands to billions of years old or to precisely measure trace abundances of chemical elements at concentrations as low as parts per billion. A partnership of the U.S. Geological Survey and the Stanford University School of Earth Sciences operates a large SIMS instrument, the Sensitive High-Resolution Ion Microprobe with Reverse Geometry (SHRIMP–RG) on the Stanford campus.

Chemical analyses and calculation of isotopic compositions of high-burnup UO{sub 2} fuels and MOX fuels

Energy Technology Data Exchange (ETDEWEB)

Matsumura, Tetsuo; Sasahara, Akihiro [Central Research Inst. of Electric Power Industry, Tokyo (Japan)

2001-08-01

Chemical analysis activities of isotopic compositions of high-burnup UO{sub 2} fuels and MOX fuels in CRIEPI and calculation evaluation are reviewed briefly. C/E values of ORIGEN2, in which original libraries and JENDL-3.2 libraries are used, and other codes with chemical analysis data are reviewed and evaluated. Isotopic compositions of main U and Pu in fuels can be evaluated within 10% relative errors by suitable libraries and codes. Void ratio is effective parameter for C/E values in BWR fuels. JENDL-3.2 library shows remarkable improvement compared with original libraries in isotopic composition evaluations of FP nuclides. (author)

Calculation of relativistic and isotope shifts in Mg I

International Nuclear Information System (INIS)

Berengut, J.C.; Flambaum, V.V.; Kozlov, M.G.

2005-01-01

We present an ab initio method of calculation of the isotope and relativistic shifts in atoms with a few valence electrons. It is based on an energy calculation involving the combination of the configuration-interaction method and many-body perturbation theory. This work is motivated by analyses of quasar absorption spectra that suggest that the fine-structure constant α was smaller at an early epoch. Relativistic shifts are needed to measure this variation of α, while isotope shifts are needed to resolve systematic effects in this study. The isotope shifts can also be used to measure isotopic abundances in gas clouds in the early universe, which are needed to study nuclear reactions in stars and supernovae and test models of chemical evolution. This paper shows that the isotope shift in magnesium can be calculated to very high precision using our method

Molecular diffusion of stable water isotopes in polar firn as a proxy for past temperatures

Science.gov (United States)

Holme, Christian; Gkinis, Vasileios; Vinther, Bo M.

2018-03-01

Polar precipitation archived in ice caps contains information on past temperature conditions. Such information can be retrieved by measuring the water isotopic signals of δ18O and δD in ice cores. These signals have been attenuated during densification due to molecular diffusion in the firn column, where the magnitude of the diffusion is isotopologue specific and temperature dependent. By utilizing the differential diffusion signal, dual isotope measurements of δ18O and δD enable multiple temperature reconstruction techniques. This study assesses how well six different methods can be used to reconstruct past surface temperatures from the diffusion-based temperature proxies. Two of the methods are based on the single diffusion lengths of δ18O and δD , three of the methods employ the differential diffusion signal, while the last uses the ratio between the single diffusion lengths. All techniques are tested on synthetic data in order to evaluate their accuracy and precision. We perform a benchmark test to thirteen high resolution Holocene data sets from Greenland and Antarctica, which represent a broad range of mean annual surface temperatures and accumulation rates. Based on the benchmark test, we comment on the accuracy and precision of the methods. Both the benchmark test and the synthetic data test demonstrate that the most precise reconstructions are obtained when using the single isotope diffusion lengths, with precisions of approximately 1.0 °C . In the benchmark test, the single isotope diffusion lengths are also found to reconstruct consistent temperatures with a root-mean-square-deviation of 0.7 °C . The techniques employing the differential diffusion signals are more uncertain, where the most precise method has a precision of 1.9 °C . The diffusion length ratio method is the least precise with a precision of 13.7 °C . The absolute temperature estimates from this method are also shown to be highly sensitive to the choice of fractionation factor

Analysis of Gas Membrane Ultra-High Purification of Small Quantities of Mono-Isotopic Silane

Energy Technology Data Exchange (ETDEWEB)

de Almeida, Valmor F [ORNL; Hart, Kevin J [ORNL

2016-09-01

A small quantity of high-value, crude, mono-isotopic silane is a prospective gas for a small-scale, high-recovery, ultra-high membrane purification process. This is an unusual application of gas membrane separation for which we provide a comprehensive analysis of a simple purification model. The goal is to develop direct analytic expressions for estimating the feasibility and efficiency of the method, and guide process design; this is only possible for binary mixtures of silane in the dilute limit which is a somewhat realistic case. Among the common impurities in crude silane, methane poses a special membrane separation challenge since it is chemically similar to silane. Other potential problematic surprises are: ethylene, diborane and ethane (in this order). Nevertheless, we demonstrate, theoretically, that a carefully designed membrane system may be able to purify mono-isotopic, crude silane to electronics-grade level in a reasonable amount of time and expenses. We advocate a combination of membrane materials that preferentially reject heavy impurities based on mobility selectivity, and light impurities based on solubility selectivity. We provide estimates for the purification of significant contaminants of interest. To improve the separation selectivity, it is advantageous to use a permeate chamber under vacuum, however this also requires greater control of in-leakage of impurities in the system. In this study, we suggest cellulose acetate and polydimethylsiloxane as examples of membrane materials on the basis of limited permeability data found in the open literature. We provide estimates on the membrane area needed and priming volume of the cell enclosure for fabrication purposes when using the suggested membrane materials. These estimates are largely theoretical in view of the absence of reliable experimental data for the permeability of silane. Last but not least, future extension of this work to the non-dilute limit may apply to the recovery of silane from

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

Precision mass measurements for studies of nucleosynthesis via the rapid neutron-capture process. Penning-trap mass measurements of neutron-rich cadmium and caesium isotopes

Energy Technology Data Exchange (ETDEWEB)

Atanasov, Dinko

2016-07-06

Although the theory for the rapid neutron-capture process (r-process) was developed more than 55 years ago, the astrophysical site is still under a debate. Theoretical studies predict that the r-process path proceeds through very neutron-rich nuclei with very asymmetric proton-to-neutron ratios. Knowledge about the properties of neutron-rich isotopes found in similar regions of the nuclear chart and furthermore suitable for r-process studies is still little or even not existing. The basic nuclear properties such as binding energies, half-lives, neutron-induced or neutron-capture reaction cross-sections, play an important role in theoretical simulations and can vary or even drastically alternate results of these studies. Therefore, a considerable effort was put forward to access neutron-rich isotopes at radioactive ion-beam facilities like ISOLDE at CERN. The goal of this PhD thesis is to describe the experimental work done for the precision mass measurements of neutron-rich cadmium ({sup 129-131}Cd) and caesium ({sup 132,146-148}Cs) isotopes. Measurements were done at the on-line radioactive ion-beam facility ISOLDE by using the four-trap mass spectrometer ISOLTRAP. The cadmium isotopes are key nuclides for the synthesis of stable isotopes around the mass peak A = 130 in the Solar System abundance.

Improved sample utilization in thermal ionization mass spectrometry isotope ratio measurements: refined development of porous ion emitters for nuclear forensic applications

Energy Technology Data Exchange (ETDEWEB)

Baruzzini, Matthew Louis [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

2017-05-08

The precise and accurate determination of isotopic composition in nuclear forensic samples is vital for assessing origin, intended use and process history. Thermal ionization mass spectrometry (TIMS) is widely accepted as the gold standard for high performance isotopic measurements and has long served as the workhorse in the isotopic ratio determination of nuclear materials. Nuclear forensic and safeguard specialists have relied heavily on such methods for both routine and atypical e orts. Despite widespread use, TIMS methods for the assay of actinide systems continue to be hindered by poor ionization e ciency, often less than tenths of a percent; the majority of a sample is not measured. This represents a growing challenge in addressing nextgeneration nuclear detection needs by limiting the ability to analyze ultratrace quantities of high priority elements that could potentially provide critical nuclear forensic signatures. Porous ion emitter (PIE) thermal ion sources were developed in response to the growing need for new TIMS ion source strategies for improved ionization e ciency, PIEs have proven to be simple to implement, straightforward approach to boosting ion yield. This work serves to expand the use of PIE techniques for the analysis of trace quantities of plutonium and americium. PIEs exhibited superior plutonium and americium ion yields when compared to direct lament loading and the resin bead technique, one of the most e cient methods for actinide analysis, at similar mass loading levels. Initial attempts at altering PIE composition for the analysis of plutonium proved to enhance sample utilization even further. Preliminary investigations of the instrumental fractionation behavior of plutonium and uranium analyzed via PIE methods were conducted. Data collected during these initial trial indicate that PIEs fractionate in a consistent, reproducible manner; a necessity for high precision isotope ratio measurements. Ultimately, PIEs methods were applied for

Extending and refining the mass surface around $^{208}$Pb by high-precision Penning-trap mass spectrometry with ISOLTRAP

CERN Multimedia

Herfurth, F; Stora, T; Blaum, K; Beck, D; Kowalska, M; Schwarz, S; Stanja, J; Herlert, A J; Yamaguchi, T

We propose high-precision mass spectrometry of nuclides around the doubly magic $^{208}$Pb. On the neutron-rich side, we aim to extend the knowledge of Fr, At, Hg, and Au masses to study the robustness of the N = 126 shell closure and to provide mass data necessary for modeling the rapid-neutron-capture process. On the proton-rich side, we aim at high-resolution mass spectrometry of selected Au, At, and Fr isotopes to verify the predicted existence of very low-lying isomeric states. The proposal will make use of newly-available laser-ionization schemes for Au and At. Finally, the recently implemented multi-reflection time-of-flight mass separator for auxiliary isobaric purification now allows measurements which were not feasible before.

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)

High-precision ground-based photometry of exoplanets

Directory of Open Access Journals (Sweden)

de Mooij Ernst J.W.

2013-04-01

Full Text Available High-precision photometry of transiting exoplanet systems has contributed significantly to our understanding of the properties of their atmospheres. The best targets are the bright exoplanet systems, for which the high number of photons allow very high signal-to-noise ratios. Most of the current instruments are not optimised for these high-precision measurements, either they have a large read-out overhead to reduce the readnoise and/or their field-of-view is limited, preventing simultaneous observations of both the target and a reference star. Recently we have proposed a new wide-field imager for the Observatoir de Mont-Megantic optimised for these bright systems (PI: Jayawardhana. The instruments has a dual beam design and a field-of-view of 17' by 17'. The cameras have a read-out time of 2 seconds, significantly reducing read-out overheads. Over the past years we have obtained significant experience with how to reach the high precision required for the characterisation of exoplanet atmospheres. Based on our experience we provide the following advice: Get the best calibrations possible. In the case of bad weather, characterise the instrument (e.g. non-linearity, dome flats, bias level, this is vital for better understanding of the science data. Observe the target for as long as possible, the out-of-transit baseline is as important as the transit/eclipse itself. A short baseline can lead to improperly corrected systematic and mis-estimation of the red-noise. Keep everything (e.g. position on detector, exposure time as stable as possible. Take care that the defocus is not too strong. For a large defocus, the contribution of the total flux from the sky-background in the aperture could well exceed that of the target, resulting in very strict requirements on the precision at which the background is measured.

Precision two-photon spectroscopy of alkali elements

Indian Academy of Sciences (India)

2014-07-18

Jul 18, 2014 ... A review of various techniques adopted for measuring absolute frequencies of the atomic transitions and precision measurements of isotope shifts and hyperfine structures (HFS) is presented. Some of the recent works on precision measurements of HFS constants of 6 2 S 1 / 2 level of 39 K and 41 K, 9 2 ...

High precision relative position sensing system for formation flying spacecraft

Data.gov (United States)

National Aeronautics and Space Administration — We propose to develop and test an optical sensing system that provides high precision relative position sensing for formation flying spacecraft.  A high precision...

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.

Optimization to improve precision in neutron activation analysis

International Nuclear Information System (INIS)

Yustina Tri Handayani

2010-01-01

The level of precision or accuracy required in analysis should be satisfied the general requirements and customer needs. In presenting the results of the analysis, the level of precision is expressed as uncertainty. Requirement general is Horwitz prediction. Factors affecting the uncertainty in the Neutron Activation Analysis (NAA) include the mass of sample, mass standards, concentration in standard, count of sample, count of standard and counting geometry. Therefore, to achieve the expected level of precision, these parameters need to be optimized. A standard concentration of similar materials is applied as a basis of calculation. In the calculation NIST SRM 2704 is applied for sediment samples. Mass of sample, irradiation time and cooling time can be modified to obtain the expected uncertainty. The prediction results show the level of precision for Al, V, Mg, Mn, K, Na, As, Cr, Co, Fe, and Zn eligible the Horwitz. The predictive the count and standard deviation for Mg-27 and Zn-65 were higher than the actual value occurred due to overlapping of Mg-27 and Mn-54 peaks and Zn-65 and Fe-59 peaks. Precision level of Ca is greater than the Horwitz, since the value of microscopic cross section, the probability of radiation emission of Ca-49 and gamma spectrometer efficiency at 3084 keV is relatively small. Increased precision can only be done by extending the counting time and multiply the number of samples, because of the fixed value. The prediction results are in accordance with experimental results. (author)

A Fourier transform infrared trace gas and isotope analyser for atmospheric applications

Directory of Open Access Journals (Sweden)

D. W. T. Griffith

2012-10-01

Full Text Available Concern in recent decades about human impacts on Earth's climate has led to the need for improved and expanded measurement capabilities of greenhouse gases in the atmosphere. In this paper we describe in detail an in situ trace gas analyser based on Fourier Transform Infrared (FTIR spectroscopy that is capable of simultaneous and continuous measurements of carbon dioxide (CO₂, methane (CH₄, carbon monoxide (CO, nitrous oxide (N₂O and ¹³C in CO₂ in air with high precision. High accuracy is established by reference to measurements of standard reference gases. Stable water isotopes can also be measured in undried airstreams. The analyser is automated and allows unattended operation with minimal operator intervention. Precision and accuracy meet and exceed the compatibility targets set by the World Meteorological Organisation – Global Atmosphere Watch for baseline measurements in the unpolluted troposphere for all species except ¹³C in CO₂.

The analyser is mobile and well suited to fixed sites, tower measurements, mobile platforms and campaign-based measurements. The isotopic specificity of the optically-based technique and analysis allows its application in isotopic tracer experiments, for example in tracing variations of ¹³C in CO₂ and ¹⁵N in N₂O. We review a number of applications illustrating use of the analyser in clean air monitoring, micrometeorological flux and tower measurements, mobile measurements on a train, and soil flux chamber measurements.

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

Conditions to obtain precise and true measurements of the intramolecular {sup 13}C distribution in organic molecules by isotopic {sup 13}C nuclear magnetic resonance spectrometry

Energy Technology Data Exchange (ETDEWEB)

Bayle, Kevin [EBSI Team, Interdisciplinary Chemistry: Synthesis, Analysis, Modelling (CEISAM), University of Nantes-CNRS UMR 6230, 2 Rue de la Houssinière, BP 92208, F-44322, Nantes Cedex 3 (France); Gilbert, Alexis [Department of Environmental Chemistry and Engineering, Tokyo Institute of Technology, 4259 Nagatsuta-cho, Midori-ku, Yokohama, Kanagawa 226-8503 (Japan); Earth–Life Science Institute, Tokyo Institute of Technology, Meguro, Tokyo 152-8551 (Japan); Julien, Maxime [EBSI Team, Interdisciplinary Chemistry: Synthesis, Analysis, Modelling (CEISAM), University of Nantes-CNRS UMR 6230, 2 Rue de la Houssinière, BP 92208, F-44322, Nantes Cedex 3 (France); Yamada, Keita [Department of Environmental Chemistry and Engineering, Tokyo Institute of Technology, 4259 Nagatsuta-cho, Midori-ku, Yokohama, Kanagawa 226-8503 (Japan); Silvestre, Virginie; Robins, Richard J.; Akoka, Serge [EBSI Team, Interdisciplinary Chemistry: Synthesis, Analysis, Modelling (CEISAM), University of Nantes-CNRS UMR 6230, 2 Rue de la Houssinière, BP 92208, F-44322, Nantes Cedex 3 (France); Yoshida, Naohiro [Department of Environmental Chemistry and Engineering, Tokyo Institute of Technology, 4259 Nagatsuta-cho, Midori-ku, Yokohama, Kanagawa 226-8503 (Japan); Earth–Life Science Institute, Tokyo Institute of Technology, Meguro, Tokyo 152-8551 (Japan); Remaud, Gérald S., E-mail: gerald.remaud@univ-nantes.fr [EBSI Team, Interdisciplinary Chemistry: Synthesis, Analysis, Modelling (CEISAM), University of Nantes-CNRS UMR 6230, 2 Rue de la Houssinière, BP 92208, F-44322, Nantes Cedex 3 (France)

2014-10-10

Highlights: • Evaluation of the trueness and precision criteria of isotopic {sup 13}C NMR spectrometry. • Use of bi-labelled [1,2-{sup 13}C{sub 2}]acetic acid to determine the performance of the instrumental response. • Inter-calibration of the {sup 13}C intramolecular composition of acetic acid using the technique GC-Py–irm-MS. - Abstract: Intramolecular {sup 13}C composition gives access to new information on the (bio) synthetic history of a given molecule. Isotopic {sup 13}C NMR spectrometry provides a general tool for measuring the position-specific {sup 13}C content. As an emerging technique, some aspects of its performance are not yet fully delineated. This paper reports on (i) the conditions required to obtain satisfactory trueness and precision for the determination of the internal {sup 13}C distribution, and (ii) an approach to determining the “absolute” position-specific {sup 13}C content. In relation to (i), a precision of <1% can be obtained whatever the molecule on any spectrometer, once quantitative conditions are met, in particular appropriate proton decoupling efficiency. This performance is a prerequisite to the measurement of isotope fractionation either on the transformed or residual compound when a chemical reaction or process is being studied. The study of the trueness has revealed that the response of the spectrometer depends on the {sup 13}C frequency range of the studied molecule, i.e. the chemical shift range. The “absolute value” and, therefore, the trueness of the {sup 13}C NMR measurements has been assessed on acetic acid and by comparison to the results obtained on the fragments from COOH and CH{sub 3} by isotopic mass spectrometry coupled to a pyrolysis device (GC-Py–irm-MS), this technique being the reference method for acetic acid. Of the two NMR spectrometers used in this work, one gave values that corresponded to those obtained by GC-Py–irm-MS (thus, the “true” value) while the other showed a bias, which was

Laser technology for high precision satellite tracking

Science.gov (United States)

Plotkin, H. H.

1974-01-01

Fixed and mobile laser ranging stations have been developed to track satellites equipped with retro-reflector arrays. These have operated consistently at data rates of once per second with range precision better than 50 cm, using Q-switched ruby lasers with pulse durations of 20 to 40 nanoseconds. Improvements are being incorporated to improve the precision to 10 cm, and to permit ranging to more distant satellites. These include improved reflector array designs, processing and analysis of the received reflection pulses, and use of sub-nanosecond pulse duration lasers.

Analysis and Optimization of Dynamic Measurement Precision of Fiber Optic Gyroscope

Directory of Open Access Journals (Sweden)

Hui Li

2013-01-01

Full Text Available In order to improve the dynamic performance of high precision interferometer fiber optic gyroscope (IFOG, the influencing factors of the fast response characteristics are analyzed based on a proposed assistant design setup, and a high dynamic detection method is proposed to suppress the adverse effects of the key influencing factors. The assistant design platform is built by using the virtual instrument technology for IFOG, which can monitor the closed-loop state variables in real time for analyzing the influence of both the optical components and detection circuit on the dynamic performance of IFOG. The analysis results indicate that nonlinearity of optical Sagnac effect, optical parameter uncertainty, dynamic characteristics of internal modules and time delay of signal detection circuit are the major causes of dynamic performance deterioration, which can induce potential system instability in practical control systems. By taking all these factors into consideration, we design a robust control algorithm to realize the high dynamic closed-loop detection of IFOG. Finally, experiments show that the improved 0.01 deg/h high precision IFOG with the proposed control algorithm can achieve fast tracking and good dynamic measurement precision.

Precise determination of the neutron scattering length of lead isotopes 204Pb,207Pb and 208Pb by neutron interferometry

International Nuclear Information System (INIS)

Ioffe, A.; Ermakov, O.; Karpikhin, I.; Krupchitsky, P.; Mikula, P.; Lukas, P.; Vrana, M.

2000-01-01

The neutron scattering length of lead isotopes 204 Pb, 207 Pb and 208 Pb are determined by a set of neutron interferometry experiments. The obtained values b (208) =9.494(30) fm, b (207) =9.286(16) fm, b (204) =10.893(78) fm have much higher accuracy then current table data. Together with the precise value of b for natural lead, these results represent a complete set of data and allow one to calculate b (206) =9.221(69) fm, which is in the very good agreement with the present day experimental value. (orig.)

Determination of tungsten in high-alloy steels and heat resisting alloys by isotope dilution-spark source mass spectrometry

International Nuclear Information System (INIS)

Saito, Morimasa; Yamada, Kei; Okochi, Haruno; Hirose, Fumio

1983-01-01

Tungsten in high-alloy steels and heat-resisting alloys was determined by isotope dilution method combined with spark source mass spectrometry by using 183 W enriched tungsten. The spike solution was prepared by fusing tungsten trioxide in sodium carbonate. A high-alloy steel sample was dissolved in the mixture of sulfuric acid and phosphoric acid together with the spike solution; a sample of heat resisting alloy was similarly dissolved in the mixture of hydrochloric acid, nitric acid, sulfuric acid, and phosphoric acid. The solution was evaporated to give dense white fumes. Tungsten was separated from the residue by a conventional cinchonine salt-precipitation method. The salt was ignited, and the residue was mixed with graphite powder and pressed into electrodes. The isotope 183 W and 184 W were measured. The method was applied to the determination of tungsten in JSS and NBS standard high-alloy steels and JAERI standard nickel- and NBS standard cobalt-base heat resisting alloys containing more than 0.05% tungsten. The results were obtained with satisfactory precision and accuracy. However, the results obtained for JSS standard high- speed steels containing molybdenum tended to be significantly lower than the certified values. (author)

Use of the Isomass 54E thermal ionisation mass spectrometer at AEE Winfrith. Part II: plutonium analysis

International Nuclear Information System (INIS)

Knight, A.P.

1982-06-01

This report describes the application of the Isomass 54E Thermal ionisation mass spectrometer for the isotopic analysis of plutonium, and gives details of the development of a method for quantitative determination of plutonium in sample solutions using isotopic dilution. A computer program for the control of the 54E is also described. Isotope dilution was used to compare results of plutonium content of twelve zebra reactor fuel pellets with results obtained by titrimetry. The Isomass 54E is shown to be capable of high precision analysis of plutonium sample solutions for both isotopic content and total plutonium concentration using an isotope dilution technique. (U.K.)

Lithium Isotopes in Geothermal Fluids from Iceland

Science.gov (United States)

Millot, R.; Asmundsson, R.; Sanjuan, B.

2008-12-01

One of the main objectives of the HITI project (HIgh Temperature Instruments for supercritical geothermal reservoir characterization and exploitation), partially funded by the European Union, is to develop methods to characterize the reservoir and fluids of deep and very high temperature geothermal systems. The chemical composition of geothermal waters in terms of major and trace elements is related to the temperature, the degree of water/rock interaction and the mineralogical assemblage of the bedrock. Traditional geothermometers, such as silica, Na-K, Na-K-Ca or K-Mg applied to geothermal waters, make it possible to estimate the temperature at depth of the reservoir from which the waters are derived. However, the values estimated for deep temperature are not always concordant. The chemical geothermometer Na/Li which presents the singularity of associating two chemical elements, one a major element (sodium) and the other a trace element (Li), can be also used and gives an additional temperature estimation. The primary objective of this work was to better understand the behavior of this last geothermometer using the isotopic systematics of Li in order to apply it at very high temperature Icelandic geothermal systems. One particularly important aspect was to establish the nature, extent and mechanism of Li isotope fractionation between 100 and 350°C during water/rock interaction. For that purpose, we measured Li isotopes of about 25 geothermal waters from Iceland by using a Neptune MC-ICP-MS that enabled the analysis of Li isotopic ratios in geothermal waters with a level of precision of ±0.5‰ (2 standard deviations) on quantities of 10-50 ng of Li. Geothermal waters from Reykjanes, Svartsengi, Nesjavellir, Hveragerdi, Namafjall and Krafla geothermal systems were studied and particular emphasis was placed on the characterization of the behavior of Li isotopes in this volcanic context at high temperature with or without the presence of seawater during water

A miniaturized laser-ablation mass spectrometer for in-situ measurements of isotope composition on solar body surfaces

Science.gov (United States)

Riedo, A.; Meyer, S.; Tulej, M.; Neuland, M.; Bieler, A.; Iakovleva, M.; Wurz, P.

2012-04-01

space instrument would have a cylindrical shape with a length of 120 mm, and a diameter of 60 mm, and a weight of about 1.5 kg (all electronics included). The mass analyzer supports high dynamic range of about 107 and a typical mass resolution of m/Δm~700. A computer-controlled optimizer controls the reproducibility of the performance of the mass analyzer, the laser fluence and the positioning of the sample. The system supports highly sensitive studies of elemental composition with sub-ppm detection limits. Our studies show that high accuracy and precision measurements can also be achieved in the investigations of isotopic patterns. Our initial studies of lead isotopic pattern indicated an accuracy and precision in the per mile range, which are comparable to that achieved by other - well known in isotopic analysis - mass spectrometric techniques, i.e., TIMS, SIMS, LA-ICP-MS used in the laboratory. The initial studies were conducted with Galena minerals and NIST standards. Hence, the miniaturized laser ablation time-of-flight mass spectrometer is a powerful instrument for in-situ measurements for the further investigation in surface characterization.

Stable isotopes in Lithuanian bioarcheological material

Science.gov (United States)

Skipityte, Raminta; Jankauskas, Rimantas; Remeikis, Vidmantas

2015-04-01

Investigation of bioarcheological material of ancient human populations allows us to understand the subsistence behavior associated with various adaptations to the environment. Feeding habits are essential to the survival and growth of ancient populations. Stable isotope analysis is accepted tool in paleodiet (Schutkowski et al, 1999) and paleoenvironmental (Zernitskaya et al, 2014) studies. However, stable isotopes can be useful not only in investigating human feeding habits but also in describing social and cultural structure of the past populations (Le Huray and Schutkowski, 2005). Only few stable isotope investigations have been performed before in Lithuanian region suggesting a quite uniform diet between males and females and protein intake from freshwater fish and animal protein. Previously, stable isotope analysis has only been used to study a Stone Age population however, more recently studies have been conducted on Iron Age and Late medieval samples (Jacobs et al, 2009). Anyway, there was a need for more precise examination. Stable isotope analysis were performed on human bone collagen and apatite samples in this study. Data represented various ages (from 5-7th cent. to 18th cent.). Stable carbon and nitrogen isotope analysis on medieval populations indicated that individuals in studied sites in Lithuania were almost exclusively consuming C3 plants, C3 fed terrestrial animals, and some freshwater resources. Current investigation demonstrated social differences between elites and country people and is promising in paleodietary and daily life reconstruction. Acknowledgement I thank prof. dr. G. Grupe, Director of the Anthropological and Palaeoanatomical State Collection in Munich for providing the opportunity to work in her laboratory. The part of this work was funded by DAAD. Antanaitis-Jacobs, Indre, et al. "Diet in early Lithuanian prehistory and the new stable isotope evidence." Archaeologia Baltica 12 (2009): 12-30. Le Huray, Jonathan D., and Holger

Charge radii and electromagnetic moments of Li and Be isotopes from the ab initio no-core shell model

International Nuclear Information System (INIS)

Forssen, C.; Caurier, E.; Navratil, P.

2009-01-01

Recently, charge radii and ground-state electromagnetic moments of Li and Be isotopes were measured precisely. We have performed large-scale ab initio no-core shell model calculations for these isotopes using high-precision nucleon-nucleon potentials. The isotopic trends of our computed charge radii and quadrupole and magnetic-dipole moments are in good agreement with experimental results with the exception of the 11 Li charge radius. The magnetic moments are in particular well described, whereas the absolute magnitudes of the quadrupole moments are about 10% too small. The small magnitude of the 6 Li quadrupole moment is reproduced, and with the CD-Bonn NN potential, also its correct sign

Application of Stable Isotope in Detection of Veterinary Drug Residues

International Nuclear Information System (INIS)

Wang Wei; Liu Zhanfeng; Du Xiaoning

2010-01-01

In recent years, there has happened a series of significant food safety events worldwide, which lower down consumers' confidence in food safety, and they are taking increasing care about the sources of their foods. The safety problem of animal-origin foods has become a global topic for discussion. Therefore, it is a pressing task to establish a precise, sensitive and reliable method for analyzing veterinary drug residue. An introduction of the present status regarding veterinary drug residue analysis was made in the paper, and it briefly summarized the limit of detection (LOD) and quantification (LOQ) which could be reached in veterinary drug residue analysis by isotopic internal standard method domestically and abroad. The paper also made a review of the progress in applied research of stable isotope labeled compound in veterinary drug residue analysis of, such as, antibiotic medicines, furans and sulfonamides. The paper elucidated the great importance of the application of stable isotopes in the sane development of China's food safety system. (authors)

Decoupling of the leading contribution in the discrete BFKL analysis of high-precision HERA data

Energy Technology Data Exchange (ETDEWEB)

Kowalski, H. [Deutsches Elektronen-Synchrotron DESY, Hamburg (Germany); Lipatov, L.N. [St. Petersburg State University, St. Petersburg (Russian Federation); Petersburg Nuclear Physics Institute, Gatchina (Russian Federation); Ross, D.A. [University of Southampton, School of Physics and Astronomy, Southampton (United Kingdom); Schulz, O. [Max Planck Institute for Physics, Munich (Germany)

2017-11-15

We analyse, in NLO, the physical properties of the discrete eigenvalue solution for the BFKL equation. We show that a set of eigenfunctions with positive eigenvalues, ω, together with a small contribution from a continuum of eigenfunctions with negative ω, provide an excellent description of high-precision HERA F{sub 2} data in the region, x < 0.001, Q{sup 2} > 6 GeV{sup 2}. The phases of the eigenfunctions can be obtained from a simple parametrisation of the pomeron spectrum, which has a natural motivation within BFKL. The data analysis shows that the first eigenfunction decouples completely or almost completely from the proton. This suggests that there exists an additional ground state, which is naturally saturated and may have the properties of the soft pomeron. (orig.)

High-precision performance testing of the LHC power converters

CERN Document Server

Bastos, M; Dreesen, P; Fernqvist, G; Fournier, O; Hudson, G

2007-01-01

The magnet power converters for LHC were procured in three parts, power part, current transducers and control electronics, to enable a maximum of industrial participation in the manufacturing and still guarantee the very high precision (a few parts in 10-6) required by LHC. One consequence of this approach was several stages of system tests: factory reception tests, CERN reception tests, integration tests , short-circuit tests and commissioning on the final load in the LHC tunnel. The majority of the power converters for LHC have now been delivered, integrated into complete converter and high-precision performance testing is well advanced. This paper presents the techniques used for high-precision testing and the results obtained.

Triple oxygen isotopes in biogenic and sedimentary carbonates

Science.gov (United States)

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

2014-09-01

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

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.

Reassessment of the C-13/C-12 and C-14/C-12 isotopic fractionation ratio and its impact on high-precision radiocarbon dating