Knowledge Base

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  • GC-IRMS
  • Gas Chromatography
  • Oxygen isotopes

A novel methylation derivatization method for ?18O analysis of individual carbohydrates by gas chromatography/pyrolysis– isotope ratio mass spectrometry

Marco M. Lehmann (1), Maria Fischer (2), Jan Blees (1), Michael Zech (3), Rolf T. W. Siegwolf (1) and Matthias Saurer (1)

1) Laboratory of Atmospheric Chemistry, Paul Scherrer Institute, PSI, CH-5232 Villigen, Switzerland, 2) Laboratory of Nanoscale Materials Science, Empa, Überlandstrasse 129, CH-8600 Dübendorf, Switzerland, 3) Department of Soil Biogeochemistry, Martin-Luther-University Halle Wittenberg, Von-Seckendorff-Platz 3, D-06120 Halle, Germany

Rapid Communications in Mass Spectrometry (2016), V30, pp221–229, doi: 10.1002/rcm.7431

Goal: The oxygen isotope ratio (?18O) 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, ?18O analyses are often performed on carbohydrate bulk material, while compound-specific ?18O analyses remain challenging and methods for a wide range of individual carbohydrates are rare. To improve the ?18O 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.

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  • GC-IRMS
  • Gas Chromatography
  • Combustion
  • Carbon isotopes

Purification and Gas Chromatography–Combustion–Isotope Ratio Mass Spectrometry of Aroma Compounds from Green Tea Products and Comparison to Bulk Analysis

Ariaki Murata (1), Ulrich H. Engelhardt (2), Peter Fleischmann (2), Keita Yamada (3), Naohiro Yoshida (3), Dieter Juchelka (4), Andreas Hilkert (4), Toshiyuki Ohnishi (5), Naoharu Watanabe (1) and Peter Winterhalter (2)

1) Graduate School of Science and Technology, Shizuoka University, 836 Ohya, Shizuoka 422-8529, Japan, 2) Institute of Food Chemistry, Technische Universität Braunschweig, Schleinitzstrasse 20, DE-38106 Braunschweig, Germany, 3) Department of Environmental Chemistry and Engineering, Interdisciplinary Graduate School of Science and Engineering, Tokyo Institute of Technology, Yokohama 226-8502, Japan, 4) Thermo Fisher Scientific (Bremen) GmbH, Hanna-Kunath-Strasse 11, 28199 Bremen, Germany, 5) Graduate School of Agriculture, Shizuoka University, 836 Ohya, Suruga-ku, Shizuoka 422-8529, Japan

Journal of Agricultural and Food Chemistry (2013), V61(47), pp 11321–11325, doi: 10.1021/jf403605a

Goal: A method for carbon isotope ratio (d13C) analysis was developed for compound-specific isotope analysis of tea volatiles, and the values were compared with the d13C value from bulk isotope analyses. The d13C value of 2-phenylethanol liberated via enzymatic hydrolysis of the 2-phenylethyl ß-primeveroside standard was examined first. Isotope fractionations for 2-phenylethyl ß-primeveroside from preparative high-performance liquid chromatography (HPLC) were also analyzed. The enzymatic treatment and the preparative HPLC process did not cause carbon isotope fractionations, substantiating the strategies available for d13C analysis of volatile compounds. On the basis of the gas chromatography–combustion–isotope ratio mass spectrometry data from 2-phenylethanol, it was possible to derive the conditions for enzyme treatment and preparative HPLC of the glycoconjugates of 2-phenylethanol, (Z)-3-hexenol, and benzyl alcohol isolated from green tea leaves.

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  • GC-IRMS
  • O isotopes
  • Sugar

A novel methodological approach for ?18O analysis of sugars using gas chromatography-pyrolysis-isotope ratio mass spectrometry

Michael Zech (1,2), Matthias Saurer (3), Mario Tuthorn (1), Katja Rinne (3), Roland A. Werner (4), Rolf Siegwolf (3), Bruno Glaser (2) and Dieter Juchelka (5)

1) Department of Soil Physics and Chair of Geomorphology, University of Bayreuth, Bayreuth, Germany, 2) Institute of Agronomy and Nutritional Sciences, Soil Biogeochemistry, Martin-Luther-University, Halle-Wittenberg, Germany, 3) Paul Scherrer Institute, Villigen, Switzerland, 4) Institute of Agricultural Sciences, ETH Zürich, Switzerland, 5) Thermo Fisher Scientific, Bremen, Germany

Isotopes in Environmental and Health Studies (2013), Volume 49(4), pp492–502, doi: 10.1080/10256016.2013.824875

Goal: Although the instrumental coupling of gas chromatography-pyrolysis-isotope ratio mass spectrometry (GC-Py-IRMS) for compound-specific d18O analysis has been commercially available for more than a decade, this method has been hardly applied so far. Here we present the first GC-Py-IRMS d18O results for trimethylsilyl-derivatives of plant sap-relevant sugars and a polyalcohol (glucose, fructose, sucrose, raffinose and pinitol). Particularly, we focus on sucrose, which is assimilated in leaves and which is the most important transport sugar in plants and hence of utmost relevance in plant physiology and paleoclimate studies.

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  • GC-IRMS
  • LC-IRMS
  • Bone Collagen

Comparison of liquid chromatography–isotope ratio mass spectrometry (LC/IRMS) and gas chromatography–combustion– isotope ratio mass spectrometry (GC/C/IRMS) for the determination of collagen amino acid d13C values for palaeodietary and palaeoecological reconstruction

Philip J. H. Dunn, Noah V. Honch and Richard P. Evershed

Organic Geochemistry Unit, Bristol Biogeochemistry Research Center, School of Chemistry, University of Bristol, Cantock’s Close, Bristol BS8 1TS, UK

Rapid Communications in Mass Spectrometry (2011), V25, pp2995–3011, doi: 10.1002/rcm.5174

Goal: Results are presented of a comparison of the amino acid (AA) delta13C values obtained by gas chromatography- combustion-isotope ratio mass spectrometry (GC/C/IRMS) and liquid chromatography- isotope ratio mass spectrometry (LC/IRMS). Although the primary focus was the compound-specific stable carbon isotope analysis of bone collagen AAs, because of its growing application for palaeodietary and palaeoecological reconstruction, the results are relevant to any field where AA delta13C values are required. We compare LC/IRMS with the most up-to-date GC/C/IRMS method using N-acetyl methyl ester (NACME) AA derivatives.

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  • GC-IRMS
  • Authenticity
  • Wine

Progress in wine authentication: GC–C/P–IRMS measurements of glycerol and GC analysis of 2,3-butanediol stereoisomers

Jochen Jung, Tatjana Jaufmann, Uwe Hener, Andreas Münch, Mirjam Kreck, Helmut Dietrich and Armin Mosandl

Institut für Lebensmittelchemie, Biozentrum J.W. Goethe-Universität, Marie-Curie-Str. 9, 60439 Frankfurt/Main, Germany

Eur Food Res Technol (2006), V223(6), pp811-820, doi: 10.1007/s00217-006-0274-4

Goal: The determination of glycerol and 2,3-butanediol by photometric or enzymatic methods is well established. This paper reports on the direct assessment of glycerol and stereoselective analysis of 2,3-butanediol isomers in wine using capillary GC without any derivatisation.

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  • GC-IRMS
  • Authenticity
  • Lavender Oil

Comprehensive authenticity assessment of lavender oils using multielement/multicomponent isotope ratio mass spectrometry analysis and enantioselective multidimensional gas chromatography–mass spectrometry

Jochen Jung, Sabine Sewenig, Uwe Hener and Armin Mosandl  

Institut für Lebensmittelchemie, Biozentrum J.W. Goethe-Universität, Marie-Curie-Str. 9, 60439 Frankfurt/Main, Germany

European Food Research and Technology (2005), V220(2), pp232–237, doi: 10.1007/s00217-004-1049-4

Goal: Delta13CV-PDB, delta2HV-SMOW and delta18OV-SMOW multielement isotope ratio mass spectrometry analysis of linalool and linalyl acetate, the main components of lavender oils, is reported. Self-prepared and commercially available lavender oils, as well as samples of linalool and linalyl acetate labelled as synthetic and natural products respectively, were investigated. Multielement/multicomponent isotope ratio mass spectrometry analysis and-as far as possible-in conjunction with enantioselective analysis is judged to be the most comprehensive basis of authenticity assessment in flavour and essential oil analysis.

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  • Noble Gas MS
  • Helix MC Plus
  • Xe isotopes
  • Meteorites

Chondritic xenon in the Earth’s mantle

Antonio Caracausi (1,2), Guillaume Avice (2), Peter G. Burnard (2), Evelyn Füri (2) and Bernard Marty (2); 1) Instituto Nazionale di Geofisica e Vulcanologia, Sezione di Palermo, 90146 Palermo, Italy, 2) Centre de Recherches Pétrographiques et Géochimiques, UMR 7358, Université de Lorraine, CNRS, 54501 Vandoeuvre-lès-Nancy, France

Nature (2016), V533, pp82-85, doi: 10.1594/IEDA/100582

Goal: Noble gas isotopes are powerful tracers of the origins of planetary volatiles, and the accretion and evolution of the Earth. Here we show, using high-precision analysis of magmatic gas from the Eifel volcanic area (in Germany), that the light xenon isotopes identify a chondritic primordial component that differs from the precursor of atmospheric xenon. This is consistent with an asteroidal origin for the volatiles in the Earth’s mantle, and indicates that the volatiles in the atmosphere and mantle originated from distinct cosmochemical sources. Furthermore, our data are consistent with the origin of Eifel magmatism being a deep mantle plume.

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  • Noble Gas MS
  • Helix MC Plus
  • Xe, Kr isotopes
  • Meteorites

A comprehensive study of noble gases and nitrogen in “Hypatia”, a diamond-rich pebble from SW Egypt

Guillaume Avice (1), Matthias M.M. Meier (1,2), Bernard Marty (1), Rainer Wieler (2), Jan D. Kramers (3), Falko Langenhorst (4), Pierre Cartigny (5), Colin Maden (2), Laurent Zimmermann (1), Marco A.G. Andreoli (6)

1) CRPG-CNRS, Université de Lorraine, UMR 7358, 15 rue Notre-Dame des Pauvres, BP 20, 54501 Vandoeuvre-lès-Nancy Cedex, France, 2) Department of Earth Sciences, ETH Zürich, Clausiusstrasse 25, CH-8092 Zürich, Switzerland, 3) Department of Geology, University of Johannesburg, Auckland Park 2006, Johannesburg, South Africa, 4) Institut für Geowissenschaften, Friedrich-Schiller-Universität Jena, Carl-Zeiss-Promenade 10, D-07745 Jena, Germany, 5) Équipe de Géochimie des Isotopes Stables, Institut de Physique du Globe de Paris, Sorbonne Paris Cité, Univ. Paris Diderot, UMR 7154 CNRS, F-75005 Paris, France, 6) School of Geosciences, University of the Witwatersrand, PO Box 3, Wits 2050, South Africa

Earth and Planetary Science Letters (2015), V432, pp243-253, doi: 10.1016/j.epsl.2015.10.013

Goal: This is a follow-up study of a work by Kramers et al. (2013) on a very unusual diamond-rich rock fragment found in the area of south west Egypt in the south-western side of the Libyan Desert Glass strewn field. This pebble, called Hypatia, is composed of almost pure carbon. We also analyzed concentrations and isotopic compositions of all five noble gases and nitrogen in several ?mg sized Hypatia samples. These data confirm the conclusion by Kramers et al. (2013) that Hypatia is extra-terrestrial. The sample is relatively rich in trapped noble gases with an isotopic composition being close to the Q component found in many types of meteorites. 40Ar/36Ar ratios in individual steps are as low as 0.4±0.3.

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  • TIMS
  • Triton
  • U-Pb
  • Zircons

High-precision U–Pb dating of complex zircon from the Lewisian Gneiss Complex of Scotland using an incremental CA-ID-TIMS approach

Q.G. Crowley (1), R. Key (2), S.R. Noble (3)

1) School of Natural Sciences, Department of Geology, Trinity College, Dublin 2, Ireland, 2) British Geological Survey, Murchison House,West Mains Road, Edinburgh EH9 3LA, UK, 3) NERC Isotope Geosciences Laboratory, British Geological Survey, Kingsley Dunham Centre, Keyworth, Nottingham NG12 5GG, UK

Gondwana Research (2015), V27, pp1381–1391, doi: 10.1016/j.gr.2014.04.001

Goal: A novel approach of thermally annealing and sequentially partially dissolving single zircon grains prior to high-precision Isotope Dilution Thermal Ionization Mass Spectrometry (ID-TIMS) is presented. This technique is applied to complex zircon from the Precambrian Lewisian Gneiss Complex of Scotland. Up to six partial dissolutions were conducted at incrementally higher temperatures and analysed at each successive step. Using this technique of pseudo-spatial resolution coupled with high-precision analysis it is possible to recognise discrete Pb-loss and multiple stages of zircon growth or isotopic resetting within single grains to within 0.1–0.2% error (2?) on individual 207Pb/206Pb ages. This method has relevance to U–Pb zircon geochronology where conventional micro-beam techniques are unable to resolve between separate ages within single grains.

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  • MC-ICPMS
  • Neptune
  • Sr isotopes
  • Anthropology

Mobility Histories of 7th–9th Century AD People Buried at Early Medieval Bamburgh, Northumberland, England

S.E. Groves (1), C.A. Roberts (1), S. Lucy (2), G. Pearson (3), D.R. Gröcke (4), G. Nowell (4), C.G. Macpherson (4) and G. Young (5)

1) Department of Archaeology, Durham University, South Road, Durham DH1 3LE, UK, 2) Newnham College, University of Cambridge, Sidgwick Avenue, Cambridge CB3 9DF, 3) Department of Earth and Atmospheric Sciences, 1-26 Earth Sciences Building, University of Alberta, Edmonton AB T6G 2E3, Canada; 4) Department of Earth Sciences, Durham University, Science Labs, Durham DH1 3LE, UK; 5) Bamburgh Research Project, 23, Kingsdale Avenue, Blyth, Northumberland NE24 4EN, UK

American Journal of Physical Anthropology (2013), V151(3), pp462–476, doi: 10.1002/ajpa.22290

Goal: Early Medieval England is described historically as a time when people migrated from the Continent to English shores. This study tests the hypothesis that those buried in the Bowl Hole cemetery, Bamburgh, Northumberland were nonlocally born, because of its royal status. Ninety-one male and female adult, and nonadult, skeletons were studied. Isotope ratios of strontium (87Sr/86Sr) and oxygen (d18O) were generated for 78 individuals (28 females, 27 males, five “adults,” 18 nonadults).

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  • MC-ICPMS
  • Neptune
  • Sr isotopes
  • NIST SRM-1515

Determination of 87Sr/86Sr and ?88/86Sr ratios in plant materials using MC-ICP-MS

Hou-Chun Liu (1,2), Chuan-Hsiung Chung (1,2), Chen-Feng You (1,2) and Yi-Hsuan Chiang (1)

1) Department of Earth Sciences, National Cheng Kung University, 70101 Tainan, ROC, Taiwan, 2) Earth Dynamic System Research Center, National Cheng Kung University, 70101 Tainan, ROC, Taiwan

Analytical and Bioanalytical Chemistry (2016), V408, pp387–397, doi: 10.1007/s00216-015-9070-y

Goal: A protocol for highly accurate and precise determination of Sr isotope ratios in plant materials, (87)Sr/(86)Sr and ? (88/86)Sr, by multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS) is presented in this study. An Eichrom Sr resin was used for matrix separation and an improved Zr empirical external normalization coupled with standard-sample bracketing method (Zr EEN-SSB) was applied to mass bias correction during Sr isotope MC-ICP-MS measurements. Potential influences of matrix elements, and polyatomic and isobaric interferences on the Sr isotopic determination were further evaluated using NIST SRM 987 Sr isotopic standard spiked with various amount of Ca, Mg, and Rb contents.

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  • MC-ICPMS
  • Neptune
  • Si isotopes
  • Weathering

Silicon isotope systematics of acidic weathering of fresh basalts, Kilauea Volcano, Hawai’i

Steven M. Chemtob (1,2), George R. Rossman (1), Edward D. Young (3), Karen Ziegler (4), Fréderic Moynier (5), John M. Eiler (1), Joel A. Hurowitz (6)

1) Divison of Geological and Planetary Sciences, California Institute of Technology, Pasadena, CA 91125, United States, 2) Department of Earth and Planetary Sciences, Washington University, St. Louis, MO 63130, United States, 3) Department of Earth, Planetary, and Space Sciences, University of California, Los Angeles, CA 90095, United States, 4) Institute of Meteoritics, University of New Mexico, Albuquerque, NM 87131, United States, 5) Institut de Physique du Globe de Paris, Institut Universitaire de France, Université Paris Diderot, Paris, France, 6) Department of Geosciences, Stony Brook University, Stony Brook, NY 11794, United States

Geochimica et Cosmochimica Acta (2015), V169, pp63–81, doi: 10.1016/j.gca.2015.07.026

Goal: Silicon stable isotopes are fractionated by a host of low-temperature aqueous processes, making them potentially useful as a weathering proxy. Here we characterize the silicon isotope signature of surficial chemical weathering of glassy basaltic lava flows at Kilauea Volcano, Hawaii. Our results indicate that (1) altering fluid chemistry and fluid–rock ratio impact the Si isotope signature of chemical weathering and (2) ?30Si of solids produced by low temperature aqueous alteration may diverge sharply from watershed- or landscape-scale weathering trends.

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  • MC-ICPMS
  • Neptune
  • Hf isotopes
  • U-Pb geochrononolgy

Clarifying the zircon Hf isotope record of crust–mantle evolution

Jeffery D. Vervoort (1), Anthony I.S. Kemp (2)

1) School of the Environment, Washington State University, Pullman, WA 99163, USA, 2) School of Earth and Environment, The University of Western Australia, Crawley, WA, Australia

Chemical Geology (2016), V425, pp65-75, doi: 10.1016/j.chemgeo.2016.01.023

Goal: In this paper we review several important issues related to unraveling the complexities of integrated U–Pb age and Hf isotope datasets, especially with respect to understanding crust–mantle evolution. In particular, we address the potential difficulty of assigning accurate initial Hf isotope compositions as well as some of the inherent problems associated with so-called “depleted-mantle model ages”. Finally, we make some suggestions regarding the optimum analytical approach and presentation of the Hf (and Nd) isotope data to obtain the clearest record of Earth's chemical evolution

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  • MC-ICPMS
  • Neptune
  • Hg isotopes
  • Gold trap

Indirect gold trap–MC-ICP-MS coupling for Hg stable isotope analysis using a syringe injection interface

Jeroen E. Sonke, Thomas Zambardi and Jean-Paul Toutain

Observatoire Midi-pyrénées, Laboratoire des Mécanismes et Transferts en Géologie, CNRS/IRD/Université Paul Sabatier Toulouse 3, 14 avenue Edouard Belin, Toulouse, 31400, France

Journal of Analytical Atomic Spectrometry (2008), V23, pp569–573, doi: 10.1039/b718181g

Goal: Gold traps are part of standard instrumentation to quantitatively pre-concentrate gaseous elemental mercury, Hg0 (g), and are a pre-requisite for atmospheric Hg0 (g) analysis. High precision mercury stable isotope ratio analysis by on-line coupling of gold traps to multi collector-inductively coupled plasma mass spectrometry (MC-ICP-MS) has up to now been problematic due to the transient nature of the signal. We present a new off-line technique, where amalgamated elemental Hg0 is volatilized from the gold trap in an argon gas stream and temporarily stored in a large volume gas tight syringe.

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  • MC-ICPMS
  • Neptune
  • S isotopes
  • Gas Chromatography

Compound-Specific ?34S Analysis of Volatile Organics by Coupled GC/Multicollector-ICPMS

Alon Amrani, Alex L. Sessions, and Jess F. Adkins

Division of Geological and Planetary Sciences, California Institute of Technology, 1200 East California Boulevard, Pasadena California, USA

Analytical Chemistry (2009), V81(21), pp9027–9034, doi: 10.1021/ac9016538

Goal: We have developed a highly sensitive and robust method for the analysis of ?34S in individual organic compounds by coupled gas chromatography (GC) and multicollector inductively coupled plasma mass spectrometry (MC-ICPMS). The system requires minimal alteration of commercial hardware and is amenable to virtually all sample introduction methods. Isobaric interference from O2+ is minimized by employing dry plasma conditions and is cleanly resolved at all masses using medium resolution on the Thermo Neptune MC-ICPMS.