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New Approaches for Stable Isotope Ratio Measurements IAEA-TECDOC-1247 New approaches for stable isotope ratio measurements Proceedings of an Advisory Group meeting held in Vienna, 20–23 September 1999 October 2001 The originating Section of this publication in the IAEA was: Isotope Hydrology Section International Atomic Energy Agency Wagramer Strasse 5 P.O. Box 100 A-1400 Vienna, Austria NEW APPROACHES FOR STABLE ISOTOPE RATIO MEASUREMENTS IAEA, VIENNA, 2001 IAEA-TECDOC-1247 ISSN 1011–4289 © IAEA, 2001 Printed by the IAEA in Austria October 2001 FOREWORD The practice of stable isotope ratio determination has undergone profound changes during the past decade. While this analytical task used to be the artwork of a small but very active group of experimentalists, it has now largely shifted to the hands of laboratory operators. Rapid technical developments in the last few years, particularly in the areas of non-mass spectrometric and mass spectrometric analysis of organic and inorganic matter have enabled a multitude of new applications in biogeochemistry and related fields. An IAEA Advisory Group meeting was held in September 1999 to identify and discuss these recent technical advances as well as new scientific opportunities and analytical challenges. There was an expressed need by the scientific community for concurrent development of suitable, high-quality stable isotope reference materials, standardized methods and calibration procedures. By consensus of participants, the Advisory Group established a list of candidate reference materials that would improve transferability of results and ultimately enable broader application of isotope techniques. This report includes a summary of discussions at the meeting and contributions on isotope applications in a range of specific biogeochemical fields using the new analytical techniques. It is expected to serve as a useful reference for researchers and laboratory managers who plan to develop or apply state-of-the-art stable isotope techniques. The papers were reviewed by W. Brand, of the Max Planck Institute for Geochemistry, Jena, Germany. The IAEA officers responsible for this publication were M. Gröning, of the Agency’s Laboratories, Seibersdorf and Vienna, and P. Aggarwal, of the Division of Physical and Chemical Sciences. EDITORIAL NOTE This publication has been prepared from the original material as submitted by the authors. The views expressed do not necessarily reflect those of the IAEA, the governments of the nominating Member States or the nominating organizations. The use of particular designations of countries or territories does not imply any judgement by the publisher, the IAEA, as to the legal status of such countries or territories, of their authorities and institutions or of the delimitation of their boundaries. The mention of names of specific companies or products (whether or not indicated as registered) does not imply any intention to infringe proprietary rights, nor should it be construed as an endorsement or recommendation on the part of the IAEA. The authors are responsible for having obtained the necessary permission for the IAEA to reproduce, translate or use material from sources already protected by copyrights. CONTENTS Summary.................................................................................................................................................. 1 OPTICAL SPECTROSCOPIC TECHNIQUES Laser spectrometry applied to the simultaneous determination of the @2H, @17O, and @18O isotope abundances in water................................................................................................................. 7 E.R.T. Kerstel, R. Van Trigt, N. Dam, J. Reuss, H.A.J. Meijer Laser assisted ratio analysis — An alternative to GC/IRMS for CO2 .................................................. 15 D.E. Murnick CF-TECHNIQUES APPLIED FOR STABLE ISOTOPES IN ORGANIC MATERIALS On-line measurement of 13C/12C and 15N/14N ratios by E/A-diluter-IRMS........................................... 25 H. Förstel, M. Boner, H. Prast High temperature pyrolysis: A new system for isotopic and elemental analysis.................................. 33 M. Gehre Isotope methods for the control of food products and beverages ......................................................... 39 C. Guillou, F. Reniero Methods in the use of GC/C/IRMS for the analysis of biochemical and pollutant isotope signatures of compounds .................................................................................................................... 55 S.A. Macko, M.H. Engel Stable carbon isotope ratios of lipid biomarkers and their applications in the marine environment.... 67 I. Tolosa, S. de Mora Challenges of 13C/12C measurements by CF-IRMS of biogeochemical samples at sub-nanomolar levels ...................................................................................................................... 75 M.J. Whiticar, M. Eek CF-TECHNIQUES APPLIED TO INORGANIC COMPOUNDS Taking the atmosphere’s pulse: The application of GC-IRMS to stable isotopes in atmospheric trace gases .................................................................................................................. 99 D.C. Lowe, D.J. Ferretti, R.J. Francey, C.E. Allison Isotope ratio analysis on water: A critical look at developments........................................................ 105 H.A.J. Meijer On-line stable isotope measurements during plant and soil gas exchange ......................................... 113 D. Yakir Continuous flow IRMS application to CH4, NMHCs, and N2O in the atmosphere and the oceans ... 131 N. Yoshida, U. Tsunogai, S. Toyoda ANNEX............................................................................................................................................... 137 WORKING GROUP REPORTS: A — Atmosphere................................................................................................................................. 138 B — Biogeochemistry, Food and Ecology.......................................................................................... 141 C — Hydrology and Oceanography.................................................................................................... 143 D — Labelled Componds.................................................................................................................... 144 List of Participants .............................................................................................................................. 149 SUMMARY New analytical techniques for stable isotope ratio measurements have become popular over the past decade. These include non-mass spectrometric techniques using laser spectroscopy, and mass- spectrometric techniques with on-line or continuous flow apparatus for sample introduction. Two non mass spectrometric techniques have emerged to be most promising for high precision stable isotope analysis. The first technique is infrared laser absorption spectrometry applied to small water samples (10 µL) injected into evacuated chambers for the direct and parallel determination of @2H, @18O and @17O in the produced water moisture. In this method the intensities of individual isotope selective absorption lines caused by rotational-vibrational transitions in the water molecule are measured using a tuneable infrared laser system. The precision obtained so far is 0.7‰ for @2H, and 0.5‰ for both @18O and @17O. The second technique, called laser assisted isotope ratio analysis 13 12 13 (LARA), is suitable for @ C analysis of CO2 samples using two fixed frequency CO2 and CO2 lasers by measurement of the electrical response of a gas discharge induced by the laser optogalvanic effect. This technique finally measures an electrical discharge signal being proportional to the concentration of the isotopic species measured. The precision obtained so far is better than 1‰ for @13C and about 0.5‰ for @18O. The non mass spectrometric methods share the advantage of avoiding isobaric corrections that are inherent in mass spectrometric measurement. Due to the optical character of the measurements, they can be used for the parallel measurement of several samples and standards at the same time, limited ultimately only by space and budget considerations for the installation of multiple measurement chambers. The infrared laser absorption method provides means for the simultaneous measurement of all stable isotope ratios directly from one water sample without any sample preparation effort, but requires expensive laser equipment; costs which could be minimized only by the development of special diode lasers tuneable in the near infrared spectrum. The LARA method is a relatively cheap and robust method for direct CO2 analysis in gas mixtures with 5% CO2 in N2, but of course needs a suitable conversion of the sample material into CO2 gas as in the case of mass spectrometric methods. Further research is currently carried out for the measurement of other isotopic ratios such as @18O with the LARA method. The development of similar systems for @17O and @2H analysis seems possible. In view of their demonstrated usefulness and identifiable avenues for improvement, there is likely a promising future for these techniques, which in some cases could replace mass spectrometry by simpler and more robust alternatives. Commercial interest in those techniques will be crucial for their further development. For now, the majority of stable isotope ratio determinations are still performed by mass spectrometry. The on-line or continuous flow technique already accounts for a majority
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