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Studies on the Preparation of Small 14C Samples with an RGA and 13C-Enriched Material

Published online by Cambridge University Press:  18 July 2016

Jakob Liebl
Affiliation:
Vienna Environmental Research Accelerator (VERA), Faculty of Physics, Isotope Research, University of Vienna, Währinger Straße 17, A-1090 Vienna, Austria
Roswitha Avalos Ortiz
Affiliation:
Vienna Environmental Research Accelerator (VERA), Faculty of Physics, Isotope Research, University of Vienna, Währinger Straße 17, A-1090 Vienna, Austria
Robin Golser
Affiliation:
Vienna Environmental Research Accelerator (VERA), Faculty of Physics, Isotope Research, University of Vienna, Währinger Straße 17, A-1090 Vienna, Austria
Florian Handle
Affiliation:
Vienna Environmental Research Accelerator (VERA), Faculty of Physics, Isotope Research, University of Vienna, Währinger Straße 17, A-1090 Vienna, Austria
Walter Kutschera
Affiliation:
Vienna Environmental Research Accelerator (VERA), Faculty of Physics, Isotope Research, University of Vienna, Währinger Straße 17, A-1090 Vienna, Austria
Peter Steier*
Affiliation:
Vienna Environmental Research Accelerator (VERA), Faculty of Physics, Isotope Research, University of Vienna, Währinger Straße 17, A-1090 Vienna, Austria
Eva Maria Wild
Affiliation:
Vienna Environmental Research Accelerator (VERA), Faculty of Physics, Isotope Research, University of Vienna, Währinger Straße 17, A-1090 Vienna, Austria
*
Corresponding author. Email: peter.steier@univie.ac.at.
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Abstract

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The minimum size of radiocarbon samples for which reliable results can be obtained in an accelerator mass spectrometry (AMS) measurement is in many cases limited by carbon contamination introduced during sample preparation (i.e. all physical and chemical steps to which samples were subjected, starting from sampling). Efforts to reduce the sample size limit down to a few μg carbon require comprehensive systematic investigations to assess the amount of contamination and the process yields. We are introducing additional methods to speed up this process and to obtain more reliable results. A residual gas analyzer (RGA) is used to study combustion and graphitization reactions. We could optimize the reaction process at small CO2 pressures and identify detrimental side reactions. Knowing the composition of the residual gas in a graphitization process allows a reliable judgment on the completeness of the reaction. Further, we use isotopically enriched 13C (≥98% 13C) as a test material to determine contamination levels. This offers significant advantages: 1) The measurement of 12C/13C in CO2 is possible on-line with the RGA, which significantly reduces turnaround times compared to AMS measurements; 2) Both the reaction yield and the amount of contamination can be determined from a single test sample.

The first applications of isotopically enriched 13C and the RGA have revealed that our prototype setup has room for improvements via better hardware; however, significant improvements of our sample processing procedures were achieved, eventually arriving at an overall contamination level of 0.12 to 0.15 μg C during sample preparation (i.e. freeze-drying, combustion, and graphitization) of μg-sized samples in aqueous solution, with above 50% yield.

Type
Sample Preparation
Copyright
Copyright © 2010 by the Arizona Board of Regents on behalf of the University of Arizona 

References

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