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Ultra Small-Mass Graphitization by Sealed Tube Zinc Reduction Method for AMS 14C Measurements

Published online by Cambridge University Press:  09 February 2016

Xiaomei Xu ,
Pan Gao  and
Eric G Salamanca
Xiaomei Xu*
Affiliation:
Keck Carbon Cycle AMS Laboratory, Department of Earth System Science, University of California, Irvine, California 92697-3100, USA
Pan Gao
Affiliation:
Keck Carbon Cycle AMS Laboratory, Department of Earth System Science, University of California, Irvine, California 92697-3100, USA Department of Geography, Peking University, Beijing 100871, China
Eric G Salamanca
Affiliation:
Keck Carbon Cycle AMS Laboratory, Department of Earth System Science, University of California, Irvine, California 92697-3100, USA
*
2Corresponding author. Email: xxu@uci.edu.
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Abstract

A modified sealed tube Zn reduction method based on Khosh et al. (2010) has been developed to graphitize ultra small-mass samples ranging from 4–15 μg carbon (C) for accelerator mass spectrometry (AMS) radiocarbon measurements. In this method, the reagent TiH2 is removed from the previous method while the amounts of Zn and Fe powder remain the same. The volume of the sealed reactor is further reduced by ∼40% to ∼0.75 cm3 and the graphitization temperature is lowered to 450 °C. Graphite targets produced by this method generally yield 12C+1 currents of about 0.5 μA per 1 μg C, similar to the small mass (15–100 μg C) sealed tube Zn reduction method previously reported by Khosh et al. (2010) when measured on the same AMS system at KCCAMS, University of California, Irvine. Change of Fe powder to Sigma-Aldrich (400-mesh) has yielded further improved backgrounds over Fe powder of Alfa Aesar (325-mesh). Modern C background from combustion and graphitization is estimated to be 0.2–0.8 μg C, and dead-C background to be 0.1–0.4 μg C. The accuracy and precision of ultra small-mass samples prepared by this method are size and 14C content dependent, but is usually ±4–5% for the smallest sample size of ∼4–5 μg C with modern 14C content. AMS on-line δ13C measurement that allows for correction of both graphitization and machine-induced isotopic fractionation is the key for applying the sealed tube Zn reduction method to ultra small-mass sample graphitization.

Type
Articles
Information
Radiocarbon , Volume 55 , Issue 2: Proceedings of the 21st International Radiocarbon Conference (Part 1 of 2) , 2013 , pp. 608 - 616
Copyright
Copyright © 2013 by the Arizona Board of Regents on behalf of the University of Arizona 

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