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Testing sealed-tube Graphitization at the NERC Radiocarbon facility, east Kilbride

Published online by Cambridge University Press:  09 September 2019

Luz Maria Cisneros-Dozal*
Affiliation:
NERC Radiocarbon Facility, East Kilbride, G75 0QF, UK
Xiaomei Xu
Affiliation:
KCCAMS Laboratory, Department of Earth System Science, University of California, Irvine, CA, 92697, USA
Sheng Xu
Affiliation:
SUERC AMS Laboratory, East Kilbride, G75 0QF, UK Current address:Institute of Surface-Earth System Science, Tianjin University, Tianjin 300072, China
*
*Corresponding author. Email: malu.cisneros@glasgow.ac.uk.

Abstract

Graphitization of 0.5–1.5 mg C, and of smaller samples to a lesser extent, is routinely done at our Facility by reduction over zinc. The method yields low background, good accuracy but offers a limited throughput, requires dedicated equipment and considerable operator time. Sealed-tube graphitization is faster, easier and cost-efficient producing as many graphites as CO2 can be purified in one day with low background, good accuracy and precision, provided precise measurements of δ13C values can be attained by accelerator mass spectrometry (AMS) to correct for isotope fractionation (Xu et al. 2007). We tested sealed-tube graphitization on 0.1 to 1.0 mg C samples and found that while we were able to obtain low backgrounds of >57,000 ±1000 yr BP for ∼1.7 mg C and 41,230 ± 430 yr BP for ∼0.09 mg C (0.0008 ± 0.0001 and 0.0059 ± 0.0003 Fraction Modern, respectively), results were variable for sample sizes <0.5 mg C. Measurements of FIRI Belfast Cellulose and TIRI Barleymash showed 0.3–0.6% precision and 1% accuracy for most sample sizes. We found better results in our laboratory by introducing the following modifications: (1) shorter inner tube (2 cm long), (2) short flame-seal length (∼7–8 cm) and (3) keeping the inner tube with iron separate from the outer tube containing zinc and titanium hydride during cleaning.

Type
Conference Paper
Copyright
© 2019 by the Arizona Board of Regents on behalf of the University of Arizona 

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Footnotes

Selected Papers from the 23rd International Radiocarbon Conference, Trondheim, Norway, 17–22 June, 2018

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