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Please use this identifier to cite or link to this item: http://apo.ansto.gov.au/dspace/handle/10238/3589

Title: A first step toward small-mass AMS radiocarbon analysis at Nagoya University
Authors: Minami, M
Miyata, Y
Nakamura, T
Hua, Q
Keywords: Graphitization
Currents (beam)
Mass
Sem (microscopy)
Carbon 14
Preparation (sample)
Issue Date: 22-Mar-2010
Citation: Minami, M., Miyata, Y., Nakamura, T., Hua, Q., (2011). A first step toward small-mass AMS radiocarbon analysis at Nagoya University. 12th International Conference on Accelerator Mass Spectrometry (AMS 12), 20th - 25th March 2011. Museum of New Zealand: Te Papa Tongarewa, Wellington, New Zealand.
Abstract: We have started to establish a small-mass sample preparation system at Nagoya University. In the first step, NIST Ox-II standard samples <0.5 mgC, graphitized using our regular sample preparation protocol, were measured for 14C. The 14C/12C ratios of these small-mass samples were affected by the decrease in beam current intensity and incomplete graphitization especially for samples <0.3 mgC. In the second step, we have designed a compact graphitization system suitable for small-mass samples and compared its performance to that of our regular graphitization system. During the graphitization reaction following our regular protocol, by-product water vapor was incompletely trapped, which resulted in low graphite yield or no graphitization for samples of <0.5 mgC. Meanwhile graphite was successfully produced for samples of 0.2mgC using the new reactor. The SEM images of small-samples using the new reactor show spotted graphite covering the spherical iron particles. No or very little graphite was observed for the samples graphitized using our regular graphitization system. During the graphitization reaction using the sealed tube method, water vapor was incompletely trapped, which resulted in low graphite yield especially for samples of <0.5 mgC. Meanwhile graphite was successfully produced for samples of 0.2mgC using the new reactor. The cold trap at −80°C employed in the new graphitization system was effective in trapping water for small-mass samples. The combination of lower temperature for trapping water and a reduction in reactor volume delivered higher graphitization efficiency for small samples. We are now ready for 14C analysis of samples of around 0.2mgC. We also report an example of stepwise combustion of samples containing sulfur in a closed tube to produce graphite successfully. Copyright (c) 2010 AMS12
URI: http://apo.ansto.gov.au/dspace/handle/10238/3589
http://www.gns.cri.nz/ams12/
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