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Ultra-Small Graphitization Reactors for Ultra-Microscale 14C Analysis at the National Ocean Sciences Accelerator Mass Spectrometry (NOSAMS) Facility

Sunita R Shah Walter, Alan R Gagnon, Mark L Roberts, Ann P McNichol, Mary C Lardie Gaylord, Elizabeth Klein

Abstract


In response to the increasing demand for 14C analysis of samples containing less than 25 µg C, ultra-small graphitization reactors with an internal volume of ~0.8 mL were developed at NOSAMS. For samples containing 6 to 25 µg C, these reactors convert CO2 to graphitic carbon in approximately 30 min. Although we continue to refine reaction conditions to improve yield, the reactors produce graphite targets that are successfully measured by AMS. Graphite targets produced with the ultra-small reactors are measured by using the Cs sputter source on the CFAMS instrument at NOSAMS where beam current was proportional to sample mass. We investigated the contribution of blank carbon from the ultra-small reactors and estimate it to be 0.3 ± 0.1 µg C with an Fm value of 0.43 ± 0.3. We also describe equations for blank correction and propagation of error associated with this correction. With a few exceptions for samples in the range of 6 to 7 µg C, we show that corrected Fm values agree with expected Fm values within uncertainty for samples containing 6–100 µg C.

DOI: 10.2458/azu_rc.57.18118


Keywords


ultra-microscale; carbon dioxide; graphite; accelerator mass spectroscopy; methods; sample preparation

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