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Improvements in Procedural Blanks at NOSAMS: Reflections of Improvements in Sample Preparation and Accelerator Operation

Published online by Cambridge University Press:  18 July 2016

A.P. McNichol ,
A. R. Gagnon ,
E. A. Osborne ,
D. L. Hutton ,
K.F. Von Reden  and
R. J. Schneider
A.P. McNichol
Affiliation:
National Ocean Sciences Accelerator Mass Spectrometer Facility, Department of Marine Geology and Geophysics, Woods Hole Oceanographic Institution, Woods Hole, Massachusetts 02543 USA
A. R. Gagnon
Affiliation:
National Ocean Sciences Accelerator Mass Spectrometer Facility, Department of Marine Geology and Geophysics, Woods Hole Oceanographic Institution, Woods Hole, Massachusetts 02543 USA
E. A. Osborne
Affiliation:
National Ocean Sciences Accelerator Mass Spectrometer Facility, Department of Marine Geology and Geophysics, Woods Hole Oceanographic Institution, Woods Hole, Massachusetts 02543 USA
D. L. Hutton
Affiliation:
National Ocean Sciences Accelerator Mass Spectrometer Facility, Department of Marine Geology and Geophysics, Woods Hole Oceanographic Institution, Woods Hole, Massachusetts 02543 USA
K.F. Von Reden
Affiliation:
National Ocean Sciences Accelerator Mass Spectrometer Facility, Department of Marine Geology and Geophysics, Woods Hole Oceanographic Institution, Woods Hole, Massachusetts 02543 USA
R. J. Schneider
Affiliation:
National Ocean Sciences Accelerator Mass Spectrometer Facility, Department of Marine Geology and Geophysics, Woods Hole Oceanographic Institution, Woods Hole, Massachusetts 02543 USA
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Abstract

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During the four years the Sample Preparation Laboratory (SPL) at the National Ocean Sciences Accelerator Mass Spectrometer (NOSAMS) Facilty has been in operation we have accumulated much data from which we can assess our progress. We evaluate our procedural blanks here and describe modifications in our procedures that have improved our analyses of older samples. In the SPL, we convert three distinct types of samples—seawater, CaCO3 and organic carbon—to CO2 prior to preparing graphite for the accelerator and have distinct procedural blanks for each procedure. Dissolved inorganic carbon (∑CO2) is extracted from acidified seawater samples by sparging with a nitrogen carrier gas. We routinely analyze “line blanks” by processing CO2 from a 14C-dead source through the entire stripping procedure. Our hydrolysis blank, IAEA C-1, is prepared by acidifying in vacuo with 100% H3PO4 at 60° overnight, identical to our sample preparation. We use a dead graphite, NBS-21, or a commercially available carbon powder for our organic combustion blank; organic samples are combusted at 850° for 5 h using CuO to provide the oxidant. Analysis of our water stripping data suggests that one step in the procedure contributes the major portion of the line blank. At present, the contribution from the line blank has no effect on our seawater analyses (fraction modern (fm) between 0.7 and 1.2). Our hydrolysis blanks can have an fm value as low as 0.0006, but are more routinely between 0.0020 and 0.0025. The fm of our best organic combustion blanks is higher than those routinely achieved in other laboratories and we are currently altering our methods to reduce it.

Type
V. Advances in Measurement Techniques
Information
Radiocarbon , Volume 37 , Issue 2 , 1995 , pp. 683 - 691
Copyright
Copyright © the Department of Geosciences, The University of Arizona 

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