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Carbon-isotopic analysis of dissolved acetateHeating of dried, acetate-containing solids together with oxalic acid dihydrate conveniently releases acetic acid for purification by gas chromatography. For determination of the carbon-isotopic composition of total acetate, the acetate-containing zone of the chromatographic effluent can be routed directly to a combustion furnace coupled to a vacuum system allowing recovery, purification, and packaging of CO2 for mass-spectrometric analysis. For analysis of methyl carbon, acetic acid can be cryogenically trapped from the chromatographic effluent, then transferred to a tube containing excess NaOH. The tube is evacuated, sealed, and heated to 500 degrees C to produce methane by pyrolysis of sodium acetate. Subsequent combustion of the methane allows determination of the 13C content at the methyl position in the parent acetate. With typical blanks, the standard deviation of single analyses is less than 0.4% for acetate samples larger than 5 micromoles. A full treatment of uncertainties is outlined.
Document ID
20040089981
Acquisition Source
Legacy CDMS
Document Type
Reprint (Version printed in journal)
External Source(s)
Authors
Gelwicks, J. T.
(Inc. Rahway, NJ 07065-0904, United States)
Hayes, J. M.
Date Acquired
August 21, 2013
Publication Date
January 1, 1990
Publication Information
Publication: Analytical chemistry
Volume: 62
ISSN: 0003-2700
Subject Category
Exobiology
Funding Number(s)
CONTRACT_GRANT: NGR15003-118
Distribution Limits
Public
Copyright
Other
Keywords
Non-NASA Center
NASA Discipline Number 52-30
NASA Discipline Exobiology
NASA Program Exobiology

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