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Vacuum Electrolysis Reactor Technique for Quantitation of 13-carbon Isotope Enrichment at the C1-position of Formic Acid and Acetic Acid

Vacuum Electrolysis Reactor Technique for Quantitation of 13-carbon Isotope Enrichment at the C1-position of Formic Acid and Acetic Acid

Michael May, John Kuo, C T Tan

Anal Chem. 2004 Sep 15;76(18):5313-8.

PMID: 15362887

Abstract:

A specialized vacuum electrolysis reactor was designed, constructed, and utilized for 13-carbon isotope analysis of formic acid-13C and acetic acid-13C, each highly enriched at the C1-position. This reusable reactor was equipped with two platinum wire electrodes, miniature stir bar, and sidearm reaction chamber. The associated technique developed for 13-carbon isotope analysis is based upon electrolytic generation of carbon dioxide into the preevacuated reactor followed by gas inlet mass spectrometry. It proved practical to degas and electrolyze 95% formic acid (without added electrolyte) due to adequate ionic conductivity. Formic acid-13C (nominally 99 at. % 13C) was measured by electrolytic CO2 generation to be 98.9 at. % 13C. To analyze various 13C-isotopic permutations of acetic acid, lithium and acid were separately added to reactor compartments, vacuum degassed, and stirred to produce an acidic solution. Thus, acetic acid-1-13C that was nominally 99 at. % 13C1 was determined by vacuum electrolysis to be 98.9 at. % 13C1. Further, acetic acid-2-13C that was isotope depleted at the C1-position (and known to be 99 at. % 13C at C2) gave 0.8 at. % 13C by mass spectrometry.

Chemicals Related in the Paper:

Catalog Number	Product Name	Structure	CAS Number	Price
AP1563797	Acetic acid-1-13C		1563-79-7	Price
AP1563800	Acetic acid-2-13C		1563-80-0	Price

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