Purge-and-Trap Gas Chromatography/Mass Spectrometry for the Analysis of Carboxylic Acids by Esterification.

EHARA Yasushi, SAKAMOTO Kazuhiko

doi:10.2116/analsci.16.283

Purge-and-Trap Gas Chromatography/Mass Spectrometry for the Analysis of Carboxylic Acids by Esterification.

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EHARA Yasushi

Criminal Investigation Laboratory, Saitama Prefectural Police Headquarters Department of Environmental Science and Human Engineering, Graduate School of Science and Engineering, Saitama University
SAKAMOTO Kazuhiko

Department of Environmental Science and Human Engineering, Graduate School of Science and Engineering, Saitama University

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This report describes the application of purge-and-trap (P&T) gas chromatography/mass spectrometry (GC/MS) to analyze carboxylic acids (CAs) using esterification. The optimum analytical conditions were determined based on the esterification recoveries using 10 mmol L^-1 of a CAs methanol solution. P&T sampling was carried out with a Curiepoint head-space sampler. The optimum instrumental conditions were: purging, 150°C for 10 min; trap temperature, -10°C; desorption, 358°C for 20 s. A comparison of pyrolysis (Py)-GC/MS, P&T-GC/MS, and solvent extraction-GC/MS was made based on conversions of the CAs into the corresponding CA methylesters. The merits of the P&T method for the other two methods were validated according to quantitative data, the coefficient of variation, and the lower limit of determination calculated from the standard deviation. As a result, we concluded that the P&T method is more useful than the pyrolysis and solvent extraction methods.