Ferrocenoyl piperazide as derivatizing agent for the analysis of isocyanates and related compounds using liquid chromatography/electrochemistry/mass spectrometry (LC/EC/MS)

B. Seiwert, H. Henneken, U. Karst

Research output: Contribution to journalArticleAcademicpeer-review

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Abstract

Ferrocenoyl piperazide is introduced as a new pre-column derivatizing agent for the analysis of various isocyanates in air samples using reversed-phase liquid chromatographic separation, electrochemical oxidation/ionization, and mass spectrometry. The nonpolar derivatives can be separated well using a phenyl-modified stationary phase and a formic acid/ammonium formate buffer of pH 3, which yields excellent separations, especially for one problematic group of isocyanates consisting of 2,4- and 2,6-toluylenediisocyanate (2,4- and 2,6-TDI) and hexamethylenediisocyanate (HDI). Electrochemical oxidation at low potentials (0.5 V versus Pd/H2) leads to formation of charged products, which are nebulized in a commercial atmospheric pressure chemical ionization (APCI) source, with the corona discharge operated only at low voltage. Limits of detection between 6 and 20 nmol/L are obtained for the isocyanate derivatives, and calibration is linear over at least two decades of concentration. The method is applied for the analysis of air after thermal degradation of a polyurethane foam, and it is demonstrated that it is suitable as well for the analysis of carboxylic acid chlorides and of isothiocyanates.
Original languageEnglish
Pages (from-to)1727-1736
Number of pages10
JournalJournal of the American Society for Mass Spectrometry
Volume15
Issue number12
DOIs
Publication statusPublished - 2004

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