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

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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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formic acid
Electrochemistry
Isocyanates
Liquid chromatography
Liquid Chromatography
Mass spectrometry
Mass Spectrometry
Electrochemical oxidation
Air
Isothiocyanates
Derivatives
Atmospheric Pressure
Ion sources
Carboxylic Acids
Calibration
Atmospheric pressure
Ionization
Limit of Detection
Chlorides
Buffers

Cite this

@article{2f848f8643e64cde87293394a57123df,
title = "Ferrocenoyl piperazide as derivatizing agent for the analysis of isocyanates and related compounds using liquid chromatography/electrochemistry/mass spectrometry (LC/EC/MS)",
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.",
author = "B. Seiwert and H. Henneken and U. Karst",
year = "2004",
doi = "10.1016/j.jasms.2004.09.002",
language = "English",
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pages = "1727--1736",
journal = "Journal of the American Society for Mass Spectrometry",
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Ferrocenoyl piperazide as derivatizing agent for the analysis of isocyanates and related compounds using liquid chromatography/electrochemistry/mass spectrometry (LC/EC/MS). / Seiwert, B.; Henneken, H.; Karst, U.

In: Journal of the American Society for Mass Spectrometry, Vol. 15, No. 12, 2004, p. 1727-1736.

Research output: Contribution to journalArticleAcademicpeer-review

TY - JOUR

T1 - Ferrocenoyl piperazide as derivatizing agent for the analysis of isocyanates and related compounds using liquid chromatography/electrochemistry/mass spectrometry (LC/EC/MS)

AU - Seiwert, B.

AU - Henneken, H.

AU - Karst, U.

PY - 2004

Y1 - 2004

N2 - 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.

AB - 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.

U2 - 10.1016/j.jasms.2004.09.002

DO - 10.1016/j.jasms.2004.09.002

M3 - Article

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EP - 1736

JO - Journal of the American Society for Mass Spectrometry

JF - Journal of the American Society for Mass Spectrometry

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