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
SN - 1044-0305
VL - 15
SP - 1727
EP - 1736
JO - Journal of the American Society for Mass Spectrometry
JF - Journal of the American Society for Mass Spectrometry
IS - 12
ER -