Journal of Chromatography A 2006-11-17

Validation of a diffusive sampling method for airborne low-molecular isocyanates using 4-nitro-7-piperazinobenzo-2-oxa-1,3-diazole-impregnated filters and liquid chromatography-tandem mass spectrometry.

Hartmut Henneken, Heiko Hayen, Martin Vogel, Uwe Karst

Index: J. Chromatogr. A. 1134(1-2) , 112-21, (2006)

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Abstract

A diffusive sampling method for the determination of low-molecular isocyanates as their 4-nitro-7-piperazinobenzo-2-oxa-1,3-diazole (NBDPZ) derivatives using tandem mass spectrometry (MS/MS) after atmospheric pressure chemical ionisation (APCI) is presented. Isocyanic acid (ICA), methyl isocyanate (MIC), ethyl isocyanate (EIC) and phenyl isocyanate (PhIC) are collected on NBDPZ-impregnated polystyrene divinyl benzene (SDB) filter tapes. The method was validated for MIC, EIC and PhIC for concentrations between 0.5 and 50 ppb at relative humidity (RH) conditions from 10 up to 90%. Validation was carried out by active sampling using 1-(2-methoxyphenyl)piperazine (2-MP) as derivatising agent. Sampling periods applied were between 15 min and more than 8 h. The sampling rates were determined to be 21.0 mL/min for MIC with a relative standard deviation (RSD) of 9.0% for 184 samplers, 15.6 mL/min for EIC (RSD 11.6%; N = 154) and 11.5 mL/min for PhIC (RSD 8.4%; N = 87). The limits of quantification were 1.4 ppb for MIC and 1.3 ppb for EIC and PhIC applying 15 min sampling periods. Owing to high background signals, isocyanic acid could only be determined when it was present in concentrations in the high ppb range.