A laboratory comparison of analytical methods used for isocyanates

作者:Ceballos Diana M; Whittaker Stephen G; Yost Michael G*; Dills Russell L; Bello Dhimiter; Thomasen Jennifer M; Nylander French Leena A; Reeb Whitaker Carolyn K; Peters Phillip M; Weiland Elisa C; Suydam Wallace W
来源:Analytical Methods, 2011, 3(11): 2478-2487.
DOI:10.1039/c1ay05225j

摘要

Monomeric and oligomeric 1,6-hexamethylene diisocyanate (HDI) and isophorone diisocyanate (IPDI) are components of catalyst hardeners in two-part polyurethane coating systems. Exposure to these isocyanates in the collision repair industry has been associated with increased risk for work-related asthma; however their quantitation remains a challenging task. Four analytical methods were compared: modified version of the National Institute for Occupational Safety and Health Method 5525 (NIOSH); liquid chromatography and mass spectrometry (LC/MS) using 1-(2-methoxyphenyl)piperazine (MPP) as the derivatizing reagent; modified version of the Occupational Health and Safety Administration Method 42/PV2034 (OSHA); and modified version of the Omega ISO-CHEK (R) Method (WA-DOSH). Five levels of a widely used clear coat hardener were spiked onto sampling media. A reference value was calculated by using a hardener NCO titration and manufacturer composition data. Intra-and inter-method variability was determined. All methods measuring NCO-HDI monomer, NCO-IPDI monomer, NCO-IPDI oligomers, and total NCO mass (except OSHA method) compared well against the reference values (slopes >= 0.816, R(2) > 0.90). The NCO-HDI oligomer results for the NIOSH method compared well with the reference values (slope - 1.161, standard error - 0.046 and R(2) - 0.98, p < 0.001) while WA-DOSH were above (slope = 2.293, standard error = 0.055 and R(2) = 0.99, p < 0.001) and LC/MS were below (slope = 0.264, standard error = 0.011 and R(2) = 0.98, p < 0.001) the reference values. The principal challenges associated with comparing methods were: 1) the reporting metrics were not always directly comparable and 2) not all methods reported all isocyanate species of interest. Although this present study provided valuable information, a more extensive investigation is required in order to critically evaluate these methodological differences.

  • 出版日期2011-11