Applied occupational and environmental hygiene

Regulated workplace ketones and their interference in the PFBHA method for aldehydes.

PMID 11062931


Ketones are the major positive interferences for an aldehyde dynamic air sampler that consists of 200-mg 20 percent (w/w) O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine hydrochloride (PFBHA) on Tenax TA contained in a Pyrex tube 7-mm OD, 5-mm ID, and 70-mm in length, that utilizes a personal battery-powered pump at 10-50 mL/min. The ketone O-oxime derivatives were synthesized to allow absolute quantitation of O-oximes formed during sampling. Wet spiking allowed ketone recoveries to be found. Ketone vapors of known concentrations were generated statically in Tedlar gas bags. The O-oximes were desorbed with hexane, and an aliquot injected for gas chromatographic analysis on a nonpolar capillary column with mass spectrometric or electron capture detection. Gas phase recoveries up to 200 ppm-hour loadings exceeded 75 percent at 25 degrees C for chloroacetone, cyclohexanone, diacetone alcohol, diethyl ketone, dipropyl ketone, ethyl butyl ketone, methyl amyl ketone, methyl butyl ketone, 2-methylcyclohexanone, methyl ethyl ketone, methyl isobutyl ketone, methyl isopropyl ketone, and methyl propyl ketone. The recoveries for acetophenone, 2-chloroacetophenone, and ethyl amyl ketone were lower than 75 percent, and were caused by steric hindrance. Sampling for both aldehydes and ketones is recommended at 10 mL/min for TLV concentrations.