Determination of 1,3-butadiene down to sub-part-per-million levels in air by collection on charcoal and high-resolution gas chromatography.
Lunsford-RA; Gagnon-YT; Palassis-J; Fajen-JM; Roberts-DR; Eller-PM
Appl Occup Environ Hyg 1990 May; 5(5):310-320
The development and validation of NIOSH Method 1024 for determining 1,3-butadiene (106990) (BUT) in air was discussed. The method involved collecting air samples on tandem 400 and 200 milligram coconut shell charcoal sampling tubes, desorbing the tubes with dichloromethane, and analyzing desorbates by high resolution capillary gas chromatography. Recovery and desorption efficiency tests utilizing samplers spiked with 4.64 to 463 micrograms (microg) BUT and air volumes of 0 to 32.4 liters (l) were conducted. Recoveries ranged from 80 to 129.4% and desorption efficiencies from 91.2 to 103.8%. The optimum sample volume was 25l. The overall mean relative standard deviation was 0.033. The accuracy was within +/-25%. In stability tests, storage at -4 degrees resulted in no loss of analyte. Storage at room temperature resulted in a BUT loss of 1.50% per day. The detection limit determined by analyzing blind quality control samples during an industrial hygiene survey of five BUT monomer production factories was 25microg per sample. This was equivalent to 0.82 parts per million in a 25l air sample. The detection limit was dependent on the desorption efficiency. It was found necessary during the field study to fit a back flushable fused silica precolumn to the chromatographic column to protect it against high boiling or polar contaminants. Experiments leading to optimization of the sampling and desorption procedure and problems encountered during field use were discussed.
NIOSH-Author; Gas-chromatography; Air-sampling; Adsorbents; Industrial-hygiene; Solvent-extraction; Hydrocarbons; Butadienes
DPSE; EID; DSHEFS
Applied Occupational and Environmental Hygiene