Determination of 1,3-Butadiene down to Sub-part-per-million Levels in Air by Collection on Charcoal and High-Resolution Gas Chromatography

Abstract

The need for a more sensitive method for the determination of 1,3-butadiene in air led to the development of NIOSH Method 1024, in which samples are collected on tandem 400- and 200-mg coconut-shell charcoal samplers; desorbed in dichloromethane; separated by gas chromatography on an aluminum oxide, porous-layer, open-tubular, fused silica capillary column fitted with a backflushable precolumn; and detected by flame ionization. This article reports the development of the method and an assessment of its performance based on laboratory evaluations and field use. A sample volume of 25 L is recommended for 1,3-butadiene concentrations up to 100 ppm. Samples stored in a freezer are stable; a loss of 1.5 percent per day occurs at ambient temperature. The lower quantitation limit, based on maintaining desorption efficiency ≥ 75 percent, is about 40 μg/sample. The estimated limit of detection is 0.2 μg/sample. The estimated precision of the total sampling and analytical method is 6 percent relative standard deviation. The accuracy is within ± 25 percent, based on the analysis of blind quality control samples ranging from 20 to 663 μg/sample.