Analytical reference materials. Part V. Development of a sediment reference material for chlorobenzenes and hexachlorobutadiene

Abstract

The development of the first lake sediment reference material for the determination of chlorobenzenes and hexachlorobutadiene is described. Approximately 500 kg of lake sediment were collected, freeze-dried, crushed, sieved and blended before 5000 sub-samples were bottled and stored at 4 °C in the dark. Sub-samples were extracted using a Soxhlet apparatus, cleaned with Florisil and analysed by gas chromatography using both OV-1 and Carbowax 20M capillary columns interfaced to either an electron-capture or a mass-selective detector. Reference concentrations for six chlorobenzenes and hexachlorobutadiene were generated and no sign of loss or degradation for those components in the reference material was observed after 4 years of cold storage. This sample is suitable for long-term in-house or inter-laboratory quality assurance applications.