Optimized pressure-pulse splitless injection and electron-capture, negative ionization detection for the congener specific determination of compounds of technical toxaphene

Abstract

The goal of the study is the optimization of the congener specific determination of compounds of technical toxaphene (CTTs). For this reason GC/ECNI-MS and CTT standard mixtures are applied. The splitless injection is improved by pressure-pulse injection which yields significantly higher abundance of the CTTs than by the conventional constant flow injection technique. The abundance of low volatile CTTs like B9-1025 (Parlar #62) is increased by factor 3 or more. The pressure-pulse injection can easily be integrated in standard (constant flow splitless injection) methods without influencing the retention times and reproducibility. The GC oven program and the flow are optimized for the separation of CTTs on a non-polar CP-Sil 2 column. Problems caused by oxygen in the ion source are discussed.