Interference of the gas chromatography- mass spectrometry instrumental background on the determination of trace cyclic volatile methylsiloxanes and exclusion of it by delayed injection

Abstract

Cyclic volatile methylsiloxanes (cVMS) have been widely found in various types of environmental media and attracted increasing attention as new pollutants. However, there is still a great challenge in the accurate quantification of trace cVMS, due to their volatility, and the high background originating from GC/MS accessories and surroundings. In this work, the main sources of the high background were investigated in detail for octamethylcyclotetrasiloxane (D4), decmethylcyclopentasiloxane (D5) and dodecmethylcyclohexosiloxane (D6). Several effective measures were employed to minimize these backgrounds, including the delayed injection method to minimize the interference from the injection septum. Then, a GC–MS method was developed for the accurate determination of D4, D5 and D6, with a linear range of 2 - 200 μg/L. The coefficient of determination was 0.9982–0.9986, the limit of detection (LOD) was 0.40–0.52 μg/L, and the quantitative range was 1.88–190 μg/L. Good reproducibility and recovery were obtained, indicating the reliability of the established analytical method.