Effects of sorbent materials on the cryofocusing analysis of gaseous reduced sulphur compounds

Abstract

The relative performance of different sorbent materials employed in the cryofocusing (e.g. in cold trap (CT) unit) stage was investigated at sub-ambient temperature by the thermal desorption (TD)–gas chromatography (GC)–pulsed flame photometric detector. To this end, the TD-based calibration of five reduced sulphur compounds (RSC: H ₂S, CH ₃SH, CS ₂, DMS and DMDS) and SO ₂ was carried out via the Peltier cooling system with five types of sorbent combinations such as two single-bed (Tenax TA and Silica gel) plus three multibed types (a combination of either two from the following three sorbents: Tenax TA, Silica gel and Carbopack B). Relative performance of each of all five CT options, if evaluated in terms of response factors for each compound, demonstrated that each CT composition acts as an important criterion to distinguish detection properties between light and heavy sulphur species. Although the relative response of H ₂S and CH ₃SH was systematically distinguishable between the CT types, that of SO ₂ was the most complicated to interpret. According to this study, the two CT types consisting of Carbopack B and Silica gel (CS-0.4 and CS-0.6) were the optimum choices for sulphur gas analysis in terms of basic QA parameters (sensitivity, reproducibility and linearity).

Keywords:

• reduced sulphur compound
• cold trap
• cryofocusing
• sorbent material
• analytical bias

Funding

This study was supported by a National Research Foundation of Korea (NRF) Grant funded by the Ministry of Education, Science and Technology (MEST) [No. 2009-0093848].