The fundamental properties of the direct injection method in the analysis of gaseous reduced sulfur by gas chromatography with a pulsed flame photometric detector

Abstract

In this study, the fundamental aspects of gas chromatography with a pulsed flame photometric detector were investigated through the calibration of gaseous reduced sulfur compounds based on the direct injection method. Gaseous standards of five reduced sulfur compounds (hydrogen sulfide, methane thiol, dimethyl sulfide, carbon disulfide, and dimethyl disulfide) were calibrated as a function of injection volume and concentration level. The results were evaluated by means of two contrasting calibration approaches: fixed standard concentration method (variable volumetric injection of standard gases prepared at a given concentration) and fixed standard volume method (injection of multiple standards with varying concentrations at a given volume). The optimum detection limit values of reduced sulfur compounds, when estimated at 100 μL of injection volume, ranged from 2.37 pg (carbon disulfide) to 4.89 pg (dimethyl sulfide). Although these detection limit values improved gradually with decreasing injection volume, the minimum detectable concentration (e.g., in nmol mol −1 scale) remained constant due to a balance by the sample volume reduction. The linearity property of pulsed flame photometric detector also appeared to vary dynamically with changes in its sensitivity. According to this study, the performance of pulsed flame photometric detector, when tested by direct injection method, is highly reliable to precisely describe the behavior of reduced sulfur compounds above ∼20 nmol mol −1.