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We describe a simple, sensitive, and robust method for sulfur isotope ratio (S/S) analysis of ppm-level organic sulfur compounds (OSCs) in the presence of percent-level HS. The method uses a gas chromatograph (GC) coupled with a multicollector inductively coupled plasma mass spectrometer (MC-ICPMS). The GC, equipped with a gas inlet and a valve that transfers the HS to a thermal conductivity detector (TCD), enables a precise heart cut and prevents the saturation of the MC-ICPMS. The sensitivity and accuracy of the method are better than 0.3‰ for OSCs at a concentration of 25 pmol or 1.4 ppm, and better than 0.5‰ for concentrations ≥0.7 ppm of OSCs. An order of magnitude increase in sensitivity, with no effect on accuracy, can be achieved if the loop volume (0.5 mL) is changed to 5 mL. High concentrations of methane (95% v/v) and/or HS (20% v/v) had no effect (within 0.5‰) on the precision and accuracy of the gas sample containing 2 ppm of OSCs after heart cut. The applicability and robustness of this method are demonstrated on a gas sample (10% v/v HS) that was produced by pyrolysis of sulfur-rich kerogen. The results show good precision and reveal sulfur isotope variability between individual OSCs that may represent key processes during formation and degradation of OSCs.

An experimental study has been performed to determine the factors affecting the stability of hydrogen sulfide calibration mixtures at concentrations below 1 ppm. Quantitative data was obtained that illustrates that material selection and surface treatment are major factors affecting the shelf life of low concentration reactive gas mixtures. With the proper material selection and surface treatment, hydrogen sulfide and carbonyl sulfide standard mixtures on the order of 50-100 ppb can be maintained for at least 18 months.

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