Volatile organic sulfur compounds (VOSCs) are important sources of unpleasant odor in wastewater systems. However, the study of VOSCs is usually hindered by their complicated measurement method and highly reactive nature. In this work, a static headspace method utilising gas chromatography (GC) with a sulfur chemiluminescence detector (SCD) was developed to quantitatively analyze VOSCs in wastewater matrices. The method has low detection limits and requires no pre-concentration treatment. Three typical VOSCs, namely methanethiol (MT), dimethyl sulfide (DMS) and dimethyl disulfide (DMDS), were chosen as examples for this study. The calibration curves of all three compounds covering a wide range from 0.5 ppb to 500 ppb showed good linearity (R(2) > 0.999). The method detection limits (MDL) were 0.08, 0.12 and 0.21 ppb for MT, DMS and DMDS, respectively. The reproducibility (relative standard deviation) was approximately 2%. The recovery ratio of MT, DMS and DMDS in spiked wastewater samples were 83 ± 4%, 103 ± 4% and 102 ± 3%, respectively. Sample preservation tests showed that VOSCs in wastewater samples could be preserved in vials without headspace under acidified conditions (pH ∼1.1) for at least 24 h without significant changes (<1.8 ppb). The analysis of real wastewater samples from both a laboratory-scale sewer system and a full-scale sewer pipe demonstrated the suitability of this method for routine wastewater VOSC measurement.
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