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Volatile sulfur compounds (VSCs) are important sources of unpleasant odours in biosolid emissions. However, the study of VSCs may be limited by complications in their gas phase measurements due to reactivity, transformations and varying reported odour detection thresholds. A range of methods were used to quantitatively analyse VSCs in wastewater biosolid emissions. VSCs were identified in aged biosolid emissions by gas chromatography (GC) with a sulfur chemiluminescence detector (SCD) and mass spectrometry coupled with olfactory detection port (MS/O). In total, 10 VSC's were identified with two volatile organic sulfur compounds (VOSCs), allyl methyl sulfide and methyl propyl sulfide being reported for the first time in biosolid emissions. The emission patterns of different VSCs varied as the biosolids aged. Initially, the median concentrations of H₂S, dimethyl sulfide (DMS), dimethyl trisulfide (DMTS …