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), methanethiol (MeSH) and ethanethiol (EtSH) were orders of magnitude greater than their reported odour detection threshold, suggesting they would contribute to the odorous impact of the biosolids. The maximum H₂S value was equal to 59.9 × 10³ μg/m³ and was at least one magnitude higher compared to VOSCs, such as dimethyl disulfide (DMDS) (3.8×10³ μg/m³), DMS (4.53 × 10³ μg/m³), EtSH (2.83 × 10³ μg/m³) and MeSH (3.25 × 10³ μg/m³). Among the identified VSCs, H₂S was the prominent odorant in terms of the magnitude and the frequency of detection, both initially as well as throughout storage. However, DMTS should be considered as a high priority or key odorant due to its odour activity value (OAV) and frequency of detection (sensorially detected in more than 75% of samples, with an OAVs higher than 1).