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Opportunities for the beneficial re-use of biosolids are limited by nuisance odour emissions. Volatile organic compounds (VOCs) from anaerobically stabilised biosolids were measured to identify compounds that could contribute to the overall odour character of nuisance emissions. Flux hood sampling and chemical analysis were used to identify VOCs emitted from biosolids as they were stored in ambient conditions. Compounds emitted varied as the biosolid cakes were stored for a period of 50 days. VOCs detected in the biosolids are likely to occur from catchment sources as well as abiotic and biotic generation in the wastewater processing and the biosolids as they are stored. Odour activity values (OAVs) were used to compare odorants. Trimethylamine was the only VOC detected that exceeded the sulfur compounds in terms of OAVs. Other compounds such as limonene, ethyl methyl benzene and acetic acid were detected at concentrations exceeding their olfactory detection limits, however at lower OAVs than sulfur compounds.