A study was conducted to quantify volatiles generated from Indian mustard (Brassica juncea L. Czerniak) tissue incorporated into soils under controlled conditions. Mustard residues were incorporated into noncovered and covered soils that varied by texture, temperature, moisture, pH, or sterility (autoclaved or nonautoclaved). Sandy loam soil had 38% more allyl isothiocyanate (AITC) than clay loam soil. AITC concentration in 45 °C soil was 81% higher than in soil at 15 °C, and 56% higher in covered compared to noncovered treatments. The microbial catabolism of AITC was suggested by the result that AITC concentration in autoclaved soils was over three times that measured in nonautoclaved soils. The highest AITC level detected (1.71 μmol·L–1) occurred in the autoclaved covered soil. Several factors also influenced CO2 evolution. At 30 or 45 °C, CO2 concentration was at least 64% higher than at 15°C. The covered soil had over twice the CO2 found in the noncovered soil, and the nonautoclaved soil treatment yielded twice the CO2 measured in the autoclaved soil. There were no main effect differences among soil moisture, soil pH, and soil texture treatments for CO2 concentrations. This information could be helpful in defining ideal soil conditions for field scale experiments. Additionally, this study demonstrates a sampling technique for testing fumigation potential of biofumigation and solarization systems that may have the potential to replace methyl bromide.