The analysis of pesticide and PCB residues presents analytical challenges for a number of reasons. Considerable pressure for lower detection limits of these compounds prompts laboratories to seek methods that enable them to reproducibly attain results in the pg/L range. By combining a large volume splitless injection with full scan gas chromatography/ mass spectrometry, low level analysis can be accomplished with decreased sample preparation time. A large volume splitless injection technique was developed. This technique was then evaluated using standards containing pesticides and PCB's at concentrations ranging from 1.25-250 pg/L (1.25-250 ppb) in hexane.