A personal exposure monitoring program has been carried out to field-test methodologies for sample collection and analysis. The basic study involved the collection of personal air, breath, and water samples. Quality assurance procedures were implemented during the sampling period and included exposing field controls and blanks and the collection of duplicates, some of which were analyzed by a reference laboratory. The analysis of the air/breath collections on Tenax GC® and water samples were performed by capillary column gas chromatography/mass spectrometry (GC/MS) and GC methods, respectively. Twenty-two volatile halogenated and aromatic compounds were selected as target compounds. Daily checks on instrument performance and calibration were performed, and precision quality control charts were maintained. The analysis of performance audit samples on Tenax GC was a major component of the quality assurance protocol. These results clearly show that background on the sampling devices adversely affect data quality and must be monitored closely.