A high-speed gas chromatograph coupled with a high-speed time-of-flight mass spectrometer was used to gain a six-fold increase in overall rate of analytical throughput for analysis of EPA Method TO-14 target compounds. One hundred mass spectra per second, ranging from 35 to 270 mass units, were collected. Sing.'e ion chromatograms were searched at appropriate retention times for chromatographic peaks, which were integrated. Thirty-eight of the forty-one TO-14 target compounds were calibrated using standards at five concentrations from 2.5 to 40 ppb. Four grab samples of ambient air were collected at four different locations at an automobile repair facility, and two grab samples were collected less than one minute apart at a site near a chemical plant, just before and just after passage of three large diesel trucks. All samples were analyzed on the same day they were collected.