One of the main problems encountered in chemical analysis operations in the field is collecting sufficient sample from the source and transferring that sample to the measurement instrument for fast separation and identification. I have been involved in developing a field-portable gas chromatography-mass spectrometry (GC-MS) system with solid phase microextraction (SPME) sampling for point detection of chemical agents. The objective is to minimize the analysis time between sampling and detection of a potential chemical threat. SPME offers a convenient means for sampling gaseous and liquid samples, concentrating the analytes, and transferring the analytes to the injection port of a GC system for separation and identification. GC-MS has advantages of high efficiency, speed, and applicability for field analysis. Work was done to optimize the SPME fiber coating, capillary column dimensions, and GC operating conditions to provide complete analysis within 3 minutes. Since isothermal operation of the GC was a prior requirement, many components in the chromatograms were unresolved. Therefore, a peak de-convolution algorithm was applied to allow for identification and quantitation of poorly resolved and often completely obscured trace components. Details of the instrumentation and optimization of operating conditions are described in this thesis.