This study assessed the analysis method for measuring volatile organic silicon compounds (namely as siloxanes) by usinggas chromatography with flame ionization detector. Calibration standard gas was made in a laboratory by using six volatileorganic silicons as model gas. Two different types of working gas were prepared to evaluate quality control in GC-FIDanalysis. Less than 0.2 RSD% of repeatability of retention time was observed in the analysis of calibration standard gas. Inthe linearity test, the highest coefficient of determination (R2) was found to be 0.997 for L2 among volatile organic siliconcompounds. This study demonstrated that quantification of volatile organic silicon compounds can be performed by usingGC-FID analysis with direct injection mode, and the GC calibration can be covered by the gas-phase standard method.