Abstract: Fugitive emissions of benzene series compounds and total hydrocarbons pose irreversible harm to the ecological environment and human health. The rapid and accurate analysis of these compounds has long been a research focus in ambient air monitoring. A quick method for the analysis of total hydrocarbons, methane, benzene, toluene, ethylbenzene, p-xylene, m-xylene, o-xylene, and styrene was developed using a multi-dimensional gas chromatograph with dual FID detectors. The results show that the target components can be accurately analyzed within 12 minutes with a single injection, and the components exhibit good linearity and repeatability across the measurement range. This method demonstrates excellent detection limits, with accuracy ranging from −7.7% to 0.2%. The method can be applied for on-line calibration of analytical instruments in various spatiotemporal scenarios, showing potential application value in field mobile monitoring of ambient air.