Abstract: To address the traceability issue in gas chromatography-mass spectrometry (GC-MS), standard substances are necessitated. A three-component mixed solution, comprising octafluoronaphthalene, benzophenone, and methyl stearate dissolved in isooctane, was meticulously prepared using the gravimetric method for the purpose of gas quality calibration. Analysis was carried out utilizing a gas chromatography equipped with a hydrogen flame ionization detector (GC-FID). Rigorous evaluation was conducted by employing F-tests and regression analysis to assess the homogeneity and stability of the prepared standard substances, as well as the associated uncertainty in the obtained results. Each component in the mixed standard substance yielded calibration values of 3.00 ng/μL with a relative expanded uncertainty U_rel of 3%, at a coverage factor (k) of 2. Comprehensive experimentation involving raw material analysis, preparation of standard materials, assessment of uniformity and stability, and comparison of quantitative values confirmed that the developed standard material fulfills the criteria for national secondary standard substances. Consequently, it has been officially accredited with a certificate number GBW (E) 130677, enabling its utilization in the calibration of GC-MS instruments, specifically for the repeatability testing of retention times.