The objective of this example case was to maximize peak height and minimize peak width of 11 iodinated standards analyzed using gas chromatography-mass spectrometry (GC-MS). Seven parameters (split ratio, carrier gas flow rate, inlet temperature, injection volume, auxiliary line temperature, oven temperature ramp rate, and capillary column film thickness) were chosen due to their known impact on GC−MS performance metrics (i.e., minimized peak width and maximized peak height) optimized in this study. To limit the number of experiments required for the surface response experiments, screening experiments were performed to determine the statistically significant parameters. A two-level fractional factorial design was created with 32 distinct observations (methods) with a resolution of 4 and a defining aliasing pattern of ABCF = CDEFG = I. The data was collected using an Agilent GC-MS (7890 GC, 7010C mass spectrometer, Agilent Technologies, Santa Clara, CA) operated in full scan mode. Chromatographic separation was performed using a Restek Rtx-1701 GC column (30 m × 0.25 mm ID; Restek Corporation, Bellefonte, PA). The source temperature was held at 230 °C and the quadrupoles were held at 150 °C. An emission current of 100 μA and ionization energy of 70 eV were used. The oven temperature program was held at 35 °C for 5 minutes and then increased at the chosen oven temperature ramp rate to 280 °C and held for 15 minutes. The attached CSV files contain the fractional factorial design (ffd.csv), the raw chromatographic data for the 32 distinct methods (TIC_Method_#.csv), and the retention times (rts.csv) for each iodinated standard.