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). Once the significant (or most significant) parameters have been determined in a prior screening experiment, another set of experiments must be designed in which a response surface objective experiment is performed to collect data for optimization. In this example case, surface response experiments were performed using a 3-level Box-Behnken design in which each statistically significant parameter (e.g. split ratio, carrier gas flow rate, oven temperature ramp rate, and capillary column film thickness) was assigned a “low”, “middle”, and “high” value. For these experiments, the three nonsignificant parameters, inlet temperature, injection volume, and auxiliary line temperature, were fixed at 200 °C, 2 μL, and 280 °C, respectively. The experiments were conducted in the same manner as described in the screening experiments section. The attached CSV files contain the Box-Behnken design (bbd.csv), the raw chromatographic data for the 25 distinct methods (Method #.csv), and the retention times (bb_rts.csv) for each iodinated standard.