During the acquisition of data for the final data sets, all data for each column were measured within 5 days using an autosampler. RT were extracted from chromatograms using GCMSsolution GCMS Postrun Analysis (version 4.50) software. The RT was recorded at the top of the peak. The fraction of compounds (randomly selected) was remeasured after ~15 days after the end of the first acquisition in order to estimate the reproducibility and measurement error. The mean deviations (the average of deviations for multiple compounds) between the results of the first and later measurements are 0.066, 0.026, and 0.030 min. for the Bis4MPyC6, Bis2MPyC9, and Hex4MPy columns, respectively. The mean percentage deviations are 0.53%, 0.44%, and 0.67% for these three columns, respectively. The Bis4MPyC6 column is the longest and the most polar, so the absolute values of the RT are the largest for this column. Due to this, the absolute mean deviation is the largest, while the relative deviation is not.