Cationization of cotton fabrics was performed utilizing 3-chloro-2-hydroxypropyltrimethylammonium chloride (CHPTAC) in a cold pad batch procedure. Cotton fabrics were cationized at three levels 2.11, 4.23, and 8.45 % on weight of fabric of CHPTAC. Different neutralization schemes were employed on each cationization level to determine the effect of pH and process parameters on minimizing the amount of free trimethyl amine (TMA) in cationized cotton. Employing a solvent extraction method and gas chromatography/flame ionization detection (GC/FID), TMA was extracted and determined in parts per million (ppm) from the neutralized and sealed and aged cationized fabric. The results show that it is straightforward to quantify the concentration of TMA in cationized fabric and that the lowest levels of TMA in cationized cotton are achieved with by an initial warm rinse to remove excess sodium hydroxide, followed by acidification bath to achieve an acidic pH, and ending with a subsequent cold final rinse.