A gas chromatographic (GC) method with flame ionization detection was developed to separate and quantitate p-chloroaniline (PCA) from other components in a chlorhexidine digluconate (CHG)-containing alcohol foam surgical scrub product. A simple sample preparation method was developed in which 1-butanol was used to dissolve the foam and precipitate the CHG, which otherwise would interfere with the GC analysis. The method was validated with respect to linear dynamic range, precision, accuracy, selectivity, limit of detection, and limit of quantitation.