A capillary gas chromatographic procedure is described for the analysis of glutaraldehyde and phenol present in germicidal formulations. Glutaraldehyde breaks down over time following activation with alkaline-buffered media and products must be used within certain time limits. Some germicidal products contain either glutaraldehyde or phenol and these are also used in combination. It is necessary to have suitable methodology for determining the concentration of glutaraldehyde and phenol as a means of evaluating the effective levels of these active ingredients. Various analytical methods are described in the literature for the determination of either glutaraldehyde or phenol. Using capillary gas chromatography with a column for compounds of intermediate polarity, both ingredients can be assayed from a single determination.