Gas chromatography, coupled with controlled temperature pyrolysis, provides a rapid and significant method for the determination of acrylic acid content in acrylic copolymers synthesized from unsaturated monomers and acrylic acid. After pyrolysis, the resulting pyrolyzates are fed directly into a gas chromatograph by means of a gas sampling valve. We have found that direct probe pyrolysis at high temperatures may be used to determine the presence of acrylic acid. During the pyrolysis, among other things, the formation of water was observed and practically used for determination of acrylic acid in the polymer backbone in synthesized and commercial acrylic polymers containing carboxylic groups.