An experiment for the identification of synthetic polymers and copolymers by analytical pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) was developed and performed in the polymer analysis courses for third-year undergraduate students of chemistry with material sciences, and for first-year postgraduate students of polymer sciences. In order to illustrate this analytical technique, polystyrene (PS) and poly(acrylonitrile-co-1,3-butadiene-co-styrene) (ABS) were selected for identification. The students were able to complete this experiment in a single 6 h (a 45 min) or in two 3 h (a 45 min) laboratory sessions. The success rate in the determining of PS was 100%. Because the task of identifying ABS is more demanding, the success rate was about 80-90%. Successful completion of the laboratory experiments and a laboratory report are required of students to obtain a permit for the examination in the polymer analysis course.