A multi-instrument approach has been applied to the efficient identification of polymers in an upper-division undergraduate instrumental analysis laboratory course. Attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR) is used in conjunction with differential scanning calorimetry (DSC) to identify 18 polymer samples and to determine whether polyethylene samples are high density or low density and whether nylon samples are composed of nylon-6 or nylon-6,6. This experiment introduces students to the use of two different instruments to qualitatively analyze several polymers in an efficient manner.