Temperature programmed oxidation (TPO) coupled with in situ Raman spectroscopy has been used as an effective qualitative and quantitative analysis of raw and purified single-walled carbon nanotubes (SWNT) samples. The incorporation of Raman facilitates the identification of the nature of the oxidation peaks present in a TPO profile. Using different samples it was possible to evaluate the potential of the technique for quantifying different impurities in the SWNT samples as well as in SWNT-polymer composites. (C) 2003 Elsevier B.V. All rights reserved.