Anodic alumina (Al2O3) and titania (TiO2) nanoporous oxide membranes are among the most widely studied self-organized nanopore templates, formed by uniform and well aligned arrays of synthetized nanometric pores or tubes. Here, we perform a comparative study of the depth profiling analysis in self-ordered alumina and titania nanoporous membrane templates by means of the radiofrequency glow discharge coupled to optical emission spectrometry (rf-GD-OES) technique. The densely packed columnar arrays of hexagonally self-ordered nanoporous alumina membranes investigated, with an average inner pore diameter of 35 nm and 105 nm interspacing, give an uniform thickness pore length about more than 5 µm, depending on the anodization time. Meanwhile, the analysis of the anodized titania nanotubes, with an average inner pore diameter of 100 nm and 40 nm wall thickness, shown to be about 300 nm in length. Each type of membranes were also studied in both cases, when the nanopores were empty and after filling with electrodeposited Ni. The direct analysis by rf-GD-OES reveals the ability of this technique to control the quality of these so synthesized nanocomposites formed by electrodeposited Ni nanowires into the alumina and titania nanoporous templates. (© 2006 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim)