Thermal gravimetric analysis (TGA) combining the use of digital microbalances, gas-chromatography and mass spectroscopy is demonstrated as a highly sensitive technique for the determination of thermal behaviour of polymeric materials obtained in very low quantities in laser-induced chemical processes. The article is a brief review on some authors' TGA studies of materials prepared by laser ablation of polymers, laser-induced chemical vapour deposition and laser back-side etching in the gas phase. The TGA-diagnosed materials are (i) chemical vapour-deposited N-containing polyoxocarbosilane and Fe/polyoxocarbosilane composites, (ii) crosslinked polymers ablatively deposited from pure and metal particles-loaded poly(vinyl acetate), poly(vinyl chloride-co-vinyl acetate) (PVACVC) and poly[oxy(tetramethyldisilane-1,2-diyl) (POTMD), and (iii) carbon/polyoxocarbosilane composites obtained through gas-phase etching process. (C) 2008 Elsevier B.V. All rights reserved.