This article deals with the development of methods for characterization and structural elucidation of N-methylmelamine resins as well as the cured material and composites made with these products. Resin characterization was achieved by ESI-ion trap MS and HPLC=PDA=MS n , which made the assignment of each species in the mixture possible. GPC as well as MS were used to follow the curing of the resin. Completely cured resins and composites are no more soluble in any solvent, and, therefore, the characterization was carried out with analytical pyrolysis and thermally assisted hydrolysis and methylation (THM) hyphenated to a GC=MS system.