An effluent gas detection (EGD) system by programmed temperature gas chromatography had been developed for measuring the micro contents of thermovolatile and volatile thermodecomposition components evolved from the liquid and solid thin films，fibers，powders etc，during the heating of cited materials. These micro contents Were difficult to measure by the conventional methods of thermal analysis (Such as TG，DTG and DTA). The EGD data of evolved gases from the powdered sample of CuSO₄?5H₂O and the film samples of hydroxy terminated polybutadiene(HTPB) and dibutyl phthatate(DBP)，measured by EGD system were compared with the correspondent data obtained from TG-DTG-DTA technique. The anodic oxidation aluminum foil in boric acid bath，carbon fibre and silicon carbide fibre Were also measured by cited EGD system. The advantages and procedure Were described.