In this study, a simple process for fabricating a novel micromachined preconcentrator (mu PCT) and a gas chromatographic separation column (mu SC) for use in a micro gas chromatograph (mu GC) using one photomask is described. By electroless gold plating, a high-surface-area gold layer was deposited on the surface of channels inside the mu PCT and mu SC. For this process, (3-aminopropyl) trimethoxysilane (APTMS) was used as a promoter for attaching gold nanoparticles on a silicon substrate to create a seed layer. For this purpose, a gold sodium sulfite solution was used as reagent for depositing gold to form heating structures. The microchannels of the mu PCT and mu SC were coated with the adsorbent and stationary phase, Tenax-TA and polydimethylsiloxane (DB-1), respectively. mu PCTs were heated at temperatures greater than 280 degrees C under an applied electrical power of 24 W and a heating rate of 75 degrees C s(-1). Repeatable thermal heating responses for mu PCTs were achieved; good linearity (R-2 > 0.9997) was attained at three heating rates for the temperature programme for the mu SC (0.2, 0.5 and 1 C-circle s(-1)). The volatile organic compounds (VOCs) toluene and m-xylene were concentrated over the mu PCT by rapid thermal desorption (peak width of half height (PWHH) < 1.5 s); preconcentration factors for both VOCs are > 7900. The VOCs acetone, benzene, toluene, m-xylene and 1,3,5-trimethylbenzene were also separated on the mu SC as evidenced by their different retention times (47-184 s).