The simultaneous separation of 13 kinds of organic solvents has been carried out with Hitachi model 163 gas chromatograph equipped with a flame ionization detector, using a stainless steel column (3 mm × 4) packed with 10% silicone gum SE 30 on chromosorb W 80-l00 mesh (AW, DMCS) and as a carrier gas, nitrogen gas of flow rate of 20ml/min. The satisfactory separation has been achieved only when the column temperature first was set at 80℃ and then increased at the temperature ratio of 10℃/min immediately after benzene peak appeared. The retention time was the smallest in methyl alcohol, followed by ethyl alcohol, acetone, methyl ethyl ketone, ethyl acetate, isobutyl alcohol, benzene, methyl iso-butyl ketone, iso-butyl acetate, toluene, n-butyl acetate, iso-amyl acetate, ethylene glycol monobutyl ether, in order of retention time.