We intended to make the activated carbon fibers which could separate, remove and recover the volatile organic compounds of benzene, toluene, acetone and methanol. Changing activation temperature and time, large specific surface area and narrow pore distribution could be obtained. The activated carbon fibers have large adsorption capacity and selectivility for those organic compounds. We characterized the adsorption capability of the activated carbon fibers for benzene, toluene, acetone and methanol by BET specific surface area and pore size and micropore volume measurements. In the result of activation, the maximum value of BET specific surface area of the fibers was $1100m^2$/g at $800^{circ}C$ for 60 minutes and $K_2$O was reduced actively in this condition. Their average pore size was 5.8~5.9$AA$. The activated carbon fibers prepared in this work had high adsorption rate to saturation and the selectibility for the above organic compounds. The adsorbed amount of acetone and methanol(diameter of$ 4.3AA$ and $4.4AA$ respectively) which are smaller than micropore diameter in size was 43~49%, which was larger value than benzene and toluene(in the same diameter as $5.9AA$).