Toluene adsorption characteristics in the adsorption bed packed with activated carbon fiber (ACF) were studied. Experimental apparatus is composed of VOC generation equipment, adsorption bed, and analytical instrument. Breakthrough characteristics were investigated with length of the adsorption bed which consisted of 3 or 5 sheets of the ACF and flow rate when toluene concentration are 400 ppm and 800 ppm respectively. When mass transfer zone (MTZ) comes out of the adsorption bed, toluene concentration is increased sharply and reached plateau region by saturation. Experimental results are compared with semi-empirical gas adsorption model proposed by Yoon and Nelson. In order to investigate the movement of the MTZ with adsorption time in the adsorption bed packed with ACFs, weight increment of each ACF was measured with the location of ACF at each run. When the weight increment of ACF by toluene adsorption which located at the exit of the bed reaches about 20%, toluene started to be detected.