Synthesis of carbon fibers from cotton fiber by pyrolysis process has been described. Synthesis parameters are optimized using Taguchi optimization technique. Synthesized carbon fibers are used for studying hydrogen adsorption capacity using Seivert's apparatus. Transmission electron microscopy analysis and X-ray diffraction of carbon fiber from cotton suggested it to be very transparent type material possessing graphitic nature. Carbon synthesized from cotton fibers under the conditions predicted by Taguchi optimization methodology (no treatment of cotton fiber prior to pyrolysis, temperature of pyrolysis 800℃, Argon as carrier gas and paralyzing time for 2 h) exhibited 7.32 wt% hydrogen adsorption capacity.