The adsorption method for heavy metal removal from wastewater is focused because of its simplicity and high versatility, and sulfur-impregnated carbonaceous adsorbent is expected as heavy metal adsorbent with high performance at low cost. In this study, sulfur-impregnated carbonaceous filter for removing heavy metals were prepared by pyrolysis of cotton immersed in sulfur solution, K 2 S, Na 2 S and NaHS, and the adsorption behavior of nickel was investigated. A nickel adsorption experiment was carried out using a syringe. The sulfur-immersed carbonaceous filter was prepared from cotton via pyrolysis at 400 °C for 1 h after immersing to sulfur solution for 12 h. In the experiment, a syringe which filled with 1 g of the obtained filter and glass wool was used, and a nickel solution was passed through the syringe. The filter with nickel adsorption can be prepared using all sulfur solutions, especially the product prepared by using Na 2 S has higher adsorption ability than the products using K 2 S and NaHS. The product obtained using over 0.4 M K 2 S solution was effective for nickel adsorption. The equilibrium data of nickel adsorption on the product using 1 M K 2 S was found to Langmuir isotherm model better than Freundlich, and the calculated maximum adsorption capacity is 0.215 mmol/g.