JIS A 1901for Small chamber method has been established in 2003 for the precise measurement method of chemicals emission. JIS A 1902-2 for sampling and preparation of test specimens and testing condition of an adhesive using a glass plate has been revised in December 2006. However, this current method had the problem that it was different from using condition of an adhesive in actual construction. It has led to develop a new measurement method using a calcium silicate board (CSB) [1] for VOCs emissions from an adhesive. In this paper, three VOCs: toluene, xylene, and ethylbenzene emissions through the CSB have been measured by the cup method [2] and the small chamber method. The effective diffusion coefficient (De) of the CSB was measured by the cup method in some VOCs mixing conditions. De decreased in the conditions that toluene was included in mixtures. The mass changes per unit time (m) for mixtures were equal to the mean value of those for pure substances. VOCs emission rates from four kinds of adhesives: E (Epoxide resin adhesive for woody floor materials), U (Polyurethane resin adhesive for subfloors), S (Chloroprene rubber adhesive for wall and ceiling boards (using solvent)), and W (Ethylene vinyl acetate emulsion copolymerization adhesive) were measured by the small chamber method using CSB in the conditions added with three VOCs mixture, which ranged from 0.025%Wt to 0.25%Wt. VOCs emission rates of the first sampling day were the highest in all test periods and they decreased over time. Additionally, the more VOCs were added the higher emission rates were.