A recently published method for measurement of hydrolysis rate constants for volatile organic compounds in aqueous samples was adopted for use in the laboratory. In applying the method, the authors developed the capability to make the zero-headspace reaction bulbs and used them to measure the hydrolysis rate constant for 1,1,1-trichloroethane. After establishing and mastering the critical points of the technique, they were able to determine an acceptable neutral hydrolysis rate constant (kn=7.98 E-2, 115 C) that was within 17% of the value calculated using the Arrhenius parameters of Jeffers' method. A detailed description of their experiences while learning this technique and becoming proficient in its use is provided in the belief that the experience would benefit other analytical chemists. (Copyright (c) Marcel Dekker, Inc., 1991.)