The Master Analytical Scheme (MAS) for Organic Compounds in Water provides for analysis of purgeable and extractable, as well as neutral and ionic-water-soluble, organics in surface and drinking water and in leachates and various effluents. This report describes experiments in the development of the scheme; the MAS protocols are presented in Master Analytical Scheme for Organic Compounds in Water, and the state-of-the-art in the analytical methodology is reviewed through December 1981 in Literature Review for the Development of the Master Analytical Scheme for Organic Compounds in Water. The protocols report stands alone as the handbook for implementation. As part of the experimental development, existing techniques were compared to identify optimal methods for recovery of each class of organic compound in water, the applicability of new techniques was investigated, and questions necessary to the development of the scheme were answered. In addition, the viability of the analytical protocol was tested by applying it to a variety of water types and chemical compounds. The MAS was designed to permit application of all protocols or just those for particular organic groups of interest. Recoveries were obtained for about 260 model compounds of a wide variety of chemical classes and physical properties dosed into representative samples of several types of water.