The original thrust of this effort was towards improving ion chromatographic methods to detect all major ions. This technique was developed for the determination of chloride, nitrite, sulfite, phosphate, sulfate, nitrate, thiosulfate, and thiocyanate in a single run. A qualitative indication of total organic acids is also obtained. Sodium, ammoniacal-N, and K were determined separately by ion chromatography. Because the chloride peak occurred in a crowded portion of the ion chromatogram, an independent method was developed for chloride involving a digestion and titration. Measurements for pH and electrical conductivity were then made in order to check the accuracy of these individual measurements. However, it soon became clear that modified procedures for these measurements had to be developed in order to compensate for the high ionic strength of the synfuel samples. A computer program was developed to check the accuracy and completeness of the analyses by calculating ion balances, electrical conductivity, and total sulfur based on the individual determinations. Application of this program to a set of synfuel wastewaters indicated an acceptable agreement for most samples. However, it also became apparent that for some waters a major category of negative ions was missing, and for other samples the individual sulfur components did not account for the total sulfur found. For this reason additional efforts were directed towards determining the missing components. A gas chromatographic procedure involving a bonded-phase, carbowax capillary column was developed for the light organic acids. Efforts to develop a practical method for polysulfides, which were suspected as the missing sulfur component, were largely unsuccessful. 33 references, 14 figures, 12 tables.