Procedures employing thiocyanate and dithiol complexes of molybdenum have been developed for the determination of the metal in the presence of large quantities of ferric iron. The procedures are developed for field application and it is possible to complete 200 analyses per day with laboratory accuracy. Use is made of sulphuric acid extraction and ascorbic acid reduction in the case of the thiocyanate procedure whilst the reducing system in the dithiol procedure is potassium iodide-sodium sulphite. Using a simple photometer the range of determination possible is 0-10~g for the thiocyanate procedure and 0-5 g for dithioI.INTRODUCTIONOf the many colorimetric procedures that have been developed for the determination of molybdenum only those using the thiocyanate or toluene-3, 4-dithiol complexes of the metal are sufficiently free from interference to be of use in geochemical prospecting. Rapid methods based on both these complexes 'have been developed at the. Broken Hill Division of The University of New South Wales as part of a general programme designed to improve geochemical procedures. Whilst speed rather than high accuracy is the important factor in prospecting, the aim of the programme is to develop procedures which will allow determination of 200 samples per man-day without loss of normal laboratory accuracy for the methods concerned.In most geochemical procedures visual estimation of a coloured complex is used in the determination of the quantity of metal present. At the high rate of sample determination of the improved methods this procedure places severe strain on the eyes. For this reason all methods are designed for determination by means of a simple filter photometer...