Two methods were developed for the determination of uranium metal in UF3 with other fluoride compounds. A simplified method of determination which has a relatively high degree of precision (coefficient of variation 2 per cent) is carried out by decomposing the hydride in an atmosphere of carbon dioxide and subsequently measuring the hydrogen over an aqueous solution of potassium hydroxide. The ignition of the hydride in an atmosphere of oxygen and volumetric measurement of the water at reduced pressures provide a more sensitive method of determination. The coefficient of variation of the latter procedure is 7 per cent. The yield of gas from the reaction of the hydride with ammonia and gaseous hydrogen chloride was found to be neither stoichiometric nor reproducible.