Procedures are described for both a titrimetric and a gravimetric determination of hafnium in aluminum -hafnium alloys. The gravimetric procedure is used if the hafnium is to be recovered; otherwise, the titrimetric procedure is preferred. The sample is dissolved in aqua regia. Any undissolved hafnium is taken into solution via pyrosulfate fusion. The hafnium is separated from the aluminum and contaminants in the aluminum by precipitation as the mandelate. In the gravimetric procedure the hafnium mandelate is heated to the oxide, then weighed. In the titrimetric procedure the mandelate is destroyed with nitric, sulfuric, and perchloric acids. The hafuium then is determined by adding a measured excess of EDTA and back titrating the excess EDTA with a standard bismuth solution to a xylenol orange end point. (auth)