This investigation describes the application of the Beckman Model DU flame spectrophotometer to the rapid determination of iron in siliceous materials such as alumina refractories and limestone. The arc emission line at 386.0 mg was used to measure the iron radiation.Cobalt was incorporated in the samples in order that the cobalt 387.1-mg arc line could serve as an internal standard. An oxyacetylene flame was the excitation source.The radiative interference of many elements normally associated with iron in siliceous samples could be corrected by using an internal standard. None of the alkalies or alkaline earths offered interference when present in the amounts usually encountered, and large concentrations of aluminum can be tolerated.Magnesium offers serious interference, and when present, the separation of iron as the hydrous oxide is necessary. The optimum concentration range for iron is between 25 and 200 p.p.m. The standard deviation from the mean of replicate samples is approximately 3%. The method has been successfully applied to limestone and several varieties of alumina refractories.