The available methods for the determination of total sulfur in plant and animal tissue were found to be either cumbersome or of low degree of precision. A simple procedure utilizing nitric and perchloric acid oxidation was developed, which gives precise and accurate results for sulfur comparable with those obtained by the AOAC magnesium nitrate method on a great variety of plant and animal products, and the amino acids, cystine, cysteine, and methionine. Sulfur recoveries in standard materials were within 2% of theory. The same sample preparation can serve for the determination of calcium, magnesium, potassium, sodium, and phosphorus, as well as sulfur. The sulfate was determined gravimetrically as barium sulfate, but the prepared solution can be adapted for the indirect flame spectrophotometric or any other desired method of sulfur determination.