Determination of traces of impurities in chloro-silanes and high purity silica are important in the preparation of semiconductor grade silicon. The author have developed an indirect method for the determination of phosphorus in these materials. Phosphorus is extracted as phosphoantimonyl molybdate complex in methyl isobutyl ketone. The concentration of phorphorus is calculated by determining the concentration of antimony by atomic absorption spectrophotometer as antimony and phosphorus are present in 1:1 molar ratio in the complex. The method is selective and enables the determination of 0.1 ppm of phosphorus.