A rapid, selective and sensitive liquid-liquid extraction and spectrophotometric method for the separation and microgram determination of uranium using PSAHA is described. Uranium is extracted with PSAHA into chloroform at pH 6.0–6.8. The U-PSAHA chelate is orange red in color having maximum absorbance at 410 nm and molar absorptivity 1.2·104l·mol–1·cm–1. The system obeys Beer's Law in the range of 1.2 to 22.00 ppm of uranium. The uranium is determined in sea water and rock samples.