An alternating current phase-selective anodic stripping (PSAS) method is described for determining trace amounts of gallium in spiked bovine tissue. Sharp, gaussian a.c. anodic stripping peaks were obtained at high solution ionic strength and in the presence of thiocyanate anion. Tissue samples were ashed completely using a low temperature, radio-frequency excited oxygen plasma. Interference from copper and zinc naturally present in the tissue was eliminated by isopropyl ether extraction of HGaC14 from 7 molar hydrochloric acid solution.