In the proposed method, a 12.5-g sample is digested with nitric acid and evaporated to dryness; the excess nitric acid is removed by reaction with formic acid. Tellurium is extracted from the dried residue into hydrobromic acid and is then coprecipitated with arsenic, using hypophosphorous acid as the reducing agent. The precipitate is dissolved in a solution of hydrobromic acid and bromine, from which the tellurium is extracted into 0.6 ml of methyl isobutyl ketone. Tellurium content is estimated by atomic absorption spectrophotometry. Recovery of tellurium from nitric acid solutions carried through the procedure approached 100 percent through the analytical range 5-200 ppb. The relative standard deviation of five consecutive analyses of USGS standard rock GSP-1 was 5.26 percent at a mean concentration of 20.8 ppb. Under optimum conditions an average of 20 samples may be analyzed per man-day.