Abstract: The trace elements of fourteen kinds of Mg, Si, S, Mn, ect., in high purity Sb were analyzed by glow discharge mass spectrometer (GDMS). The working parameters of measuring were optimized. The correlation of concentration for impurity in samples versus sputtering time, the influence of spectral interference on measurement results and the accuracy and repeatability of measurement were discussed. The results showed the surface contamination produced in sample preparation and treatment can be eliminated if the sample was sputtered for enough time. The characteristics can help to establish the scientific basis for measuring the other high purity materials. GDMS is one of most efficient tools to analyze these materials.