A quantitative spectral method is usod to determino the various impurities contained in the 99.99% pure antimony. The antimony metal is ground to powder form as sample. A cortain amount of chemical salt, one of its component is the impurity element to be determined, in the form of powder is added to the sample, to secure a series of standards by several times of dilution. All the samples and standards are placed in the respective craters drilled on carbon rods. Each sample is photographed for five times by a Zeiss Qu-24 medium size quartz spec-trograph in same spectral plate. The result is obtained by linear interpolation method. The interrupted arc with longest interrupted time and exposure time is found to be a suitable source.Several impurities, including Ca, Si, Mg, Cu Fe, Al and Pb are analysed successfully at sensitivities from 10-5 to 10-6. The experimental error is only estimated about 30-