Abstract: The determination of Cd, Cr, Cu, Zn, Ni and Pb in the dust-fall ofcoal ash by spark source mass spectrometry (SSMS) without standard samplehas been reported in the present paper. In our work, two methods--theContent Increment SSMS by which six elements Cd, Zn, Cu, Ni, Cr and Pbwere determined, and the Solid Isotope Dilution SSMS by which fourelements Zn, Cu, Ni and Pb were determined, have been used. Generally,the results of the two methods are showing no differences. The variationcoefficents are within 30% for the former and 10% for the latter. The bothdetection limits are below 1 ppm. Here the problem concerning correction ofoverlapped disturbance has also been discussed.