The application of square-wave voltammetry (SWV) for the determination of eight elements viz. Cd(II), Pb(II), Cu(II), Zn(II), Co(II), Ni(II), Cr(VI), and Mo(VI) in soil and indoor-airborne particulate matter has been examined and optimized. The cathodic and anodic types of the SWV technique were examined for the detection of these metal ions. It was found that the square-wave anodic stripping voltammetry is the conventional technique for the determination of Zn(II), Cd(II), Pb(II), and Cu(II), but square-wave adsorptive cathodic stripping voltammetric method is used for the determination of Co(II), Ni(II), Mo(VI) and Cr(VI). Various experimental parameters, which influenced the response of the mercury film electrode to these metal ions, were optimized. The detection limits of these metal ions were 0.03, 0.4, 0.04, 0.1, 0.15, 0.05, 0.2, and 3.2μg/kg for Cd(II), Pb(II), Cu(II), Zn(II), Co(II), Ni(II), Cr(VI), and Mo(VI), respectively, with very good accuracy (standard deviation is below 2%). Interference from coexisting ions was successfully investigated. A comparison of analytical data for analyzing real samples was carried out between the SWV method and the graphite furnace atomic absorption spectrophotometric (GFAAS) method. By the standard addition method, the recoveries were 96.6–104% with SD of 0.75–2.5%. The great advantage of SWV is the simplicity, selectivity, sensitivity, and shortening analysis time over the GFAAS method.