Various investigations were conducted to establish quantification of microelements in iron and steel using ICP-MS with solid-phase extractive separation capable of separating the matrix simply and rapidly as a pretreatment. A "zero-emission type analysis" free from EDTA as a masking agent and buffering agents used for pH adjustment was sought. To do so, an anion-exchange type solid-phase extraction disk was used as the solid-phase extraction agent, along with "skill-free analysis" requiring no cumbersome manipulations, and "quick analysis" for assessment in an extremely short period of time. Results show a target element in a solid-phase disk, whereas the sample solution at separation was maintained at higher than pH 1.8. The pH adjustment was conducted by dilution of the sample solution with about 400 cm(3) of water. The target element held in the solid-phase disk was eluted with 10 cm(3) of 3 kmol/m(3) nitric acid. The detection limitations [3 sigma; ng/g (ppb)] were the following: Ti 0.043, Ge 0.014, Zr 0.013, Nb 0.025, Mo 1.06, Sn 0.030, Hf 0.010, Ta 0.019, and W 0.12.