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.