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It has been investigated what kind of characteristic X-ray in electron probe micro-analyzer (EPMA) is effective for the determination of compounds of Si series materials. After comparing the characteristic X-rays among the primary and secondary lines in K α and K β obtained from the Si series standard samples, it was found that the secondary line of K α exhibited the most informative spectrum although the intensity was considerably weak. As a result of analyzing the spectrum shapes of the Si series standard samples, the spectrum shape of the secondary line of K α for SiC was different from those for other Si compounds. To grasp the characteristics of the shape, a line was perpendicularly drawn from the peak top to base line in order to divide a spectrum into two areas. The area ratio of right to left was defi ned to call as the asymmetry index here. As a result, the asymmetry index value of the SiC was greater than one, while those of other Si compounds were less than one. It was found from the EPMA analysis that identifi cation of SiC became successful to distinguish from other Si compounds and this method was applicable for micro-sized compounds in a practical composite material.