In this paper, the alcoholysis products synthesized by MeSiHCl₂ and MeOH in xylene are examined by IR and ¹H-NMR. The results indicated that the concentration of each composition can be calculated using the Si-H bond and phenyl group absorption peak as spectrum-band of quantitative analysis through the calibration curve and the scaling method in the IR analytical means, and also it can be established using the normalization method through the analysis of the different chemical shift parton H and a series of quantitative analytic calculations in ¹H-NMR. Both methods are simple and rapid. The results of the two methods are compared.