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Quantification of individual phases within a multiphase amorphous material has been achieved using a newly developed technique based on X-ray powder diffraction. The quantification method was developed during a study of an amorphous silica-poly(methyl methacrylate) (SiO2-PMMA) hybrid nanocomposite. The efficiency of the method as a quantifying tool for individual phases was demonstrated for samples of SiO2-PMMA prepared either by polymerization of methyl methacrylate in the presence of amorphous SiO2 or by mechanically mixing known quantities of the individual and pre-prepared SiO2 and PMMA materials. The weight percentages of amorphous SiO2 in the nanocomposites as determined by application of the new technique were analogously found to be 29%, a result that was supported by thermogravimetric analysis and helium picnometry measurements.