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Proton spin resonance spectra were recorded for the three binary mixtures, benzene-dioxane, benzene-hexamethylsiloxane and dioxane-cyclooctaphenyltetrasiloxane whose mixing ratios were varied. The peak area due to resonating proton of methyl or phenyl group was found to be directly proportional for all systems to the number of protons which give the peak of respective groups over a wide range of recording conditions. With the results obtained, the determination of methyl and phenyl groups in methyl-phenyl-siloxane polymer was carried out by the use of the inner reference method using dioxane. Siloxane polymer was mixed with dioxane and the spectrum was recorded for the mixture, the number of each group being calculated from the obtained peak area. The results were compared with those obtained from the infrared analysis and they were in good agreement within the experimental error.

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