Infrared Analysis of Phenylchlorosilanes in the CsBr Region

Abstract

The infrared spectra of seven phenylchlorosilanes have been meassured from 2 to 30 microns The spectra of certain phenylchlorosilanes are very similar in the 2–15 micron wavelength region but show marked differences in the 15–30 micron range, where there are Si-Cl stretching and aromatic-ring deformation vibrations. Based on these differences, methods for the quantitative analysis of mixtures of phenylchlorosilanes have been developed using a double-beam, double-pass spectrometer equipped with a CsBr prism and a new, low-cost KBr spectrometer With double-beam compensation, low concentrations of phenyltrichlorosilane in diphenyldichlorosilane can be determined Techniques for the quantitative analysis of mixtures of phenyltrichlorosilane, diphenyldichlorosilane, and chlorobenzene are described. Because atmospheric water vapor absorbs strongly in the CsBr region, flushing the spectrometer with dry air or nitrogen improves the accuracy of absorbance measurements.

Analysis of Multicomponent Methyl- and Phenylchlorosilane Solutions

“…Mixtures of chlorosilanes have been previously analyzed in our laboratories by analytical distillation, but this is time-consuming. Data in a recent article (7) show that mixtures of the type described in this article might be analyzed by infrared techniques.…”

“…In this report, specifications are recommended for the conventional apparatus used in connection with oxygen flask combustion procedures (7,8). Types of apparatus employing electric ignition (2,6,6) are not included be-cause of lack of experience with these forms.…”

Report on Recommended Specifications for Microchemical Apparatus. Oxygen Combusiton Flask

“…In this report, specifications are recommended for the conventional apparatus used in connection with oxygen flask combustion procedures (7,8). Types of apparatus employing electric ignition (2, 6,6) are not included be-cause of lack of experience with these forms.…”

“…(6) Martin, A. J., Deveraux, H., Ibid., 31, 1932 (1959). (7) (8) Steyermark, A., "Quantitative Organic Microanalysis," 2nd ed., p. 292, Academic Press, New York, 1961. Received for review August 9, 1961.…”