Fourier transform (FT)-Raman spectroscopy has been applied to the online analysis and control of a PCI<sub>3</sub> reactor. This particular analytical technique was selected from a consideration of the Raman scattering efficiencies of the constituents of the reaction and the ability of the fiberoptic-coupled, near-IR, FT-Raman systems to remotely sample the toxic and potentially hazardous reaction mixture. In this communication we describe the Raman spectra of P<sub>4</sub>, PCl<sub>3</sub>, PCl<sub>5</sub>, and P<sub>4</sub> dissolved in PCl<sub>3</sub>, as well as related compounds, along with relative band intensities of the constituents of the reaction. Factors leading to the optimum FT-Raman configuration for this particular process control problem are discussed in detail.
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