The ability of Raman microspectroscopy to distinguish between rutile and anatase forms of the inorganic pigment titanium dioxide (TiO<sub>2</sub>) and to make quantitative measurements of titania loading in fibers is demonstrated. Issues that affect the validity of the Raman measurements include the spatial heterogeneity of TiO<sub>2</sub> in the fiber, the polarization of the laser beam, and the polarizing properties of the fiber itself. The amount of titanium dioxide in single delustered polyamide fibers was quantitated at concentration levels ranging from 0 to 7.1% TiO<sub>2</sub>. Fiber polarization and orientation effects were shown to be minimized by scrambling the polarization of the laser.
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