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A measurement and data evaluation technique for the separate determination of the scattering and absorption properties of loose pharmaceutical powders is described. The equation of radiative transfer for diffuse reflectance and transmittance is analytically solved by using a three-flux approximation. Combined transmittance and reflectance measurements then allow one to derive both the scattering and the absorption coefficients. The scattering and absorption coefficients provide more information about particle size, degree of agglomeration, and chemical composition of the samples in comparison to the usual determination of only the ratio of the coefficients from diffuse reflectance measurements on optically thick samples. Furthermore, the theory of diffuse reflectance of optically thick samples according to Kubelka and Munk is compared to the three-flux approximation. The influence of the particle size on the scattering and absorption coefficient is investigated, and it is shown that the assumption of a wavelength-independent scattering coefficient, though often made in reflectance spectroscopy, is not generally valid.

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A method is described to determine quantitatively the infrared-optical properties of loose powder beds via directional-hemispherical transmission and reflection measurements. Instead of the integration of the powders into a potassium bromide (KBr) or a paraffin oil matrix, which would drastically alter the scattering behavior, the powders are placed onto supporting layers of polyethylene (PE) and KBr. A commercial spectrometer is supplemented by an external optics, which enables measurements on horizontally arranged samples. For data evaluation we use a solution of the equation of radiative transfer in the 3-flux approximation under boundary conditions adapted to the PE or KBr/powder system. A comparison with Kubelka–Munk’s theory and Schuster’s 2-flux approximation is performed, which shows that 3-flux approximation yields results closest to the exact solution. Equations are developed, which correct transmission and reflection of the samples for the influence of the supporting layer and calculate the specific extinction and the albedo of the powder and thus enables us to separate scattering and absorption part of the extinction spectrum. Measurements on TiO2 powder are presented, which show the influence of preparation techniques and data evaluation with different methods to obtain the albedo. The specific extinction of various TiO2 powders is presented.