The effect of particle size on Raman intensity has been measured for a number of crystalline solids with a fiber-optic-based Raman spectrometer. Particle sizes ranged from 76 to 605 μm. Materials examined were sodium nitrate, sodium chlorate, sodium bromate, potassium ferrocyanide, potassium ferricyanide, and copper(II) sulfate. Raman intensity was found to decrease with increasing particle size. The factors responsible for this trend are discussed. We conclude that the major factor is diffuse reflectance that enhances the overlap between the excitation and collection beams. The depth of sample contributing to the Raman signal has been examined for both powders and tablets as a function of powder particle size. Materials examined in this study were sodium nitrate, sodium sulfate, sodium chlorate, sodium bromate, potassium ferrocyanide, potassium ferricyanide, and copper(II) sulfate. For nonabsorbing powders, the depth of sample contributing to the signal exceeded 15 mm. The effect of the pressure used in forming tablets on the Raman signal strength and reproducibility has been examined for sodium nitrate. The Raman intensity was found to decrease with increasing pressure until a tablet of constant density was formed. The effect of particle size and particle size mismatch on the sodium nitrate Raman signal in binary mixtures with potassium chloride, potassium bromide, and potassium iodide has been examined. Good reproducibility was found to require matching of component particle sizes.

The utility of FT-Raman spectroscopy in characterizing ion-exchange resins has been demonstrated. Measurements have been made on strong acid-type cation-exchange resin beads of a sulfonated polystyrene-divinyl benzene copolymer. Spectra are compared for the resin with 10 different cations. Classical least-squares fitting is used to quantitate the amounts of different cations in binary mixtures. On-column determinations are demonstrated for displacement of H+ by Na+ and Na+ by Ag+.

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