Effects of Sample Dilution and Particle Size/Morphology on Diffuse Reflection Spectra of Carbohydrate Systems in the Near- and Mid-Infrared. Part I: Single Analytes

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Abstract
The mid- and near-infrared diffuse reflection spectra of three carbohydrates—microcrystalline cellulose, wheat starch, and sucrose—are examined to determine whether dilution is necessary in either spectral region in order to avoid the effects of specular reflection. As expected, it was found that dilution was not necessary to obtain valid diffuse reflection spectra of samples in the near-infrared, but that dilution was necessary for measuring mid-infrared diffuse reflection spectra free of the effects of specular reflection. The effects of particle size and sample morphology were investigated for sucrose crystals up to 2 mm in dimension. Depending upon the particle size and orientation, the effects of specular reflection can be observed in both near- and mid-infrared diffuse reflection spectra of sucrose. Surface roughness can allow a diffuse reflection component to be measured in the spectra of very large particles where a specular reflection mechanism would typically be expected to predominate.