A simple, inexpensive near-IR spectrophotometer is described that employs single fiber-optic strands in a diffuse-transmission geometry. The instrument can examine unusually small sample volumes and offers sufficient throughput to perform multicomponent analyses on diffusely transmitting powdered samples. Control of the effective optical path-length is found to be critical in obtaining reproducible results when scattering samples are to be analyzed. A pseudo-double-beam arrangement is employed to reduce instrument noise and to set the optical pathlength independently for each sample. Sample sizes of only a few tens of milligrams are required for analysis. The resulting performance is nearly equivalent to that of a commercial reflectance instrument. An average standard error of prediction of 2.77% w/w was obtained for four-component mixtures of benzoic acid derivatives. The single-fiber transmission geometry is shown to be useful also in the near-IR analysis of microliter volumes of liquids. A standard error of cross-validation of 17 mM sodium chloride dissolved in water was achieved.

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