The ability of near-infrared (NIR) diffuse reflectance spectroscopy to perform rapid bulk composition analyses of poly(ether urethane urea) (PEUU) block copolymers is demonstrated. Six polymer samples with known elemental compositions were used to construct calibration models using the method of classical least-squares (CLS). Results indicate that NIR diffuse reflectance spectroscopy can determine hard-segment and soft-segment contents of the bulk polymers within 2.6% mass over a range of 31% mass. Errors in the calibrations were caused by nonrepresentative NIR sampling of the polymers and by the presence of side products in the polymers. NIR spectra of model hard- and soft-segment materials are used to assign NIR bands to specific functional groups in the polymers.

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