X-ray powder diffraction (XRD) is utilized for determination of polymorphism in crystalline organic materials. Though convenient to use in a laboratory setting, XRD is not easily adapted to in situ monitoring of synthetic chemical production applications or thin film depositions. Nearinfrared spectroscopy (NIR) can be adapted to in situ manufacturing schemes by use of a source/detector probe. Conversely, NIR is unable to conclusively define the existence of polymorphism in crystalline

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... By combining the two techniques, a novel simultaneous NIR/XRD instrument has been developed. During material's analysis, results from XRD allowed for the determination of the existence of polymorphic phases, and NIR data were collected as a fingerprint for each of the observed polymorphs. These NIR fingerprints allowed for the development of a library, which can be referenced during the use of a NIR probe in manufacturing settings. The NIR/XRD instrument was also used to monitor materials during exposure to ambient air. XRD can detect crystalline phase changes and NIR can monitor solvent loss and/or water uptake.