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Materials characterization using a novel simultaneous near-infrared/X-ray diffraction instrument

Published online by Cambridge University Press:  06 March 2012

Tom Blanton*
Affiliation:
Eastman Kodak Company, Imaging Materials Research and Development, Rochester, New York 14650-2106
Craig Barnes
Affiliation:
Eastman Kodak Company, Imaging Materials Research and Development, Rochester, New York 14650-2106
Julie Putrelo
Affiliation:
Eastman Kodak Company, Imaging Materials Research and Development, Rochester, New York 14650-2106
Agyare Yeboah
Affiliation:
Eastman Kodak Company, Imaging Materials Research and Development, Rochester, New York 14650-2106
Steve Switalski
Affiliation:
Eastman Kodak Company, Imaging Materials Research and Development, Rochester, New York 14650-2106
*
a)Electronic mail: [email protected]

Abstract

X-ray powder diffraction (XRD) is utilized for the 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. Near-infrared 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 materials. 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.

Type
Technical Articles
Copyright
Copyright © Cambridge University Press 2004

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