In Situ Monitoring of Calcium Carbonate Polymorphs during Batch Crystallization in the Presence of Polymeric Additives Using Raman Spectroscopy

Parminder Agarwal, Kris A. Berglund

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    Abstract

    Polycarboxylic acids are well-known to affect calcium carbonate crystallization. Agarwal et al. (Ind. Eng. Chem. Res. 2003, in press) reported previously the synthesis of polymaleimide by a variety of techniques and initiators. In the present work, the effect of these polymers on calcium carbonate crystallization was studied by a variety of techniques. Crystallization experiments were carried out in a 1-L LABMAX automated batch reactor, and the concentration of calcium in solution was determined in real time. Raman spectroscopy was used to determine the relative amount of various calcium carbonate polymorphs as the crystallization occurred. However, Raman spectroscopy is a scattering technique, which may make it surface selective, and therefore results from solids may not be representative of bulk of sample. X-ray diffraction (XRD) was used to compare the results obtained by Raman spectroscopy. Peak intensity ratios were used for both Raman spectroscopy and XRD for calibration and measurement purposes. The results obtained by these two techniques for final percent vaterite for calcium carbonate crystallization in the presence of polymeric additives were in agreement within 2%. Therefore, use of Raman spectroscopy for in situ measurement of polymorph composition during calcium carbonate crystallization appears accurate. Scanning electron microscopy (SEM) data were useful in understanding the crystal morphology and to determine crystal size.

    Original languageEnglish (US)
    Pages (from-to)941-946
    Number of pages6
    JournalCrystal Growth and Design
    Volume3
    Issue number6
    DOIs
    StatePublished - Nov 2003

    Profile

    Crystallization
    crystallization
    Calcium carbonate
    Raman spectroscopy
    calcium carbonates
    Experimental Liver Cirrhoses
    Polymorphism
    Erythrocyte Volume
    X ray diffraction
    Crystals
    diffraction
    Buccal Administration
    Octanols
    Carcinoid Tumor
    Fetal Development
    Batch reactors
    Calcium
    Calibration
    Scattering
    Scanning electron microscopy

    ASJC Scopus subject areas

    • Chemistry(all)
    • Materials Science(all)
    • Condensed Matter Physics

    Cite this

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    abstract = "Polycarboxylic acids are well-known to affect calcium carbonate crystallization. Agarwal et al. (Ind. Eng. Chem. Res. 2003, in press) reported previously the synthesis of polymaleimide by a variety of techniques and initiators. In the present work, the effect of these polymers on calcium carbonate crystallization was studied by a variety of techniques. Crystallization experiments were carried out in a 1-L LABMAX automated batch reactor, and the concentration of calcium in solution was determined in real time. Raman spectroscopy was used to determine the relative amount of various calcium carbonate polymorphs as the crystallization occurred. However, Raman spectroscopy is a scattering technique, which may make it surface selective, and therefore results from solids may not be representative of bulk of sample. X-ray diffraction (XRD) was used to compare the results obtained by Raman spectroscopy. Peak intensity ratios were used for both Raman spectroscopy and XRD for calibration and measurement purposes. The results obtained by these two techniques for final percent vaterite for calcium carbonate crystallization in the presence of polymeric additives were in agreement within 2%. Therefore, use of Raman spectroscopy for in situ measurement of polymorph composition during calcium carbonate crystallization appears accurate. Scanning electron microscopy (SEM) data were useful in understanding the crystal morphology and to determine crystal size.",
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