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.

LanguageEnglish (US)
Pages941-946
Number of pages6
JournalCrystal Growth and Design
Volume3
Issue number6
DOIs
StatePublished - Nov 2003

Profile

Calcium Carbonate
calcium carbonates
Calcium carbonate
Crystallization
Polymorphism
Raman spectroscopy
crystallization
Monitoring
X ray diffraction
selective surfaces
Crystals
crystal morphology
Batch reactors
initiators
in situ measurement
diffraction
calcium
Calcium
Polymers
x rays

ASJC Scopus subject areas

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

Cite this

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