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Updated: Jul 13, 2025

Calcium Carbonate Formation in the Presence of Biopolymeric Additives
Published on: May 14, 2019
X-ray Absorption Spectroscopy as a Process Analytical Technology: Reaction Studies for the Manufacture of
Thokozile A Kathyola1,2, Sin-Yuen Chang2, Elizabeth A Willneff3
1School of Chemical and Process Engineering, University of Leeds, Leeds LS2 9JT, U.K.
Abstract:
Process analytical technologies are widely used to inform process control by identifying relationships between reagents and products. Here, we present a novel process analytical technology system for operando XAS on multiphase multicomponent synthesis processes based on the combination of a conventional lab-scale agitated reactor with a liquid-jet cell. The preparation of sulfonate-stabilized CaCO3 particles from polyphasic Ca(OH)2 dispersions was monitored in real time by Ca K-edge XAS to identify changes in Ca speciation in the bulk solution/dispersion as a function of time and process conditions. Linear combination fitting of the spectra quantitatively resolved composition changes from the initial conversion of Ca(OH)2 to the Ca(R-SO3)2 surfactant to the ultimate formation of nCaCO3·mCa(R- SO3)2 particles. The system provides a novel tool with strong chemical specificity for probing multiphase synthesis processes at a molecular level, providing an avenue to establishing the relationships between critical quality attributes of a process and the quality and performance of the product.
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