Real-Time Raman Monitoring of Calcium Phosphate Precipitation in a Semi-Batch Stirred Crystallizer

Bing Han; Marjatta Louhi-Kultanen

doi:10.1021/acs.cgd.7b01587

Real-Time Raman Monitoring of Calcium Phosphate Precipitation in a Semi-Batch Stirred Crystallizer

Bing Han^*, Marjatta Louhi-Kultanen

^*Corresponding author for this work

Research output: Contribution to journal › Article › Scientific › peer-review

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Abstract

Semi-batch precipitation of calcium monohydrogen phosphate dihydrate (CaHPO₄·2H₂O; also termed dicalcium phosphate dihydrate, DCPD) from a homogeneous reaction of KH₂PO₄ and CaCl₂ was studied with inline Raman spectroscopy. In the reaction, hydroxyapatite (HAP, Ca₅OH(PO₄)₃) formed first and transferred to DCPD throughout the entire precipitation process. Raman calibration models were created with a series of KH₂PO₄-NaOH-water solutions. The reliability of the calibration models was validated with offline measurement of phosphate concentration in the mother liquor. Real-time changes in HPO₄ ^2- and H₂PO₄ ^- concentration were monitored and predicted. Comprehensive kinetic information was obtained from liquid and solid analysis. It was found that the influence of the mixing rate on the precipitation was not significant, whereas the reactant feeding rate had a remarkable impact.

Original language	English
Pages (from-to)	1622-1628
Number of pages	7
Journal	Crystal Growth and Design
Volume	18
Issue number	3
DOIs	https://doi.org/10.1021/acs.cgd.7b01587
Publication status	Published - 7 Mar 2018
MoE publication type	A1 Journal article-refereed

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title = "Real-Time Raman Monitoring of Calcium Phosphate Precipitation in a Semi-Batch Stirred Crystallizer",

abstract = "Semi-batch precipitation of calcium monohydrogen phosphate dihydrate (CaHPO4·2H2O; also termed dicalcium phosphate dihydrate, DCPD) from a homogeneous reaction of KH2PO4 and CaCl2 was studied with inline Raman spectroscopy. In the reaction, hydroxyapatite (HAP, Ca5OH(PO4)3) formed first and transferred to DCPD throughout the entire precipitation process. Raman calibration models were created with a series of KH2PO4-NaOH-water solutions. The reliability of the calibration models was validated with offline measurement of phosphate concentration in the mother liquor. Real-time changes in HPO4 2- and H2PO4 - concentration were monitored and predicted. Comprehensive kinetic information was obtained from liquid and solid analysis. It was found that the influence of the mixing rate on the precipitation was not significant, whereas the reactant feeding rate had a remarkable impact.",

author = "Bing Han and Marjatta Louhi-Kultanen",

note = "TARKISTA ONKO T{\"A}M{\"A} AVATTU 2019.",

year = "2018",

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doi = "10.1021/acs.cgd.7b01587",

language = "English",

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journal = "Crystal Growth and Design",

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T1 - Real-Time Raman Monitoring of Calcium Phosphate Precipitation in a Semi-Batch Stirred Crystallizer

AU - Han, Bing

AU - Louhi-Kultanen, Marjatta

N1 - TARKISTA ONKO TÄMÄ AVATTU 2019.

PY - 2018/3/7

Y1 - 2018/3/7

N2 - Semi-batch precipitation of calcium monohydrogen phosphate dihydrate (CaHPO4·2H2O; also termed dicalcium phosphate dihydrate, DCPD) from a homogeneous reaction of KH2PO4 and CaCl2 was studied with inline Raman spectroscopy. In the reaction, hydroxyapatite (HAP, Ca5OH(PO4)3) formed first and transferred to DCPD throughout the entire precipitation process. Raman calibration models were created with a series of KH2PO4-NaOH-water solutions. The reliability of the calibration models was validated with offline measurement of phosphate concentration in the mother liquor. Real-time changes in HPO4 2- and H2PO4 - concentration were monitored and predicted. Comprehensive kinetic information was obtained from liquid and solid analysis. It was found that the influence of the mixing rate on the precipitation was not significant, whereas the reactant feeding rate had a remarkable impact.

AB - Semi-batch precipitation of calcium monohydrogen phosphate dihydrate (CaHPO4·2H2O; also termed dicalcium phosphate dihydrate, DCPD) from a homogeneous reaction of KH2PO4 and CaCl2 was studied with inline Raman spectroscopy. In the reaction, hydroxyapatite (HAP, Ca5OH(PO4)3) formed first and transferred to DCPD throughout the entire precipitation process. Raman calibration models were created with a series of KH2PO4-NaOH-water solutions. The reliability of the calibration models was validated with offline measurement of phosphate concentration in the mother liquor. Real-time changes in HPO4 2- and H2PO4 - concentration were monitored and predicted. Comprehensive kinetic information was obtained from liquid and solid analysis. It was found that the influence of the mixing rate on the precipitation was not significant, whereas the reactant feeding rate had a remarkable impact.

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