Raman and ATR FTIR spectroscopy in reactive crystallization: Simultaneous monitoring of solute concentration and polymorphic state of the crystals

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Raman and ATR FTIR spectroscopy in reactive crystallization : Simultaneous monitoring of solute concentration and polymorphic state of the crystals. / Qu, Haiyan; Alatalo, Hannu; Hatakka, Henry; Kohonen, Jarno; Louhi-Kultanen, Marjatta; Reinikainen, Satu P.; Kallas, Juha.

In: Journal of Crystal Growth, Vol. 311, No. 13, 15.06.2009, p. 3466-3475.

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Qu, Haiyan ; Alatalo, Hannu ; Hatakka, Henry ; Kohonen, Jarno ; Louhi-Kultanen, Marjatta ; Reinikainen, Satu P. ; Kallas, Juha. / Raman and ATR FTIR spectroscopy in reactive crystallization : Simultaneous monitoring of solute concentration and polymorphic state of the crystals. In: Journal of Crystal Growth. 2009 ; Vol. 311, No. 13. pp. 3466-3475.

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@article{8e71627aa39a45f6b2b03791511f656f,
title = "Raman and ATR FTIR spectroscopy in reactive crystallization: Simultaneous monitoring of solute concentration and polymorphic state of the crystals",
abstract = "Batch-reactive crystallization of the two polymorphs of l-glutamic acid was studied using in-line Raman and ATR FTIR spectroscopy. It was observed that the barrier to the nucleation of the stable β-form was higher, and thus the occurrence of β-form nucleation requires a higher supersaturation level. The local supersaturation level inside the reactive crystallizer is significantly affected by the feeding manner of the reactant. When the reactant was fed to a poorly mixed zone, such as the surface of the liquid, a high local supersaturation level was generated near the feeding point. This high local supersaturation level drastically increased with the increase in the concentrations of the reactants. As a consequence, the fraction of the β-form increased with the increase in reactants concentrations. On the other hand, feeding the reactant to a well-mixed zone near the impeller can avoid the occurrence of high local supersaturation, and therefore the dependence of the polymorphic composition of the final product on the concentration of the reactants can be reduced. The information obtained from the spectroscopy leads to improved understanding of the precipitation process and offers great potential for process optimization and control of crystalline quality.",
keywords = "A1. Polymorphism, A2. Industrial crystallization, A2. Precipitation, B3. ATR FTIR spectroscopy, B3. In-line monitoring, B3. Raman spectroscopy",
author = "Haiyan Qu and Hannu Alatalo and Henry Hatakka and Jarno Kohonen and Marjatta Louhi-Kultanen and Reinikainen, {Satu P.} and Juha Kallas",
year = "2009",
month = "6",
day = "15",
doi = "10.1016/j.jcrysgro.2009.04.018",
language = "English",
volume = "311",
pages = "3466--3475",
journal = "Journal of Crystal Growth",
issn = "0022-0248",
publisher = "Elsevier",
number = "13",

}

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TY - JOUR

T1 - Raman and ATR FTIR spectroscopy in reactive crystallization

T2 - Simultaneous monitoring of solute concentration and polymorphic state of the crystals

AU - Qu, Haiyan

AU - Alatalo, Hannu

AU - Hatakka, Henry

AU - Kohonen, Jarno

AU - Louhi-Kultanen, Marjatta

AU - Reinikainen, Satu P.

AU - Kallas, Juha

PY - 2009/6/15

Y1 - 2009/6/15

N2 - Batch-reactive crystallization of the two polymorphs of l-glutamic acid was studied using in-line Raman and ATR FTIR spectroscopy. It was observed that the barrier to the nucleation of the stable β-form was higher, and thus the occurrence of β-form nucleation requires a higher supersaturation level. The local supersaturation level inside the reactive crystallizer is significantly affected by the feeding manner of the reactant. When the reactant was fed to a poorly mixed zone, such as the surface of the liquid, a high local supersaturation level was generated near the feeding point. This high local supersaturation level drastically increased with the increase in the concentrations of the reactants. As a consequence, the fraction of the β-form increased with the increase in reactants concentrations. On the other hand, feeding the reactant to a well-mixed zone near the impeller can avoid the occurrence of high local supersaturation, and therefore the dependence of the polymorphic composition of the final product on the concentration of the reactants can be reduced. The information obtained from the spectroscopy leads to improved understanding of the precipitation process and offers great potential for process optimization and control of crystalline quality.

AB - Batch-reactive crystallization of the two polymorphs of l-glutamic acid was studied using in-line Raman and ATR FTIR spectroscopy. It was observed that the barrier to the nucleation of the stable β-form was higher, and thus the occurrence of β-form nucleation requires a higher supersaturation level. The local supersaturation level inside the reactive crystallizer is significantly affected by the feeding manner of the reactant. When the reactant was fed to a poorly mixed zone, such as the surface of the liquid, a high local supersaturation level was generated near the feeding point. This high local supersaturation level drastically increased with the increase in the concentrations of the reactants. As a consequence, the fraction of the β-form increased with the increase in reactants concentrations. On the other hand, feeding the reactant to a well-mixed zone near the impeller can avoid the occurrence of high local supersaturation, and therefore the dependence of the polymorphic composition of the final product on the concentration of the reactants can be reduced. The information obtained from the spectroscopy leads to improved understanding of the precipitation process and offers great potential for process optimization and control of crystalline quality.

KW - A1. Polymorphism

KW - A2. Industrial crystallization

KW - A2. Precipitation

KW - B3. ATR FTIR spectroscopy

KW - B3. In-line monitoring

KW - B3. Raman spectroscopy

UR - http://www.scopus.com/inward/record.url?scp=66649132475&partnerID=8YFLogxK

U2 - 10.1016/j.jcrysgro.2009.04.018

DO - 10.1016/j.jcrysgro.2009.04.018

M3 - Article

VL - 311

SP - 3466

EP - 3475

JO - Journal of Crystal Growth

JF - Journal of Crystal Growth

SN - 0022-0248

IS - 13

ER -

ID: 10772487