Evaluation of nucleation rate by in‐situ focused beam reflectance measurement in an unseeded batch cooling crystallization

Kim, Junwoo; Kim, Jung-Wook; Lee, Keundeuk; Koo, Kee-Kahb

doi:10.1002/crat.201300288

Cited by 10 publications

(10 citation statements)

References 35 publications

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“…Crystal nucleation rate decreases and crystal growth rate increases with increasing reaction temperature [22,23]. Thus, the number of generated crystals decreases and the size of crystals increases.…”

Section: Reactant Concentrationmentioning

confidence: 95%

Preparation, characterization, and in vitro cytotoxicity of COM and COD crystals with various sizes

Sun

Ouyang

Liu

et al. 2015

Materials Science and Engineering: C

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Section: Reactant Concentrationmentioning

confidence: 95%

Preparation, characterization, and in vitro cytotoxicity of COM and COD crystals with various sizes

Sun

Ouyang

Liu

et al. 2015

Materials Science and Engineering: C

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“…Crystal16 2 /Crystalline, colorimeter) 47,48 FBRM 49 (e.g. Lasentec "ParticleTrack" probe) 42,43,48,50 Naked eye 49 Turbidity via in-situ camera 51,52 3D Optical reflectance measurement (ORM) 53 Turbidity probe 54…”

Section: Detection Of the First Crystalmentioning

confidence: 99%

A Review of Experimental Methods for Nucleation Rate Determination in Large-Volume Batch and Microfluidic Crystallization

Devos

Gerven

Kuhn

2021

Crystal Growth & Design

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Experimental nucleation rate determination for crystallization in solution has been acknowledged as an important topic for a long time, as it improves the design and control of industrial crystallization processes, and offers insights into the mechanisms of nucleation. Characterization of nucleation rates in large volume batch crystallizers has been widely studied in the past, which has led to the development of a variety of models linking the nucleation rate to the metastable zone width and induction time. These methods remain important due to their role in industrial crystallization. More recently, the use of microfluidic platforms has resulted in the development of methods to obtain nucleation rates based on the stochastic nature of nucleation. This has opened new pathways for understanding nucleation on a molecular level. This review presents a critical overview of nucleation rate determination methods: large volume batch crystallizer models (Part I), and microfluidic and microvial models (Part II) are presented in terms of equations, advantages and limitations. Published experimental nucleation rate values are summarized (SI). A critical discussion of experimental nucleation rate determination is given (Part III). The objective of the review is to be a starting point for researchers attempting to experimentally characterize nucleation behavior.

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“…The justification of these empirical assumptions and their implementation will be discussed thoroughly in this contribution. This approach will then be used to determine whether primary nucleation rates obtained from the stochastic model are comparable with direct measurements via in situ laser-backscattering technique , and in situ Raman spectroscopy using p -aminobenzoic acid (PABA) and l -glutamic acid (LGA) as model compounds.…”

Section: Introductionmentioning

confidence: 99%

Direct Measurements of Primary Nucleation Rates of p-Aminobenzoic Acid and Glutamic Acid and Comparison with Predictions from Induction Time Distributions

Cedeno

Maosoongnern

Flood

2018

Ind. Eng. Chem. Res.

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The model-based estimation of primary nucleation rates from the probability distribution of induction time measurements has been used extensively in the literature; however, there has been no experimental validation of this approach via direct measurements of nucleation rates. In this work, we compared the nucleation rates obtained from the probability distribution model against that measured from in situ optical reflectance measurement (ORM) with p-aminobenzoic acid and l-glutamic acid as model compounds. Results reveal that the primary nucleation rates obtained from stochastic models are several orders of magnitude lower than those measured from a direct particle-counting technique. Although differences in fluid dynamics due to agitation and crystallizer geometry may have an effect, this tremendous discrepancy provides strong evidence that primary nucleation rates obtained from induction time measurements are not scalable and should not be used for interpretation of nucleation rates in industrial applications.

show abstract

Evaluation of nucleation rate by in‐situ focused beam reflectance measurement in an unseeded batch cooling crystallization

Cited by 10 publications

References 35 publications

Preparation, characterization, and in vitro cytotoxicity of COM and COD crystals with various sizes

Preparation, characterization, and in vitro cytotoxicity of COM and COD crystals with various sizes

A Review of Experimental Methods for Nucleation Rate Determination in Large-Volume Batch and Microfluidic Crystallization

Direct Measurements of Primary Nucleation Rates of p-Aminobenzoic Acid and Glutamic Acid and Comparison with Predictions from Induction Time Distributions

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