Real‐time product morphology monitoring in crystallization using imaging technique

Anda, J. Calderon De; Wang, X. Z.; Lai, Xiaojun; Roberts, Kevin J.; Jennings, Kevin H.; Wilkinson, Mike; Watson, D.; Roberts, D.

doi:10.1002/aic.10410

Cited by 99 publications

(38 citation statements)

References 29 publications

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“…Recently, 2D [8,13,14,39,40] and morphologically based [41][42][43] population balance models have been developed. The latter case offers a significant improvement in that the multi-dimensional characteristic lengths are defined with respect to the growth rates of the individual crystal habit faces.…”

Section: Overall Linear Growth Ratementioning

confidence: 99%

“…This approach has been enhanced through the use of stroboscopic techniques together with computational methods for analysis of crystallisation processes within agitated batch vessels [7][8][9][10]. High speed imaging processes has also been used to capture high resolution images on-line and perform real-time, in situ particle analysis [10,13,14,54].…”

Section: Crystal Growth Rate Measurement Techniquesmentioning

confidence: 99%

“…through the measurement of the characteristic dimensions (such as length, width, and equivalent diameter etc.) associated with the growth of the crystals [7][8][9][10][11][12][13][14]. Linking these two, quite distinctive, sets of measurements is a challenge mindful of the quite different hydrodynamic environments involved.…”

Section: Introductionmentioning

confidence: 99%

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Precision measurement of the growth rate and mechanism of ibuprofen {001} and {011} as a function of crystallization environment

et al. 2014

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Article:Nguyen, TTH, Hammond, RB, Roberts, KJ et al. (2 more authors) (2014) Precision measurement of the growth rate and mechanism of ibuprofen {001} and {011} as a function of crystallization environment. CrystEngComm, 16 (21). 4568 -4586. ISSN 1466-8033 https://doi.org/10.1039/c4ce00097h eprints@whiterose.ac.uk https://eprints.whiterose.ac.uk/ Reuse Unless indicated otherwise, fulltext items are protected by copyright with all rights reserved. The copyright exception in section 29 of the Copyright, Designs and Patents Act 1988 allows the making of a single copy solely for the purpose of non-commercial research or private study within the limits of fair dealing. The publisher or other rights-holder may allow further reproduction and re-use of this version -refer to the White Rose Research Online record for this item. Where records identify the publisher as the copyright holder, users can verify any specific terms of use on the publisher's website. TakedownIf you consider content in White Rose Research Online to be in breach of UK law, please notify us by emailing eprints@whiterose.ac.uk including the URL of the record and the reason for the withdrawal request. acetonitrile. The crystal growth rates of the {001} and {011} faces of spontaneously nucleated crystals are precisely measured in-situ using optical microscopy revealing that their respective growth rates increase with increasing supersaturation to different extents, depending on the solvent type, with concomitant impact on the crystal habit. The measured aspect ratios, as a function of supersaturation, are generally higher at the 15 mL than the 0.5 mL scale size.Analysis of the growth rates versus supersaturation is consistent with a 2-D surface nucleation (Birth and Spread) model for both faces and at both scale sizes. The growth rates of the {001} and {011} faces exhibit much less growth rate dispersion when compared to literature data for a stirred batch crystallizer. 2The data is rationalized by examining the surface chemistry of the growing faces revealing, e.g. that polar protic solvents inhibit the growth rate of faces containing available binding sites for hydrogen bonding formation, such as carboxylic acid groups.

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Section: Overall Linear Growth Ratementioning

confidence: 99%

Section: Crystal Growth Rate Measurement Techniquesmentioning

confidence: 99%

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Precision measurement of the growth rate and mechanism of ibuprofen {001} and {011} as a function of crystallization environment

et al. 2014

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“…Compared with the laser-based method which is commonly used for crystal size measurement [13][14][15], challenges in the study of crystal size by electrical impedance spectroscopy exist because the impedance data is easily affected by several factors, such as the concentration of the solid LGA phase, the concentration of solute, temperature and crystal size [16]. The relationship between the crystal size and electrical impedance spectra can't be obtained straightforwardly, but has to rely on the establishing and solving of mathematical model.…”

Section: Introductionmentioning

confidence: 99%

On-line monitoring of the crystallization process: relationship between crystal size and electrical impedance spectra

Zhao

Yao

Wang

2016

Meas. Sci. Technol.

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On-line monitoring of crystal size in the crystallization process is crucial to many pharmaceutical and fine-chemical industrial applications. In this paper, a novel method is proposed for the on-line monitoring of the cooling crystallization process of L-glutamic acid (LGA) using electrical impedance spectroscopy (EIS). The EIS method can be used to monitor the growth of crystal particles relying on the presence of an electrical double layer on the charged particle surface and the polarization of double layer under the excitation of alternating electrical field. The electrical impedance spectra and crystal size were measured on-line simultaneously by an impedance analyzer and focused beam reflectance measurement (FBRM), respectively. The impedance spectra were analyzed using the equivalent circuit model and the equivalent circuit elements in the model can be obtained by fitting the experimental data. Two equivalent circuit elements, including capacitance (C 2 ) and resistance (R 2 ) from the dielectric polarization of the LGA solution and crystal particle/solution interface, are in relation with the crystal size. The mathematical relationship between the crystal size and the equivalent circuit elements can be obtained by a non-linear fitting method. The function can be used to predict the change of crystal size during the crystallization process.

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“…Effort was also made to extract particle shape information from FBRM CLD measurements such as the imaginative work of (Ma et al, 2001;Yamamoto et al, 2002), but concern remains on the magnitude of error that is introduced in the conversion from CLD to crystal shape. Microscopy imaging is considered as probably the most promising technique for measuring particle shape since one can see the shape of the particles, as a result has attracted much attention in recent years De Anda et al (Calderon De Anda et al, 2005a;Calderon De Anda et al, 2005b;De Anda et al, 2005), Wang et al (Wang et al, 2007) and Larsen et al (Larsen and Rawlings, 2009;Larsen et al, 2006Larsen et al, , 2007 used a GSK imaging system with non-invasive high-speed camera to record images and monitor the particle shape and size in a stirred batch crystalliser. Zhou et al (Zhou et al, 2011;Zhou et al, 2009) used image analysis to automatically extract the maximum possible information from in situ digital particle vision and measurement (PVM) images, which was employed to monitor particle shape and size distribution on-line.…”

Section: Introductionmentioning

confidence: 99%

On-line measurement of the real size and shape of crystals in stirred tank crystalliser using non-invasive stereo vision imaging

Zhang

Cai

Liu

et al. 2015

Chemical Engineering Science

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Non-invasive stereo vision imaging technique was applied to monitoring a cooling crystallisation process in a stirred tank for real-time characterisation of the size and shape of needle-like Lglutamic acid (LGA)  polymorphic crystals grown from solution. The instrument consists of two cameras arranged in an optimum angle that take 2D images simultaneously and are synchronised with the lighting system. Each 2D image pair is processed and analysed and then used to reconstruct the 3D shape of the crystal. The needle shaped LGA  form crystal length thus obtained is found to be in good agreement with the result obtained from off-line analysis of crystal samples, and is about three times larger than that estimated using 2D imaging technique. The result demonstrates the advantage of 3D imaging over 2D in measurement of crystal real size and shape.

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Real‐time product morphology monitoring in crystallization using imaging technique

Cited by 99 publications

References 29 publications

Precision measurement of the growth rate and mechanism of ibuprofen {001} and {011} as a function of crystallization environment

Precision measurement of the growth rate and mechanism of ibuprofen {001} and {011} as a function of crystallization environment

On-line monitoring of the crystallization process: relationship between crystal size and electrical impedance spectra

On-line measurement of the real size and shape of crystals in stirred tank crystalliser using non-invasive stereo vision imaging

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