Skip to main content Accessibility help

We use cookies to distinguish you from other users and to provide you with a better experience on our websites. Close this message to accept cookies or find out how to manage your cookie settings.

Close cookie message
×
Hostname: page-component-77c89778f8-gq7q9 Total loading time: 0 Render date: 2024-07-16T18:31:22.220Z Has data issue: false hasContentIssue false

9 - Measuring techniques

Published online by Cambridge University Press:  05 July 2015

Alison Lewis ,
Marcelo Seckler ,
Herman Kramer  and
Gerda van Rosmalen
Alison Lewis
Affiliation:
University of Cape Town
Marcelo Seckler
Affiliation:
Universidade de São Paulo
Herman Kramer
Affiliation:
Technische Universiteit Delft, The Netherlands
Gerda van Rosmalen
Affiliation:
Technische Universiteit Delft, The Netherlands
Get access

Summary

Why this chapter is important

Industrial crystallizers may be seen as devices that create a certain level of supersaturation as the driving force for the generation of the product crystals. Measurement of the supersaturation is therefore of paramount importance to control crystallization processes, as it determines the mechanisms and the rates of elementary crystallization processes such as nucleation, crystal growth and agglomeration. These elementary processes eventually lead to the formation of crystals of a wide spectrum of sizes. The so-called crystal size distribution (CSD), or more generally particle size distribution (PSD), is also a very important product characteristic that not only determines the performance of the crystalline product, but also the efficiency of the downstream processes like filtration and drying, as well as product stability during storage, as explained in Chapter 2.

In this chapter, you will learn various techniques used to measure the supersaturation and the CSD/PSD. In addition, you will have the knowledge to select the most convenient measuring technique according to a given measuring objective and crystallization system. With these tools, you will be able to understand and improve the process as well as the product quality of an industrial crystallization process.

Sampling and dilution procedures

Process measurements can be classified according to the sampling procedure: (a) inline, with a probe inserted in the process; (b) online, recirculating a side stream between the process and the instrument; (c) offline, in a laboratory. In the latter two procedures, a suspension sample must be withdrawn from the crystallizer, diluted and sometimes separated into solids and pure liquid. For the solids characterization, careful attention has to be paid to these procedures; otherwise the measurements are drastically affected (Allen, 2003, Gerla, 1995, Jager, 1990).

Type
Chapter
Information
Industrial Crystallization
Fundamentals and Applications
 , pp. 192 - 209
Publisher: Cambridge University Press
Print publication year: 2015

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

References

Allegra, J. R. and Hawley, S. A. 1972. Attenuation of sound in suspensions and emulsions: theory and experiments. Journal of the Acoustical Society of America, 51, 1545–1564.CrossRefGoogle Scholar
Allen, T. 2003. Powder Sampling and Particle Size Determination, Elsevier.Google Scholar
Bohren, C. F. and Huffman, D. R. 1983. Absorption and Scattering of Light by Small Particles, John Wiley & Sons.Google Scholar
Boxman, A. 1992. Particle Size Measurement for the Control of Industrial Crystallizers. PhD Thesis, Delft University of Technology.Google Scholar
Calderon de Anda, J., Wang, X. Z., Lai, X. and Roberts, K. J. 2005. Classifying organic crystals via in-process image analysis and the use of monitoring charts to follow polymorphic and morphological changes. Journal of Process Control, 15, 785–797.CrossRefGoogle Scholar
Chianese, A. K. M. and Mazzarotta, B. 1995. Nucleation kinetics of pentaerythritol. The Chemical Engineering Journal, 58, 209–214.Google Scholar
Cornel, J., Lindenberg, C. and Mazzotti, M. 2008. Quantitative application of in situ ATR-FTIR and Raman spectroscopy in crystallization processes. Industrial and Engineering Chemistry Research, 47, 4870–4882.CrossRefGoogle Scholar
Dunuwila, D. D. and Berglund, K. A. 1997. ATR-FTIR spectroscopy for in situ measurement of supersaturation. Journal of Crystal Growth, 179, 185–193.CrossRefGoogle Scholar
Févotte, G. 2007. In situ Raman spectroscopy for in-line control of pharmaceutical crystallization and solids elaboration processes: a review. Chemical Engineering Research and Design, 85, 906–920.CrossRefGoogle Scholar
Gerla, J. H. 1995. Modelling, Measurement and Manipulation of Crystallizers, PhD Thesis, Delft University of Technology.Google Scholar
Helt, J. E. and Larson, M. A. 1977. Effects of temperature on the crystallization of potassium nitrate by direct measurement of supersaturation. AIChE Journal, 23, 822–830.CrossRefGoogle Scholar
Hojjati, H. and Rohani, S. 2005. Cooling and seeding effect on supersaturation and final crystal size distribution (CSD) of ammonium sulfate in a batch crystallizer. Chemical Engineering and Processing: Process Intensification, 44, 949–957.CrossRefGoogle Scholar
Hsieh, C. H., Billeter, J., McNally, M. E. P., Hoffman, R. M. and Gemperline, P. J. 2013. Kinetic modeling of dissolution and crystallization of slurries with attenuated total reflectance UV-visible absorbance and near-infrared reflectance measurements. Analytical Chemistry, 85, 5367–5375.CrossRefGoogle ScholarPubMed
Jager, J. 1990. Control of Industrial Crystallizers: The Physical Aspects, PhD Thesis, Delft University of Technology.Google Scholar
Kadam, S. S., Mesbah, A., Van Der Windt, E. and Kramer, H. J. M. 2011. Rapid online calibration for ATR-FTIR spectroscopy during batch crystallization of ammonium sulfate in a semi-industrial scale crystallizer. Chemical Engineering Research and Design, 89, 995–1005.CrossRefGoogle Scholar
Kadam, S. S., Vissers, J. A. W., Forgione, M. et al. 2012. Rapid crystallization process development strategy from lab to industrial scale with PAT tools in skid configuration. Organic Process Research and Development, 16, 769–780.CrossRefGoogle Scholar
Kapembwa, M., Rodríguez-Pascual, M. and Lewis, A. E. 2014. Heat and mass transfer effects on ice growth mechanisms in pure water and aqueous solutions. Crystal Growth and Design, 14, 389–395.CrossRefGoogle Scholar
Kohl, M., Puel, F., Klein, J. P., Hoff, C. and Monnier, O. 2004. Investigation of the growth rate of b-cyclodextrin in water during both flow-cell and batch experiments. Journal of Crystal Growth, 270, 633–645.CrossRefGoogle Scholar
Lee, M.-J., Seo, D.-Y., Wang et al. 2012. Quantitative in-line monitoring of solvent-mediated polymorphic transformation of sulfamerazine by near-infrared spectroscopy. Journal of Pharmaceutical Science, 101, 1578–1586.CrossRefGoogle ScholarPubMed
Lindenberg, C., Cornel, J., Scholl, J. and Mazzotti, M. 2012. ATR-FTIR Spectroscopy. In Industrial Crystallization Process Monitoring and Control, Chianese, A. and Kramer, H. J. M. (eds.), Wiley-VCH Verlag GmbH & Co, 81–91.Google Scholar
Lowe, D. 1987. Three dimensional objet recognition from single two-dimensional images. Artificial Intelligence, 31, 355–395.CrossRefGoogle Scholar
Markande, A., Fitzpatrick, J., Nezzal, A., Aerts, L. and Redl, A. 2013. Application of in-line monitoring for aiding interpretation and control of dextrose monohydrate crystallization. Journal of Food Engineering, 114, 8–13.CrossRefGoogle Scholar
Matthews, H. B. and Rawlings, J. B. 1998. Batch crystallization of a photochemical: modeling, control, and filtration. AIChE Journal, 44, 1119–1127.CrossRefGoogle Scholar
Mullin, J. W. and Leci, C. L. 1972. Desupersaturation of seeded citric acid solutions in a stirred vessel. AIChE Symposium Series, 68, 8–20.Google Scholar
Myreen, K. 2012. In-line process refractometer for concentration measurement in sugar crystal-lizers. In Industrial Crystallization Process Monitoring and Control, Chianese, A. and Kramer, H. J. M. (eds.), Wiley-VCH Verlag GmbH & Co. KGaA, 71–79.Google Scholar
Nývlt, J., Rychlý, R., Gottfried, J. and Wurzelová, Z. 1970. Metastable zone-width of some aqueous solutions. Journal of Crystal Growth, 6, 151–162.CrossRefGoogle Scholar
Perry, R. H. and Chilton, C. H. 2008. Perry's Chemical Engineers' Handbook, McGraw-Hill.Google Scholar
Redman, T., Rohani, S. and Strathdee, G. 1997. Control of the crystal mean size in a pilot plant potash crystallizer. Chemical Engineering Research and Design, 75, 183–192.CrossRefGoogle Scholar
Redman, T. P. and Rohani, S. 1994. On-line determination of supersaturation of KCl-NaCl aqueous solution based on density measurement. Canadian Journal of Chemical Engineering, 72, 64–71.CrossRefGoogle Scholar
Rozsa, L. 1998. The SeedMaster device: for online supersaturation measurement and automatic crystallizer seeding. International Sugar Journal, 100, 601–607.Google Scholar
Schorsch, S., Ochsenbein, D. R., Vetter, T., Morari, M. and Mazzotti, M. 2014. High accuracy online measurement of multidimensional particle size distributions during crystallization. Chemical Engineering Science, 105, 155–168.CrossRefGoogle Scholar
Silva, W. K., Chicoma, D. L. and Giudici, R. 2011. In-situ real-time monitoring of particle size, polymer, and monomer contents in emulsion polymerization of methyl methacrylate by near infrared spectroscopy. Polymer Engineering and Science, 51, 2024–2034.CrossRefGoogle Scholar
Su, W., Hao, H., Barrett, M. and Glennon, B. 2010. The impact of operating parameters on the polymorphic transformation of D-mannitol characterized in situ with Raman spectroscopy, FBRM, and PVM. Organic Process Research and Development, 14, 1432–1437.CrossRefGoogle Scholar
Takubo, H. 1990. Refractive index as a measure for saturation and supersaturation in crystal growth of water-soluble substances. Journal of Crystal Growth, 104, 239–244.CrossRefGoogle Scholar
Trifkovic, M., Rohani, S. and Sheikhzadeh, M. 2012. Kinetics estimation and polymorphic transformation modeling of buspirone hydrochloride. Journal of Crystal Process Technology, 2, 31–43.CrossRefGoogle Scholar
Ulrich, J. and Jones, M. J. 2012. Speed of sound. In Industrial Crystallization Process Monitoring and Control, Chianese, A. and Kramer, H. J. M. (eds.), Wiley-VCH Verlag GmbH & Co, 59–69.Google Scholar
Verma, S. and Shlichta, P. J. 2008. Imaging techniques for mapping solution parameters, growth rate, and surface features during the growth of crystals from solution. Progress in Crystal Growth and Characterization of Materials, 54, 1–120.CrossRefGoogle Scholar
Worlitschek, J. and Mazzotti, M. 2004. Model-based optimization of particle size distribution in batch-cooling crystallization of paracetamol. Crystal Growth and Design, 4, 891–903.CrossRefGoogle Scholar
Wu, J. X., Xia, D., Van Den Berg, F. et al. 2012. A novel image analysis methodology for online monitoring of nucleation and crystal growth during solid state phase transformations. International Journal of Pharmaceutics, 433, 60–70.CrossRefGoogle ScholarPubMed

Save book to Kindle

To save this book to your Kindle, first ensure coreplatform@cambridge.org is added to your Approved Personal Document E-mail List under your Personal Document Settings on the Manage Your Content and Devices page of your Amazon account. Then enter the ‘name’ part of your Kindle email address below. Find out more about saving to your Kindle.

Note you can select to save to either the @free.kindle.com or @kindle.com variations. ‘@free.kindle.com’ emails are free but can only be saved to your device when it is connected to wi-fi. ‘@kindle.com’ emails can be delivered even when you are not connected to wi-fi, but note that service fees apply.

Find out more about the Kindle Personal Document Service.

Available formats
×

Save book to Dropbox

To save content items to your account, please confirm that you agree to abide by our usage policies. If this is the first time you use this feature, you will be asked to authorise Cambridge Core to connect with your account. Find out more about saving content to Dropbox.

Available formats
×

Save book to Google Drive

To save content items to your account, please confirm that you agree to abide by our usage policies. If this is the first time you use this feature, you will be asked to authorise Cambridge Core to connect with your account. Find out more about saving content to Google Drive.

Available formats
×