Application of Laser‐Backscattering Instruments for In Situ Monitoring of Crystallization Processes – A Review

Laser-backscattering instruments, such as the focused beam reflectance measurement or threefold dynamical optical reflectance measurement, are promising tools to aid crystallization process development, allowing an in situ, real-time, and nondestructive measurement of particle size distributions. Besides the instrument principles, in detail geometrical and optical models are discussed which deconvolute the recorded chord length distribution. Emphasis is thereby laid on the influence of the suspension density on instrument recordings. The application of laser-backscattering devices for determination of kinetic constants is discussed and future directions and perspectives are given.

[1]  Joachim Ulrich,et al.  Data Preprocessing of In Situ Laser‐Backscattering Measurements , 2011 .

[2]  Niall A. Mitchell,et al.  Nucleation kinetics of paracetamol-ethanol solutions from induction time experiments using Lasentec FBRM® , 2011 .

[3]  Ulrich Bröckel,et al.  Anwendbarkeit der Lasermessverfahren FBRM und 3D ORM SMF in Batch‐Kristallisationen , 2011 .

[4]  J. Ulrich,et al.  Crystallization kinetics of α-ammonium chloride monitored by in-situ measurement techniques , 2011 .

[5]  Michael J. Hounslow,et al.  Influence of electronic antifouling on agglomeration of calcium carbonate , 2011 .

[6]  A. Seidel-Morgenstern,et al.  Application of a recent FBRM-probe model to quantify preferential crystallization of DL-threonine , 2010 .

[7]  Z. Nagy,et al.  Investigation of the Effect of Temperature Cycling on Surface Features of Sulfathiazole Crystals during Seeded Batch Cooling Crystallization , 2010 .

[8]  R. Tan,et al.  Implementation of Focused Beam Reflectance Measurement (FBRM) in Antisolvent Crystallization to Achieve Consistent Product Quality , 2010 .

[9]  J. Herri,et al.  Chord length distributions measurements during crystallization and agglomeration of gas hydrate in a water-in-oil emulsion: Simulation and experimentation , 2010 .

[10]  A. Chen,et al.  Study on growth kinetics of phosphoric acid hemihydrate using FBRM , 2009 .

[11]  W. Gille Geometric figures with the same chord length probability density function: Six examples , 2009 .

[12]  Wolfgang Marquardt,et al.  Estimation of particle size distributions from focused beam reflectance measurements based on an optical model , 2009 .

[13]  Wolfgang Marquardt,et al.  Process Analysis by Means of Focused Beam Reflectance Measurements , 2009 .

[14]  Andreas Seidel-Morgenstern,et al.  Parameterization of population balance models for polythermal auto seeded preferential crystallization of enantiomers , 2009 .

[15]  Ali N. Saleemi,et al.  The impact of direct nucleation control on crystal size distribution in pharmaceutical crystallization processes , 2009 .

[16]  R. Braatz,et al.  Robust Bayesian estimation of kinetics for the polymorphic transformation of L‐glutamic acid crystals , 2008 .

[17]  Carolyn A. Koh,et al.  Measuring the particle size of a known distribution using the focused beam reflectance measurement technique , 2008 .

[18]  Marco Mazzotti,et al.  Measurement of particle size and shape by FBRM and in situ microscopy , 2008 .

[19]  B. Glennon,et al.  Comparison of Morphological Characteristics of Streptomyces natalensis by Image Analysis and Focused Beam Reflectance Measurement , 2008, Biotechnology progress.

[20]  Carolyn A. Koh,et al.  Hydrate formation from high water content-crude oil emulsions , 2008 .

[21]  W. Marquardt,et al.  Analysis of FBRM measurements by means of a 3D optical model , 2008 .

[22]  Weili Yu,et al.  Chord length characterization using focused beam reflectance measurement probe - methodologies and pitfalls , 2008 .

[23]  Michael J. Hounslow,et al.  Determining kinetics of calcium carbonate precipitation by inline technique , 2008 .

[24]  Sohrab Rohani,et al.  Kinetics Estimation and Single and Multi-Objective Optimization of a Seeded, Anti-Solvent, Isothermal Batch Crystallizer , 2008 .

[25]  D. Wilkinson,et al.  Characterization of Organic and Inorganic Chemicals Formed by Batch-Cooling Crystallization: Shape and Size , 2008 .

[26]  M. Sheikhzadeh,et al.  Real-time optimal control of an anti-solvent isothermal semi-batch crystallization process , 2008 .

[27]  Zoltan K. Nagy,et al.  Special Issue: Pharmaceutical Engineering , 2007 .

[28]  Guido Dünnebier,et al.  FDA PAT Initiative – Eine Anwendersicht zu technischen Möglichkeiten und aktueller industrieller Umsetzung , 2007 .

[29]  H. Masuhara,et al.  Crystallization of Glycine by Photon Pressure of a Focused CW Laser Beam , 2007 .

[30]  Don W. Green,et al.  Perry's Chemical Engineers' Handbook , 2007 .

[31]  Jingkang Wang,et al.  The influence of impurities on phosphoric acid hemihydrate crystallization , 2007 .

[32]  Wolfgang Marquardt,et al.  Advanced Geometrical Modeling of Focused Beam Reflectance Measurements (FBRM) , 2007 .

[33]  D. Ramkrishna,et al.  Transformation of the chord-length distributions to size distributions for nonspherical particles with orientation bias , 2007 .

[34]  M. Sheikhzadeh,et al.  Control of Supersaturation in a Semibatch Antisolvent Crystallization Process Using a Fuzzy Logic Controller , 2007 .

[35]  J. Chew,et al.  Comparison between Open-Loop Temperature Control and Closed-Loop Supersaturation Control for Cooling Crystallization of Glycine , 2007 .

[36]  M. Morbidelli,et al.  Modeling Focused Beam Reflectance Measurement and its Application to Sizing of Particles of Variable Shape , 2006 .

[37]  M. Morbidelli,et al.  Sizing Polydisperse Dispersions by Focused Beam Reflectance and Small Angle Static Light Scattering , 2006 .

[38]  A. Myerson,et al.  Laboratory Scale Batch Crystallization and the Role of Vessel Size , 2006 .

[39]  Kumar Patchigolla,et al.  Obtaining Particle Size Distribution from Chord Length Measurements , 2006 .

[40]  M. Morbidelli,et al.  Aggregation of concentrated polymer latex in stirred vessels , 2006 .

[41]  M. Pons,et al.  Modeling of chord length distributions , 2006 .

[42]  Ronald W. Rousseau,et al.  Batch and Tubular-Batch Crystallization of Paracetamol: Crystal Size Distribution and Polymorph Formation , 2006 .

[43]  P. Bahri,et al.  Polymer flocculation of calcite: Population balance model , 2006 .

[44]  M. Mazzotti,et al.  In Situ Monitoring and Modeling of the Solvent-Mediated Polymorphic Transformation of l-Glutamic Acid , 2006 .

[45]  Ronald W. Rousseau,et al.  Utilization of Focused Beam Reflectance Measurement in the Control of Crystal Size Distribution in a Batch Cooled Crystallizer , 2006 .

[46]  M. Mazzotti,et al.  Precipitation of L‐Glutamic Acid: Determination of Nucleation Kinetics , 2006 .

[47]  M. Hounslow,et al.  In Situ Observation of the Conversion of Sodium Carbonate to Sodium Carbonate Monohydrate in Aqueous Suspension , 2005 .

[48]  Marco Mazzotti,et al.  Restoration of PSD from Chord Length Distribution Data using the Method of Projections onto Convex Sets , 2005 .

[49]  Kumar Patchigolla,et al.  Determination of non-spherical particle size distribution from chord length measurements. Part 2: Experimental validation , 2005 .

[50]  E. Kougoulos,et al.  Modelling particle disruption of an organic fine chemical compound using Lasentec focussed beam reflectance monitoring (FBRM) in agitated suspensions , 2005 .

[51]  D. Wilkinson,et al.  Comparison of Particle Size Distributions Measured Using Different Techniques , 2005 .

[52]  Mingzhong Li,et al.  Determination of non-spherical particle size distribution from chord length measurements. Part 1: Theoretical analysis , 2005 .

[53]  Pui Shan Chow,et al.  Effects of operating conditions on agglomeration and habit of paracetamol crystals in anti-solvent crystallization , 2005 .

[54]  Panagiota Angeli,et al.  Drop size distribution in highly concentrated liquid–liquid dispersions using a light back scattering method , 2005 .

[55]  A. Seidel-Morgenstern,et al.  Crystal Growth Kinetics via Isothermal Seeded Batch Crystallization: Evaluation of Measurement Techniques and Application to Mandelic Acid in Water , 2005 .

[56]  Joachim Ulrich,et al.  Industrial Crystallization: Developments in Research and Technology , 2004 .

[57]  B. Glennon,et al.  Monitoring of cell growth using the focused beam reflectance method , 2004 .

[58]  R. Braatz,et al.  Parameter Estimation and Optimization of a Loosely Bound Aggregating Pharmaceutical Crystallization Using in Situ Infrared and Laser Backscattering Measurements , 2004 .

[59]  N. Kubota,et al.  Process Control of Seeded Batch Cooling Crystallization of the Metastable α-Form Glycine Using an In-Situ ATR-FTIR Spectrometer and an In-Situ FBRM Particle Counter , 2004 .

[60]  M. Mazzotti,et al.  Model-Based Optimization of Particle Size Distribution in Batch-Cooling Crystallization of Paracetamol , 2004 .

[61]  Terence Allen,et al.  Powder Sampling and Particle Size Determination , 2003 .

[62]  B. Glennon,et al.  Focussed beam reflectance measurement (FBRM) monitoring of particle size and morphology in suspension cultures of Morinda citrifolia and Centaurea calcitrapa , 2003, Biotechnology Letters.

[63]  R. Braatz,et al.  Measurement of particle size distribution in suspension polymerization using in situ laser backscattering , 2003 .

[64]  E. Wynn,et al.  Relationship between particle-size and chord-length distributions in focused beam reflectance measurement: stability of direct inversion and weighting , 2003 .

[65]  C. Nascimento,et al.  In-line monitoring of crystallization processes using a laser reflection sensor and a neural network model , 2003 .

[66]  M. Mazzotti,et al.  Choice of the Focal Point Position Using Lasentec FBRM , 2003 .

[67]  R. Braatz,et al.  Paracetamol Crystallization Using Laser Backscattering and ATR-FTIR Spectroscopy: Metastability, Agglomeration, and Control , 2002 .

[68]  Parisa A. Bahri,et al.  Estimating Average Particle Size by Focused Beam Reflectance Measurement (FBRM) , 2002 .

[69]  J. W. Goodwin,et al.  Factors governing emulsion droplet and solid particle size measurements performed using the focused beam reflectance technique , 2001 .

[70]  R. Braatz,et al.  Solute concentration prediction using chemometrics and ATR-FTIR spectroscopy , 2001 .

[71]  F. Puel,et al.  On-line ATR FTIR measurement of supersaturation during solution crystallization processes. Calibration and applications on three solute/solvent systems , 2001 .

[72]  Karen A. McDonald,et al.  Characterization of plant suspension cultures using the focused beam reflectance technique , 2001, Biotechnology Letters.

[73]  K. Sommer 40 Years of Presentation Particle Size Distributions–Yet Still Incorrect? , 2001 .

[74]  P. Langston,et al.  Non‐Spherical 2‐Dimensional Particle Size Analysis from Chord Measurements using Bayes' Theorem , 2001 .

[75]  M. Mazzotti,et al.  Modeling and Experimental Analysis of PSD Measurements through FBRM , 2000 .

[76]  B. Glennon,et al.  In‐line FBRM Monitoring of Particle Size in Dilute Agitated Suspensions , 1999 .

[77]  S. Rohani,et al.  Determination of Particle Size Distribution by Par-Tec® 100: Modeling and Experimental Results , 1998 .

[78]  Michael J. Hounslow,et al.  Coincidence correction for electrical-zone (Coulter-counter) particle size analysers , 1997 .

[79]  A. J. Bale,et al.  Adaptation of focused beam reflectance measurement to in-situ particle sizing in estuaries and coastal waters , 1997 .

[80]  J. Klein,et al.  Particle Size Determination by Laser Reflection: Methodology and problems , 1996 .

[81]  J. Ulrich Entwicklungen bei der Lösungskristallisation in den letzten Jahren , 1994 .

[82]  C. Dobbs,et al.  The Use of Laser Backscatter Instrumentation for the on-line measurement of the particle size distribution of emulsions , 1993 .

[83]  Richard A. Williams,et al.  In situ measurement of particle aggregation and breakage kinetics in a concentrated suspension , 1992 .

[84]  Hiroshi Takubo,et al.  Refractive index as a measure for saturation and supersaturation in crystal growth of water-soluble substances , 1990 .

[85]  S. D. Wicksell,et al.  THE CORPUSCLE PROBLEM. SECOND MEMOIR CASE OF ELLIPSOIDAL CORPUSCLES , 1926 .

[86]  S. D. Wicksell,et al.  THE CORPUSCLE PROBLEM. A MATHEMATICAL STUDY OF A BIOMETRIC PROBLEM , 1925 .

[87]  Z. Nagy,et al.  Adaptive concentration control of cooling and antisolvent crystallization with laser backscattering measurement , 2009 .

[88]  Reginald B. H. Tan,et al.  Recent Advances in Crystallization control: An Industrial Perspective , 2007 .

[89]  Richard D. Braatz,et al.  Experimental design and inferential modeling in pharmaceutical crystallization , 2001 .

[90]  Terence Allen,et al.  Modern Methods of On-Line Size Analysis for Particulate Process Streams†‡ , 1991 .

[91]  J. Ulrich,et al.  Use of the laser diffraction technique for particle size measurement at high suspension densities , 1990 .

[92]  John Garside,et al.  Industrial crystallization from solution , 1985 .

[93]  Kurt Leschonski,et al.  Representation and Evaluation of Particle Size Analysis Data , 1984 .