The Impact of Operating Parameters on the Polymorphic Transformation of <scp>d</scp>-Mannitol Characterized in Situ with Raman Spectroscopy, FBRM, and PVM

Su, Weiyi; Hao, Hongxun; Barrett, Mark; Glennon, Brian

doi:10.1021/op100228f

Cited by 49 publications

(51 citation statements)

References 20 publications

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“…For the sake of completeness, some more unusual techniques for studying catalytic reactions should also be described, which enable monitoring of changes in solid particles such as phase transformations and crystallization [24][25][26]. This could be of interest for heterogeneously catalyzed reactions, too, because coupling with spectroscopic methods, such as Raman, ATR-FTIR, and UV-vis, can provide more detailed structural information.…”

Section: Methods Couplingmentioning

confidence: 99%

“…Su et al [24] studied the polymorphic transformation of d-mannitol by in situ Raman spectroscopy coupled with FBRM (focused beam reflectance measurement) and PVM (particle vision measurement). In this way, relationships between fine particles and metastable-form dissolution, and also between coarse particles and stable-form crystallization, could be defined.…”

Section: Methods Couplingmentioning

confidence: 99%

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Reaction Monitoring in Multiphase Systems: Application of Coupled In Situ Spectroscopic Techniques in Organic Synthesis

Knöpke

Bentrup

2013

Heterogeneous Catalysts for Clean Technology

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In situ spectroscopy is the only approach to obtain reliable information on mechanisms and the role of intermediates in chemical reactions as well as on structure-reactivity relationships in catalysis [1][2][3][4][5]. Especially, in heterogeneous catalysis, the application of a variety of in situ methods has gained a lively development during the recent two decades. But also in homogeneous catalysis, as well as in catalytic multiphase systems, in situ characterization methods are increasingly applied. A survey of techniques, which are most commonly applied in gas/solid and multiphase systems and the method-specific information, is presented in Table 3.1.The vibrational spectroscopies, Raman and Fourier transform infrared spectroscopy (FTIR) provide complementary information. While FTIR spectroscopy requires groups with a permanent dipole moment, Raman spectroscopy needs groups that have polarizable bonds. As a result, certain vibrations of functional groups are active or inactive in the infrared or Raman spectra, respectively. Thus, the spectra of molecules such as water or carbon monoxide show strong bands in the infrared spectra but only very weak bands in the Raman spectra. However, this is advantageous for measurements in aqueous systems. Furthermore, bands resulting from metal-nonmetal vibrations can be observed well with Raman spectroscopy. A disadvantage of Raman spectroscopy is the possible damage or fluorescence of the sample when irradiated with Raman laser light. In particular, the analysis of condensed aromatic systems can be perturbed by fluorescence. Consequently, the combination of both methods provides comprehensive information about the vibrational state of molecules or adsorbed species.Ultraviolet-visible (UV-vis) spectroscopy gives less distinct information about the molecular structure than infrared and Raman spectroscopies. Typically, the bands appearing in UV-vis spectra are rather broad. This is because of the simultaneous excitation of rotational, vibrational, and electronic transitions. The bands appearing in the UV-vis spectra of organic molecules are prominent for chromophores. These chromophores can be small parts of the sample molecule, but in extreme cases also the complete electronic shell of the sample molecule.

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Section: Methods Couplingmentioning

confidence: 99%

Section: Methods Couplingmentioning

confidence: 99%

Reaction Monitoring in Multiphase Systems: Application of Coupled In Situ Spectroscopic Techniques in Organic Synthesis

Knöpke

Bentrup

2013

Heterogeneous Catalysts for Clean Technology

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“…Barrett et al [25,61] used the PVM imaging probe in the determination of the metastable zone of an inorganic compound and also for tracking the polymorphic transformation process of D-Mannitol crystals. Patience and Rawlings [18] investigated the use of the PVM for measuring the shape and size information of sodium chlorate crystals with support from Pfizer.…”

Section: Two-dimensional Imaging Approachesmentioning

confidence: 99%

“…However, several researchers found that it is not trivial to apply these software systems directly to images obtained under an on-line process environment, e.g. for slurries of particles which are suspended in solution [19,25,61]. The major challenges in such situations lie in the fact that the slurries in a stirred tank reactor are in continuous motion, and that the variation of distances from the camera lens to particles captured in a snapshot makes some particles rather poorly resolved and fuzzy in definition as compared to others, reflecting the depth of focus for the microscope objective lens system.…”

Section: Image Analysis and 3d Reconstructionmentioning

confidence: 99%

“…Braatz and co- Detailed simulation and experimental studies showed that by controlling concentration instead of temperature profile, the control strategy can have much lower sensitivities to most practical disturbances and to variations in the nucleation and growth kinetics [183]. Barrett et al [61] proposed an approach to use solute-specific ATR-FTIR absorption peak heights for solute solubility and dissolved concentration, in turn, supersatuation, for the optimization of cooling crystallisation processes. Louhi-Kultanen and co-workers [155,156,184,185] investigated the feedback control of a reactive semi-batch precipitation process of LGA, and proposed a control structure to control the driving force of the reactive crystallisation using the feeding rate of the added acid.…”

Section: Optimisation and Control Of Crystal Size Distribution (Csd)mentioning

confidence: 99%

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Measurement, modelling, and closed-loop control of crystal shape distribution: Literature review and future perspectives

2016

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Crystal morphology is known to be of great importance to the end-use properties of the crystal product and affect the down-stream processing such as in filtration and drying, but was previously regarded as too challenging to achieve automatic closed-loop control. As a consequence, previous work has focused on control the crystal size distribution (CSD) where the size of a crystal is often defined as the diameter of a sphere that has the same volume of the crystal. This paper reviews very promising new advances made in recent years in morphological population balance models for modelling and simulation of crystal shape distribution (CShD), measurement and estimation of crystal facet growth kinetics, as well as in 2D and 3D imaging for on-line characterisation of crystal morphology and CShD. A framework is presented integrating various components in order to achieve the ultimate objective of model-based closed-loop control of CShD. The knowledge gaps and challenges that require further research are also identified.

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Raman Spectroscopy in Process AnalysisUpdate based on the original article by M. Anne Leugers and Elmer D. Lipp, Encyclopedia of Analytical Chemistry , © 2000, John Wiley & Sons, Ltd.

Lipp

Leugers

Chen

et al. 2012

Encyclopedia of Analytical Chemistry

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Process analysis involves the on‐line measurement of chemical or physical properties of a process, generally a manufacturing process, which provides timely data so that the process can be monitored and conditions adjusted if necessary. As a tool for process analysis, Raman spectroscopy has some desirable attributes. Foremost among these are the options for sampling. The use of visible and near‐infrared (NIR) light for the Raman measurement allows the use of commonly available fiber optics for both delivery of light to a sampling point, and then collection of the scattered light and return to a spectrometer. The probes can be insertable into a process or fully noncontact. The noncontact probes operate through windows on the process and provide one of the few means of collecting analytical information without disturbing the process. Raman spectra often provide a high level of chemical and structural information, and the seconds to minutes time frame of the measurement is well suited to process control. In this article, we discuss modern Raman instrumentation and provide a number of application examples, both conventional manufacturing processes and unconventional applications, where the principles and goals of process analysis still apply.

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The Impact of Operating Parameters on the Polymorphic Transformation of d-Mannitol Characterized in Situ with Raman Spectroscopy, FBRM, and PVM

Cited by 49 publications

References 20 publications

Reaction Monitoring in Multiphase Systems: Application of Coupled In Situ Spectroscopic Techniques in Organic Synthesis

Reaction Monitoring in Multiphase Systems: Application of Coupled In Situ Spectroscopic Techniques in Organic Synthesis

Measurement, modelling, and closed-loop control of crystal shape distribution: Literature review and future perspectives

Raman Spectroscopy in Process AnalysisUpdate based on the original article by M. Anne Leugers and Elmer D. Lipp, Encyclopedia of Analytical Chemistry , © 2000, John Wiley & Sons, Ltd.

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