Microreaction Systems for Education

Liauw, Marcel; Treu, Dlna E.

doi:10.1002/9780470431870.ch12

Cited by 3 publications

(4 citation statements)

References 19 publications

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“…Those include lightfibre optics, sample desk probes, imaging systems, optimised detectors, progress in miniaturisation and use of chemometrics to correlate the spectral data with physical and chemical properties of the samples [6]. In-and online methods could be developed to perform kinetic studies and to control and monitor automated processes, including chemical [7,8] and polymer applications [9 -11]. NIRS is considered superior to mid-IR (MIR) for industrial applications, due to the fact that in the range from 12 500 to 4000 cm -1 (780 -2500 nm), overtone and combination vibrations appear which are less intense than the fundamental vibrations in the MIR [11] and therefore allow the use of much larger sample thickness.…”

Section: Introductionmentioning

confidence: 99%

Fast, noninvasive and simultaneous near‐infrared spectroscopic characterisation of physicochemical stationary phases' properties: From silica particles towards monoliths

Petter

Heigl

Bonn

et al. 2008

J of Separation Science

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The design of novel stationary phases is a permanent demanding challenge in chromatographic separation science to enable analysis with enhanced selectivity, specificity and speed. Therefore, the characterisation of chemical and physical properties is next to calculation of chromatographic parameters essential. Conventionally, chemical parameters including surface coverage are determined by burning combustion or frontal analysis, physical parameters including particle size, pore size, pore volume and surface area are determined by SEM, mercury intrusion porosimetry (MIP) and Brunauer-Emmett-Teller (BET). All these methods are time consuming, invasive and require besides special equipment some special trained laboratory staff. Therefore, we introduced near-infrared spectroscopy (NIRS) as a noninvasive, easy-to-handle technology with wavenumber ranging from 4000 to 10,000 cm(-1) enabling analysis within only a few seconds at higher precision than the conventional methods. Investigated materials comprise porous and nonporous silica gel, carbon-based nanomaterials (fullerenes), polymer beads and monoliths. Different carriers themselves and their kind of derivatisations (RP, normal-phase, ion-exchanger, IMAC (immobilised metal affinity chromatography), affinity) can be determined by applying principal component analysis (PCA) of recorded spectra. Partial least square regression (PLSR) enables the determination of particle size, pore size, pore volume, porosity, total porosity and surface area with one single measurement. For the optimised design of well-defined polymer beads and monoliths, real-time in situ monitoring to control, e. g. particle and pore sizes as well as monomer content during the polymerisation process, can be extremely helpful. In this article, the advantages of this fast, noninvasive high-throughput NIRS methods are summarised, discussed in detail and different applications of the individual characterised materials are shown.

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Section: Introductionmentioning

confidence: 99%

Fast, noninvasive and simultaneous near‐infrared spectroscopic characterisation of physicochemical stationary phases' properties: From silica particles towards monoliths

Petter

Heigl

Bonn

et al. 2008

J of Separation Science

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“…In the 1980s the method became quite popular, which can be attributed to the availability of stand-alone NIR instruments offering enhanced reproducibility, instrumental accessories and statistical software including light-fiber optics, sample desk probes, imaging systems, optimized detectors, progress in miniaturization and use of chemometrics to correlate the spectral data with physical and chemical properties of the sample [2]. In-and on-line methods could be developed to perform kinetic studies and to control and monitor automated processes, including chemical [3] and polymer applications [4]. Near-IR spectroscopy shows higher performance compared to mid-IR (MIR) for industrial applications, due to overtone and combination vibrations appearing in the range from 4,000 to 10,000 cm -1 , allowing the use of much larger sample thickness.…”

Section: Introductionmentioning

confidence: 99%

Infrared Spectroscopy: A Novel Tool for the Physicochemical Characterization of Particulate, Monolithic and Coated Stationary Phases

Huck

Bittner

2011

Chromatographia

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The design of novel stationary phases is a permanent demanding challenge in chromatographic and electrophoretic separation science to enable analysis with enhanced selectivity, specificity and speed. Therefore, the characterization of chemical and physical properties is next to calculation of chromatographic parameters essential. Conventionally, column performance is checked by a test run which only enables to prove efficiency column by column. Chemical parameters including surface coverage is normally analyzed by burning combustion or frontal analysis, physical parameters including particle size, pore size, pore volume and surface area by SEM, mercury intrusion porosimetry and Brunauer Emmett Teller. All these methods are extremely time consuming, invasive and require, beside special equipment, some specially trained lab staff. In order to enable a fast high-throughput control of chemical and physical parameters we introduced near-infrared spectroscopy (NIRS, 4,000-10,000 cm -1 ) as a non-invasive, easy-to-handle technology enabling simultaneous analysis within only a few seconds at higher precision than the conventional applied methods. The method is applicable to porous/non-porous silica gel, carbon-based nano-materials (e.g. fullerenes), polymer beads, monoliths for solidphase extraction, liquid chromatography, micro-liquid chromatography, material-enhanced laser desorption ionization and coated capillaries for capillary electrophoresis and capillary electrochromatography. Different carriers themselves and their kind of chemical derivatization (reversed-phase, normal-phase, ion-exchanger, immobilized affinity chromatography, affinity, endcapping) can be determined by applying principal component analysis of spectra recorded. Partial least square regression enables the determination of physical parameters particle size, pore size, pore volume, porosity, total porosity and surface area with one single measurement in an established quantitative model. For a detailed investigation NIRS imaging, which benefits from the combination of a NIR spectrometer with a microscope, allows to analyze materials of interest with resolution down to 4 lm. For the optimized design of polymeric phases real-time in situ monitoring to control polymerization progress can be highly helpful. In this article, the advantages of this novel infrared-based method for the fast high-throughput quality control are introduced.

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“…Zur vollen Entfaltung des Potenzials der Mikroverfahrenstechnik wird es aber erst kommen, wenn sie bereits in der Ausbildung als Alternative zu den etablierten verfahrenstechnischen Ansätzen vermittelt wird, auch wenn die neue Technologie noch nicht vollständig ausgreift ist [2]. Eine aktuelle Übersicht zu laufenden nationalen und internationalen Aktivitäten haben Liauw und Treu zusammengestellt [3]. Zu den deutschen Hochschulen, die die Integration mikroverfahrenstechnischer Inhalte in die Lehre seit einigen Jahren vorantreiben, gehören unter anderem die RWTH Aachen [2,3], die FriedrichSchiller-Universität Jena [4 -6] und die TU Ilmenau [7].…”

Section: Introductionunclassified

“…Eine aktuelle Übersicht zu laufenden nationalen und internationalen Aktivitäten haben Liauw und Treu zusammengestellt [3]. Zu den deutschen Hochschulen, die die Integration mikroverfahrenstechnischer Inhalte in die Lehre seit einigen Jahren vorantreiben, gehören unter anderem die RWTH Aachen [2,3], die FriedrichSchiller-Universität Jena [4 -6] und die TU Ilmenau [7]. Von der DECHEMA wird seit 2003 ein entsprechender Weiterbildungskurs angeboten [8].…”

Section: Introductionunclassified

μ‐Consortium: Installation of a mobile Plant for Education and Training in Micro Process Engineering

Knochen

Kunz

Turek

et al. 2010

Chemie Ingenieur Technik

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Microreaction Systems for Education

Cited by 3 publications

References 19 publications

Fast, noninvasive and simultaneous near‐infrared spectroscopic characterisation of physicochemical stationary phases' properties: From silica particles towards monoliths

Fast, noninvasive and simultaneous near‐infrared spectroscopic characterisation of physicochemical stationary phases' properties: From silica particles towards monoliths

Infrared Spectroscopy: A Novel Tool for the Physicochemical Characterization of Particulate, Monolithic and Coated Stationary Phases

μ‐Consortium: Installation of a mobile Plant for Education and Training in Micro Process Engineering

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