36333
2016
eng
698
709
6
88
article
Wiley-VCH Verlag GmbH & Co. KGaA
Weinheim, Germany
1
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Quantitative online NMR spectroscopy in a nutshell
Online NMR spectroscopy is an excellent tool to study complex reacting multicomponent mixtures and gain process insight and understanding. For online studies under process conditions, flow NMR probes can be used in a wide range of temperature and pressure. This paper compiles the most important aspects towards quantitative process NMR spectroscopy in complex multicomponent mixtures and provides examples. After NMR spectroscopy is introduced as an online method and for technical samples without sample preparation in deuterated solvents, influences of the residence time distribution, pre-magnetization, and cell design are discussed. NMR acquisition and processing parameters as well as data preparation methods are presented and the most practical data analysis strategies are introduced.
Chemie Ingenieur Technik
10.1002/cite.201500120
0009-286X
27.06.2016
Nicolai Zientek
Klas Meyer
Simon Kern
Michael Maiwald
deu
uncontrolled
Prozessanalytik
eng
uncontrolled
Process analytical technology
eng
uncontrolled
Online NMR spectroscopy
eng
uncontrolled
Online monitoring
Analytische Chemie
Verlagsliteratur
Datei im Netzwerk der BAM verfügbar ("Closed Access")
44847
2018
eng
3349
3360
14
410
article
Springer
Berlin, Heidelberg
1
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Online low-field NMR spectroscopy for process control of an industrial lithiation reaction—automated data analysis
Monitoring specific chemical properties is the key to chemical process control. Today, mainly optical online methods are applied, which require time- and cost-intensive calibration effort. NMR spectroscopy, with its advantage being a direct comparison method without need for calibration, has a high potential for closed-loop process control while exhibiting short set-up times. Compact NMR instruments make NMR spectroscopy accessible in industrial and rough environments for process monitoring and advanced process control strategies.
We present a fully automated data analysis approach which is completely based on physically motivated spectral models as first principles information (Indirect Hard Modelling – IHM) and applied it to a given pharmaceutical lithiation reaction in the framework of the European Union’s Horizon 2020 project CONSENS. Online low-field NMR (LF NMR) data was analysed by IHM with low calibration effort, compared to a multivariate PLS-R (Partial Least Squares Regression) approach, and both validated using online high-field NMR (HF NMR) spectroscopy.
Analytical and Bioanalytical Chemistry
10.1007/s00216-018-1020-z
https://link.springer.com/article/10.1007/s00216-018-1020-z
1618-2642
1618-2650
07.05.2018
Simon Kern
Klas Meyer
Svetlana Guhl
Patrick Gräßer
Andrea Paul
R. King
Michael Maiwald
eng
uncontrolled
Online NMR spectroscopy
eng
uncontrolled
Process analytical technology
eng
uncontrolled
Partial Least Squares Regression
eng
uncontrolled
Indirect Hard Modeling
eng
uncontrolled
Benchtop NMR Spectroscopy
eng
uncontrolled
Smart Sensors
eng
uncontrolled
CONSENS
Analytische Chemie
1 Analytische Chemie; Referenzmaterialien
1.4 Prozessanalytik
Umwelt
Chemie und Prozesstechnik
Chemische Charakterisierung und Spurenanalytik
Verlagsliteratur
Datei im Netzwerk der BAM verfügbar ("Closed Access")
Sensorik