Analytische Chemie
Filtern
Dokumenttyp
- Vortrag (4)
- Posterpräsentation (2)
Sprache
- Englisch (6)
Referierte Publikation
- nein (6)
Schlagworte
- Process Monitoring (6) (entfernen)
Organisationseinheit der BAM
- 1.4 Prozessanalytik (6) (entfernen)
Eingeladener Vortrag
- nein (4)
Modular chemical production is a tangible implementation of the digital transformation of the specialty chemicals process industry. In particular, it enables acceleration of process development and thus faster time to market by flexibly interconnecting and orchestrating standardized physical modules and bringing them to life. For this purpose, specific (chemical) sensors of process analytics are needed, preferably without lengthy calibration or spectroscopic model development.
An excellent example of a "direct" analytical method is online nuclear magnetic resonance (NMR) spectroscopy. NMR spectroscopy meets the requirements of a direct analytical method because of the direct correlation between the signal area in the spectrum ("counting" the nuclear spins) and the analyte amount of substance concentrations. It is also extremely linear over the concentration range.
With the availability of compact benchtop NMR instruments, it is now possible to bring NMR spectroscopy directly into the field, in close proximity to specialized laboratory facilities, pilot plants, and even industrial-scale production facilities. The first systems are in TRL 8 (Qualified System with Proof of Functionality in the Field).
The presentation will discuss the many building blocks of online nuclear magnetic resonance spectroscopy, from flow cells to automated data analysis.
The departure from the current automation landscape to next generation automation concepts for the process industry has already begun. Smart functions of sensors simplify their use and enable plug-and-play integration, even though they may appear to be more complex at first sight. Monitoring specific information (i.e., “chemical” such as physico-chemical properties, chemical reactions, etc.) is the key to “chemical” process control.
The talk introduces a smart online NMR sensor module provided in an explosion proof housing as example. This sensor was developed for an intensified industrial process (pharmaceutical lithiation reaction step) funded by the EU’s Horizon 2020 research and innovation programme (www.consens-spire.eu). Due to NMR spectroscopy as an “absolute analytical comparison method”, independent of the matrix, it runs with extremely short set-up times in combination with “modular” spectral models. Such models can simply be built upon pure component NMR spectra within a few hours (i.e., assignment of the NMR signals to the components) instead of tedious calibrations runs.
Industry 4.0, IIoT, or Lab 4.0 will enable us to handle more complex processes in shorter time. Intensified production concepts require for adaptive analytical instruments and control technology to realize short set-up times, modular control strategies. They are based on a digitized Laboratory 4.0.
The departure from the current automation landscape to next generation automation concepts for the process industry has already begun. Smart functions of sensors simplify their use and enable plug-and-play integration, even though they may appear to be more complex at first sight. Monitoring specific information (i.e., “chemical” such as physico-chemical properties, chemical reactions, etc.) is the key to “chemical” process control.
The talk introduces a smart online NMR sensor module provided in an explosion proof housing as example. This sensor was developed for an intensified industrial process (pharmaceutical lithiation reaction step) funded by the EU’s Horizon 2020 research and innovation programme (www.consens-spire.eu). Due to NMR spectroscopy as an “absolute analytical comparison method”, independent of the matrix, it runs with extremely short set-up times in combination with “modular” spectral models. Such models can simply be built upon pure component NMR spectra within a few hours (i.e., assignment of the NMR signals to the components) instead of tedious calibrations runs.
The talk also generally covers current aspects of high-field and low-field online NMR spectroscopy for reaction monitoring and process control and gives also an overview on direct dissolution studies of API cocrystals.
Compact nuclear magnetic resonance (NMR) instruments make NMR spectroscopy and relaxometry accessible in industrial and harsh environments for reaction characterization and process control. Robust field integration of NMR systems have to face explosion protection or integration into process control systems with short set-up times. This paves the way for industrial automation in real process environments.
The design of failsafe, temperature and pressure resistant flow through cells along with their NMR-specific requirements is an essential cornerstone to enter industrial production plants and fulfill explosion safety requirements. Additionally, if fast reactions are monitored, suitable mixing devices need to be placed in close vicinity to the measuring volume to mix the reactants properly.
NMR-specific requirements aim at full quantitative pre-magnetization and acquisition with maximum sensitivity while reducing sample transfer times and dwell-times. All parameters are individually dependent on the applied NMR instrument.
Luckily, an increasing number of applications are reported together with an increasing variety of commercial equipment. However, these contributions have to be reviewed thoroughly.
The performance of sample flow cells commonly used in online analytics and especially for low-field NMR spectroscopy was experimentally and theoretically investigated by 1H-NMR experiments and numerical simulations. Especially, the applicability of 3D printed zirconium dioxide for innovative flow cell designs was of interest. Here, we demonstrate and discuss an automated test method to determine the critical parameters of flow through cells for quantitative online NMR spectroscopy. The setup is based on randomized setpoints of flow rates in order to reduce temperature related effects. Five flow cells and tubing were assessed and compared for high-field as well as low-field NMR spectrometers.
The departure from the current automation landscape to next generation automation concepts for the process industry has already begun. Smart functions of sensors simplify their use and enable plug-and-play integration, even though they may appear to be more complex at first sight. Monitoring specific information (i.e., “chemical” such as physico-chemical properties, chemical reactions, etc.) is the key to “chemical” process control. Here we introduce our smart online NMR sensor module provided in an explosion proof housing as example.
Due to NMR spectroscopy as an “absolute analytical comparison method”, independent of the matrix, it runs with extremely short set-up times in combination with “modular” spectral models. Such models can simply be built upon pure component NMR spectra within a few hours (i.e., assignment of the NMR signals to the components) instead of tedious calibrations runs. We present a range of approaches for the automated spectra analysis moving from statistical approach, (i.e., Partial Least Squares Regression) to physically motivated spectral models (i.e., Indirect Hard Modelling and Quantum Mechanical calculations).
Based on concentration measurements of reagents and products by the NMR analyzer a continuous production and direct loop process control were successfully realized for several validation runs in a modular industrial pilot plant and compared to conventional analytical methods (HPLC, near infrared spectroscopy). The NMR analyser was developed for an intensified industrial process funded by the EU’s Horizon 2020 research and innovation programme (“Integrated CONtrol and SENsing”, www.consens-spire.eu).
The departure from the current automation landscape to next generation automation concepts for the process industry has already begun. Smart functions of sensors simplify their use and enable plug-and-play integration, even though they may appear to be more complex at first sight. Monitoring specific information (i.e., “chemical” such as physico-chemical properties, chemical reactions, etc.) is the key to “chemical” process control.
The talk introduces a smart online NMR sensor module provided in an explosion proof housing as example. This sensor was developed for an intensified industrial process (pharmaceutical lithiation reaction step) funded by the EU’s Horizon 2020 research and innovation programme (www.consens-spire.eu). Due to NMR spectroscopy as an “absolute analytical comparison method”, independent of the matrix, it runs with extremely short set-up times in combination with “modular” spectral models. Such models can simply be built upon pure component NMR spectra within a few hours (i.e., assignment of the NMR signals to the components) instead of tedious calibrations runs.
The talk also generally covers current aspects of high-field and low-field online NMR spectroscopy for reaction monitoring and process control giving an overview from direct dissolution studies of API cocrystals to studies of emulsions for a hydroformylation.