TY - CONF A1 - Wander, Lukas A1 - Kern, Simon A1 - Meyer, Klas A1 - Guhl, Svetlana A1 - Maiwald, Michael T1 - Assessment and validation of various flow cell designs for quantitative online NMR spectroscopy N2 - Compact nuclear magnetic resonance (NMR) instruments make NMR spectroscopy and relaxometry accessible in industrial and harsh environments for reaction 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. 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. 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 tubings were assessed and compared for high-field as well as low-field NMR spectrometers. T2 - Small Molecule NMR Conference (SMASH) CY - Baveno, Italy DA - 17.09.2017 KW - Online NMR spectroscopy KW - Reaction monitoring KW - Flow cell KW - Process control KW - SMASH PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-419485 UR - http://www.smashnmr.org/conference/program AN - OPUS4-41948 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kern, Simon A1 - Guhl, Svetlana A1 - Meyer, Klas A1 - Paul, Andrea A1 - Maiwald, Michael T1 - Reading between the lines – Automated data analysis for low field NMR spectra N2 - For reaction monitoring and process control using NMR instruments, in particular, after acquisition of the FID the data needs to be corrected in real-time for common effects using fast interfaces and automated methods. When it comes to NMR data evaluation under industrial process conditions, the shape of signals can change drastically due to nonlinear effects. Additionally, the multiplet structure becomes more dominant because of the comparably low-field strengths which results in overlapping of multiple signals. However, the structural and quantitative information is still present but needs to be extracted by applying predictive models. 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 Modeling). By using the benefits of traditional qNMR experiments data analysis models can meet the demands of the PAT community (Process Analytical Technology) regarding low calibration effort/calibration free methods, fast adaptions for new reactants, or derivatives and robust automation schemes. T2 - Small Molecule NMR Conference (SMASH) CY - Baveno, Italy DA - 17.09.2017 KW - Online NMR spectroscopy KW - Data analysis KW - Chemometrics KW - Indirect hard modeling KW - Spectral modeling KW - Line prediction KW - CONSENS KW - SMASH PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-419498 UR - http://www.smashnmr.org/conference/program AN - OPUS4-41949 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael A1 - Kern, Simon A1 - Meyer, Klas A1 - Guhl, Svetlana A1 - Paul, Andrea A1 - Wander, Lukas T1 - Design and validation of a compact online NMR module N2 - Monitoring chemical reactions is the key to process control. Today, mainly optical online methods are applied, which are calibration intensive. NMR spectroscopy has a high potential for direct loop process control while cutting the calibration and validation needs to an minimum and thus exhibiting short set-up times. Compact NMR instruments make NMR spectroscopy accessible in industrial and harsh environments for advanced process monitoring and control. Intensified continuous processes are in focus of current research. Flexible (modular) chemical plants can produce different products using the same equipment with short down-times between campaigns and quick introduction of new products to the market. In continuous flow processes online sensor data and tight closed-loop control of the product quality are mandatory. Data analysis techniques are available but currently mostly used for off-line data analysis to detect the causes of variations in the product quality. This is addressed within the EU’s Research Project CONSENS by the development and integration of a smart NMR module for process monitoring. The presented NMR module is provided in a mobile explosion proof housing and involves a compact spectrometer together with an acquisition unit and a programmable logic controller for automated data preparation (phasing, baseline correction), and evaluation. Such “smart sensors” provide the basis for the future project “Industrie 4.0”, and Industrial Internet of Things (IIoT), along with current requirements to process control, model based control, or soft sensing. The module transforms the acquired online spectra of various technically relevant reactions to either conventional 4‒20 mA signals as well as WiFi based OPC-UA communication protocols, which enables NMR-based advanced process control and funny discussions with plant managers along with automation and safety engineers. T2 - Small Molecule NMR Conference (SMASH) CY - Baveno, Italy DA - 17.09.2017 KW - Online NMR spectroscopy KW - CONSENS KW - Reaction monitoring KW - Process control KW - Process analytical technology KW - Indirect hard modeling KW - Industrie 4.0 KW - Smart sensors KW - SMASH PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-419473 UR - http://www.smashnmr.org/conference/program AN - OPUS4-41947 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -