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Immer im Bild mittels Prozess-Spektroskopie - Spektroskopische Methoden für die Prozessanalytik
(2012)
Spektroskopische Methoden sind in der Regel zerstörungsfrei und liefern stetig Informationen, die zur Prozess-Steuerung eingesetzt werden können. Präzise Messungen unter Prozessbedingungen wurden vor allem durch die Entwicklung leistungsfähiger Sonden und Durchfluss-Systeme möglich. In Kombination mit multivariater Datenanalyse lassen sich diese Methoden auch zur Identifizierung und Quantifizierung von Stoffströmen einsetzen.
Quantitative online NMR spectroscopy of technical mixtures: on the fly quantification of fluids
(2014)
In this paper quantitative NMR spectroscopy is demonstrated as a tool for process analytical technology (PAT) in order to obtain real time information from dynamic processes. Different methods for quantification are presented and as a result the limit of detection for NMR measurement could be determined to 3.3 mg kg-1 (ethanol in water). As model processes esterification reactions and dissolution of pharmaceutical formulations are presented and important process parameters are extracted. Furthermore it is demonstrated that not only 1H-NMR spectroscopy can be used for process monitoring but also 13C-NMR for technical mixtures.
Establishing ZIF‐8 as a reference material for hydrogen cryoadsorption: An interlaboratory study
(2024)
Hydrogen storage by cryoadsorption on porous materials has the advantages of low material cost, safety, fast kinetics, and high cyclic stability. The further development of this technology requires reliable data on the H2 uptake of the adsorbents, however, even for activated carbons the values between different laboratories show sometimes large discrepancies. So far no reference material for hydrogen cryoadsorption is available. The metal‐organic framework ZIF‐8 is an ideal material possessing high thermal, chemical, and mechanical stability that reduces degradation during handling and activation. Here, we distributed ZIF‐8 pellets synthesized by extrusion to 9 laboratories equipped with 15 different experimental setups including gravimetric and volumetric analyzers. The gravimetric H2 uptake of the pellets was measured at 77 K and up to 100 bar showing a high reproducibility between the different laboratories, with a small relative standard deviation of 3–4 % between pressures of 10–100 bar. The effect of operating variables like the amount of sample or analysis temperature was evaluated, remarking the calibration of devices and other correction procedures as the most significant deviation sources. Overall, the reproducible hydrogen cryoadsorption measurements indicate the robustness of the ZIF‐8 pellets, which we want to propose as a reference material.
qNMR - The handbook
(2023)
Quantitative NMR (qNMR) has been around for a long time, but also has great potential to solve future problems in any quantitative analysis. As a primary method, it differs fundamentally from chromatographic methods: it is better described as a quantum mechanical balance. Succesful implementation of qNMR requires certain attention to detail. "qNMR - the handbook" is intended to be a guide for analysts to help understand the fundamental principles of NMR and the significant points relating to its implementation for quantitation. Regulatory considerations of qNMR adoption are explained. NMR fundamentals are explained to provide understanding. Together with many useful examples, the book is a compelling addition to the laboratory's reference library, providing all the tools that any practitioner should know to successfully implement qNMR.
The authors are qNMR pioneers and come from a variety of backgrounds including business, government and academia.