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Industrial Analytical Instrumentation

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Nuclear Magnetic Resonance (NMR) spectroscopy

Magritek release new reaction monitoring
solutions for their Spinsolve benchtop NMR

Magritek, a leading provider of compact NMR and MRI instruments, have released new solutions that enable straightforward reaction monitoring on the Spinsolve benchtop NMR spectrometer. This is complemented with a series of applications notes illustrating the multiple uses for the Spinsolve benchtop NMR spectrometer.

The development of benchtop NMR spectroscopy no longer requires specialist high technology systems with specialist laboratories and highly qualified operators. The use of new, cryogen-free magnet technology and a system that is easily used on the lab bench or made readily portable on a trolley between locations makes NMR analysis available to a wide audience.

One of the largest growth areas for benchtop NMR is reaction monitoring where it is being broadly applied in chemistry and pharmaceutical sciences. NMR has a range of advantages for reaction monitoring. Spectra are chemically specific, enabling measurements to be sensitive to molecular structure and reaction kinetics. With high stability and spectral resolution Magritek's Spinsolve delivers measurements that are quantitative with only minimal calibration. The signal has a linear response to concentration and it is generally not sensitive to the matrix. Results are representative of the complete sample and the measurement is non-destructive.

To enable the Spinsolve spectrometer for reaction monitoring Magritek have created full solutions with either glass flow cells or PTFE flow tubing that fit through the completely clear bore of the instrument. The glass flow cell option offers a large sample volume in the sampling region of the spectrometer and a narrow internal diameter outside of that zone. This gives the maximum signal to noise output with minimal fluid in the flow system. The hardware kit is completed with a peristaltic pump, appropriate tubing, and a stand to provide access below the spectrometer. Complementing the hardware is the full experiment scripting capability and pump control available in the latest instrument software. Stop-flow or continuous flow monitoring is straightforward to set up.

Images: Magritek's comprehensive reaction monitoring solution kit is shown with the Spinsolve benchtop NMR spectrometer. The schematic on the right shows two possible sample kit configurations.

A range of application notes available on the Magritek website help Spinsolve users solve specific problems. For example, consider fermentation processes. This is a naturally occurring chemical event. One application note describes how easy it is to monitor a simple fermentation process - to follow the conversion of fructose and glucose into ethanol and carbon dioxide - and to easily get chemical conversion rates and to see where the optimal end point has occurred. The note shows that a simple flow loop setup allows on-line reaction monitoring on a lab bench. While shimming was performed at the start of the experiment on the reactant itself, no extra shimming was required during the ten day experiment. Even gas bubbles in the measurement volume did not disrupt subsequent measurements.

Benchtop NMR reaction monitoring may also be used for kinetic profiling. Another application note describes the study the hydrolysis of acetic anhydride by water. Rate constants can easily and reliably be obtained by plotting the peak height or integral of a characteristic peak as a function of reaction time. The activation energy of the process can be determined by carrying out the reaction at different temperatures.

Magritek in profile
Magritek provides complete NMR and MRI solutions and applications for Chemical, Pharmaceutical, Oil and Gas, Food and Construction Industries as well as components and subsystems suitable for Research Laboratories and Academic Education. Magritek has offices in Aachen, Germany, San Diego, USA, and Wellington, New Zealand and a global network of distributors and agents to support customers. The initial NMR technology and IP used in Magritek products grew out of decades of world-class research by Ampere prize winner Professor Bernhard Bluemich's group at RWTH Aachen University, and Gunther Laukien prize winner Paul Callaghan's team at Massey University and Victoria University of Wellington.

To see the full list of application notes and other downloads available free from the Magritek,view website: Magritek's Spinsolve benchtop NMR spectrometer is supplied worldwide to academics in teaching and research; to industry for research and reaction monitoring through to product quality control.
Refer to page 901

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