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Industrial Analytical Instrumentation

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Nuclear Magnetic Resonance (NMR) spectroscopy

Magritek reports on how undergraduate chemists
at Samford University are using the Spinsolve benchtop
NMR system in their research and education programs

Magritek, a leading provider of compact NMR and MRI instruments, report on the use of their Spinsolve Benchtop NMR spectrometer in the Chemistry Department of Samford University located in Birmingham, Alabama. It is being applied in research in the areas of organic synthesis, reaction methodology and medicinal chemistry.

Dr Paul Wiget is an assistant professor of chemistry at Samford University in Birmingham, Alabama. He first became interested in the Spinsolve instrument when he began interviewing for his current position knowing that his research interests would require a work-around for the lack of a local high-field NMR. Spinsolve, as a two-channel system with indirect-detection, was potentially the answer. The ability to perform 13C, DEPT, HSQC, HMBC experiments was most important. This would be very versatile and helpful in reducing the amount of time formerly needed to spend traveling to and from the high-field instruments used across town at the University of Alabama, Birmingham. Dr Wiget also saw the scripting function as extraordinarily helpful as it would enable the running of a HSQC experiment and followed by an HMBC routine allowing extraction from the 13C data overnight even when measuring dilute samples.

Image: Dr Paul Wiget discusses the value of performing an HMBC experiment and how it gives useful information about a molecule. He is talking with one of his undergraduate students, Ellie Berry, a user of the Magritek Spinsolve Carbon at Samford University, Birmingham, Alabama.

Now having used Spinsolve Carbon system for several months, Dr Wiget describes his array of experiments used in both research and teaching. "We use NMR in our second semester organic laboratory as means to adequately characterize the intermediate and product of a two-step synthesis, an independent project that makes up about two thirds of the students' grade. We have found that often the carbon channel is most useful in this project due to the inherently low dispersion associated with the proton channel; this is in conjunction with IR, GC-MS, UV-Vis, and melting-point analysis. We also have fluorescence and ICP atomic absorption available."

"We also use the reaction monitoring function to obtain kinetic data for our physical chemistry course. This is particularly useful because the experiment we monitor is the esterification of triflouroacetic acid with various alcohols. With the simultaneous 19F and 1H "nested" monitoring scripts, we can get reinforcing data by monitoring the reaction progress via two nuclei instead of just one. Additionally, when the dispersion issue arises during that experiment, we no longer have to abandon the more substituted alcohols because we can simply monitor the reaction via the 19F spectra."

Continuing to describe the benefits of Spinsolve, Dr Wiget says "the greatest benefit of the system is its ease of use and low-level of training for student operation. We are also very fond of no longer needing an air source for spinning. The instrument is very fast and reliable compared to the old, larger, 60 MHz instrument we had. The requirement of consistent spin and the finicky nature of the software made the instrument less practical for student use, and very challenging for research purposes."

Dr Wiget's first publications are ready for submission so keep checking the Magritek blog for news of their release or view their website via the banner link

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.

For further information, view website: http://www.magritek.com   
Refer to page 232

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