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Thought Leader Interview: Prof Patrick Giraudeau

February 19th, 2018, by

A fascinating thought leader interview with Prof Patrick Giraudeau from the University of Nantes discusses how his group uses their Spinsolve benchtop NMR spectrometer for applications such as reaction monitoring, edible oil analysis and implementing ultrafast 2D NMR.

Benchtop NMR systems are better suited to reaction monitoring than high-field systems

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NMR spectroscopy outdoors at a natural gas plant

February 7th, 2018, by

Professor Mike Johns at the University of Western Australia shared this story about doing NMR outdoors with one of their Spinsolve spectrometers. The outdoor environment presents a number of challenges for any analytical instrument and not normally a place you would find NMR spectrometers. Great to hear the trial was successful. Details and pictures below.

In collaboration with Chevron and Woodside, the Fluid Science and Resources Research Group at the University of Western Australia (UWA) trialled a ppm oil-in water measurement protocol built around solid phase extraction and a Magritek 1H 43 MHz Spinsolve benchtop NMR spectrometer. This occurred in October 2017 on the Woodside Pluto LNG plant in North West Australia. Measurements were performed outside, adjacent to the waste water treatment plant, using the SPE-NMR apparatus shown below. The trial was successful with measurements being consistent with laboratory data over a two week period.

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Silicon NMR on Spinsolve – Part 2

August 30th, 2017, by

In my last blog post I introduced silicon NMR on Spinsolve and showed a variety of 1D 29Si{1H} and 29Si-1H DEPT spectra. In this post I’m moving on to talk about some 2D experiments that are useful for silicon studies. One of the most useful and widely used of those is the 1H-29Si HMBC experiment, which correlates proton and silicon chemical shifts over two or more chemical bonds. For example, Figure 1 below shows a 1H-29Si HMBC spectrum of the 1,1,3,3,5,5-hexamethyltrisiloxane sample I used before, collected in around 17 minutes. The 1H spectrum is shown along the horizontal axis of the 2D spectrum, and the 29Si spectrum is shown along the vertical axis.

Fig. 1. 1H-29Si HMBC spectrum of 1,1,3,3,5,5-hexamethyltrisiloxane

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Chemistry Department at Lyon College, Arkansas, uses Spinsolve for research and teaching

July 26th, 2017, by

Dr Irosha Nawarathne is an Assistant Professor in the Chemistry Department at Lyon College, a selective liberal arts institution in rural Arkansas. Her work bridges biomedical research to teaching students the practical use of instrumentation to prepare them for employment and the challenges of the chemical industry. She summarizes her experience with the Spinsolve, which was added to the Chemistry Department in 2015:

Spinsolve has become the most popular among faculty and students of our chemistry program. It is used in organic chemistry, instrumental analysis, and advanced inorganic chemistry laboratories. We plan to extend the usage to other areas too. Students have become very interested in the concept of NMR because of this instrument. Their knowledge of NMR is improved tremendously after the incorporation of Spinsolve in the chemistry program. It is easy to operate, provides quick analysis, and requires very low maintenance. Spinsolve is definitely the best fit for a small college like ours. We formerly had a cryogenic NMR spectrometer at Lyon but the chemistry program has not been able to maintain the instrument in the long term. Spinsolve is low cost and its low maintenance is key for its great fit to Lyon chemistry program. It is also used in recruiting keen students as they get really excited about the instrument and its capabilities during frequent campus tours.

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Ley Group at Cambridge uses Spinsolve Benchtop NMR as part of their flow chemistry and organic synthesis research

June 22nd, 2017, by

Professor Steven Ley’s laboratories are located in the Department of Chemistry at the University of Cambridge. Their research specialises in flow chemistry and organic synthesis. They are renowned for collaborations with academic and industrial partners. Précising their work, Steve says

“Complex synthesis remains a challenging occupation requiring an exceptional level of experimental skill, extensive knowledge of both mechanistic and molecular reactivity, and a bold, inventive, and creative spirit. It is the combination of these qualities that transforms the synthesis process from one of simple logistics to an art form.”

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RIVM in the Netherlands uses the Spinsolve benchtop NMR spectrometer to investigate illegal drugs

June 8th, 2017, by

Dr Peter Keizers is a scientist in the Centre for Health Protection at RIVM, the Dutch National Institute for Public Health and the Environment based in Bilthoven. As a chemist, he investigates (illegal) drugs, medical devices and other medicinal products. His group studies the composition of these products and specifically look for active pharmaceutical ingredients, preferably in a quantitative way.


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Spinsolve as an optimisation tool for a catalyst-free flow reaction

February 15th, 2018, by

The group of Professor Yoshida at the Department of Synthetic Chemistry and Biological Chemistry of Kyoto University has recently published an article showing how Spinsolve benchtop NMR spectroscopy can be used to optimise the reactions of aminating reagents to achieve an efficient C–N bond formation without using any catalyst.


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New Publications on Real-Time Reaction Monitoring

December 14th, 2017, by

Two recent publications (link here and here) in international journals highlight the potential of using the Spinsolve benchtop NMR for real time chemical reaction monitoring.  Interest in using NMR spectroscopy to monitor chemical reactions has been increasing as the information can be used to optimise yield and minimise waste in order to enhance sustainability of the production process.

One of papers from the Ley group at Cambridge University (Musio et al., ACS Sustainable Chem. Eng, 2017) describes how real-time reaction monitoring on Fluorine can be used to optimise the reaction and reduce the environmental impact in the synthesis of functional fluorinated products. The other paper from the Blümich group at RWTH Aachen (Singh et al., Anal. Bioanal. Chem., 409, pp 7223–7234, 2017) evaluates the on-line benchtop NMR reaction monitoring method against off-line GC and high-field NMR methods and finds excellent agreement between them.

Magritek and Quantum Design announce distribution partnership for Spinsolve in South America

August 30th, 2017, by

San Diego 10th August 2017: Magritek, a leading provider of compact NMR and MRI instruments, and Quantum Design, a leading manufacturer and distributor of scientific and industrial instrumentation announce their new distribution partnership. Under the new agreement, Quantum Design South America will distribute Magritek’s product line of Spinsolve Benchtop NMR Spectrometers in South America.

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Silicon NMR on Spinsolve – Part 1

June 22nd, 2017, by

Silicon is one of the most widespread elements in the natural world and, as such, this makes it a very interesting and useful element to study using NMR. Over the past few decades, a wide range of silicon-containing compounds have been investigated using both solid- and liquid-state NMR techniques. For example, siloxane polymers, which are extensively used in biomedical and cosmetic applications, have been extensively studied by NMR to understand their structure and individual building blocks. Similarly, the structure of silicates, zeolites and other materials have been studied by silicon NMR. Silicon NMR has been shown to be a powerful tool for the determination of active end groups, cross-linking moieties and polymer sequencing.

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Using Spinsolve as chemically sensitive online detector for Size-Exclusion Chromatography (SEC–NMR)

February 8th, 2018, by

Manfred Wilhelm’s group of the Institute for Chemical Technology and Polymer Chemistry at Karlsruhe Institute of Technology (KIT) recently published an article evaluating the use of 62 MHz Spinsolve benchtop NMR as a chemically sensitive online detector for size-exclusion chromatography (SEC) of polymers.

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New Publications Featuring Spinsolve in Education

October 4th, 2017, by

Two nice educational applications of Spinsolve benchtop NMR have been published recently as open access in international journals. These papers can be downloaded for free from the links given below. The first one describes a simple method to measure the octanol-water partition coefficient of an organic compound. The second one demonstrates a method to determine the pKa value of some biologically active pyridine-based drugs.

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University College Leuven Limburg use Spinsolve in their undergraduate organic chemistry laboratory program

August 23rd, 2017, by

Dr Hilde Roex is the co-ordinator of the second year organic chemistry laboratory course of the Chemistry Program (Gasthuisberg campus, Faculty Management & Technology). Here, the students apply NMR in their organic chemistry laboratory to identify the molecular structure of their synthesized products. They are taught to see the value of NMR for quality control and its use alongside other analytical methods including gas and liquid chromatography. Their goal is to be able to interpret proton NMR spectra and to learn that proton NMR and FT-IR spectroscopy are complementary techniques. This helps to make students familiar with NMR showing them applications of its wide use in industry.

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13C NMR of Cholesterol on an 80 MHz magnet

June 14th, 2017, by

Cholesterol is an essential molecule found in all animals and is a structural component of animal cell membranes. It is the reason why animal cells are flexible and animals can move, unlike plant cells which have rigid cell walls. Cholesterol is a sterol and the cells in your body synthesize about 1 gram every day.

With recent advances in the performance of benchtop NMR, such as the 80 MHz Spinsolve 80, it is interesting to see the 13C NMR spectra from molecules such as Cholesterol.  With a molecular weight of 386 g/mol and 27 carbon atoms it is a larger molecule than is typical measured on a Carbon-13 capable benchtop NMR spectrometer. Because there are more peaks to resolve, both the sensitivity and resolution of the instrument are tested with this measurement.

The 1D proton-decoupled 13C NMR spectrum of a 400 mM sample of Cholesterol measured by a Spinsolve 80 is shown in the figure below. Because 13C has a lower gyromagnetic ratio than protons, the 13C Larmor frequency is 20 MHz. The region between 20 ppm and 45 ppm has been expanded to show how the carbon peaks are resolved.