This week our team is at the excellent Magnetic Moments in Central Europe conference in Prague. Our applications team are there with a working Spinsolve and would be delighted to show you the Spinsolve NMR spectrometer in action. If you are attending please come by our booth to say hi and see the best benchtop NMR for yourself.
There are two naturally occurring NMR active nuclei of Boron, 11B (80.1%) and 10B (19.9%). Both nuclei are quadrupolar with spin of greater than ½. 11B has a spin of 3/2 and 10B is spin 3. In terms of sensitivity, 11B is the better nucleus to use as it has a higher natural abundance, a higher gyromagnetic ration, and a lower quadrupole moment. A Spinsolve benchtop NMR spectrometer with a proton frequency of 60 MHz can be configured to measure the 11B NMR signal which has a frequency of 19.2 MHz.
The 11B NMR spectrum of a 0.23 M solution Sodium tertraphenylborate in MeOH-d4 is shown below. The first spectrum shows the excellent sensitivity of Spinsolve using just 8 scans to acquire a spectrum in only 16 seconds.
In my first two posts on using 1D and 2D NMR methods to assign the peaks of quinine (Figure 1), I looked at the 1H and 13C spectra.
Figure 1. Structure of quinine
In this post, I’m moving on to look at the 1H-13C HSQC spectrum. It’s worth spending a brief moment recapping what HSQC is all about and what info it gives you. In a nutshell, the HSQC experiment correlates proton and carbon chemical shifts over one chemical bond. Another way to put this is that a cross-peak in an HSQC spectrum says, “The proton with this chemical shift is directly attached to the carbon with that chemical shift”. By convention, HSQC spectra are presented with 1H shifts along the horizontal axis and 13C shifts along the vertical axis.
Some variants of HSQC also encode into the phases of the cross-peaks additional information about how many hydrogen atoms are attached to each carbon atom. This is sometimes referred to as multiplicity or DEPT editing. In the multiplicity-edited HSQC spectrum, it is conventional for the CH and CH3 groups to have positive phase, and the CH2 groups to have negative phase, just as in a DEPT-135 spectrum. Figure 2 shows the multiplicity-edited HSQC (“HSQC-ME”) spectrum of our 400 mM quinine sample. The CH2 signals are shown in blue and the CH and CH3 signals in red.
At the Achema conference this week in Frankfurt we have a joint booth with Corning Advanced Flow Reactors. We are running a live Spinsolve Benchtop NMR reaction monitoring setup in combination with a Corning Advanced Flow Reactor. If you are Achema, please come and visit us at our joint booth with Corning AFR Hall 9.2 / Booth A32 and see the powerful combination of Corning Flow Reactors and Magritek Benchtop NMR.
We are very excited to announce the launching of our new Spinsolve Autosampler. It enables up 20 separate samples to be measured in any order and can be fitted to all Spinsolve models. We have been developing this for some time, and already have quite a number of units with some of our reference customers who tell us they are delighted with its operation, functionality and high quality construction.
The Autosampler is particularly useful for customers who often have a series of samples to run on their benchtop NMR and want to save the hassle of having to keep coming back to exchange samples. Another benefit is the ability to increase utilization by setting up a queue of experiments to run on their Spinsolve overnight.
The benchtop NMR business is significantly expanding and therefore Magritek is seeking for an Application Scientist based in our European Headquarters in Aachen, Germany, capable of making a significant contribution to the future success of our company.
Dr Catherine Santai is an Associate Professor of Chemistry & Biochemistry and Program Lead of the Integrative Sciences program at Harrisburg University of Science & Technology. The program utilizes a number of analytical techniques teaching undergraduates about their use, giving them the experience ahead of entering research or industrial roles in later life. So far, the Magritek 60 MHz Spinsolve Benchtop NMR Spectrometer has been used in the Organic Chemistry and Biochemistry laboratory sessions. These provide invaluable hands-on lessons about NMR techniques and analysis of a variety of compounds. NMR is used alongside FTIR (Fourier transfer infrared), AAS (atomic absorption), UV-VIS (ultraviolet – visible) and fluorescence spectroscopies.
Malvern, PA, USA, 4th December 2018: Magritek announces that it has been awarded a major contract by the US Drug Enforcement Administration (DEA) for two Spinsolve 80 Carbon benchtop NMR spectrometers. The purchase was made through a competitive award process and will allow DEA laboratories in Virginia and California to utilize the latest benchtop NMR technology to assist in forensic analysis applications.
Speaking about this prestigious award, Magritek Inc’s CEO, Dr Hector Robert, says
“We are very excited to be awarded this contract by the DEA. The selection of the 80 MHz Spinsolve instrument with 1H, 19F and 13C nuclei provides a versatile system suited to the analysis of many substances studied in forensic science. The systems are supplied with autosamplers which enable the measurement of multiple samples with an automated and efficient workflow.”
The group of Professor Lee Cronin at the University of Glasgow has combined machine learning with a chemical reaction system to speed up the discovery of new chemical reactions, which is an inherently unpredictable and time consuming process. This new approach of an Organic Synthesis Robot uses a Spinsolve Benchtop NMR spectrometer as an integral component. Their work has just been published in the prestigious journal Nature: J. M. Granda, L. Donina, V. Dragone, D.-L. Long and L. Cronin, Nature559, 377–381 (2018), DOI: 10.1038/s41586-018-0307-8
Photograph of the chemical robot
The photo shows the impressive setup of the chemical robot with 27 pumps, valves and six reactors, as well as NMR, IR and MS spectrometers for real-time analytics.
The permitted hydrocarbon content of discharged water from offshore oil and gas exploration is becoming increasingly limited by more stringent legislation. This creates the demand for measurement methods that are sensitive enough to detect contaminants at ppm level, but also compact and robust to field conditions. The group of Professor Mike Johns at the University of Western Australia in Perth has developed a benchtop NMR method to quantify the hydrocarbon content in water at the ppm level.