Category Archives: solid-state NMR

[NMR] Solid-state NMR specialist at EPFL

The Institute of Chemistry and Chemical Engineering at EPFL (ISIC; https://www.epfl.ch/schools/sb/research/isic/) is currently looking for a full-time specialist in solid-state NMR for its NMR platform (https://www.epfl.ch/schools/sb/research/isic/platforms/nuclear_magnetic_resonance/). 

As solid-state NMR specialist, you will have the responsibility to advise and guide EPFL researchers wishing to characterize their samples by solid-state NMR. A major part of the work will be dedicated to the preparation and measurement of these samples.

You will be in charge of the solid-state spectrometers of the ISIC NMR platform (two 400 MHz routine spectrometers, and four research spectrometers at 400, 500 and 900 MHz able to work at low temperature (100 K), fast MAS (100 kHz) with possible coupling to DNP. 

The user pool is large and diverse, (chemistry, material sciences, life sciences, physics …), and we are thus looking for an open-minded, well organized and flexible person with a modern vision and knowledge of solid state NMR and service, who will integrate smoothly into our existing team.
Candidates should submit their application online before 15.01.2021.

More details on the position and the application process here: https://recruiting.epfl.ch/Vacancies/1606/Description/2Contact :
For additional information, please contact Dr Aurélien Bornet (NMR platform leader, aurelien.bornet@epfl.ch) or Prof. Sandrine Gerber (Responsible for ISIC Platforms, sandrine.gerber@epfl.ch).
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[NMR] Open Position of Research Engineer in Solid State NMR – TOTAL Research & Technology Feluy – Belgium

Position of Research Engineer in NMR

The Analytical Department of the Research Center of Feluy (Belgium) being part of the R&D of TOTAL is looking for a Research Engineer specialized in Solid State NMR for a fixed-term contract of 24 months leading to permanent contract.

Under the responsibility of the Structure, Functionality and Morphology Service Manager, the applicant mission will be to:

  • Design, conduct and implement developments in high resolution NMR to provide the key chemical information required by the R&D departments of TOTAL company in the field of materials for energy such as catalysts, polymers, batteries, etc… and in this way participate in the development of new products and resolution of problems encountered by customers or in the Business Units.
  • Evaluate and develop new methods and new equipments.
  • Adapt practices to customer requests and products.
  • Operate High Resolution Solid State NMR equipment.
  • Realize assays, analyze results, draw conclusions, make the necessary recommendations and draft synthetic documents
  • Ensure reliable analytical results,
  • Propose and follows works done with academics in her/his area of ​​competence,
  • Propose equipment investments, maintenance schedules, ensures the availability of machines and consumables,
  • Tutor trainees,

Required Profile:       PhD in chemistry or analytical science. HR SS NMR specialty on battery problematics.

Moreover, Knowledge or experience in High Resolution Liquid NMR and Low Field NMR as well as a background on Catalyst and/or Polymer domains would be highly appreciated

Specific abilities:

  • Great interpersonal skills
  • Project management
  • Strong written and oral communication skills in French and in English.
  • To have an analytical turn of mind
  • To work as a team

To join the NMR reference laboratory of Total R&D in a pluri-disciplinary analytical team, send a curriculum vitae and a motivation letter to: vincent.livadaris@total.com

Vincent LIVADARIS
Raffinage-ChimieDirection Recherche et Développement
Responsable du Service Structure, Fonctionnalité & Morphologie
Tél : +32 (0)64 51 41 18Fax : +32 (0)64 51 08 65vincent.livadaris@total.com
trait.jpg logo.jpgTotal Research & Technology FeluyDépartement AnalyseZone Industrielle
B-7181 Feluy

TOTAL Classification: Restricted Distribution TOTAL – All rights reserved
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ssNMR/DNP ZOOMinar (4/29) : Matthias Ernst and Songi Han #DNPNMR

From the ssNMR mailing list

Date: Sun, 26 Apr 2020 15:10:25 +0000

From: Kong Ooi Tan <kongooi@mit.edu>

Subject: [ssNMR] ssNMR/DNP ZOOMinar (4/29) : Matthias Ernst and Songi Han

Hi all,

I would like to announce our second ZOOMinar session on 4/29, Wed 11 am Boston / 5 pm Zurich / 8 am California. Our speakers are Prof. Matthias Ernst (ETHZ) and Prof. Songi Han (UCSB), the details are:

Zoom link: https://mit.zoom.us/j/91253458660 <https://mit.zoom.us/j/91253458660>

Duration: 1 hr, i.e. 30 mins (23 mins talk + 7 mins Q&A) per speaker

1st speaker: Matthias Ernst, ?Residual Line Width in FSLG Decoupled Proton MAS Spectra?

Recorded (Yes/No): No

-PhD studies with Prof. Richard R. Ernst at ETHZ.

-Postdoc with Prof. Alex Pines at UC Berkeley for 2 years

-Staff scientist with Prof. Beat H. Meier at University of Nijmegen

-Joined ETHZ as a senior scientist in Beat?s group, and promoted to adjunct Professor in 2011.

2nd speaker: Songi Han, ?Asymmetry in Electron Spin Polarization and Coupling drives Cross-Effect and Thermal Mixing DNP?

Recorded (Yes/No): Yes

She received her Doctoral Degree from Aachen University of Technology (RWTH), Germany, in 2001. She pursued her postdoctoral studies at the Max-Planck Institute for Polymer Research, Mainz, and the University of California Berkeley. She joined the faculty at UCSB in 2004, and was promoted to full professor in 2012.

Regards,

Kong

Dr. Kong Ooi Tan

Postdoctoral Fellow

Francis Bitter Magnet Laboratory

Massachusetts Institute of Technology

77 Massachusetts Avenue, NW14-4112

Cambridge, MA 02139

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Structure determination of supra-molecular assemblies by solid-state NMR: Practical considerations #DNPNMR

Demers, Jean-Philippe, Pascal Fricke, Chaowei Shi, Veniamin Chevelkov, and Adam Lange. “Structure Determination of Supra-Molecular Assemblies by Solid-State NMR: Practical Considerations.” Progress in Nuclear Magnetic Resonance Spectroscopy 109 (December 2018): 51–78.

https://doi.org/10.1016/j.pnmrs.2018.06.002

In the cellular environment, biomolecules assemble in large complexes which can act as molecular machines. Determining the structure of intact assemblies can reveal conformations and inter-molecular interactions that are only present in the context of the full assembly. Solid-state NMR (ssNMR) spectroscopy is a technique suitable for the study of samples with high molecular weight that allows the atomic structure determination of such large protein assemblies under nearly physiological conditions.

This review provides a practical guide for the first steps of studying biological supramolecular assemblies using ssNMR. The production of isotope-labeled samples is achievable via several means, which include recombinant expression, cell-free protein synthesis, extraction of assemblies directly from cells, or even the study of assemblies in whole cells in situ. Specialized isotope labeling schemes greatly facilitate the assignment of chemical shifts and the collection of structural data. Advanced strategies such as mixed, diluted, or segmental subunit labeling offer the possibility to study inter-molecular interfaces.

Detailed and practical considerations are presented with respect to first setting up magicangle spinning (MAS) ssNMR experiments, including the selection of the ssNMR rotor, different methods to best transfer the sample and prepare the rotor, as well as common and robust procedures for the calibration of the instrument. Diagnostic spectra to evaluate the resolution and sensitivity of the sample are presented. Possible improvements that can reduce sample heterogeneity and improve the quality of ssNMR spectra are reviewed.

Solid state NMR service across the world #ssNMR

This article is not directly about DNP-NMR spectroscopy. However, since DNP is predominantly used in solid-state NMR spectroscopy it is interesting to see how solid-state NMR is becoming more popular across the worl.

Barrow, Nathan S., and Paul Jonsen. “Solid State NMR Service across the World.” Solid State Nuclear Magnetic Resonance 105 (February 2020): 101626. 

https://doi.org/10.1016/j.ssnmr.2019.101626

In 2013 the EPSRC published a report on the NMR equipment base serving the physical and life sciences community in the UK. Whilst this included both solution and solid state NMR, the report omitted equipment from industry or outside of the UK. This report originated as a means of benchmarking industrial solid state NMR facilities around the world. A survey of 24 SSNMR laboratories was conducted in the first half of 2019, primarily by face-to-face interviews or via telephone. Aggregated statistics relating to service throughput, equipment, and staff are presented, along with discussions about barriers to accessing SSNMR. We found that the hardware profile seen in the earlier UK-only report was representative of the worldwide view, and that the main barrier to access was a lack of knowledge about what SSNMR can do. Publishing this survey provides a strong benchmark for SSNMR laboratories, which will hopefully allow them to identify barriers that might be preventing them from performing to their optimal level in solving materials science problems.

High-sensitivity protein solid-state NMR spectroscopy #DNPNMR

Mandala, Venkata S, and Mei Hong. “High-Sensitivity Protein Solid-State NMR Spectroscopy.” Current Opinion in Structural Biology 58 (October 2019): 183–90.

https://doi.org/10.1016/j.sbi.2019.03.027

The sensitivity of solid-state nuclear magnetic resonance (SSNMR) spectroscopy for structural biology is significantly increased by 1H detection under fast magic-angle spinning (MAS) and by dynamic nuclear polarization (DNP) from electron spins to nuclear spins. The former allows studies of the structure and dynamics of small quantities of proteins under physiological conditions, while the latter permits studies of large biomolecular complexes in lipid membranes and cells, protein intermediates, and protein conformational distributions. We highlight recent applications of these two emerging SSNMR technologies and point out areas for future development.

[NMR] Postdoc: Solid-state NMR at 1.2 GHz

Postdoc position at ETH Zurich:

for the development of fast MAS methods and biomolecular applications at high field (in particular at 1.2 GHz) in the group of Beat Meier (http://nmr.ethz.ch), we look for a postdoctoral researcher with a strong experimental background in solid-state NMR. Experience with NMR hardware and with biomolecular applications and structural biology is an asset. Spectrometers at 600 and 850 MHz are available and a 1.2 GHz system is expected in the first half of 2020.

The position is available from January 1, 2020 (or later) and is initially planned for for 1 year (renewable). Candidates should send a CV and the names of at least two references to Beat Meier (beme@ethz.ch)

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[NMR] Postdoc: Solid-state NMR at 1.2 GHz

Postdoc position at ETH Zurich: for the development of fast MAS methods and biomolecular applications at high field (in particular at 1.2 GHz) in the group of Beat Meier (http://nmr.ethz.ch), we look for a postdoctoral researcher with a strong experimental background in solid-state NMR. Experience with NMR hardware and with biomolecular applications and structural biology is an asset. Spectrometers at 600 and 850 MHz are available and a 1.2 GHz system is expected in the first half of 2020.

The position is available from January 1, 2020 (or later) and is initially planned for for 1 year (renewable). Candidates should send a CV and the names of at least two references to Beat Meier (beme@ethz.ch)

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TmDOTP: An NMR-based thermometer for magic angle spinning NMR experiments

Knowing the actual sample temperature in a solid-state NMR experiment is crucial in many ways. Many different approaches exist from measuring the chemical shift difference in spectra of ethylene glycol (solution-state NMR spectroscopy) to measuring the peak position in lead nitrate or the T1 relaxation times of KBr (solid-state NMR spectroscopy). All of these methods have their pros and cons. This approach using TmDOTP, having a temperature coefficient of 1ppm/K and being inert to biopolymers is a valuable addition to the ssNMR toolbox.

Zhang, Dongyu, Boris Itin, and Ann E. McDermott. “TmDOTP: An NMR-Based Thermometer for Magic Angle Spinning NMR Experiments.” Journal of Magnetic Resonance 308 (November 1, 2019): 106574.

https://doi.org/10.1016/j.jmr.2019.106574

Solid state NMR is a powerful tool to probe membrane protein structure and dynamics in native lipid membranes. Sample heating during solid state NMR experiments can be caused by magic angle spinning and radio frequency irradiation such heating produces uncertainties in the sample temperature and temperature distribution, which can in turn lead to line broadening and sample deterioration. To measure sample temperatures in real time and to quantify thermal gradients and their dependence on radio frequency irradiation or spinning frequency, we use the chemical shift thermometer TmDOTP, a lanthanide complex. The H6 TmDOTP proton NMR peak has a large chemical shift (−176.3 ppm at 275 K) and it is well resolved from the protein and lipid proton spectrum. Compared to other NMR thermometers (e.g., the proton NMR signal of water), the proton spectrum of TmDOTP, particularly the H6 proton line, exhibits very high thermal sensitivity and resolution. In MAS studies of proteoliposomes we identify two populations of TmDOTP with differing temperatures and dependency on the radio frequency irradiation power. We interpret these populations as arising from the supernatant and the pellet, which is sedimented during sample spinning. In this study, we demonstrate that TmDOTP is an excellent internal standard for monitoring real-time temperatures of biopolymers without changing their properties or obscuring their spectra. Real time temperature calibration is expected to be important for the interpretation of dynamics and other properties of biopolymers.

Solid-state NMR of nanocrystals #DNPNMR

Gutmann, Torsten, Pedro B. Groszewicz, and Gerd Buntkowsky. “Solid-State NMR of Nanocrystals.” In Annual Reports on NMR Spectroscopy, 97:1–82. Elsevier, 2019.

https://doi.org/10.1016/bs.arnmr.2018.12.001

Recent advances in solid-state nuclear magnetic resonance (NMR) spectroscopy and dynamic nuclear polarization (DNP) of nanostructured materials are reviewed. A first group of materials is based on crystalline nanocellulose (CNC) or microcrystalline cellulose (MCC), which are used as carrier materials for dye molecules, catalysts or in combination with heterocyclic molecules as ion conducting membranes. These materials have widespread applications in sensorics, optics, catalysis or fuel cell research. A second group are metal oxides such as V-Mo-W oxides, which are of enormous importance in the manufacturing process of basic chemicals. The third group are catalytically active nanocrystalline metal nanoparticles, coated with protectants or embedded in polymers. The last group includes of lead-free perovskite materials, which are employed as environmentally benign substitution materials for conventional lead-based electronics materials. These materials are discussed in terms of their application and physicochemical characterization by solid-state NMR techniques, combined with gas-phase NMR and quantum-chemical modelling on the density functional theory (DFT) level. The application of multinuclear 1H, 2H, 13C, 15N and 23Na solid state NMR techniques under static or MAS conditions for the characterization of these materials, their surfaces and processes on their surfaces is discussed. Moreover, the analytic power of the combination of these techniques with DNP for the identification of low-concentrated carbon and nitrogen containing surface species in natural abundance is reviewed. Finally, approaches for sensitivity enhancement by DNP of quadrupolar nuclei such as 17O and 51V are presented that enable the identification of catalytic sites in metal oxide catalysts

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