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Varian VNMRS Level 500 MHz Spectrometer

This instrument is one of the specialty instruments. It is primarily used for solid-state, biological samples, HRMAS, ¹H, ¹³C, and multinuclear NMR spectroscopy. It is capable of 1D and 2D NMR experiments. The age of the instrument requires manual tuning of the spectrometer. The low ¹¹B background in the broadband probe makes this instrument the instrument of choice for compounds containing boron. This instrument is the easiest to reserve for long-term NMR experiments. This instrument is capable of analyzing biological in addition to agricultural samples (e.g. seeds, flowers, pollen, etc.) and is the instrument of choice for solid-state and HRMAS analysis.

• Varian VNMRS Console and various probes
• Nalorac H{CN}Triple Resonance probe with Z-axis PFG – Mainly for biological NMR, protein structural analysis
• Nalorac Dual Broad Band probe (tunable from 22 to 225 MHz with quartz inserts for low ¹¹B background) with Z-axis PFG–manually tune X-channel for direct observation of heteronuclei with proton decoupling  (Click here to see available nuclei)
• Nalorac HF dual tuned probe with Z-axis gradients (includes filters for {¹H}¹⁹F and {¹⁹F}¹H experiments) – primarily for fluorine NMR, but also has strongest gradient coils of any of our probes for DOSY experiments
• Nalorac H{CPN} Quad Resonance probe with XYZ-axis PFG – specialty probe for phosphorus containing biological molecules
• Varian High Resolution Magic Angle Spinning probe (Nanoprobe), two channel H-observe, X-decouple
• Z-axis gradients
• Oxford 11.75 T, 51 mm magnet
• Oxford 28 gradient shim set
• 4 channel console, 1 full band channel and 3 broadband channels with waveform generators on each channel.
• Triaxial Pulsed Field Gradient amplifier
• Deuterium gradient shimming and decoupling switches
• Variable temperature: -80 °C to +90 °C

Bruker Avance Neo 500 MHz Spectrometer

This instrument is the new instrument in the NMR Spectroscopy Lab. Users are trained on this instrument only upon request. It is primarily used for diffusion and solid-state experiments, but it is also capable of solution-based ¹H, ¹³C, and multinuclear NMR spectroscopy (1D and 2D NMR experiments). The presence of a 24 sample SampleCase autosampler allows for automated data collection for data collection during off-peak hours. We currently have the iProbe available.

• Bruker iProbe two-channel: ¹H and broadband (¹⁹F/³¹P–¹⁹⁹Hg/¹⁷O– ¹⁰⁹Ag),
• Bruker TXI probe – triple resonance probe (¹H, ¹⁵N, ¹³C)
• Both probes have extended range beyond our current probes: up to 130 °C cooler and 50 °C hotter.
• Cryo probe provides twice the sensitivity of a room temperature probe, allowing for high sensitivity measurements at lower analyte concentrations than a room temperature probe – e.g., 25% of the time for a typical ¹³C acquisition.
• Diffusion probe allows for a 20-fold reduction in acquisition time – e.g., < 10 min. acquisition vs > 3 hours for a diffusion experiment on our current equipment-for low molecular weight species.
• HRMAS package spins 5-6 times as fast as our current HRMAS probes, eliminating spinning side bands and include an auto-loading mechanism, eliminating the need to remove the probe to change samples

Varian DD2 600 MHz Spectrometer

This instrument is one of the specialty instruments. It is primarily used for biological samples and ¹H, ¹³C, and multinuclear NMR spectroscopy. It is capable of 1D and 2D NMR experiments. It is capable of HRMAS and analysis of solid-state samples but is more difficult to book long-term experiments than with the 500 MHz NMR spectrometer due to the demand for routine multinuclear analysis. HRMAS and solid-state samples can be analyzed with prior notice (3 days). The ability to autotune to many nuclei makes this the instrument of choice for multinuclear NMR spectroscopy (Click here to see the available nuclei). This is the instrument of choice for variable temperature experiments.

• Oxford 14.1T 51mm bore magnet
• 4 channel console, 1 high band, 3 low band
• Varian 40 channel shim set
• Z-axis pulsed field gradients
• 5 mm triple resonance probe, ¹H detect {¹³C,¹⁵N} decouple–biological NMR, protein structural analysis
• 5 mm broadband OneProbe, ¹⁵N to ³¹P tuning range (60 to 250 MHz), automatic tuning, and 12-position autosampler
• 4mm Solid State NMR probe with high power High-band amplifier
• Variable temperature: -80 °C to +90 °C

Description – Rates are per Hour	Varian 500 MHz	Bruker 500 MHz	Agilent 600 MHz	Service/Advanced Training
WSU Clients (Federal Funding)	$ 12.00	$ 15.00	$ 13.00	$ 30.00
WSU Clients (Non-Federal Funding)	$ 13.04	$ 16.30	$ 14.13	$ 32.61
Other Non-Profits or Small Business/Startup (with Current SBIR/STTR Funding)	$ 77.00	$ 82.00	$ 82.00	$ 60.00
Corporate	$ 117.00	$ 125.00	$ 125.00	$ 90.00

The PC in Fulmer B3 runs Varian/Agilent’s latest software VnmrJ that is compatible with all the NMR software versions running on the spectrometers in the facility. Data from the spectrometers can be analyzed here and processed. The results can be saved to a USB drive and printed at a local printer in the WSU NMR lab.

Freeware

Here are a few freeware NMR processing software that are popular.

• VnmrJ is now open source software as OpenVnmrJ. It requires working knowledge with UNIX.
• SpinWorks This is a software developed by Kirk Marat from University of Manitoba. SpinWorks is freely available for download and works on Windows based computers. The author comments that some people have successfully tried it with Wine to run on Linux platforms and with SoftWindows on Mac as well. 
• NMRPipe This is a nice software that is an outgrowth of dedicated effort by Frank Delaglio of NIH (part of his graduate work) and what more it is free ! Nevertheless, this runs only on a Unix or Unix-like operating system (including Linux) and probably more suited to do 2D and 3D NMR data than a routine 1D spectrum processing. It requires working knowledge with UNIX.
• matNMR 3 This software was developed by Jacco van Beek, and published in J. Magn. Res. It is a toolbox for processing 1D and 2D NMR spectra under MATLAB, and is free. It has been tested under Solaris and MS Windows 95. Additionally, it works on MacOS 7.5 and 8.0), and on Windows NT.
• iNMR is a software available on Mac or Windows you can download in demo mode for use of select features with no expiration. You can upgrade to a commercial product from Mestrlab for full use, and all future versions.
• Topspin is also freely available to academic users. Topspin is the software package for NMR data analysis and the acquisition and processing of NMR spectra provided with Bruker NMR spectrometers.

Commercial Software

At present no other third party software is available for distribution by the facility. But here are some links you can explore and buy the software if found suitable for your own use.

• ACDNMR A 1D and 2D processing version is available in this suite. Interface is user friendly and can read many NMR fid formats including Bruker’s.
• MNOVA from Mestrelab Research has more than one flavor of this software available for purchase and one can also download a trial version by registering. The WSU chemistry department currently owns a departmental license to this software. For users that are members of the WSU chemistry department, directions on installing this software can be seen here.
• NUTS This program can run both on Windows and Mac computers. If you need simple 1D processing, this is the most affordable software. A 2D version is available for a higher price.

• WSU NMR Lab YouTube Channel
• Preparation of a liquid NMR sample
• Using the NMR Lab and Training on the 500 MHz Varian NMR Spectrometer
• Using IconNMR

Educational Magnetic Resonance Resources

• Animated brief introduction to NMR
• Basics of NMR Spectroscopy, online interactive textbook by Joseph P. Hornak, PhD
• Interactive demonstration for NMR signal acquisition and data processing
• Lecture notes from James Keeler, author of Understanding NMR Spectroscopy
• Modern NMR Methodology – Textbook
• Notes from Structure Determination by Spectroscopic Methods (Chem 605) taught by Hans Reich at UW-Madison
• Structure Elucidation by NMR Spectroscopy
• Structure Elucidation by NMR Spectroscopy: Practical Strategies for Organic Chemists

NMR Resources

• List of impurities observed in NMR spectra: organic & organometallic
• Technical Information on NMR Tubes
• NMR Periodic Table
• NMR solvent chart from Cambridge Isotopes
• List of pH buffers for NMR spectroscopy from Cambridge Isotope Laboratories
• Resource for information on organic compounds. Often times there are either simulated or user-submitted NMR spectra available.
• Spectral Database of Organic Compounds
• Solid state and quadrupolar NMR
• Online resource for predicting standard 1D and 2D NMR spectra
• Guide for multiplet analysis of 1H NMR spectroscopy
• Practical guide for how to shim an NMR spectrometer by hand
• NMR lab. NMR resource that includes information on both common and rare NMR nuclei, liquid-state and solid-state NMR information, multi-dimensional NMR techniques, NMR relaxation, and much more
• List of common NMR artifacts and problems, and troubleshooting suggestions

Biological NMR Resources

• Introduction to structure determination of proteins using NMR.
• Introduction to NMR Spectroscopy of Proteins
• Biological Magnetic Resonance Data Bank.  View and submit NMR spectroscopic data for biological macromolecules and metabolites.
• Guide to protein NMR – Assignment strategies, software links, general NMR information

Other NMR-Related Software

• DMFIT is a free NMR fitting software ideal for peak fitting and solid-state NMR data analysis.  Common uses are NMR peak deconvolution, and fitting static and MAS CSA patterns.
• SpinDrops – iTunes app designed to help NMR spectroscopists understand magnetic resonance experiments and concepts
• Additional list and links to NMR-related software

Suggested Reading: Magnetic Resonance Journals

• Magnetic Resonance in Chemistry
• Journal of Magnetic Resonance
• Annual Reports on NMR Spectroscopy
• Applied Magnetic Resonance
• Solid State Nuclear Magnetic Resonance
• Progress in Nuclear Magnetic Resonance Spectroscopy
• Magnetic Resonance Imaging
• Journal of Biomolecular NMR
• Concepts in Magnetic Resonance
• NMR in Biomedicine

Suggested Reading: Magnetic Resonance Books

• Understanding NMR Spectroscopy – James Keeler
• Basic One and Two Dimensional NMR Spectroscopy Experiments – Horst Friebolin
• Protein NMR Spectroscopy – John Cavanagh
• Spin Dynamics – Malcolm Levitt
• Essential Practical NMR for Organic Chemistry
• Multidimensional Solid-State NMR and Polymers – Klaus Schmidt-Rohr
• Experimental Pulse NMR: A Nuts and Bolts Approach – Fukuchima, Roeder
• Principles of Magnetic Resonance Imaging – Nishimura
• Modern NMR Techniques for Chemistry Research – Andrew Derome

Videos on NMR Spectroscopy

• This collection of videos posted by ANZMAG include 14 lectures presented by James Keeler, covering many of the chapters from his excellent textbook titled Understanding of NMR Spectroscopy.
• Lectures from a graduate-level course in Organic Spectroscopy at UC Irvine, taught by Professor James Nowick.
• This playlist of videos on Youtube posted by chemtubeuk includes both introductory and advanced concepts in nuclear magnetic resonance, including a brief introduction to NMR, and how to interpret HSQC data.

WSU NMR Lab Safety Policies

There are multiple potential hazards in an NMR lab. In order to use the NMR facility at WSU, you must read and be familiar with the following safety information. Failure to comply with the correct standard operating procedures in the NMR lab can result in damage, personal injury, and even death. Please let an NMR staff member know of problems as soon as you encounter something that seems not quite right. If you can’t find a staff member, please submit a Problem Report using the form on the website.

Emergencies

1. If the fire alarm goes off, please leave the lab and evacuate the building.
2. In the event of a quench, please exit the NMR lab immediately.
3. For all emergencies, call 911.

Magnetic Field Hazards

1. The defining characteristic of an NMR lab is the presence of strong magnetic fields. Every magnet has a stray magnetic field that extends beyond the physical structure of the magnet. The safety zone, or 5 Gauss line is indicated by tape marks on the floor around each magnet. NMR  magnets are ALWAYS ON, so users must always exercise caution in the NMR lab.
2. Electronic, electrical, or mechanical medical implants may be affected or even stopped in the presence of a static or changing magnetic field. For your own safety, if you have a pacemaker or other medical implant that could be adversely affected by strong magnetic fields, do NOT enter the NMR labs.
3. Magnets can exert large attractive forces on equipment or other ferromagnetic objects when brought. Before entering the lab, think about EVERYTHING you are about to bring in.
4. Small objects (e.g., paper clips, hair pins, spatulas, wrenches, screwdrivers, etc.) can lead to significant problems in instrument performance. If such items were to get stuck in/on the instrument, the magnet would probably need to be de-energized in order to remove them. This would be very expensive and lead to extended down time.
5. Large objects (e.g., gas cylinders) would be pulled with a large force, and significantly damage the instrument, as well as likely injury someone who attempts to stop the motion once it starts. These can cause bodies or limbs to be trapped between the equipment and the magnet.
6. Users must never bring ferromagnetic objects (i.e., materials that are strongly attracted to a magnetic field) close enough to the instruments to experience a force. Do not bring any metallic objects within the 5 Gauss line or 10 feet of any magnet.
7. Do NOT bring any compressed gas cylinders into the NMR lab without NMR personnel supervision.
8. Never put any object into the magnet except NMR tubes and sample holders.

Cryogenic Hazards

1. All of the NMR magnets are superconducting, which means they are kept in a cryostat filled with liquid helium. A concentric dewar of liquid nitrogen is placed around the helium cryostat in order to keep the helium boil-off rate low. Additionally, liquid nitrogen may be kept in portable dewars around the facility. Cryogens can pose several risks including: asphyxiation, frostbite, and chemical explosions.
2. In the event of a magnet quench, the superconducting wire inside the instrument transitions to a normal conducting state. This would boil off all of the liquid helium very quickly. The rapid expansion of helium as it vaporizes can displace the oxygen in the NMR lab and cause asphyxiation.
3. If you observe a sudden exhaust of gas from a magnet (and NMR staff are not performing a cryogen fill), exit the NMR lab immediately.
4. Direct contact with cryogens can produce cold burns on the skin. Liquid helium is 4 K, and liquid nitrogen is 77 K. The gas that is exhausted during a fill can be extremely cold.
5. Both liquid helium and liquid nitrogen are cold enough to condense liquid oxygen from the atmosphere. Violent reactions such as rapid combustion or explosion may occur if accumulated oxygen were to come in contact with combustible materials.
6. The NMR personnel must regularly refill the instruments with cryogens. During a fill, stay away from the gaseous exhaust as frostbite or asphyxiation might occur if you stand too closely.
7. During low temperature NMR, be aware of liquid nitrogen splashing. When handling cryogens, you must be wearing safety glasses and cryogenic gloves.

Chemical Safety & Housekeeping

1. The same principles of research safety apply in instrumentation laboratories when you are handling samples. Research samples, glassware, chemical storage, spills, and waste disposal must be properly handled.
2. You must wear long pants (or equivalent) and closed-toed shoes.
3. No food or beverages are allowed in the NMR lab.
4. The NMR lab is not a wet lab. All sample prep should be done in your lab. Do not prep samples at spectrometers.
5. Do not bring your lab coat or gloves into the NMR lab.
6. Should you break a sample in the NMR lab, use the items in lab to thoroughly clean up the area of the spill. Please dispose of the waste generated in your lab.
7. Sample spinners are extremely expensive, precision machined items.
8. Never take spinners out of the NMR labs.
9. Do not drop them on the floor or place them on their sides so that they may roll off the bench and on to the floor.
10. If your tube does not fit the spinner, either your tube or the spinner O-ring needs to be replaced. If you think it might be the O-ring, please contact the NMR facility staff for a replacement.
11. Keeping a shared lab clean requires the cooperation of everyone. Please do not leave KimWipes, paper towels, etc. laying around.
12. If you believe any sample may have spilled into or onto one of the instruments, please notify the NMR facility staff immediately. Place a written note on the keyboard to inform the next user.
13. Please be considerate of others. If there is a queue, please limit your session to 10 minutes.