Nuclear Magnetic Resonance
NMR Facility Overview
The Virginia Tech NMR Facility operates high-field superconducting magnets ranging from 400-600 MHz for cutting-edge research in chemistry, materials science, and related fields. Our facility provides state-of-the-art instrumentation with comprehensive user training and support.
| Instruments | Internal | Federal | External |
|---|---|---|---|
| Instrument Time | $9.90 | $15.90 | $125.00 |
| Tech Assist | $40.00 | $64.40 | $125.00 |
- Submit training request via email facility staff. or email
- Complete general facility training covering:
- Safety protocols and hazards
- Sample preparation essentials
- Instrument operation and queues
- Data download and processing
- Receive shared group credentials for:
- Instrument login
- LOGS data access
- FACES scheduling system
- Door code access (provided with facility training)
Additional training required for:
- Variable Temperature (VT) experiments (-40°C to +135°C)
- Diffusion/DOSY measurements
- Solid-State MAS (4mm rotor handling by staff only)
- Specialty Probes (10mm, DiffBB)
- Water Suppression techniques
- Quantitavtive NMR
- EPR (Electron Paramagnetic Resonance)
| Instrument Name | Vendor | Model | Field Strength | Probes |
| NEO400JACK | Bruker | Avance IV Neo | 400 MHz | 5 mm iProbe (RT) |
| 4 mm SSNMR MAS iProbe | ||||
| 10 mm probe | ||||
| DiffBB diffusion probe | ||||
| NEO400HT | Bruker | Avance IV Neo | 400 MHz | 5 mm iProbe |
| JEOL ECZL400 | JEOL | ECZL400 | 400 MHz | ROYAL HFX |
| NEO500BBO | Bruker | Avance IV Neo | 500 MHz | Prodigy BBO cryoprobe |
| NEO500OXFORD | Bruker | Avance IV Neo | 500 MHz | Prodigy BBO cryoprobe |
| NEO600TCI | Bruker | Avance IV Neo | 600 MHz | Prodigy TCI cryoprobe |
| NEO400DIFF | Bruker | Avance IV Neo | 400 MHz | DiffBB diffusion probe |
| Additional high-gradient diffusion probes |
YOUR EXPERIMENT |
BEST CHOICE |
KEY NOTES |
Quick ¹H check (<20 min) |
Neo400 HT or JEOL ECZL 400 |
20 min limit (HT), 60 min (JEOL) |
¹³C or X-nucleus, moderate time |
Neo400Jack (5mm) |
2-6 hrs daytime |
Long ¹³C or X-nucleus |
Neo500BBO or Neo500Oxford |
9-12× faster than 400 MHz |
¹H-detected 2D, dilute samples |
Neo600TCI |
Highest ¹H sensitivity |
¹⁹F experiments |
JEOL ECZL400 |
Best ¹H-¹⁹F correlation |
VT (-40 to +135°C) |
JEOL ECZL400 or Neo500Oxford |
Trained users, staff approval |
Polymers (high MW) |
Neo400Jack (10mm) or Neo500BBO |
Staff scheduled probe swap |
Diffusion/DOSY |
Neo400Jack DiffBB or Neo400Diff |
Diffusion training required |
Solid-state powders |
Neo400Jack (4mm MAS) |
Staff scheduled, rotor handling by staff |
| EXPERIMENT | WHAT IT SHOWS | TYPICAL USE | TYPICAL TIME |
|---|---|---|---|
| COSY | ³J ¹H-¹H scalar couplings (2-3 bonds) | Identify spin systems and proton connectivity | 10-30 min |
| TOCSY | Extended ¹H-¹H relayed couplings through spin systems | Map entire spin systems (e.g., sugar residues) | 30-60 min |
| Experiment | What It Shows | Typical Use | Typical Time |
|---|---|---|---|
| HSQC | ¹J ¹H-¹³C direct bonds (CH, CH₂, CH₃) | Assign protonated carbons; first hetero 2D experiment | 20-60 min |
| HMBC | ²J-⁴J ¹H-¹³C long-range couplings | Connect to quaternary carbons and resolve branching | 1-4 hrs |
| H2BC | ²J ¹H-¹³C geminal couplings only | Clean methylene (CH₂) assignments; confirm HMBC | 1-3 hrs |
| Experiment | What It Shows | Typical Use | Typical Time |
|---|---|---|---|
| NOESY | Through-space ¹H-¹H dipolar interactions (<5 Å) | Determine stereochemistry and 3D conformation (MW >800 Da) | 1-3 hrs |
| ROESY | Rotating-frame NOE (positive for all molecular weights) | Mid-sized molecules (500-1500 Da) where NOESY fails | 1-3 hrs |
Key Policies and Safety
Critical Safety Rules
DANGER: Projectile Hazard
- Never bring heavy ferromagnetic objects beyond the 5 Gauss line (marked around each magnet)
- Even small items (paper clips, bobby pins) will be attracted and can stick to the magnet impacting shims
- Heavy items (wrenches, scissors, chairs, gas cylinders) become dangerous projectiles
- Gas cylinders are absolutely prohibited unless staff authorized.
Medical Devices & Implants
STOP: If you have any of the following, you MUST get staff clearance before entering:
- Cardiac pacemakers or ICDs
- Cochlear implants
- Neurostimulators (deep brain, spinal cord, vagus nerve)
- Aneurysm clips
- Metallic foreign bodies (shrapnel, metal fragments)
"MRI Safe" ≠ "NMR Safe" — Our magnets operate at much higher fields (9.4-14.1 Tesla) than clinical MRI (1.5-3.0 Tesla)
- Remove mechanical watches before approaching magnet during sample insertion:
- Mechanical watches will be permanently magnetized and ruined
- Piercings and jewelry are generally safe, but take care if large and ferromagnetic
- NMR tube transport: Always use secondary containment (no glass containers)
- Magnet quench: If you hear loud roar/boom or see dense fog, leave immediately and contact NMR staff
- No drop-ins for staff assistance (email or call ahead)
- Instrument consoles: For acquisition only — process data offline on your computer
- Report all incidents: Spills, breakage, instrument issues, or safety concerns immediately
- Automated walkup operation: IconNMR (Bruker) or Delta interface (JEOL)
- Never work alone if handling potentially hazardous samples
- Know the location of emergency exits and safety equipment
- Keep your phone accessible for emergency communication
- If a magnet quench or safety incident occurs, evacuate immediately and contact NMR staff
Do NOT use chipped, cracked, or damaged NMR tubes.
Damaged tubes can:
- Cause instrument downtime and costly probe damage
- Get stuck in the magnet or autosampler
- Produce poor quality spectra
- Chips or cracks: Any visible damage — retire immediately
- Heavy scratches: Deep scratches affect spinning and shimming
- Bent tubes: Even slight bends cause problems
- Multiple uses: Disposable tubes should generally be used 1-3 times maximum
How to fill out an Analytical Services ISR
Supplier: "VT Chemistry NMR Lab"
Walkup Instruments (No Reservation Needed)
- Neo400HT: 20 minute hard limit per sample
- JEOL ECZL400: 60 minute daytime limit per sample
- Neo400Jack: Prioritized for scheduled use of specialty probes
- Neo500BBO & Neo600TCI: No formal limit, but experiments exceeding 2 hours should be moved to the night queue when possible
Reservation Only Instrument
- Neo500Oxford: Direct link to FACES Scheduling System
- FACES Group: VATECHNMR
- Can reserve up to the minute — No shows risk loss of privleges
In all cases, when possible run non-urgent experiments longer than 2 hours during the overnight queue to maintain fair access for all users.
Contact Ken Sharp-Knott
kknott@vt.edu
540-231-0885
When co-authorship is expected:
- Substantial intellectual contributions to experimental design, data interpretation, or manuscript preparation
- Specialized technique development or troubleshooting beyond routine support
- Custom method development, extensive troubleshooting, or data analysis assistance
When acknowledgment (not co-authorship) is sufficient:
- Routine training and instrument access
- Standard walkup experiments without significant staff involvement
- Minor troubleshooting or parameter adjustments
Best practice: Discuss authorship expectations early in your project with facility staff to avoid misunderstandings.
When describing your NMR experiments in the Methods or Experimental section of manuscripts, cite relevant instrument details from the Instruments page. Include:
- Instrument name (e.g., "Bruker Avance IV Neo 600 MHz")
- Probe type (e.g., "Prodigy TCI cryoprobe")
- Field strength and observe frequency
Example Citation:
"¹H and ¹³C NMR spectra were acquired on a Bruker Avance IV Neo 600 MHz spectrometer equipped with a Prodigy TCI cryoprobe. NMR data reported in this work were obtained at the Virginia Tech Chemistry NMR Facility (RRID:SCR_027587)."
- Specify solvent, temperature (if non-ambient), and spectrometer frequency
- Include coupling constants (J) in Hz for multiplets
- For quantitative NMR, describe relaxation delays, pulse angles, and any relaxation agents used
All data automatically uploaded to LOGS server:
URL: https://nmrsc.chem.vt.edu/asds
Login: Same credentials as FACES and instrument login
- Download datasets from LOGS to your local computer
- Process in MNova (facility standard software)
- Save MNova file (each file should contain experiments for ONE compound)
- Site license provided by facility
- Request license key via email
- Distributed automatically after training completion
- Must connect to VT network (eduroam or VPN) for validation
Technical reference materials for planning experiments, selecting parameters, and understanding NMR fundamentals.
Sample Preparation Essentials
| REQUIRMENT | SPECIFICATION |
|---|---|
| Tube | Straight, undamaged 5mm tube (high-quality for qNMR and VT) |
| Volume | ~0.6 mL (40-50mm liquid height in tube) |
| Solution | Fully dissolved, clear, no particulates or bubbles |
| Solvent | Deuterated (CDCl₃, DMSO-d₆, D₂O, CD₃OD, CD₃CN, acetone-d₆, toluene-d₈, benzene-d₆) |
| Cleanliness | Wipe tube exterior with lint-free tissue before insertion |
- FORMAT: GROUPID-USERINITIALS-SHORTSAMPLEID
- EXAMPLE: WS2-KK-SK21
- RULES: Alphanumeric characters only - no spaces, periods, or special characters
- REQUIRED: Write GROUP ID prominently around cap (required for sample identification)
- Use BLACK SHARPIE (fine-tipped) on light colored cap
- Include sample ID or your initials (strongly recommended to distinguish your samples from groupmates)
- Dark or illegible caps not allowed — slows troubleshooting and makes orphaned samples harder to track
- No tape, parafilm, or labels attached to tubes — write directly on cap only
- Damaged or poor-quality tubes: Chips, bends, or scratches make shimming harder and cause distorted peaks
- Incorrect sample volume or height: Liquid column far from 40-50mm hurts sensitivity and resolution
- Incomplete dissolution, particulates, or bubbles: Gives broad, ugly lines and unstable shims
- Sample depth set incorrectly in spinner: Always use depth gauge; incorrect depth causes weak signal
- Poor shimming: Results in broad, asymmetric peaks — more scans won't fix it
Quick Reference Guides
NUCLEUS |
SAMPLE TYPE |
TYPICAL AMOUNT (MG) |
TYPICAL TIME |
BEST INSTRUMENT |
¹H |
Small molecule |
5-20 |
5 min |
Neo400 HT or any |
¹³C |
Small molecule (quick) |
30-80 |
10-60 min |
Neo400 HT |
¹³C |
Small molecule (longer) |
10-40 |
3-8 min |
Neo500 BBO |
¹H/2D |
Very dilute |
2-10 |
10-30 min |
Neo600 TCI |
¹H |
Polymer |
10-30 |
10-30 min |
Neo400 HT or Neo400 Jack 10mm |
¹³C |
Polymer |
50-100 |
20-60 min |
Neo500 BBO |
Nucleus |
Natural Abundance (%) |
MHz/T (at 9.4T) |
Receptivity vs ¹H |
Receptivity vs ¹³C |
¹H |
99.98 |
42.58 (400 MHz) |
1.0 |
5,700-6,400 |
¹³C |
1.1 |
10.71 MHz |
1.0 (reference) |
1.0 |
¹⁵N |
0.36-0.37 |
4.32 (40 MHz) |
~50× less than ¹³C |
~0.02 |
¹⁹F |
100 |
40.05 (376 MHz) |
0.8-0.9 |
4,500-5,500 |
³¹P |
100 |
17.24 (162 MHz) |
0.06-0.07 |
350-450 |
Solvent |
Formula |
Residual ¹H Peak (ppm) |
Boiling Point (°C) |
Freezing Point (°C) |
Notes |
CDCl₃ |
Chloroform-d |
7.26 |
61 |
-64 |
Most common; good for organics |
DMSO-d₆ |
Dimethyl sulfoxide-d₆ |
2.50 |
189 |
19 |
Polar; hygroscopic; good for VT |
D₂O |
Deuterium oxide |
4.79 |
101 |
4 |
Aqueous samples; exchanges with labile H |
CD₃OD |
Methanol-d₄ |
3.31 (CHD₂), 4.87 (OH) |
65 |
-98 |
Polar; enhances with labile H |
CD₃CN |
Acetonitrile-d₃ |
1.94 |
82 |
-45 |
Polar aprotic; wide liquid range |
Acetone-d₆ |
(CD₃)₂CO |
2.05 |
56 |
-95 |
Polar; volatile |
Toluene-d₈ |
C₆D₅CD₃ |
2.09 (CD₂H), 7.00-7.20 |
111 |
-95 |
Aromatic; good for VT |
Benzene-d₆ |
C₆D₆ |
7.16 |
80 |
6 |
Aromatic; health hazard |
NMR Tubes & Consumables
- Quantitative NMR (qNMR): Use high-quality, precision tubes (e.g., Wilmad 528-PP)
- Variable Temperature (VT): VT-rated tubes (Class A) required for temperature extremes
- Cryoprobe work: Clean, undamaged tubes to protect expensive cryoprobes
| Tube Type | When to Use | Notes |
|---|---|---|
| Shigemi tubes | Limited sample volume (<300 μL) | Glass susceptibility-matched plugs; consult staff before use |
| Coaxial inserts | Lock solvent separate from sample | For samples incompatible with deuterated solvents |
| 3 mm tubes | Very limited sample quantity | Requires 3mm probe (not standard); discuss with staff |
Common deuterated solvents are available for purchase through the facility or your research group. See the Solvent Quick Reference Guide for details on each solvent.
Cost consideration: Deuterated solvents vary significantly in price. CDCl₃ and DMSO-d₆ are relatively inexpensive, while D₂O, CD₃OD, and specialty solvents (DMF-d₇, pyridine-d₅) are more costly. Plan accordingly for budget-sensitive projects.
Laboratory Hours
Staffed Hours: 9a - 5p, M-F
24/7 access for trained users
Contact NMR Staff
Ken Sharp-Knott
NMR Facility Manager
kknott@vt.edu
540-231-0885
540-267-6502 (Emergencies Only)
Murthy Shanaiah, Ph.D.
NMR Spectroscopist
nmrns@vt.edu
540-231-8256
Emergency Contact
VT Environmental Health & Safety
540-231-5364
www.ehs.vt.edu
Kenny Smith
Facilities Manager
kesmith7@vt.edu
Drew Murphy
Safety Coordinator
drewmurphy23@vt.edu
Lab Address
Hahn Hall South 002
Virginia Tech
900 W. Campus Blvd.
Blacksburg, VA 24061