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NMR-A Guide to the SCS NMR Lab
| UGL 010 | DLO - 16 May 2018 |
| ND - 3 September 2024 |
A GUIDE TO
THE SCS NMR LABORATORY
Dean Olson, Director
School of Chemical Sciences
University of Illinois
600 South Matthews, Urbana, Illinois 61801
FACILITY PERSONNEL:
Dean Olson, 244-0564;
- Lab Director
- UI400, U500, VXR500, UI500NB, CB500, B600
Prof. Liviu Mirica
- Faculty Advisor
Nikki Duay, 333-2041
- General Lab Operations, Newcomer Training, Cryogen Management, Accounting, Safety Compliance,, ChemFOM
Lingyang Zhu, 333-6283
- VNS750NB, UI600, Solution NMR, Computers, Software, System Administration
Collette Xu, 333-2586
- UI300WB, CB500WB, Solids NMR
I. INTRODUCTION
This guide provides information about the instruments and techniques available in the NMR Laboratory (NMR Lab). Scheduling and sign-up policies are described in handout UGL016. Most of the information contained herein is of a fairly general nature. If you have any questions or problems you should consult the NMR Lab handouts addressing specific topics or consult laboratory personnel. Any new user of the NMR Lab should read Handout #011 - NewUser Orientation to the NMR Lab. For full description of instrumentation, see our webpage at http://scs.illinois.edu/nmr/.
TABLE I
| NMR Instrument | 1H Freq (MHz) | Probes* | Tube Size/Rotor Size |
|---|---|---|---|
| UI300WB | 300 (7.05 Tesla) | 1H/X switchable BB 73Ge-15N BB 17O{X} 183W{X} 15N-31P BB CPMAS (ChemMag) |
5 20 mm 10 mm 20 mm 7, 4, 3.2 mm |
| UI400 | 400 (9.4 Tesla) | QUAD (1H/19F/13C/31P) | 5 mm |
| U500 | 500 (11.75 Tesla) | QUAD (1H/19F/13C/31P) | 5 mm |
| VXR500 | 500 (11.75 Tesla) | QUAD (1H/19F/13C/31P) PFG Z 13C Nanoprobe |
5 mm 70 μL |
| UI500NB | 500 (11.75 Tesla) | 1H{13C/15N} PFG Z 1H{31P/X} PFG Z 1H/X switchable BB 15N-31P BB |
5 mm 5 mm 5 mm 10 mm |
| CB500 | 500 (11.75 Tesla) | BBFO CryoProbe (1H, 19F/31P-15N) Room temperature broadband probe (1H, 31P-15N) |
5 mm |
| CB500WB (solid-state NMR) | 500 (11.75 Tesla) | Phoenix HXY MAS Probe (triple resonance mode: H: 1H-19F X: 31P-13C Y: 23Na-15N; double resonance mode: 1H-19F X: 31P-155Gd) | 6 mm |
| B600 | 600 (14.1 Tesla) | BBO Prodigy probe (1H/19F, 31P-15N/35Cl) Room temperature iTBO probe (1H/19F, 31P-15N, 19F) |
5 mm |
| UI600 | 600 (14.1 Tesla) | 1H{13C/15N}PFG X,Y,Z 15N-31P BB AutoX (15N-31P) |
5 mm 5, 10 mm 5 mm |
| VNS750NB | 750 (17.6 Tesla) | 1H{13C/15N}PFG X,Y,Z 15N-31P BB 13C{1H} 13C{1H} 15N-31P BB CPMAS (Doty) HXY MAS (Varian) |
5 mm 10 mm 3 mm 5 mm 5 mm 4 mm |
* BB = Broad Band; PFG = pulsed field gradient; X, Y, Z = available gradients; CPMAS = cross polarization magic angle spinning
Table II gives a useful comparison of 1H and 13C resolution and sensitivities for the various spectrometers and probes in the NMR Lab, as well as the variable temperature range available on the various probes.
13C: In general, the U500 and VXR500 give the best sensitivity for routine 13C measurements on 5mm samples. For example, a sample of 15 mg of a material with molecular weight <1000 in 0.5 mL solvent requires 5-10 minutes to achieve a reasonable S/N. If you are mass limited, please read the discussion in handout UGL015 for guidance in choosing the best probe for your needs. If you are solubility limited, consider using a 10 mm probe on the appropriate spectrometer.
1H: In general, routine 1H spectra can be obtained on the U400, UI400, U500 and VXR500. All inverse experiments are restricted to the UI500NB, UI600, or VNS750NB. Table II serves as a guide to the most appropriate instrument for your data collection. If you have 10-15 mg of material with molecular weight <1000, you should be able to achieve a reasonable routine 1H S/N within 1 minute on any of these spectrometers (time for shimming is, however, not included!).
TABLE II
|
NMR Instrument,
Probe
|
1H Sens
(1)
|
19F Sens (2) |
13C Sens (3) |
31P Sens (4) |
Variable Temperature Range |
| UI400, QUAD | ~120:1 | ~120:1 | ~130:1 | ~90:1 | -100 C to +100 C |
| U500, QUAD | ~260:1 | ~270:1 | ~210:1 | ~300:1 | -100 C to +100 C |
| VXR500, QUADG 1H{X} switchable |
~260:1 ~300:1 |
~280:1 | ~230:1 ~210:1 |
~200:1 | -80 C to +100 C -100 C to +100 C |
| UI500NB 1H{13C/15N} PFG Z 1H{31P/X} PFG Z |
~750:1 ~700:1 |
~80:1 NA |
-30 C to +80 C -30 C to +50 C |
||
| UI600 1H{13C/15N} X,Y,Z AutoX 15N-31P BB (10mm) |
~1000:1 ~370:1 NA |
~475:1 NA |
~125:1 ~320:1 ~1100:1 |
~200:1 ~550:1 |
-20 C to +80 C -80 C to +130 C -150 C to +150 C |
| VNS750NB 1H{13C/15N} PFG X,Y,Z 15N-31P BB (10mm) 13C{1H} 5 mm 13C{1H} 3 mm |
~1350:1 | ~180:1 ~1200:1 ~530:1 ~220:1 |
~780:1 | -20 C to +80 C -150 C to +150 C -100 C to +100 C -100 C to +100 C |
(1) 1H Sensitivity Standard: 0.1% ethylbenzene/CDCl3 (5mm tube)
(2) 19F Sensitivity Standard: 0.05% CF3C6H5/C6D6 (5mm tube)
(3) 13C Sensitivity Standard: ASTM, 40% dioxane/C6D6 (5mm tube)
(4) 31P Sensitivity Standard: 0.0485M Triphenylphosphate/ CDCl3 (5mm tube)
(5) 13C Sensitivity Standard: ASTM, 40% dioxane/C6D6 (10mm tube)
* See Handout UGL015 - 13C Sensitivity for Mass Limited Samples
TABLE III
NMR Lab Instrumentation Cost Rate Summary. See the SCS NMR Website for the current rates.
| Type of Cancellation | Time Period | Charge |
| Auto-cancel / No show | < 1 hr | 2 hrs instrument time |
| Auto-cancel / No show | > 1 hr | Time reserved + 2 hrs |
| Emergency Log-off | 1 hr | Instrument time |
II. DATA BACKUP
The NMR Lab does not take responsibility for backing up your data. You should backup your own data:
On the computers in your own lab. You should be able to map your group’s NMR data as network drives on these computers (see handout UVU403 – Data Backup Options). Backup should then be done on these computers either locally by individual users or centrally as a group, by whatever means that are available on these computers (e.g., hard disk, CD/DVD, USB memory stick, etc.). An automatic daily or weekly backup is recommended.
If you need help with data backup, contact Feng Lin.
III. INSTRUMENTATION
UI300WB - VARIAN UNITY INOVA:
(Located in 55 NL; console upgraded in 2002 to Inova from a GE GN console.) A multinuclear solution and solids FT-NMR instrument. Available probes for solutions: 15N-31P (10 mm), 73Ge-17O (20 mm), 17O{X} (10 mm), 183W{X} (20 mm). Available probes for solids cover the range 29Si-31P (7 mm) and 15N-29Si (7 mm), 15N-31P (4, 3.2 mm). A broadline 2H probe and fast digitizer allow solid state deuterium studies to be performed in the temperature range of -150 to 200 ºC. Deuterium lock and unlocked mode of operation. Homonuclear and heteronuclear proton and X nucleus decoupling for solutions. Variable temperature with a range covering -100 to +100 ºC. A variety of software is available for both one and two dimensional NMR experiments.
UI400 - VARIAN UNITY INOVA 400:
(Located in 146 RAL) A multinuclear solution FT-NMR instrument. Available probes: Nalorac QUAD probe (1H, 19F, 13C, 31P) (5 mm). Deuterium lock and unlocked mode of operation. Homonuclear and heteronuclear proton decoupling. Variable temperature range varies with the probe. A variety of software is available for both one- and two-dimensional NMR experiments.
U500 - VARIAN UNITY INOVA 500:
(Located in 150 RAL; console upgraded to an Inova console in March 2008) A multinuclear solution FT-NMR instrument. Available probes: Nalorac QUAD probe (1H, 19F, 13C, 31P) (5 mm). Deuterium lock and unlocked mode of operation. Homonuclear and heteronuclear proton decoupling. Variable temperature with a range covering -100 to +100 ºC. A variety of software is available for both one- and-two dimensional NMR experiments.
VXR500 - VARIAN UNITY INOVA 500:
(Located in 150 RAL; console upgraded to an Inova console in October 2007) A multinuclear solution FT-NMR instrument. Available probes: Nalorac QUAD gradient probe (1H, 19F, 13C, 31P) (5 mm). Deuterium lock and unlocked mode of operation. Homonuclear and heteronuclear proton decoupling. Variable temperature with a range covering -80 to +100 ºC. A variety of software is available for both one- and-two dimensional NMR experiments.
UI500NB - VARIAN UNITY INOVA 500NB:
(Located in 146 RAL) A multinuclear solution FT-NMR three channel instrument. Available probes: Varian 1H{13 C/15N} Z (5mm). Deuterium lock and unlocked mode of operation. Homonuclear and heteronuclear proton decoupling. Variable temperature with a range covering -50 to +80 ºC. A variety of software is available for both multi-dimensional NMR experiments.
UI600 - VARIAN UNITY INOVA 600:
(Located in 55 NL) A multinuclear solution FT-NMR three channel instrument. Available probes: Varian 1 H{13C/15N} X,Y,Z (5 mm) and 15N-31P BB (10 mm) probes. Deuterium lock and unlocked mode of operation. Homonuclear and heteronuclear proton decoupling. Variable temperature with a range covering -100 to +100 ºC, depending upon the probe. A variety of software is available for multi-dimensional NMR experiments.
VNS750NB - VARIAN UNITY INOVA 750
(Located in A151 CLSL; console upgraded in 2002 to allow for biomolecular solid state NMR experiments; console upgraded to VNMRS console in October 2009): (Located in 151A CLSL) A multinuclear solution FT-NMR three channel instrument. Available probes: Varian 1H{13C/15N} X,Y,Z (5 mm), 15N-31P BB (10 mm), 13C{1H} (3 mm), and 15N-31P CPMAS (5 mm) probes. Deuterium lock and unlocked mode of operation. Homonuclear and heteronuclear proton decoupling. Variable temperature with a range covering -100 to +100 oC, depending upon the probe. A variety of software is available for multi-dimensional NMR experiments.
SUNDS - SUN Data Station:
(Located in 146 RAL) This is a data station based on the SUN SPARCstation Ultra 10 computer. It has the Varian VNMR software installed for data workup. Data sets may be transferred to the SPARC via Ethernet. Data may be plotted on an HP LaserJet 5SiMX for 8.5" x 11" or 11" x 17" plots.