J.B. Stothers NMR Facility
Department of Chemistry
Western University
London, Ontario, Canada
NMR Service - Solid Samples
About Solid-State NMR Spectroscopy

The vast majority of NMR samples are studied in the liquid-state where solid samples are dissolved in the appropriate deuterated solvent. If your sample is appeciably soluble in a common solvent, you will likely want to study your sample using liquid-state NMR spectroscopy.

For samples that are not soluble in any known solvents or whose structure changes drastically when dissolved in solution then solid-state NMR spectroscopy can be used to characterize your sample. In comparison to liquid-state NMR spectroscopy, these are the major differences:
  • The resolution of solid-state NMR is inferior to that of liquid-state NMR. For nuclei other than H-1, solid-state NMR peaks are generally at least 10 times broader than liquid-state NMR peaks.
  • H-1 NMR spectra of solid organic samples are generally composed of broad, featureless peaks and usually provide no useable information.
  • The sensitivity of solid-state NMR is also inferior to that of liquid-state NMR. As a result, solid-state NMR experiments generally take a minimum of a few hours and at least 50mg of sample is required.
  • In general paramagnetic samples give better solid-state NMR spectra than liquid-state NMR spectra; however, the NMR is still much more complicated than that of diamagnetic sample and often no NMR signal is obtained.
  • Solid-state NMR can provide information about the symmetry of your molecule and the distance between certain atoms within your molecule.
Services Provided

Depending on your experience using NMR spectroscopy as a means of structural characterization, the NMR facility can perform a variety of functions. For experienced users, staff generally just acquire the NMR data and provide the raw NMR data. For novice users, NMR Facility staff can also process and help with analysis of the NMR spectra. For all service work, a report summarizing the NMR experiments performed and the experimental conditions utilized is included. The turn-around time is typically 3 - 4 weeks, but will vary considerably depending on the experiments required and number of samples.

The NMR facility can perform the following solid-state NMR experiments:
  • Experiments can be performed using magic-angle spinning (MAS), up to a maximum spinning rate of 25 kHz, or on stationary samples.
  • 1D NMR experiments can be performed on a huge variety of spin-1/2 and quadrupolar nuclei such as B-11, C-13, F-19, Al-27, Si-29, P-31 and many more nuclei.
  • 2D experiments such as MQMAS, REDOR, TRAPDOR.
  • Any of the above experiments can also be performed above room-temperature, up to a maximum of +240 °C, or below room-temperature, down a minimum of -130 °C.

Rates

Solids NMR service work is charged on a per spectrum, per sample basis. In addition, the first time a sample, or series of similar samples are studied, a one-time setup fee will be applied.

The rates for solid-state NMR service can be found in the table below. The prices are in Canadian dollars and are effective until April 30, 2019. If desired, one can also download the Solids NMR Service Rates in a PDF file.

Rates and Sample Amounts for Solid-State NMR Service
Experiment Academia / Not for Profit Industry Minimum sample amount (mg) Comments
1D NMR Experiments
Setup Fee $60 $120 N/A One time fee charged the first time a sample, or series of similar samples, is acquired in our NMR Facility. Fee covers the cost of calibrations required to optimize the experimental NMR parameters.
13C MAS $115 $200 50 Acquisition of direct detection 13C{1H} NMR spectrum.
13C CPMAS $80 $140 50 Acquisition of cross-polarization 1H-13C NMR spectrum.
19F MAS $70 $125 25 Acquisition of direct detection 19F NMR spectrum.
29Si MAS $115 $200 500 Acquisition of direct detection 29Si{1H} NMR spectrum.
29Si CPMAS $90 $160 250 Acquisition of cross-polarization 1H-29Si NMR spectrum.
31P MAS $90 $160 50 Acquisition of direct detection 31P{1H} NMR spectrum.
31P CPMAS $75 $130 50 Acquisition of cross-polarization 1H-31P NMR spectrum.
Other nuclei TBD TBD TBD Charge depends on the compound, nuclei of interest and desired NMR experiment.
Variable Temperature
> 21 °C $15 $25 N/A Charge per temperature point. Maximum temperature is +240 °C.
< 21 °C $25 $35 N/A Charge per temperature point. Minimum temperature is -120 °C.
Consultation and Interpretation of NMR Spectra
Interpretation $60/hour $120/hour N/A Charge for NMR facility staff to provide interpretation of the NMR spectra, spectral assignments and a written report explaining the interpretation.
Consultation $60/hour $120/hour N/A Charge for NMR Facility staff to do extensive research and consultation to aid with project planning and development.
Sample Submission Procedure for Western Personnel

The following procedure should be used by Western personnel when submitting a sample for service work:
  1. Contact NMR facility staff via e-mail at chemnmr@uwo.ca or phone at 519-661-2111 x. 82905 to discuss what information you are looking to obtain by using solid-state NMR, the nature of your sample and what services are required.
  2. Fill out and print Solid-State NMR Service Request - Western Personnel. Note that the form is a fillable PDF form that can be filled out electronically.
  3. Bring the appropriate amount of sample (see table above) in a screw-top vial and the completed sample submission form to the NMR facility.
  4. NMR data will generally be acquired within 4 weeks of sample receipt and will be sent via e-mail. The sample report will generally be sent via e-mail about 1 week after the data has been acquired and processed.
  5. Charges will be applied directly to the PI's account using speed code specified on the Service Request form at the end of the month in which the NMR spectra were acquired.
Sample Submission Procedure for External Clients (Non-Western Personnel)

The following procedure should be used by non-Western personnel when submitting a sample for service work:
  1. Contact NMR facility staff via e-mail at chemnmr@uwo.ca or phone at 519-661-2111 x. 82905 to discuss what information you are looking to obtain by using solid-state NMR, the nature of your sample and what services are required.
  2. Fill out and print Solid-State NMR Service Request - External Clients. Note that the form is a fillable PDF form that can be filled out electronically.
  3. Bring the appropriate amount of sample (see table above) in a screw-top vial and the completed sample submission form to the NMR facility. Alternately the sample can be mailed, along with the completed sample submission form, to:
    4. Mathew Willans
    Western University
    1151 Richmond St. N.
    Department of Chemistry
    Dock 003, Room 11
    London, ON
    N6A 5B7
  4. NMR data will generally be acquired within 4 weeks of sample receipt and will be sent via e-mail. The sample report will generally be sent via e-mail about 1 week after the data has been acquired and processed.
  5. An invoice for services rendered will be generated by Sherrie McPhee in ChemBioStores and sent via mail. Only once the invoice is received is payment required.