Hi Lacey,

  Yes it is possible to do this and there are various experiments you can apply. Usually you would need a triple resonance probe 1H, X and Y.  Depending on the sample you might need to decouple protons from 13C/31P.  Or you can use the 1Hs as a source of cross-polarisation.    Common methods would be:

1.  Heteronuclear Correlation (HETCOR) MAS NMR:  uses cross-polarisation pulse sequences.  See: Solid State Nuclear Magnetic Resonance 39 (2011) 151–157.  

2.   Alternatively, Rotational Echo DOble Resonance (REDOR) NMR.  uses Hahn-echo on 13C and pulses of 31P to interfere with the heteronuclear couplings.  See: http://www.ncbi.nlm.nih.gov/pmc/articles/PMC3246581/

If you don't have a triple resonance probe you can buy a "REDOR" box which splits the X channel into a two on a standard double resonance probe.  See http://www.nmr-service.de/redor-box.html

Hope this helps.

Paul 

Thank you, this is great! We don't have a triple resonance probe, will have to look into getting the REDOR box. Thanks again

Or maybe you should check if there is any NMR facility that has a triple resonance probe? This might be cheaper than buying (expensive) new equipment, plus they might have people that could help you with setting up the experiments.

http://nmr900.ca/index_e.html

Yes, it's what I plan to do in the meantime, thank you. Ottawa has a great facility and I've since been in contact with someone who is able to do such kind of measurements.

The Penn State NMR Facility has several spectrometers equipped with triple and quadruple resonance probes that could run these experiments.  Please contact Emmanuel Chatzakis, the new Director, at [email protected].  I'd suggest running an HSQC or HMQC with P31 observe.  You would need to revise the pulse sequence so that there was H1 decoupling during the t1 and t2 intervals.

For solid state NMR you'd need to use the methods described by Paul Wiper.  The methods I described are for liquid state samples.  Mea culpa.