The figure below shows 31P detected 31P - 13C HMQC data for dimethyl methylphosphonate with 13C decoupling during the acquisition and 1H decoupling during the entire sequence. The spectra on the top and left-hand sides of the plots are separately run one dimensional 31P and 13C spectra, respectively, both with proton decoupling. The methyl carbon of dimethyl methylphosphonate has 1JCP = 142 Hz whereas the methoxy carbons have 2JCP = 6 Hz. Two HMQC spectra were run. The one on the left was optimized for 142 Hz and the one on the right was optimized for 6 Hz. Each spectrum shows a correlation according to its coupling constant. The data were collected on a 500 MHz instrument with the appropriate bandpass filters on each channel.
2 comments:
Hello, Glenn!
I'm trying to perform the similar experiment in 1D variant on a 3-channel Bruker DRX-500 spectrometer, but it fails (very strong residual signal, no satellites). Could you kindly provide some more info about your experiment (pp used, filter&probe configuration, acquisition parameters, etc.)
Sincerely,
Sergey.
Sergey,
I used a Bruker 3 channel AVANCE 500 with a triple resonance X/31P/1H 5mm probe. The X channel of the probe was tuned to 13C. I used a 202 MHz bandpass filter on the 31P channel, a 125 MHz bandpass filter on the X channel and a 500 MHz bandpass filter on the 1H channel. I bought these filters from a a company called "DCI". I modified a standard Bruker HMQC pulse program to run the experiment. If you would like a copy of the program please email me at gafacey@uottawa.ca and I will forward it to you.
Good luck.
Glenn
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