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posted Oct 31 '12 at 03:51

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CaymanDave
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Varian VNMRJ 2.2D standard experiments

Hey folks, I was wondering if anyone else has had any issues with the experiments/pulse sequences that came standard in the VNMRJ software? I am running VNMRJ 2.2D on Red Hat Enterprise, but have yet to have much success with any experiment outside of standard 1H, 13C, 19F, and 31P. Lately we have been trying to run C13DEPT, C13APT, (HC)HMBC, (HC)HSQC, and HETCOR, and have come up with nothing usable. The DEPT experiment produces the 4 expected spectra, but three are blank/noise and the fourth is just a standard carbon scan; the APT was promising, but I noticed a peculiarity about it: if I printed out the c13 spectra, the peaks were positive/negative as expected until about halfway through, where the spectra repeated itself, only upside down and in the opposite direction (as if it were simply rotated 180 degrees around the center of the spectra); HMBC, HSQC, and HETCOR all ran, but when I try to open them, I only get the message "LP analysis failed." Any attempt to display either fid or the 2D comes up fruitless (after wft each fid independently, selecting a 2D display returns the message "No 2D data in data file"). I have been able to open the HETCOR in a separate software suite (ACD labs Spectrus Processor), and the spectra there are horrific: the proton spectra is a pooly defined mess of peaks mirror imaged around the tof, and the carbon scan comes up as simply noise.

Any help you can give for how to tweak the parameters or pulse sequence is appreciated. I feel like my job depends on it!

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posted Oct 31 '12 at 03:56

CaymanDave's gravatar image

CaymanDave
11

Varian VNMRJ 2.2D standard experiments

Hey folks, I was wondering if anyone else has had any issues with the experiments/pulse sequences that came standard in the VNMRJ software? I am running VNMRJ 2.2D on Red Hat Enterprise, but have yet to have much success with any experiment outside of standard 1H, 13C, 19F, and 31P. Lately we have been trying to run C13DEPT, C13APT, (HC)HMBC, (HC)HSQC, and HETCOR, and have come up with nothing usable. The DEPT experiment produces the 4 expected spectra, but three are blank/noise and the fourth is just a standard carbon scan; the APT was promising, but I noticed a peculiarity about it: if I printed out the c13 spectra, the peaks were positive/negative as expected until about halfway through, where the spectra repeated itself, only upside down and in the opposite direction (as if it were simply rotated 180 degrees around the center of the spectra); HMBC, HSQC, and HETCOR all ran, but when I try to open them, I only get the message "LP analysis failed." Any attempt to display either fid or the 2D comes up fruitless (after wft each fid independently, selecting a 2D display returns the message "No 2D data in data file"). I have been able to open the HETCOR in a separate software suite (ACD labs Spectrus Processor), and the spectra there are horrific: the proton spectra is a pooly defined mess of peaks mirror imaged around the tof, and the carbon scan comes up as simply noise.

Any help you can give for how to tweak the parameters or pulse sequence is appreciated. I feel like my job depends on it!

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posted Oct 31 '12 at 08:43

CaymanDave's gravatar image

CaymanDave
11

Varian VNMRJ 2.2D standard experiments

Hey folks, I was wondering if anyone else has had any issues with the experiments/pulse sequences that came standard in the VNMRJ software? I am running VNMRJ 2.2D on Red Hat Enterprise, but have yet to have much success with any experiment outside of standard 1H, 13C, 19F, and 31P. Lately we have been trying to run C13DEPT, C13APT, (HC)HMBC, (HC)HSQC, and HETCOR, and have come up with nothing usable. The DEPT experiment produces the 4 expected spectra, but three are blank/noise and the fourth is just a standard carbon scan; the APT was promising, but I noticed a peculiarity about it: if I printed out the c13 spectra, the peaks were positive/negative as expected until about halfway through, where the spectra repeated itself, only upside down and in the opposite direction (as if it were simply rotated 180 degrees around the center of the spectra); HMBC, HSQC, and HETCOR all ran, but when I try to open them, I only get the message "LP analysis failed." Any attempt to display either fid or the 2D comes up fruitless (after wft each fid independently, selecting a 2D display returns the message "No 2D data in data file"). I have been able to open the HETCOR in a separate software suite (ACD labs Spectrus Processor), and the spectra there are horrific: the proton spectra is a pooly poorly defined mess of peaks mirror imaged around the tof, and the carbon scan comes up as simply noise.

Any help you can give for how to tweak the parameters or pulse sequence is appreciated. I feel like my job depends on it!

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Added new information

posted Nov 02 '12 at 06:03

CaymanDave's gravatar image

CaymanDave
11

Varian VNMRJ 2.2D standard experiments

Hey folks, I was wondering if anyone else has had any issues with the experiments/pulse sequences that came standard in the VNMRJ software? I am running VNMRJ 2.2D on Red Hat Enterprise, but have yet to have much success with any experiment outside of standard 1H, 13C, 19F, and 31P. Lately we have been trying to run C13DEPT, C13APT, (HC)HMBC, (HC)HSQC, and HETCOR, and have come up with nothing usable. The DEPT experiment produces the 4 expected spectra, but three are blank/noise and the fourth is just a standard carbon scan; the APT was promising, but I noticed a peculiarity about it: if I printed out the c13 spectra, the peaks were positive/negative as expected until about halfway through, where the spectra repeated itself, only upside down and in the opposite direction (as if it were simply rotated 180 degrees around the center of the spectra); HMBC, HSQC, and HETCOR all ran, but when I try to open them, I only get the message "LP analysis failed." Any attempt to display either fid or the 2D comes up fruitless (after wft each fid independently, selecting a 2D display returns the message "No 2D data in data file"). I have been able to open the HETCOR in a separate software suite (ACD labs Spectrus Processor), and the spectra there are horrific: the proton spectra is a poorly defined mess of peaks mirror imaged around the tof, and the carbon scan comes up as simply noise.

Any help you * UPDATE * Since I can give for how to tweak the only comment 300 characters, I decided to add my response/update as an edited addition.

To Uli: Sample volume and depth are spot-on, aligned with the field. I have tried both manually shimming and gradient shimming, in addition to gradient shimming and then manually fine-tuning the coils. Our nuclei tuning are both done manually. All of the 1D's came up beautifully, and I have run a 13C before each DEPT and APT, and a 1H and 13C before each 2D experiment. I know wft is only for 1D, and I only used it to observe the single spectra by themselves to see what the NMR produced in 1D. Unfortunately, I seem to be lacking this magical green "auto processing" button for 2D, but have been able to process them without it. So, I can safely say shimming and tuning are not the problem :)

Interestingly enough, I changed the decoupling parameters or for a HETCOR experiment after noticing that, though the text boxes showed the pulse sequence is appreciated. I feel like my job depends on it!width and power for decoupling, entering "pp?" and "pplvl?" into the command line yielded '0' for both. I manually entered in the values, and subsequently got a 2D HETCOR; the only problem is, the carbon channel shows a mirror image of itself, (just as in the APT) making the data essentially useless. I'll try to get an image of it. I also ran an array of pw for a standard 1H scan just to ensure that the power hadn't degraded, and that came up exactly as expected, so no problem there.

Thanks for the help!

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