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We just bought a new console (with Topspin 3.2)for our Bruker 400 and noticed that not all experiments that we previously used to run are setup on the new version. For instance, 195Pt experiment is not working. The message that appeared when we tried it was: "Cannot perform getprosol. The following files are not found. Observe pulses for 195Pt. DE and Trim pulses for 195Pt". Could any one help with the step-by-step procedure for setting up this experiment? Perhaps the probe file is not populated with pulses for 195Pt. We would greatly appreciate your help.

asked Mar 19 '14 at 11:50

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IA
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Yes, your prosol file is not set up correctly. You can avoid using the getprosol command in the "new" dialog by unchecking the appropriate box. You then have to set the pulse lengths and power levels manually.

Once you have the 90 degree pulses calibrated, enter them into "edprosol" (see manual), and "edprosol" will calculate any other pulses. You will also need to enter a value for DE (6.5 to 8 usec is typical) and trim pulses (2.5 ms is typical).

It is recommended that you use "getprosol" for setting the pulses and powers.

If you have "powcheck" enabled (recommended) you may need to enter a power limit into probe file ("edhead"). If you are not sure of what power level is safe, please consult Bruker, but a power level similar to that for 13C would be reasonable.

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answered Mar 20 '14 at 10:04

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Kirk Marat
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updated Mar 20 '14 at 10:10

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Kirk is correct! But what kind of pulse program do you want to use? I got problems, using "zg", but "zgdec" works better! Also remember you have the biggest range of SW for 195 Pt ever to observe, but the NMR has only a small range to offer! User O1P to move the SW window into the correct position and region.

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answered Mar 25 '14 at 07:05

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Ulrich Haunz
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Agree with all Kirk and Ulrich say. On our 3.2 topspin, powercheck is on by default. So edhead powerlevels have to be input, then the pulsewidth calibrations into edprosol each time a new nucleus is attempted. I have found that slightly larger DE is better for 195Pt (about 20us) on our BBFO probe.

Each time I try 195Pt I relearn that the biggest problem with 195Pt is simply finding the resonance(s): the probe can observe only about 1000ppm on a 500. We make our best guess about chem shift, but the compounds are often novel enough to resist our estimates. In such cases, it helps to run 6 or seven spectra that overlap each other and cover the full spectral region queued or in automation in an overnight run. That insures that all compounds are observed (with limits of s/n).

I am curious about zgdec; that is not a sequence I see on our version TopSpin 3.2, or in 1.3 either. Is this perhaps zgdc, which adds proton decoupling? Similar then would be zgpg, decoupling that is power gated (somewhat lower during d1 to assist in not heating the sample).

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answered Mar 26 '14 at 08:20

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Charlie Fry
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Sorry - it's 'zgdc' instead of 'zgdec' ... decoupling included! Sorry! Uli - Ulrich Haunz (Apr 02 '14 at 01:07)

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It may probably be appropriate to answer this question by narrating a similar instance, and I recall such an instance of about 20 years before:- an experience with AC300 Bruker NMR Spectrometer which was in use at that time in North Eastern Hill University, Shillong, INDIA.

I was trying to implement a J-Scaling pulse sequence, from the Library of Automation Programs (set of Bruker .AU extension files provided in a Diskette). When the Program was set up and the Command was given to run, the monitor returned a prompt as if nothing has happened. No error Messages, nor any other consequence of trying to run the instruction set. (In the case of this query on 195pt, an error message seems to result). For the case of J-scaling with AC300, I sent a message to the Bruker India Scientific, and after a while I was informed that these pulse programs in the Diskette where not tried out and run in the AC300 spectrometer housed at North Eastern Hill University. Such case histories prompt me to suggest that it would be better to contact the supplier, rather than any other user of similar packages. I am not sure whether, queries in nmrwiki get answered by the Bruker Engineers. S.Aravamudhan

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answered Apr 02 '14 at 23:19

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SankarampadiAravamudhan
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updated Apr 02 '14 at 23:20

The advantage of asking questions here, especially ones of a general nature, is that others can benefit from the answers. Specific questions about broken hardware, software bugs, etc. may be better directed at your vendor. I know several Bruker enployees provide very useful answers in this group. - Kirk Marat (Apr 04 '14 at 13:48)

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Asked: Mar 19 '14 at 11:50

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