Thanks to all of you who quickly replied! Ironically, I was on the spectrometer attempting this the second time when the flood of emails started arriving! I did find my PtCl4 signal; the keys were being patient (ie, nt=128 and increasing the conc. up to ~40 mM) and the confirmation that the Varian software does indeed set tof near the PtCl6 reference, so I knew with confidence were to set tof for my -1600ppm standard. I had already discounted using the 13C filter having figured out the code, and fortunately the upfield tof (107.3 MHz) was in the right direction as we do have a FM station _at_ 107.7MHz - so I did not see interference. (I think I may have encountered spurious signals from this while searching on Monday)
The overnight run of the weak "real" sample did provide a signal in about the right location, so its all good.
Again, thanks to the couple dozen of you who had quickly responded!
Cheers,
Neal
Neal J Stolowich, PhD
NMR Facilities Manager
Department of Chemistry
University of Louisville
Louisville, KY 40292
(502) 852-7894
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>>> Neal J Stolowich <stolowich_at_louisville.edu> 03/18/09 2:12 PM >>>
Greetings all!
I went looking into the archive to find discussion about running Pt195, but the search engine doesn't appear to work?
In any event, I'm attempting to run this nuclei for the first time on my Varian Inova console. I tried ~ 10 mM Pt(Cl)4 2- , but did not see anything obvious. This shift is suppose to be -1600 ppm relative to Pt(Cl)6 as 0.0ppm, however how are these shifts relative to tof that is set by default? Any pointers from those who have run Pt would be appreciated (for instance, is the 13C 125 MHz135-35-8bb tubular filter wide enough band pass to use as well, or too high for 107 Mhz? And have I have switched to the 60 - 120 MHz 1/4 wave length cable as well. )
Thanks!
Neal
Neal J Stolowich, PhD
NMR Facilities Manager
Department of Chemistry
University of Louisville
Louisville, KY 40292
(502) 852-7894
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Received on Thu Mar 19 2009 - 05:23:49 MST