Re: Pt NMR help
Jim Breeyear (jbreeyea@zoo.uvm.edu)
Tue, 25 Feb 1997 08:17:43 -0800
Michael D. Mosher wrote:
>
> Dear All,
>
> I apologize for the cross-posting.
>
> We have a Bruker WM-360 (360MHz for 1H), widebore. I've tuned one of our
> 5mm BB probes to Pt (but can only get a 5:1 tune as measured by O-scope).
> Pt(II) has a spin 1/2, relaxation times near 1.3-0.5 sec, but a 5000ppm
> window.
> Using a 1.0 M K2PtCl4 in D2O sample, I tried to obtain a reference peak.
> Parameters were: SW 10000Hz, PW 10us, RD 2s, RG 200, PR H 1 (we have a 2 bay
> preamp, so the BB preamps were plugged into both slots), SF and SY were set
> correctly, SI 16K. The reflected signal was >20Watts, even though the probe
> was tuned as best as it could be by O-scope. After 64 pulses, we didn't see a
> thing except for noise.
>
> Does anyone have the appropriate parameters for a Bruker (using DISNMR on
> an ASPECT 3000) system? We desperately want to do Pt, Cd, and maybe Pd NMR
> (though we know the problems with Pd NMR.) ANY help would be appreciated.
>
> Thanks, in advance,
> Mike
>
> Michael D. Mosher
> Assistant Professor / Manager NMR Lab
> Department of Chemistry
> University of Nebraska at Kearney
> Kearney, NE 68849-1150
>
> Ph: (308) 865-8491
> mosherm@platte.unk.edu
Hello Mike,
I have looked at Pt IV with a wm250 and aspect 3000 with a broad-band
10mm probe. We have a 0.7M Na2Cl6, 0.15M NaPtCl6 in D2O and get a nice
peak with about 16 scans. I use the standard formula for calculating the
synth. freq.. I use a wide sweepwidth. I will get the parameters later
and send them to you.
Jim Breeyear