Two questions

From: Keith Brown (brownk@chem4823.usask.ca)
Date: Fri May 26 2000 - 08:34:28 PDT


As the subject header indicates, I have two unrelated questions to ask.

1. I am trying to do some heteronuclear noe experiments, specifically, the
hoesy experiment. The two nucleii are 1H and 19F. I tried the experiment a
couple of weeks ago but got nothing. It was set up with 1H as the F2
nucleus and 19F as the F1 nucleus. When calibrating the 19F pulses (the
first time on this particular probe) I got 26 usec for the 1H 90 degree
high power pulse and 200 usec (!) for the 19F high power pulse. These both
seemed a bit excessive to me but I used them anyway for the hoesy
experiment. What I would like ask is: has anyone done the hoesy experiment
successfully (with any heteronucleii) and has anyone done it with my two
nucleii?

2. A graduate student here is interested in looking at 195Pt however, we
cannot seem to observe it. I'm sure we're setting things up for our
broadband probe ok ... tuning, matching, spectrometer frequency etc. The
probe is functioning ok ... we can observe other nucleii without trouble.
My understanding is that 195Pt should be relatively easy to observe, being
more abundant than 13C and only slightly less sensitive. We have set
up initially with a wide window (about 2000 ppm) and have moved the
offset frequency in successive jumps of about 1000 ppm for about
10000 ppm. We're using potassium hexachloroplatinate as our reference
compound with lots in solution for the initial experiments. Are there any
words of wisdom that anyone can express concerning this nucleus?

Keith Brown
University of Saskatchewan
Saskatoon, Saskatchewan

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