RE: AMMRL: NMR - Reference Standard recommendations?

From: Bill Stevens <billstevens55_at_gmail.com>
Date: Fri, 28 Feb 2014 13:14:05 -0600

You don't want to do 90s with EtBz. In a standard sample, the T1's are
quite long - one phenyl proton over 40s.

Bill Stevens
84 Roosevelt Road
Carbondale, Illinois 62901
On Feb 28, 2014 11:49 AM, "Plant,Daniel" <dan_at_mbi.ufl.edu> wrote:

> Hi Margaret,
>
> You might be able to just get the ASTM standards for 1H and 13C.
>
> 0.1% ethyl benzene in CDCl3 and benzene-d6/dioxane 60/40.
>
>
>
> You can shoot 90's and measure S/N with these and get an idea of how your
> shims are from the shape and resolution of the quartet/triplet in the 1H
> ethylbenzene and the depth of the valleys on the benzene triplet in the 13C
> spectrum.
>
> 1H decoupling efficiency can also be calibrated and measured using the
> resolution of the decoupled dioxane peak.
>
>
>
> COSY could be a gramicidin/DMSO-d6 sample. Commercially available.
>
> Cholesterol acetate in CDCl3 is a good commercial sample for testing 13C
> APT experiments
>
>
>
> NOESY...harder if you're running organics...find something close to what you
> want to run and characterize it so you know a few peaks that should give
> NOESY peaks.
>
>
>
> There's a few others if you like to shim and measure lineshape, calibrate
> temperature, etc. but those will get you started.
>
> Dan
>
>
>
>
>
> *From:* Smallbrock, Margaret A. [mailto:Margaret.Smallbrock_at_sdsmt.edu]
> *Sent:* Wednesday, February 26, 2014 7:08 PM
> *To:* ammrl_at_ammrl.org
> *Subject:* AMMRL: NMR - Reference Standard recommendations?
>
>
>
> Greetings all,
>
>
>
> I have a lone Bruker AC300 in my facility. It does have a Tecmag DSPect
> upgrade that replaced the original computer. I have been making NMR
> reference samples as needed, but would like to purchase some reference
> standards to make it easier on me. I have been reading through a lot of the
> literature on what is available out there and would be interested in what
> all of you have out there. What would be the recommendation from the
> experts out there? I am also working on getting our COSY and NOESY working
> with the system as well, but that will need to be a made sample as I do not
> see reference samples for that.
>
>
>
> Can anyone make recommendations on what samples to purchase that would be
> in my best interest?
>
>
>
> Margaret Smallbrock
>
>
>
> Margaret Smallbrock
>
> Chemical and Instrumentation Specialist
>
> Department of Chemistry and Applied Biological Sciences
>
> SD School of Mines
>
> 501 East St. Joseph Street
>
> Rapid City, SD 57701
>
>
>
> (605) 394 - 1236 - Phone
>
> (605) 394 - 1232 - Fax
>
>
>
Received on Fri Feb 28 2014 - 09:14:07 MST

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