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Chemistry Forums for Students => Analytical Chemistry Forum => Topic started by: HailoMan on September 26, 2016, 12:49:52 AM

Title: NMR Reference
Post by: HailoMan on September 26, 2016, 12:49:52 AM
Apology in advanced if this is a silly question, but in calibrating 1H NMR spectra, can I use water residue as a reference instead of the internal solvent residue?
I did a 1H NMR measurement of gamma-valerolactone (GVL) in DMSO-d6. The DMSO residue peak (2.50 ppm) happen to overlap with 2 of the proton peaks of GVL, so I can't use the DMSO as an internal standard.
Title: Re: NMR Reference
Post by: discodermolide on September 26, 2016, 06:03:33 AM
Surely this compound should be soluble in chloroform? Then you can use that as the reference.
Title: Re: NMR Reference
Post by: Babcock_Hall on September 26, 2016, 10:13:03 AM
The chemical shift of water depends upon temperature; therefore, one would have to take this into account.
Title: Re: NMR Reference
Post by: HailoMan on September 28, 2016, 03:58:27 AM
Surely this compound should be soluble in chloroform? Then you can use that as the reference.

Unfortunately, the compound (nitrogen-doped carbon nanotubes) is non-dispersible in chloroform or other common NMR solvents.

The chemical shift of water depends upon temperature; therefore, one would have to take this into account.

Thank you for this information. I will look into it.
Title: Re: NMR Reference
Post by: Dan on September 29, 2016, 04:44:23 AM
Why not just add an internal reference that does not overlap with anything - e.g. tetramethylsilane at 0 ppm?