September 19, 2024, 06:18:17 PM
Forum Rules: Read This Before Posting


Topic: Grease in NMR  (Read 14898 times)

0 Members and 1 Guest are viewing this topic.

Offline gilgerto

  • Very New Member
  • *
  • Posts: 1
  • Mole Snacks: +0/-0
Grease in NMR
« on: May 05, 2008, 09:56:44 PM »
I often have grease in my 1H NMR (broad s 1.26 ppm and small m 0.86 ppm) of purified product when running a column on small amount of material (below 50mg). I'm doing everything I can to avoid it (gloves, use dist. hexanes, flushing column with eluant before chromatography...). Any comment on that???

Offline agrobert

  • Chemist
  • Full Member
  • *
  • Posts: 629
  • Mole Snacks: +69/-17
  • Gender: Male
  • diels alder
Re: Grease in NMR
« Reply #1 on: May 05, 2008, 10:16:18 PM »
More likely from rotovap ground glass joints and/or not so "clean" NMR tubes.  Try cleaning your NMR tubes with hexanes, methanol, and acetone.  When you are running small samples these peaks tend to show up more.
In the realm of scientific observation, luck is only granted to those who are prepared. -Louis Pasteur

Offline gericox

  • Regular Member
  • ***
  • Posts: 45
  • Mole Snacks: +0/-2
Re: Grease in NMR
« Reply #2 on: May 13, 2008, 04:32:44 PM »
Make a "blank" spectra with deutered solvent in your NMR tube to check absence grease and to be sure it's clean

Offline Mitch

  • General Chemist
  • Administrator
  • Sr. Member
  • *
  • Posts: 5298
  • Mole Snacks: +376/-3
  • Gender: Male
  • "I bring you peace." -Mr. Burns
    • Chemistry Blog
Re: Grease in NMR
« Reply #3 on: May 13, 2008, 10:20:37 PM »
Doesn't grease come out at 0 more than 1.26 ppm?
Most Common Suggestions I Make on the Forums.
1. Start by writing a balanced chemical equation.
2. Don't confuse thermodynamic stability with chemical reactivity.
3. Forum Supports LaTex

Sponsored Links