Monday, January 11, 2016

The NMR Laundromat

Source: OPRD / CNRS
The simplest, most practical solutions* are often the best.

I'm reminded of classic papers for pragmatic lab procedures, like Clark Still's on flash chromatography, or Gottlieb & Nudelman's on detecting trace NMR impurities. Everyone has encountered their lab's version of the Kugelrohr setup - run by an old electric kettle and a windshield-wiper motor!

From the ASAP of Organic Process Research and Development comes this handy one-pager: a how-to on cleaning dozens of NMR tubes simultaneously, using glassware readily available in just about any synth lab.

Seeing this instantly triggered a "Well, duh!" moment for me - the amount of time I've stood before a stoppered 500mL vacuum flask impaled with a cannula, washing single tubes by hand...I'm sure it reaches into hours, if not days.

If you try this, leave a comment; I'm really quite interested to see how it turns out. I'd also wonder if OPRD might be angling for other quick one-offs. Couldn't hurt to try, right?

*Of course, I'd be remiss if I didn't point unfamiliar readers to the treasure trove that is Not Voodoo.


  1. Thanks to your link: how did i miss hearing about the "Organikum" all these years? Sounds awesome!

  2. Looks awesome, but I don't want to put my desiccator through that

  3. You don't have to use a desiccator. The idea (Evacuate tubes face down in solvent and then back fill with air to drive the solvent up) can be applied in any vessel you can pull a vacuum on. I just did it using the bottom of a rather small vacuum trap. You could do it in a round bottom provided it was tall enough for the tubes, but it wouldn't be as convenient.

  4. We buy cheap 100 MHz tubes (for most routine spectra you really don't need anything else) and throw them away after use. Time wasted on cleaning costs more than the tubes. But that's just the industrial attitude ;)