LL-Extraction For Gently Removing Water?

So I kind of screwed up while preparing my ethanol to use in a cryo-etoh extraction. What I thought was azeotropic ethanol that I measured fresh out of my LM reflux column (warm) only ended up being 93.5%-94% when measured at room temp. Unfortunately, I discovered this post extraction when I saw a white emulsion layer while purging my ethanol on a small batch and went back to proof my solvent to see where the water came from.

The rest of my extract is still in solution, but I decided to just boil off the water in this small test-run and noticed the color darken a bit more than I anticipated by the time I boiled off all the water. It likely decarbed somewhat, which I was trying to avoid. I have read up on Beaker’s LL-extraction technique and wondered if this technique would work for removing the water in the extract. I plan on distilling off the pentane, adding a little methanol to get the extract out of the boiling flask, then allowing the solution to purge under a fume hood on a hot plate set at 60c. Does anyone see any issues with this? I have yet to acquire a vacuum oven, or else I would have just gone that route. Also, could distilled water be used in place of deionized water in the LL extraction? Thanks in advance for any input.

Taking iT to 60C is gooing to decarb more so air drying is the way to go
Do You have a vacuum vessel ?

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The collection pot of a cls can be a vacuum vessel have one of those ?

Distilled water is fine .

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Sorry miread your %

Not at the moment. I was planning on getting a vacuum oven in the next few months which is why I don’t have a vacuum chamber, but I suppose I should just shell out the $100 and order one if it means improving the quality of my extract in the meantime. I also don’t have a cls. Actually, come to think of it I do have a clean 3-gallon paint pot I was thinking of using as a pressure vessel in the future. I wonder if that would hold vacuum? I was actually considering using a vacuum chamber as a cheap vacuum oven by setting it in a warm water bath. Maybe I should consider going through with that idea in the meantime?

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I would just leave Some pentane to get out of the flask
Spread a real thin layer in the vacuum chamber and take time evaporating iT all of ppm of pentane is higher but patience can take that away

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Awesome! Thanks for that. My initial thought was to be stingy with the pentane since it costs so much more than methanol, but I guess I’m really not losing that much if it’s just enough to move the extract out of the boiling flask. The boiling point is also half of what methanol is, so that should help immensely.

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Bring the flask to 30C take out everything then Ad pentane make warm again to 30 C swirl like mad and pour

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