That's okay if it's my left eye (it don't work). He asked about the distillation specifically so I answered. I thought it was a fair example to show heating solvents is perfectly fine so long as you do it safely. Distilling serves no purpose other than letting me re-use chemicals thst are fairly hard to find and expensive where I live.

Upon latest recrystalization, all impures were removed. White supershard fluff left over. Total weigh is at 0.744+ 0.320 after re-x in hot naphtha, so 1.064g from 100g of pulverized rootbark. Excellent results imo for swims first go. Next up, a slow acetone re-x to see if solid crystals can grow.

Thx @EW , @1ce Slowly swims chemistry will improve to the understanding of this rather (seemingly) long-winded process. Chems are easy to access in swim part of the world, this is swim's lucky situation however.

Sweet!
Glad to hear of positive outcomes (:

Happy travels!

Great job man! I'm not sure about acetone.. It's miscible with water and eats plastic. So the room for error certainly is larger here. Adding boiling heptane slowly often works good for me

I think it'a you who is confused. Perhaps. DCM layer settle at the bottom. If you're doing larger extraction without a sep then you're probably being ineffective at it.

And if 'big words' you in the 'advanced chemistry' section of this forum then maybe you should avoid it for now. Although I am still unsure as to what you're relating to. Leibig?

I see many other approaches as being silly. Because it costs me money and hours of driving to go about them.

Why's that?

Overall, generally speaking, STB approaches are more likely to be "ineffective" (read: inefficient), on the whole, than not using a sep funnel (regardless of approach).

I didn't mean to generalize, a syringe does a perfectly splendid job. With bottom layer solvents like DCM a sep funnel I feel is a much better approach. I'm doing an A/B on mimosa right now and the whole process has gone substantially more smoothly than any STB I've ever done.

Seperatory funnels are key in my opinion. They simplify the whole process an immense amount. Syringes work too, but plastic syringes can be dissolved by solvents, so be careful.

I've had success using a solvent mixture of hexanes and DCM in a STB, lowering the density so the organic layer floats on the top. This way it can be siphoned off. I have found using DCM or aromatic solvents extracts the alkaloids better per pull, something like 90 to 95% in the first pull using DCM.

But as its been said, STB are inefficient and messy. The time you save omitting the filtering is lost in the work up of the messy bark sludge.

A/B is the way to go. Higher yields and cleaner extraction and of course, sep funnel.

DCM is definitely a great solvent for this extraction, but now I even lean towards toluene because it still extracts as well as DCM. Since I don't evap the solvent anymore and precipitate the salts using FASA, the high vapor pressure of DCM becomes more of a curse then a blessing.

I don't know why anyone would use Naphtha, I had to use something like 300-400mls and 3 pulls to get the same amount of product I could get from 1 pull of 50mls of DCM or toluene. (Take those numbers with a grain of salt im exaggerating slightly.)

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On another note, I think 1ce's use of 'big words' is helpful for me to understand his procedure. It's also easier to identify the problem at hand and propose a solution. Rather then making arbitrary arguments that don't solve anything. Earthwalker if you had bothered to actually read his post rather then dismissing it, you would have noticed that he was addressing something entirely different.