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Rue extraction trial with some pics

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T

tryptographer

tryptamine photographer
So I had a go with 50 grams of Rue seeds, following the Tao with some modifications.
The vinegar stinks up the whole house, next time I'll use phosphoric acid which is totally non-volatile!
I'll skip all the details... did one Manske (with phosphoric acid instead of vinegar) and this came out.

I find these strange, golden, almost velvety crystals very fascinating! So, why not take some shots and start a thread.
This closeup was made with a 3.7x microscope objective, the picture is about 5 mm wide.


Next: the freebase and separation of harmine and harmaline!
 

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Yes, thanks everyone, it's a weird material; I'll keep some of it. I was actually hoping for somewhat larger crystals. Is it the phosphoric acid, too much salt, too quick cooling?

It's very fluffy and voluminous, unfortunately I dropped my 0.01 gram scales and can only weigh in gram precision... yield seems like about 1 - 2 grams from 50 grams of harmala seeds. A part of it got stuck on the filters, I scraped very gently because I didn't want too many paper fibers in there. All remaining filter paper will be recycled in an acid wash anyway.

Next step will be freebasing into harmine and harmaline. I hope I can filter that. More to follow...!
 
Update: today I recycled the filter paper that still had quite some harmalas on it that couldn't be scraped off, going for the bicarbonate harmine/harmaline separation. Success, I think! After adding sodium bicarbonate to the redissolved harmala HCl, heating and cooling off there was a brownish precipitation that was easy to filter off (after some additional cooling in the fridge).
See attached pic: harmine freebase on the filter (impure, brownish).

I added NaOH solution to the filtrate, the precipitate was then filtered. It's now drying, pics to follow, and tomorrow similar processing of the main yield.
 

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Thanks Melodic!

Today I processed the rest:
Dissolved the HCl crystals in water, filtered out dust, fibers etc.

Added warm saturated sodium bicarbonate solution. Maybe a bit too warm, it probably lost some CO2 and got more basic.

Filtered after ~half an hour of settling, a quick wash with some ammonia. A decent pile of brown impure harmine!

Added lye to the filtrate to precipitate the harmaline. It got milky instantly, I filtered the freebase. It's a very light tan, I'm surprised how pure it already seems to be. Still drying on the filter...
The harmine could use another round of purification but not this harmaline!

Pics to follow, I have some trouble with that card reader :x
 
Here's a pic of the final yield with a centimeter scale, harmine left (impure) and harmaline right. Too bad I can't weigh it accurately at the moment... I suspect yield could be higher.

One thing that surprised me is that the bicarbonate stage seemed to purify the liquid, the harmaline came out almost white :)

I'm not sure if I'm going to purify the harmine further, maybe first extract another batch of seeds.
 

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