Syrian rue extraction failure

[ginjim]

Followed all the way the through the tao of rue

finished the manske extraction and there were just a few crystals in the bottom of the filter after later looking they look like salt crystals

(any idea where the crystals are?)

No idea where they got to.

Once your alks have settled, you want to decant as much of the basic liquid as possible.


After you have decanted the basic (high ph) lye water off the top, you want to add some hot vinegar and water to your freebase alks to redissolve everything back into the solution as harmala acetates. Once your alkaloids are redissolved, filter out anything that won't dissolve. This is mostly plant matter and oils.

after adding the lye, the solution was settled.

and the clear top part was decanted and discarded.

swim then boiled up so vinegar and added it to the cloudy alkaloid solution.

swim had 400ml solution so added 40gms salt which was dissolved.

left overnight and filtered but no crystals.


will the crystals be in the alkaloid solution? how is best to extract from here? does swim add more vinegar and more salt again?

or add more lye??
thank you

 

[ginjim]

What is the current state of the solution? (color, transparency, contents)

If you've got a cloudy solution of suspended freebase particles with too much lye, then you'll need to add vinegar until it turns dark redish brown and becomes transparent.

At that point I would probably just re-base so that you can filter them out and start with a fresh solution. Then you can dissolve the freebase alkaloids (should be a greyish color) in water, adding vinegar until they go into solution. Then you can add 100g/L salt and your alkaloids should crystalize as harmala HCl's.

Thanks for the reply

i have one which I have just added lye to. it's state it slightly thick brownish colour little cloudy.waiting to preticipate

other is now a mixture of vinegar, lye and water in a liquid state slight brown not clear high ph

and I have one more which is dark and clear which is from what I have decanted from the lye solutions

 

[arcologist]

If you are sure that the first two solutions have a high pH and haven't precipitated any white/grey/pinkish particles, then it's pretty likely that there aren't very many harmalas in them, because they should have precipitated already (like instantly as soon as you raised the pH). Let them sit to see if anything settles out. Then maybe add some more base just to make sure the pH is high. If there's still nothing lightly colored that comes out of solution then it's pretty safe to assume there's nothing there.

I'm not sure about the third solution, is the pH high? If not you could try adding more base to see if anything precipitates. Otherwise, I haven't a clue.

This isn't mentioned in any teks that I've seen, but I've noticed that a rue solution that filters clean before basing will precipitate a large amount of black/dark brown sludge after basing. I'm pretty sure these particles weren't there before basing the solution and can make it a huge pain to get the alkaloids. This is why I recommend performing the manske step first (contrary to tao of rue) because you will end up discarding the bulk of the dark sludge before it is based out of solution. It's caused me problems in the past and I'm surprised no one mentions it.

 

[Metanoia]

This isn't mentioned in any teks that I've seen, but I've noticed that a rue solution that filters clean before basing will precipitate a large amount of black/dark brown sludge after basing. I'm pretty sure these particles weren't there before basing the solution and can make it a huge pain to get the alkaloids. This is why I recommend performing the manske step first (contrary to tao of rue) because you will end up discarding the bulk of the dark sludge before it is based out of solution. It's caused me problems in the past and I'm surprised no one mentions it.

I noticed this as well, which is what I was talking about earlier about the first base being the trickiest. Your tea is as clean as you think you can get it, but when you base there's a lot of crunge that comes out and makes it a pain to filter.

The next time I do a rue extraction I'll try the manske first. I was just under the impression that you needed to base first to pull some of that nasty stuff, which doesn't really dissolve and gets filtered before the first manske anyhow.

ginjim, I assume this is your first attempt at a rue extraction. A lot of the problems you're having are normal on a first attempt, but I would recommend reading and reading and reading the tao until you're completely sick of it If you're unsure about something, consult the tao. Every single mistake I've made in any extractions I've ever done were because I wasn't completely sure about something and I made a guess at it. Like the amount of lye you were using for example. In the tao is says to slowly add a lye solution until it turns milky, then a little more to be certain you have a high enough pH and the alkaloids will all precipitate out. In my experience it only takes as little as 10 grams of lye in a solution to achieve that.

Don't take any of this personally, I'm just trying to help

 

[endlessness]

Check the Harmala Extraction and Separation Guide, maybe it seems more understandable to you.

It's kinda hard to follow what has happened.

How many grams rue did you extract?

Never throw anything away, discard any liquids or solids, before you have finished an extraction. This way if something goes wrong you can always recover the alkaloids.

Adding too much lye should not be the problem I think, the alkaloids would still have precipitated. And then when you redissolved and added the salt, the alkaloids should have precipitated again.

You have to wait a while before the harmala salts precipitate after adding the salt, like a couple of hours or a day.

If nothing happened, I'd warm it up again and add more salt, let it cool slowly again see if it precipitates. If it doesnt, probably there are no alkaloids there... ? You can try adding lye again to see if alkaloids precipitate.

If nothing works, start again.. sorry if it comes to this... next time please follow instructions carefully, maybe read the other harmala extraction guide I mentioned and see if it makes more sense to you.

And dont give up, once you got the rue extraction down, its great and not hard at all!

 

[ginjim]

thanks guys, i really appreciate your help,

i used 200 gms rue

basically I have done several high dose lye bases, mankes and filters with nothing being left in the filter, just seems to run through not leaving anything

basically I have got loads of high lye solutions and used filters.

So do you suggest I put all solutions back in the pan, warm, (add 100gm/1l salt.

then cool. and then base?

 

[ginjim]

ok on one of the solutions i was going to put in pan to warm.
but poured it back in the container so gone cloudy again

i noticed there was a little greyish sludge at bottom. about 5ml

gonna have to leave it again to rest hopefully it will settle again.
could i be expecting more of that sludge? if add more salt/vinegar etc




this is the first bit of different state/sludge i have seen since my 1st base.

 

[endlessness]

It's really hard to follow what you're doing. You are adding vinegar and salt and base and changing containers, don't mix it all! God knows what pH it is now, if it's salt saturated or not, etc... Please don't just do steps for the sake of it without having an understanding of what exactly is happening.

Unless you just let it be and recover some precipitate and attempt to purify it further, I'd just forget about this extraction and start new, going step by step as the tek says, maybe check the other harmala extraction in the wiki.

 

[ginjim]

hi the one with the little bit of residue was a manske which gave no crystals.

Last night I added a little bit more vinegar to make cloudy as suggested and then added a lye mix.

this is the 1st time I have seen alkaloids since the 1st base.

 

[armbarsalot]

easy caapi tek might be a better start. Super clear and will get you your crystals.

edit: would still need to manske after to get rid of undesired rue alks.

 

[ginjim]

It's really hard to follow what you're doing. You are adding vinegar and salt and base and changing containers, don't mix it all! God knows what pH it is now, if it's salt saturated or not, etc... Please don't just do steps for the sake of it without having an understanding of what exactly is happening.

Unless you just let it be and recover some precipitate and attempt to purify it further, I'd just forget about this extraction and start new, going step by step as the tek says, maybe check the other harmala extraction in the wiki.

hi i have one that I added lye to last night. i do see little bits floating about and some is settling.

I assume these are the alks. and waiting for these to settle even more

i do believe i have something here but just wanted it to be in a safe state so i can go from here. wasn't too sure where to started again.

i did resimmer and reduce one solution with vinegar and water because i added too much lye.

not too sure if i should base this or manske?

 

[ginjim]

ok latest update is i decanted the solution i had what was a sludge grey material and added warm vinegar water solution.

i assume these dissolved the alks.

what i have now is a light golden solution with vinegar and water and bits on the bottom.

now which is the good bit. the solution or bits at the bottom.

thank you

 

[endlessness]

Again, who knows... if you can measure pH, and its acidic, alks should be in solution. Filter to remove non-actives and base and filter again once alks have precipitated. If that doesnt work, it's because of the whole mess, so start again. Good luck

 

[ginjim]

thank you.

ph says its 8.5 now in a golden colour with bits at the bottom

but it looks like this:surprised

so i assume the good stuff is a small residue on the bottom because it's not acid?

but i put it in a vinegar water solution

 

[endlessness]

If its pH 8.5, what you see on the bottom is mostly harmine and some impurities there

Filter to retrieve it. Save it.

Then add more base to the liquid which you just filtered, to precipitate the rest of the harmine with all your harmaline

Then you can redissolev both in vinegar (separately) and reprecipitate with base or with salt again. This way you can try harmine and harmaline separately. Or you can put both together and just reprecipitate again with a base to clean up.

 

[ginjim]

had a look at the coffee filters and there seems to be crystals on there, glistens anyway could be salts

anyway i am going to try to retrieve anything from there.

so correct me if i am wrong please.

pan of vinegar and water solution to dissolve filters.

filter/ manske/filter/ dissolve in water?

or do i need to base again??:twisted:

please help and thanks

 

[endlessness]

Yes dissolve what stays in the filter in warm vinegar and water. Then filter it thoroughly through a funnel with cotton plug. Then re-base it to precipitate harmalas again. Forget the salt step for the moment.

Then you add more base to the liquid with ph 8.5, and raise it till at 11 or so, and some more alkaloids will fall out. Filter, redissolve whats in the filter with more vinegar, and re-base to precipitate again. Youre gonna be looking for pH 11 when precipitating the base.

 

[ginjim]

right last chance.

i have a solution which i have just based, there does seem to be little bits floating around and slowly sinking.

I assume these are my alks sinking.

sorry with all this converting ive done i've lost my idea of the good bits and the bad ones.

once these have sank by tomorrow i will decant this liquid and save the bits at the bottom

add hot vinegar to the bits with some water. and filter.

add salt to the solution. and rest.

this should see my 1st crystals??

 

[endlessness]

Hopefully...

 

[ginjim]

hi i binned the last one, the problem was that i added lye straight to the solution rather than in a mix.

i couldnt get any preticipation.

anyway i am on my 2nd batch and all is going well apart from one thing.

i have a solution with all my washes,bases that i have been collecting etc.

there was a little bit of alks at the bottom but lots were just floating and not doing anything.

i based this again with lye again to get it to sink but all the alks have floated and the solution is clear.

i thought they would sink.

is this good stuff?

thx