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

 

[arcologist]

Rue extractions can be tricky the first few times. It took me maybe 4 attempts before it went smoothly.

What color is the solution? (should be transparent redish brown) Did you notice a color change (from brownish to light cloudy yellow) when adding the base? Did you filter the solution adequately before basing?

You could try putting it in the fridge to lower the solubility to see if anything comes out. If you have a UV light you could shine it to see if there are any alkaloids left in the solution - it should glow bright green if they are there.

As an aside, I would probably be using sodium carbonate instead of lye if I were you. It's way safer, cheaper, and does the job just as well.

 

[ginjim]

Rue extractions can be tricky the first few times. It took me maybe 4 attempts before it went smoothly.

What color is the solution? (should be transparent redish brown) Did you notice a color change (from brownish to light cloudy yellow) when adding the base? Did you filter the solution adequately before basing?

You could try putting it in the fridge to lower the solubility to see if anything comes out. If you have a UV light you could shine it to see if there are any alkaloids left in the solution - it should glow bright green if they are there.

As an aside, I would probably be using sodium carbonate instead of lye if I were you. It's way safer, cheaper, and does the job just as well.

hi thank you for your reply

my solution is a milky brown colour
it did go a milky colour when i added the lye. this was then rested.and seperated.
i did keep murky bottom half! was that right?
I assume i had filtered adequately by the time i had finished it was going through the coffee filters no problem.

thanks will get a UV light

i did discard the

 

[Metanoia]

I found the first separation to be the trickiest. After the first base I mean. You have to get as much of the basic solution as you can out of the alkaloids. I run it through a coffee filter, which takes FOREVER. If you leave any basic solution the alkaloids won't dissolve into the vinegar properly and you'll lose some.

I use hot vinegar (no water) to dissolve my alkaloids the first time. Makes it much easier. Also make sure you filter again after your alkaloids are dissolved. Then add the salt while still very hot and allow to cool slowly.

 

[ginjim]

ok so far I have a container filled with harmalas alkaloids which is milky brown liquid
after the lye was added i let it rest. I discarded the top clear layer which was seperated and I was still left with a cloudy solution.

I added the vinegar and water solution.
I then added 40 gms rock salt.

this is still seperating with clear brown fluid (about 100 mil)

do i discard this (will any crystals be in there)

I really dont know where the crystals should be sorry

and then add vinegar and salt again??

thank you

 

[Metanoia]

When you add the lye, the alkaloids should precipitate out almost immediately. It takes several hours for them to all settle to the bottom.

You said you were left with a cloudy solution. This is the problem. You need to pour basic solution, alkaloids and all through a coffee filter to get ALL the basic solution out. Then toss the coffee filter with all your alkaloids on it in some hot vinegar (straight, no water)

They should dissolve fairly easily. If it's still moving, add more vinegar

Then once they're dissolved you filter through a coffee filter again and then add the salt. Make sure it's piping hot when you add the salt, and make sure it all fully dissolves. You need to do this in a small pot on a burner, not in a jar. Once you're at this point, then you pour it back into your jar and let it cool slowly over hours. Leave it for 24 hours or so and the crystals should form.

Then you just keep repeating the process until your alkaloids look clean enough. It's the first base that's tricky After the first manske it gets easier and easier to filter.

 

[Metanoia]

If you're unsure, don't pour anything out. Just take it and base it again with lye and see if anything precipitates, then collect that and manske it (dissolve in vinegar and add 10g salt per 100ml)

Also, for future reference, always save your filters from before you base your rue tea. If you do a vinegar wash on them you'll get lots more alkaloids.

 

[ginjim]

ok thank you. I am still at a loss.

my milk solution has gone through everything in the tao of rue.
I have a cloudy solution of rue, ly, vinegar and salts.after following the procedure but yet to see crystals.
this was filtered last night with no crystals in sight. Am I still being impatient or do I go through a process again which part do you suggest?

I really appreciate your help

 

[Metanoia]

Anything you have left, any solution, filter it and then base it. Then collect anything that precipitates out. Those will be the alkaloids. Then once you have filtered the basic solution and gotten the alkaloids out you dissolve them in hot vinegar. Filter again. Then add the salt.

Patience is definitely an important part of rue extractions

 

[ginjim]

OK i think I get you. I did remove some of the clear liquid that was on the top after the lye solution!!
would many alkaloids be in there? I assumed I was looking for a mixture still.

Sorry science wasn't a strong subject. so to get this straight

I have added more lye to my solution and let it rest over night. this hopefully collects alkaloids.

tomorrow i filter this solution and anything left in the filter I put in hot vinegar.

then I add the salt??

I can see where I went wrong then

I added lye, left to rest. basted off the top.
added hot water and vinegar
added salt. rest
filter and no crystals

 

[Metanoia]

The clear liquid you removed is just basic solution and shouldn't have any alkaloids in it. Once you raise the pH the alkaloids drop out to the bottom

You've pretty much got it. Just after you dissolve your alkaloids in hot vinegar, filter the solution again to remove anything that won't dissolve (should be nasty stuff you don't want). Then you add the salt. When you add the salt make sure you have it in a pot on the stove. As hot as you can get it without it bubbling. Then you let it cool slowly and leave it for 24 hours.

That was the mistake I made as well, basting the liquid off the top rather than just pouring the solution, alkaloids and all through a coffee filter. Base tends to be very strong compared to just vinegar, so it's important to get all that basic liquid out.

 

[ginjim]

ok well i have two lots going.

the 1st one is an alkaloid vinegar salt solution that is a clear amber colour in the manske state.(no crystals formed)

i did cock this up a bit because i dissolved in vinegar then added salt and then filtered.

there are no crystals forming or formed.

2nd one is a just after the base and have filtered the alkaloids out.

the texture is a greasy sludge.

should this be the correct consistency? anyway i am dissolving in vineger and filtering now

having a bit of a nightmare i think.

thanks for the help

 

[Kobranek]

As dioxippus stated sodium carbonate works much better, depending how much lye you used the ph isn't getting low enough for the salt step (manske) since you are adding water with the vinegar. The low ph is crucial for the alkaloids to drop out. You may have to wash the freebase after the lye step with water possibly to remove excess base for the vinegar to adequately drop the ph. Good luck!

 

[ginjim]

Thanks for your help guys. I should have paid more attention in class. I never realised chemistry could be so much fun.:d

anyway so far I have one manske in the fridge still waiting for crystals which I made this morning

and with the other failed manske I added more lye to the mix again.

it is a cloudy off yellow colour the consistency has gone quite gelatinous!!:|

 

[form is emptiness]

Manske crystals begin forming at room temperature soon after the salt is added, provided concentrations and volumes are all good. My first results were also poor, less than 100mg from 100g seed. On 2nd round first did a Easy Caapi Vine Alkaloid Extraction on the rue, then mansked half of the freebased product. Results were great.

 

[ginjim]

Manske crystals begin forming at room temperature soon after the salt is added, provided concentrations and volumes are all good. My first results were also poor, less than 100mg from 100g seed. On 2nd round first did a Easy Caapi Vine Alkaloid Extraction on the rue, then mansked half of the freebased product. Results were great.

that is not alot. i have no idea what i'm going to end up with:lol:

i have been basing, acidifying, salting and washing in no particular order now

how much lye do people normally basr with. i have been using about 70gms for 200ml is that about right?

when i did add it it solidified and then turned to salts at the bottom and with a greasy clear yellow at the top.

i decanted the top layer and tried to clean it with water:?:
now I think i am back to square 1 with having to base it.

i've kept everything just incase i need to chuck everything in a big pot againlol:

 

[arcologist]

how much lye do people normally basr with. i have been using about 70gms for 200ml is that about right?

Whoa! That's a crazy, dangerous, amount. No wonder you've had trouble neutralizing it with vinegar. You need at most maybe 20g per liter to reach pH 12 and base out all of the alkaloids. You're using like 15 times what you need, NaOH is strong! Once again, I'd really recommend sticking with sodium carbonate for rue extractions. Pick it up at your local supermarket for like $3 for 3 pounds, sold as washing soda.

 

[ginjim]

how much lye do people normally basr with. i have been using about 70gms for 200ml is that about right?

Whoa! That's a crazy, dangerous, amount. No wonder you've had trouble neutralizing it with vinegar. You need at most maybe 20g per liter to reach pH 12 and base out all of the alkaloids. You're using like 15 times what you need, NaOH is strong! Once again, I'd really recommend sticking with sodium carbonate for rue extractions. Pick it up at your local supermarket for like $3 for 3 pounds, sold as washing soda.

it said add till i found a milky colour

ok I had some lye left over from mimosa using that and I made some sodium carbonate from bicarb today

they have washing soda here but it is 30% sodium carbonate is that good enough?

where do you suggest i go from here then? I don't think my manske is going to crystalize
chuck it all in a pot with loads of water and reduce? :?:

thanks

 

[ginjim]

ok from what i gathered i have used way too much lye in my mix.

can someone recommend a way on getting this back to safe levels if possible please

 

[arcologist]

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.