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Harmine Crystals from Syrian Rue

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I'm curious.

What causes the yellow pigment in the water when performing a rue extraction?

I always figured it was traces of harmalas, but if this is so I've been pouring much of it down the sink.

What signs will show of removed impurities after cleaning beyond the brownish/white phase?
 
Hello. SWIM added HCL (a tiny little bit) on the first step of extraction - the boiling seeds part. Does that mean the alks are not going to dissolve as well if swim used vinegar?
 
Barmaley said:
Hello. SWIM added HCL (a tiny little bit) on the first step of extraction - the boiling seeds part. Does that mean the alks are not going to dissolve as well if swim used vinegar?

This is true, but a some people do use Hcl. Maybe just do a little longer soaks. That way once they're in their they won't jump out.

Just spend a little more time. If you're not happy you could always squeeze out the seeds after your first boil and then the next few times around use vinegar.
 
I decided to clean up the harmalas I have a little more. First of all I stirred them into a jar of water and then slowly started to add vinegar.

I noticed as soon as a slight colour change happened that the solution turned clear and a small layer of darker material settled on the bottom of the jar.

So rather than adding more vinegar I let the solution settle properly over night and carefully decanted the liquid of and set solids aside to dry.

Then I took the decanted liquid and slowly added sodium carbonate. This time rather than turning yellow, first of all it turned to a milky near-white colour.

It has now yellowed slightly as much of the harmalas have crashed out.


So what happened here?
 
soulfood said:
I decided to clean up the harmalas I have a little more. First of all I stirred them into a jar of water and then slowly started to add vinegar.

I noticed as soon as a slight colour change happened that the solution turned clear and a small layer of darker material settled on the bottom of the jar.

So rather than adding more vinegar I let the solution settle properly over night and carefully decanted the liquid of and set solids aside to dry.

Then I took the decanted liquid and slowly added sodium carbonate. This time rather than turning yellow, first of all it turned to a milky near-white colour.

It has now yellowed slightly as much of the harmalas have crashed out.


So what happened here?


I think it might have been a bad move for you to stop adding vinegar, because if it wasnt acidic enough, then some of the harmalas would have been remained undissolved, so they would stay together with the undissolved impurities at the bottom. I would keep adding excess vinegar, too much wont hurt, and will guarantee all the harmalas are in water-soluble acetate form.

the water changing colour is perfectly normal, look at the pictures I posted some time ago, how the colours changing are related to the different forms of the harmalas (acetate, hcl, freebase, etc) in the solution or precipitating...
 
Yeah I'm just playing about really.

I was just interested that in reality I didn't clean anything more than I already have as I didn't do the salting step or even filter after re-dissolving. Then on top of that, the substance which settled in the jar was much darker than the harmalas I put in. There wasn't very much that settled on the jar, just barely a thin covering of what looks like tiny grains of dirt. Then in the jar where I simply rebased the decanted liquid without filtering or salting I have a much brighter shade than I had before and it's not even dry yet.
 
yes its quite interesting, repeating the steps yield purer product... even if each time its just a few tiny grains of dirt or so on that are removed by decanting, this already helps...

one thing that was brought up, though, I dont remember if by amor fati or infundibulum, is that in each freebasing step, some harmine (or was it harmaline?) is 'lost', because it is a bit soluble in water, in the freebase form, and does not precipitate.. I think it was 20% or something, quite significant.. So I think the ideal to clean up and not lose so much would be to repeat many times the vinegar and the salt step, and avoid repeating the freebase step until the last part...
 
endlessness said:
I think it might have been a bad move for you to stop adding vinegar, because if it wasnt acidic enough, then some of the harmalas would have been remained undissolved, so they would stay together with the undissolved impurities at the bottom. I would keep adding excess vinegar, too much wont hurt, and will guarantee all the harmalas are in water-soluble acetate form.

the water changing colour is perfectly normal, look at the pictures I posted some time ago, how the colours changing are related to the different forms of the harmalas (acetate, hcl, freebase, etc) in the solution or precipitating...


Are you sure that adding vinegar when repeating the salting is necessary? Acetic acid is a lot weaker than HCl and I don't see how it would break up HCl salts of harmalas.

Of course if you experienced otherwise, that's a different issue...
 
no no, you are right to question that.. my own experience is only redissolving the freebase in vinegar solution, so I cannot say if the acetic acid is strong enough to turn the harmala-hcl salts in the solution into acetates.. thats a good question, maybe someone who knows more about it can say.

A way to not loose the freebase harmalas that supposedly dont crash out when raising the pH, is to saturate that solution with salt, to crash out the harmalas, and then decant/filter and put this together with the other harmalas when repeating the whole thing.
 
Acetic acid, no matter how concentrated, is a weaker acid than hydrochloric acid so you cannot turn harmala HCl salts into acetates using acetic acid. If you wanted to do that you would first have to freebase the harmala HCl salts and then add acetic acid to the freebase harmalas.
 
So really, one COULD not add any salt to the rue water, filter well (by unknown alien technology method) until simply discolored water solution with alkaloids is left and then base it with Sodium Carbonate and filter again.

1 more question. Is there any difference between ingesting freebase harmalas or a harmala acetate/chloride/etc
 
Barmaley said:
filter well (by unknown alien technology method)


hahaha I love this part! So true, we need that alien technology urgently :D

but yes one could skip the salt step BUT the salt step is what removes unwanted alkaloids such as vasicine and vasicinone, so I wouldnt skip it..

as for the last question, I dont know if anybody ever tested the difference.. theoretically it all turns into hcl salts in the stomach but different forms of substances can be absorbed quicker or whatever and make some difference.. But as far as MAOI activity goes, I would guess they are pretty much all the same, wont make much difference
 
Instead of using salt for this tech, could SWIM just add HCL to his boiled seed solution? It seems to me that this would make harmine HCL that would percipitate out, and you wouldn't have to deal with up to half your crystal actually being salts, so measuring dosage would be better.
 
it doesnt work.. the reason harmine/harmaline hcl precipitate is because they are insoluble in a salt saturated solution, but in a normal acqueous solution they are soluble..

and anyways there will be 0 salt contamination if you redissolve the harmalas in fresh water and then add a base.. you will get freebase harmalas with no salt, as the salt remains dissolved in the water
 
2 lots of 50 grams Syrian Rue' ground and boiled in 1200 ml of H2O and vinegar'
Boiled briskly for one hour' strained then filtered through a double piece of cloth and the seed pulp squeezed'
The resulant solution is left to decant' then filter through a superstenght coffee filter' it filters very easily'
split into 2 x 400ml' in large jam jars'
70 grams of sea salt added to each jar'
Each jar then shook until all the salt dissolves' the red tea turns yellow as the Harmaline acetates turn to hcl's'
Place the jars in the freezer for 3 hours' then in the fridge' the Harmaline curdles the solution and slowly falls out'
Take 1600 ml of pure water and 280 grams of sea salt and mix it to dissolve completely'

Draw off the water above the pressipitated alks' add fresh saturated salt solution' and shake the jars again'
Stick in the freezer and then in the fridge to pressipitate'
Draw off the water from above the pressipitate and add salt solution'
Shake the jars again'
Stick the jars back in the fridge to pressipitate'
Draw off he water above the alks and add more salt solution'

Leave now for 2-3 days to allow the alks to fall to the bottom'
Draw off the salt water and add fresh pure water'
Mix this well and add dropwise ammonia solution to freebase the alks'
Place the jars back in the fridge'

When the freebase has pressipitated' draw off the water'

Add fresh pure water and mix'
Add dropwise ammonia solution to freebase the alks and stick back in the fridge to pressipitate'
Draw off the water'

Shake out the resultant yellow sludge onto a clean plate and place somewhere warm to dry out completely'

Takes 8-9 days to get it clean' just keep washing the alks in saturated salt solution' until the water that seperates becomes almost clean'
Use lots of salt to prevent the alks from becoming water soluble again' hence losing them in the water'

Take a large jam jar and 3/4 fill it with pure water' then add your salt and shake the hell out of the jar until the salt has dissolved' keep adding salt until no more shall dissolve in the solution' Decant off the salt solution leaving any un-dissolved salt in the bottom of the jar'
Now have a completely saturated salt solution'
Findings of no enough salt in solution' loses untold alks to the water'

100 gram of salt per litre is insufficient'
Closer to 70-80 grams of sea salt in 400ml of pure water is very close to complete saturation'

Just to share of how to get here' needed lots of water and many big jars and lots of days'
And much salt' plus a couple of splashes of ammonia solution'

Bliss'

Pic of curdle alks pressipitating in the fridge'

Nobuoni +


Much appreciated all your input and help folks'

Blessings ~
 

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