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I f*cked it up...Harmaline Assistance Required! Options
 
spartacus
#1 Posted : 4/14/2012 2:45:28 AM
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Okay SO! hear me out, I'll describe to the best of my knowledge without the use of pictures... So I had done a basic harmaline extract from syrian rue. Took my boiled drained liquids, combined them boom. Nothing too special. Then I had added a non-iodized salt mixture to this. Okay so then I add a base (lye). All my alkaloids fall to the bottom as expected. Well I had wanted to purify this step even more before puling out the alkaloids at the bottom. So I make a hydrochloric (muriatic acid) solution, and add accordingly. Mixed it all in, and was left with a green tinted liquid that is in fact UV reactive. At the bottom of this mixture, Remained the alkaloids. So I had pulled out that greenish liquid and added yet another lye solution to the mixture. Now guess what? My salts are floating on top... And the greenish UV reactive pull still remains. What do I do? Contemplating mixing the two in attempt to recombine, or should I add more base to the floating alkaloids and hope for the best? Any response, would be appreciated. Thank you.
 

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Noman
#2 Posted : 4/14/2012 3:31:03 AM

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No need for pictures.
How about trying posting what you did and your results in a manner that I don't have to decypher instead of in a big long goofy paragraph?
 
endlessness
#3 Posted : 4/14/2012 11:45:14 AM

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spartacus wrote:
So I had done a basic harmaline extract from syrian rue.


Harmaline and harmine, you mean?

spartacus wrote:

Then I had added a non-iodized salt mixture to this. Okay so then I add a base (lye).


How much salt to how much liquid? Did you filter the rue tea before adding the salt, to make it a bit cleaner before precipitation? If not, you should have.

Did the alkaloids precipitate after you added the salt, and did you filter and discard the liquid and kept the solids, which was then redissolved in water? If not, you didnt add enough salt and didnt understand the extraction properly, read better our wiki teks. If they did precipitate and you filtered and redissolved, you should have mentioned in your description, please try to be more clear.


spartacus wrote:

Well I had wanted to purify this step even more before puling out the alkaloids at the bottom. So I make a hydrochloric (muriatic acid) solution, and add accordingly.


Did you filter the alkaloids and discard the solution? If not, again, you are not understanding the process well because you should have, otherwise you are not purifying them, you are just mixing more things in to a mix that already contains too many things.

spartacus wrote:

Remained the alkaloids. So I had pulled out that greenish liquid and added yet another lye solution to the mixture


why? Are you following any teks, or are you making this stuff up as you go? Before you improvise, you should understand what you are doing.

spartacus wrote:

My salts are floating on top...


What salts? You added a base, your alkaloids wouldnt be in salt form, they would be base which would precipitate. Whether they are on top or on the bottom doesnt matter, filter to retrieve them. If they are all on the bottom its easier because at least you can decant part of the liquid and avoid some lenghty filtering, but if some are floating, its no problem if you just have patience and use a few filters.


spartacus wrote:

or should I add more base to the floating alkaloids and hope for the best?


what would be "the best" ? What are you expecting to happen? Its hard to follow your description, it seems like you have very little understanding of what you are doing or are just having difficulties explaining.

I suggest you check out our wiki and the harmala extraction teks, like the Extraction and Separation Guide, and follow it exactly as written, until you understand whats going on.
 
spartacus
#4 Posted : 4/14/2012 3:04:47 PM
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Well I had followed this to a T https://wiki.dmt-nexus.m...Y_Harmaloid_Freebase_TEK

My salts didnt separate like his did in step 5 to step 6.

So I added Lye. Then instead of using vinegar which I have short supply of, I made a HCL solution to attempt to further purify my results.

After doing that, my liquid turned green and UV active which the "salts?" had fallen to the bottom (I'm misusing the whole salts/base terminology. ) http://en.wikipedia.org/...le:Harmaline_Harmine.jpg

I seperated this liquid and took the remains in which I had added water and a base, in attempt to precipitate the base alkaloids.

My next question is, To the jar that is now UV reactive, it obviously contains harmaline/harmine. Adding a base, should allow the crystals to precipitate? Correct?

Hoping for the best, would be me taking a shot at what I believe would be correct in order to obtain harmaline/harmine. Thankyou.

Yes Harmaline and harmine * Thank you for pointing that out.



 
endlessness
#5 Posted : 4/14/2012 6:23:18 PM

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hmmm, that tek should be reviewed, its unnecessarily complex. Next time, instead of doing all this complication of adding saturated salt solution, just add exactly 100g salt per 1l rue boiling solution, then let it cool down overnight, you'll have some nice Harmala HCl crystals that you can filter, and then redissolve in hot water and then precipitate with lye to get the freebase.

Please dont misuse the whole salt/base terminology, it makes it all more confusing. Only use the terms correctly as they mean.

When you used HCl solution, you sad there were some things that fell in the bottom, did you throw that away? In theory if you added enough HCl, all the alkaloids would be in solution, and whatever is undissolved could be discarded as its not harmalas, but since you do not mention any numbers of how much hcl, how much lye, its impossible to know. Maybe you added just a bit of hcl and the pH was still slighty basic or neutral so some of those solids on the bottom are alkaloids, while others were already dissolved.

So its VERY hard to follow what you are saying...

Do you have a way to measure pH, like papers or pH pen?

The basic facts you need to understand to extract are:

1- If the pH is acidic, 6 or under, your alkaloids will be dissolved in solution and you can filter to remove any inactive solids.

2- If the pH is basic (by adding suficient lye to over pH 9), your alkaloids should precipitate as freebase, so you decant/filter and keep the solids. If you want to clean them up, you must redissolve them with acidic solution and reprecipitate with lye or with salt as in step 3 below.

3- When you have your acidic solution with the harmalas dissolved inside, and you add 100g salt per 1l boiling solution, the alkaloids will precipitate in a couple of hours as the solution cools. They will precipitate as Harmala HCl salt crystals, and they can be filtered, keep the solids and discard the liquid. They can be easily redissolved in hot water and precipitated again as step 2 above, for purer harmalas.


If you understand these things, you should be able to figure out what you are doing. If you cant, I wont be able to either because your explanations are very complicated. If I were you I would maybe do a new extraction following this instead:

https://wiki.dmt-nexus.m...ion_and_Separation_Guide

Good luck
 
spartacus
#6 Posted : 4/14/2012 8:55:19 PM
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"just add exactly 100g salt per 1l rue boiling solution" - Well I had originally had a very nice syrian rue solution, (500ml drained from exactly 100g seeds) that I had added 23grams of sea salt to then made a solution of another 500ml of boiling salt water that wouldn't hold any more salt. Let them sit in my fridge over night. Nothing. What went wrong?

So I had taken matters into my own hands by adding lye. The solution that was UV reactive last night, Well I had added about two tablespoons of muriatic acid (way too much) per 750ml of straight water. That in which had made it UV. Alot of left overs that didn't get mixed at the bottom remained. So I had drained the UV solution, and just today added Lye to it. It's current PH reads 11.5 and sitting on the bottom low and behold is a clump of my guess Harmala's. The solution is no longer UV reactive but still has a tea-ish tint towards it.

But anyways. I was just not familiar with the whole "salt precipitation method" and was trying to conquer this in a different manner. Live and Learn, I do appreciate the input endlessness.
 
endlessness
#7 Posted : 4/14/2012 9:06:11 PM

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Now you made much more sense, thanks for clarifying and giving details!

Im not sure how much is the total salt you added but it does sound like plenty. Next time better do the 100g per 1l ratio instead of doing this thing of adding salt-saturated water, it should really work, ive done it many many times, hard to think it can fail.

If I were you, I would redissolve those harmalas that are on the bottom of your container in vinegar or HCl, and then heat it up to boil and add the salt, because at this point you are gonna have a mixture of harmine+harmaline+vasicine/vasicinone/deoxyvasicine and other possibly unwanted rue alks. If you do the salt step youll have just harmine and harmaline (and small amounts of THH if thats there). Then you can redissolve and reprecipitate the base.

Good luck!
 
spartacus
#8 Posted : 4/14/2012 10:16:40 PM
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The english language has just so many loop holes in it, it is hard for me to describe exactly what needs to be said in order for you to interpret. Ahhh.. Well anyways, Yes, my next question is, when you add the salt, does that layer stay on top and not mix with the based harmalas?

I had wished I had known that originally about adding the 100g per 1l of syrian rue solution. God, it would've saved me a lot of time. My mixture just stayed like it was, with no separation of harmalas' alkaloids overnight in the fridge, that's why I had wanted to add the base knowing it would fall. The tek I had followed had made it seem the use of a base would be unneccessary.

But yes, I will definitely have to redissolve the harmalas... Once again, Live and learn. Thanks bud!
 
endlessness
#9 Posted : 4/14/2012 10:29:26 PM

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When you mix the salt, the harmalas shouldnt be based, they should be dissolved in an acidic solution. Then you add the salt and the salt mixes with the whole thing.. Then as it cools down, harmala starts precipitating, they will be floating around and will eventually sink down to the bottom (though ive had times they just kept floating around). Its quite visible when there's precipitation. Leave it overnight just in case, in the fridge even better.
 
 
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