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Harmalas Extraction and Separation Guide Options
 
endlessness
#21 Posted : 3/18/2010 1:36:28 AM

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baking soda by itself is not enough to precipitate a considerable amount of harmaline, no... it might precipitate a tiny bit, but nearly all will be harmine. Sodium bicarbonate raises pH to smt around 8-9, while sodium carbonate will raise it to 11 or smt..

as mumbles said, amount depends on amount of acid use, so hard to make a general estimate... just add slowly and mix well, first it will just neutralize the acid, and this is one of the reasons why you shouldnt use too much acid for the first boils.. Anyways as it neutralizes, if you used vinegar, it will bubble.. Then after its neutralized, it will stop making bubbles and change colour keep adding slowly and mixing, until it stops changing colour and then bit more.. Wikipedia says sodium bicarbonate has a solubility in water of 10g/100ml at 20 degrees celcius, but this is for pure water, when one has a solution of acid and harmalas, the whole story changes a lot..

Also, even if there was sodium bicarbonate/carbonate excess, you could wash it with a basic solution and get rid of it.. But I would say just add slowly and you will be fine, any contamination will be negligible (and food-safe)
 

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plumsmooth
#22 Posted : 3/18/2010 1:52:49 PM

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Much Regards for all continuing education. I noticed one approach to be adding a certain volume of saturated Sodium Carbonate solution to harmala solution. After reading a couple of Cosmic's recipes I saw that he at one time had used up to half the volume in saturated washing soda. Then in the most recent work he seems to be using a little over 20% saturated Sodium Cabonate solution to precipitate the Harmalas. The point I am trying to make, or solve for myself (is probably one whereby an accurate PH meter capable of the upper ranges would help) is how much is actually needed to achieve the proper pka or whatever rendering all harmaloids free. Of course, thanks endless, I see the residual acid will effect this. Nevertheless, It seems that ideally one-- for a given recipe-- could hone in on the amount of saturated solution needed whereby, at least in the case of previous Manske tech, that the Salt would not compete for the H2O. I'm guessing there is a pretty sizeable window between proper achieved PH, and over saturated-- competing with Sodium Chloride. I will look around so see what meters are available that will deal with 11-12 PH properly for experimentation, however, I seem to be resistant for some stupid reason to the idea of using the color change as the primary determinative factor is ceasing basification with the carbonate. Thanks again...
 
endlessness
#23 Posted : 3/18/2010 7:14:49 PM

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plumsmooth wrote:
Much Regards for all continuing education. I noticed one approach to be adding a certain volume of saturated Sodium Carbonate solution to harmala solution. After reading a couple of Cosmic's recipes I saw that he at one time had used up to half the volume in saturated washing soda. Then in the most recent work he seems to be using a little over 20% saturated Sodium Cabonate solution to precipitate the Harmalas. The point I am trying to make, or solve for myself (is probably one whereby an accurate PH meter capable of the upper ranges would help) is how much is actually needed to achieve the proper pka or whatever rendering all harmaloids free. Of course, thanks endless, I see the residual acid will effect this. Nevertheless, It seems that ideally one-- for a given recipe-- could hone in on the amount of saturated solution needed whereby, at least in the case of previous Manske tech, that the Salt would not compete for the H2O. I'm guessing there is a pretty sizeable window between proper achieved PH, and over saturated-- competing with Sodium Chloride. I will look around so see what meters are available that will deal with 11-12 PH properly for experimentation, however, I seem to be resistant for some stupid reason to the idea of using the color change as the primary determinative factor is ceasing basification with the carbonate. Thanks again...


I understand your concern about being more exact.. It was also the case with me specially when I was making extractions for the first time.. But then one realizes there is quite an wide window of measurements and processes where it all works perfectly, given you add enough until colour stops changing Pleased ..

But anyways, just to reassure you, here's what I did to know that colour changing was a good indicator: I added sodium carbonate, mixed and let the colour stabilize.. Added more slowly, and did this until the whole brew was of a homogeneous colour and adding more would not change the colour.. Then I put the solution in the fridge for half an hour, and then filtered it.. The harmalas were on the coffee filter, the liquid was clear. So I added some more sodium carbonate to the filtered solution, and put it in the fridge, and guess what? No more precipitations Smile

You can do this yourself if you want, and then you'll see. And to answer to your idea, yeah you can raise the pH safely by adding a saturated sodium carbonate solution to the harmala solution. The drawback is of course if you already have too much liquid and it wont fit your container, but otherwise it should work perfectly.

Btw, I dont understand what you mean with 'competing with sodium chloride'.. There should be no, or not much, sodium chloride, because you will have precipitated the alkaloids with the manske, but then you filter the brew and throw away the salt-saturated solution.. So when you redissolved the precipitated salt harmalas in water, the amount of salt contamination will not interfere with your basification
 
plumsmooth
#24 Posted : 3/18/2010 8:10:00 PM

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Excuse any lack of clarity on my part, my wording/terminology may have been off too.
I was referring to information gained in reading through this fascinating thread by Trickster that you were part of, whereby 69ron discusses Salt's effect on Sodium Carbonate's dissolving ability:

https://www.dmt-nexus.me....aspx?g=posts&t=8713
 
endlessness
#25 Posted : 3/18/2010 8:21:20 PM

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when you do the manske, what you do is have the pot boiling with your harmala solution, and then keep adding salt and mixing.. when no more salt dissolves (even after a few minutes of mixing), then you just pour off the liquid from the undissolved salt, and into the fridge.. this should mean that your solution is saturated and when cools down the harmalas should precipitate, and the amount of salt present as impurities will definitely not affect the addition of sodium carbonate later on (specially because the ammount of sodium carbonate needed to raise the pH enough is very small compared to the great amounts of sodium that water can dissolve.

When I extract, say, 150g of rue seeds, the harmalas that will precipitate in the manske, I redissolve that in, say, a liter or so of warm water.. that should be plenty of water to dissolve easily all the harmalas, plus salt, plus the upcoming sodium carbonate without any trouble
 
plumsmooth
#26 Posted : 3/18/2010 9:17:40 PM

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Am I correct that that method is only using that much salt because of the "upcoming" basification with carbonate. I mean, I though the idea with the original Manske was to saturate at 100g per liter of water at room temperature. In other words, over 100g salt per liter would precipitate out after the boiling mix cools down. Of course, as my mind processes, the whole point you were probably trying to make is simply that there is room even to over saturate with salt, basify without any extra sodium carbonate precipitating into the final product. It seems though, there would have to be some left in the drying harmalas even after filtration with suction. And now, after reading that food grade Sodium Carbonate discussion I feel as though I should spent the extra dollar or two to use that. P.S. I am confused after seeing the tan and white pictures of harmaline and harmine. My Manske came out yellow needles. I think I just figured this out: Are Hydrochlorides Yellow vs the other colors of Freebase or acetates?
 
endlessness
#27 Posted : 3/18/2010 10:35:45 PM

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the 100g per liter is not the exact number, the whole equilibrium and solubility of any substance like salt changes with the harmalas and other water soluble components of rue..

The amount of sodium carbonate in your final product will be really really minimum, so small that you can disregard it when calculating doses for example.. yeah of course using food grade sodium carbonate is the best, you can make that on your own by baking sodium bicarbonate in the oven

and yeah the harmalas hcl salts are yellow, and freebases have different colours (in the guide you can see that in the pics).
 
endlessness
#28 Posted : 3/23/2010 4:44:36 PM

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some member pointed out how it was written to grind '200 seeds' , instead of 200g seeds.. I hope nobody lost their time counting 200 rue seeds hahaha!

so I just edited the first post with this small change on the file
 
plumsmooth
#29 Posted : 3/23/2010 5:26:57 PM

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In regards to grinding, I get the feeling at this point the general consensus is that it creates more trouble than worth. Especially if indeed the harmalas lie primarily in the outer regions of the seed. I know with my first Manske even not grinding left me slightly challenged for patience, even with a buchner funnel set up. By the way, maybe slightly off topic, but is there any clever way i don't know about to recover fallen precipitates in a given flask/jar. I found one of the more tedious parts to be reverse turkey basting the red liquid from the top of a small area of dirty harmalas at the bottom of jar. I heard someone mention french press with a filter as one way to separate heavier precipitates. I like the idea of being able to just pour off the top instead of slow dropper decanting. Thanks...
 
endlessness
#30 Posted : 3/23/2010 6:49:03 PM

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well I havent seen any trustable published reference of alkaloids being primarily on the outside of the seeds, and neither remember seeing anybody doing side-by-side extractions to actually checking, just some affirmations like "yeah I had good yield without grinding".. Of course I would love it if someone showed otherwise, so if you know of anything please do tell.

Just have a tall thin container and can pour off most of it before needing to filter Smile
 
DMTripper
#31 Posted : 3/26/2010 10:41:38 PM

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Can one use this tek with shredded caapi?
Or is there another tek for caapi?
––––––

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endlessness
#32 Posted : 3/26/2010 11:44:01 PM

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yeah I did this tek with caapi, results were good but I had a small yield.. Im pretty sure it was the caapi, though, which was some left-over thin caapi vines I had for ages from a friend, I tried taking the caapi orally and also had small effects

when I extracted from caapi, I did not do the manske, I went straight for basing the solution, because I had read somewhere THH doesnt precipitate as a salt in manske, but im not sure how truthfull is this affirmation.. Just to make sure, though, I avoided it.
 
plumsmooth
#33 Posted : 4/16/2010 2:18:08 PM

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After final freebasing of either Caapi or Rue Harmaloids, I would like to make a standard 50-60% gycerine/H2O tincture. I'm wondering how soluble the base form is. I noticed it is not very soluble in plain water. I'm guessing that alks are best converted to salt during tincture making process. Maybe the simplest way is to dissolve the Harmalas in the minimum amount of vinegar/water necessary to transform them, then add glycerin and apply hot water bath to evaporate the vinegar.

I'm also curious if one were to want to transform the Freebase alks back to salt form for dry storage to be used for pharma, what might be the most appropriate approach for this. I could see once again maybe dissolve in vinegar and then dehydrate. I'm not sure if the vinegar was evaporated completely with some heat, whether one would be left with 100% salt form still. This is because of q21's vinegar acetates to freebase tek stuck in my head. I guess different acetate molecules would behave differently under evaporation with heat.

Thanks for your consideration, and thanks for the valuable information provided with the technique.
 
q21q21
#34 Posted : 4/19/2010 5:38:47 AM

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LOL, just went here to thank endlessness for the pictorial, though the tek is not all that new, the pictorial drove SWIM to purchase a PH tester and do this.

Didn't expect to have an answer to the last posted question, which is yes it can be converted, YES it can be smoked (unexpectedly got visions from it) the only issue is that there would likely be a small sodium acetate contaminant that would make measurement not too precise, SWIM's still working out approximate concentrations for color in the acetate tinctures

He has a DARK red one that he measured to be ~80mg per dropper this is after 1 manske and 1 freebasing.
The next one (same 1 and 1) is much lighter, he went to measure it by evaporating and scraping and when it looked weird he though to himself about the fizzing when he put his coffee filter in the vinegar and exclaimed "shit, sodium acetate"

Other than that he's been making harmala acetate tinctures for a while, his trick for filtering such tiny amounts is to stuff part of a cotton ball into a dropper, he uses his 5ml one, then you can take off the top and fill with another dropper, and depending on your choice you can either put the top back on and squeeze, or what SWIM usually does, blow on the open end Very happy
Q21Q21's Tek: A comprehensive guide to extracting DMT
The 2 teks use non-toxic lime and vinegar and Tek 1: d-Limonene or Xylene or Tek 2: Naptha to produce very quick high yields with the greatest of ease.

I am almost never on this site anymore so I will likely not answer PMs

 
plumsmooth
#35 Posted : 4/19/2010 12:56:22 PM

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I believe what your saying Q is that Sodium Carbonate leaves a trace when going from Freebase to tincture-acetate.
Interesting, I wonder how much contaminate is left when finishing with Manske?

Although remaining expressed doubts around here has me still questioning whether Manske fully works (THH) with Caapi.
I have to admit this doubt is slightly accentuated by the simple fact/result of my last attempt to re-X freebased Caapi harmaloids using Manske tek.
Basically, at 100g Salt/1000ml liter ratio, Nothing, I repeat nothing precipitated at all out of about under a gram Caapi Harmala re-dissolved in 100-200ml salt solution.

I was really surprised and after a day in fridge just re-based them.
Then like magic they appeared.
Talk about Sodium contanimation, imagine Sodum chloride and Sodium carbonate together...

I originally though excess Vinegar may have had something to do with the lack of any precipitation, so even tried first evaporating vinegar in glass teapot and put solution back in fridge: still no Harmala precipitated.

I have never ever had this occur with Rue Harmalas!

Anyway, this led to another idea for a THH manske precipitation experiment:

Extract Caapi Harmaloids by basing twice:
Then try manske re-precipitate: (maybe adjust salt concentration upwards from 100/1000...
Then, finally re-base the Salt solution after collecting Mansked Harmalas.
IF nothing precipitates then: Does this almost Prove that THH is fully precipitated by Manske tek?
Thanks for your consideration knowledgeable ones...







 
endlessness
#36 Posted : 4/19/2010 1:32:01 PM

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yeah Im sorry about the 100g per 1000ml water number, I have adjusted that in the WIKI, and added a new picture to show what I do when saturating with salt... It might be more like 200g salt per liter water or so, so maybe what happened was you didnt add enough salt! Excess vinegar wouldnt be a problem

Im pretty sure dagger (or was it someone else?) tested and THH does precipitate in a manske, but I havent tested myself. The only time I extracted caapi I went straight for the base precipitation
 
plumsmooth
#37 Posted : 4/19/2010 1:46:22 PM

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Well I've always used the 100/1000 ratio with manske with rue.
AND it never seemed to fail precipitation, even when re-precipitating.
I'm going to try 200/1000 next time when attempting a re-precipitate with Caapi Hamalas.

I like the idea of finishing a caapi re-x with Manske becasue the salts would be easier to dissolve for tincture making process.
Taking away the need to add vinegar, and or dehydrate/evaporate the vinegar
They are also nicer to work with then the base verison, easier to handle and filter...

P.S. I'll have to take my last 100/1000 precipitated harmalas and filter, add another 100 and see if anything else comes out.
 
endlessness
#38 Posted : 4/19/2010 1:51:19 PM

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do that and report back

I dont like the manske precipitated stuff because even if one adds just enough salt, there will always be some salt contamination, I find the dosage to be innacurate. Though I would def appreciate some harmala salt to make tincture or cap it, because the taste of the freebase dissolved in orange juice is becoming quite repulsive to me Very happy
 
plumsmooth
#39 Posted : 4/19/2010 2:04:32 PM

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P.S. I still curious of any other techniques for reclaiming the salt from freebase Harmalas.
BTW, although this belongs in the "does acidified alcohol protect from harmala red" thread as well,
I did an experiment-- although it wasn't pure ascorbic acid (had bioflavanoids)-- I added a gram of Vitamin C to an ounce of alcohol and then dissolved my Rue Harmala Salt, filtered, evaporated, and seemingly no Harmala Red formed-- as per 69ron's suggestion in a thread I can not remember the title of currently. I would like to try this again, considering how nice it is to watch impurities instantly fall to the bottom and filter out, I would love to resolve the 95% Ethanol clean up of Harmaloid Salts... Of course no one necessarily want 1:1 Harmala/Vitamin C in their final product either. Maybe a dash of vinegar would do the same, or some other acid that either evaporates or will not be to strong remaining in final product...

I wish I understood more about how different acids interact, for example if one used Phosphoric to acidify the alcohol, upon evaporating, would one still have hydrochlorides or would one now have phosphates?

P.S. Just remembered, I think combining ethanol and acetic acid produces ethyl acetate or something a perfume-y smelling compound...

From Wiki...:

Ethyl acetate is the ester of ethanol and acetic acid; it is manufactured on a large scale for use as a solvent.
This colorless liquid has a characteristic sweet smell (similar to pear drops) like certain glues or nail polish removers, in which it is used.

Ethyl acetate is primarily used as a solvent and diluent, being favored because of its low cost, low toxicity, and agreeable odor. For example, it is commonly used to clean circuit boards and in some nail varnish removers (acetone and acetonitrile are also used). Coffee beans and tea leaves are decaffeinated with this solvent.[3] It is also used in paints as an activator or hardener.[citation needed] Ethyl acetate is present in confectionery, perfumes, and fruits. In perfumes, it evaporates quickly, leaving only the scent of the perfume on the skin.

Hey that would transform your freebase/orange juice taste...Wink
 
plumsmooth
#40 Posted : 4/19/2010 5:52:18 PM

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Update, Swim is working on extracting Caapi Harmalas to make a 3 gram harmala tincture.
Swim would prefer to have the Salts instead of the Freebase. Swim would probably rather have a little salt then Sodium Carbonate residue in product.
Not sure how either will dissolve, or not, in Glycerin.

About a gram of Caapi harmalas from 200G of some older shredded white vine was extracted by basifying.

This time, becasue of no precipitation last time, SWIM added 30 grams to 150ml solution, after Freebase Harmalas were dissovled in vinegar/water 50/50.

This time harmalas or salt or both immediately precipitated and solution stayed very yellow cloudy with precipitates already on bottom of jar.

Conclusion: Mankse came up with 100/1000 saltwater ratio for a reason.
At this ratio salt and harmala can freely dissolve at boiling temperature.

Update, being an impatient fellow, I re-dissolved the solution by adding another 150ml water brought to a boil; now everything clear.
Going back to fridge....

 
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