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What went wrong in my harmaline->THH zinc reduction? Options
 
Jagube
#1 Posted : 5/2/2019 10:43:01 AM

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It used to work for me and now I'm struggling with the reduction of initial ~14 grams of purported harmaline.

I've made three attempts so far, apparently all failed.

Attempt 1.
I didn't use enough vinegar, as a result only a small fraction reduced. I wasn't aware of it at first. During the basing, not knowing it was harmaline and not THH, I didn't bring the pH high enough - I stopped basing around pH 10.3. I'm assuming the supernatant still contained a significant amount of harmaline and I poured it down the drain, because after the cleanup and additionally a Manske, I was left with something like 7 grams (so a 50% loss).

Attempt 2.
I used much more vinegar, but probably still not enough, because the product still had a harmaline feel to it, although I also felt some THH.
The strange thing is it weighed closer to 10g. So how did the 7g increase to 10g? It must have been heavily contaminated.

Attempt 3.
This time I used plenty of vinegar and added some HCl.
After 9 hours the liquid was a pale yellow and didn't glow green in UV. However, the undissolved zinc looked very different: instead of the fine powder, which after the first two attempts looked almost like a liquid metal, this time it had turned into a very coarse powder and even containing porous clumps like pumice stone.

I didn't base it straight away, but let it sit overnight to let some of the residual HCl evaporate. In the morning it was dark colored again and glowed green in UV Sad So I'm assuming even if it had reduced to THH, it subsequently turned back to harmaline overnight?
 

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Jees
#2 Posted : 5/2/2019 1:54:54 PM

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Attempt 1.
Is it possible the loss was due the manske? What was the weight before/after the manske? I ask this because at pH 10.3 it would be weird to have still 50% in solution, be that DHH or THH.
I simply check pH now and then to see if there's enough vinegar left.

Attempt 2.
I can only think of zinc-salts that did not re-liquified by raising of the pH. Normally by upping pH enough the zinc salts get back into the solution. You could redissolve in vinegar and re-base with enough ammonia to be sure.

Attempt 3.
Those colors say something but might be deceiving too? You need crystal form confirmation with a microscope or another way of identifying to know if the reduction was okay or not.
And we have the taste test too, yuck for harmaline, no taste for clean THH.
 
Jagube
#3 Posted : 5/2/2019 2:54:47 PM

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Jees wrote:
Attempt 1.
Is it possible the loss was due the manske? What was the weight before/after the manske? I ask this because at pH 10.3 it would be weird to have still 50% in solution, be that DHH or THH.
I simply check pH now and then to see if there's enough vinegar left.

I don't think I weighed it before the manske, I had assumed it was still dirty before the manske, so I didn't take the time to dry it just to weigh it.

The pH after the reduction was still slightly acidic, but from what I understand we want it to be low enough for the molecules to find each other quickly so the reaction can complete within a reasonably short time.

Jees wrote:

Attempt 3.
Those colors say something but might be deceiving too? You need crystal form confirmation with a microscope or another way of identifying to know if the reduction was okay or not.
And we have the taste test too, yuck for harmaline, no taste for clean THH.

I also took 70mg of the result of Attempt 2 sublingually and it didn't taste that bad, but it definitely had a bitter taste. My reference point is the acetates though, which are yucky beyond measure; the freebase was nothing like it.

The result of Attempt 3 has been based and I'm waiting for it to settle, but I don't think it's THH. Most of the clouding occurred above pH 10.
 
blue.magic
#4 Posted : 5/3/2019 12:27:06 PM

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The problem might be the zinc because it oxidizes over time. You can try to "activate" your zinc by washing it briefly in dilute HCl. The acid will eat away the zinc oxide but leave most of the zinc metal. Use the activated zinc as soon as possible to avoid more oxidation of the wet powder. ... the vinegar solution will probably dissolve the zinc oxide anyway, but if there is excess oxide, it's better to remove it before reaction or use excess beforehand to compensate.

Another problem might be the water - any dissolved ions might skew the reaction (maybe), so use distilled or better deionised one if possible. Just to try and rule out this factor.

Make sure the concentration is not too high and add dilute enough base (ammonia). Note that excess acetic acid will form excess salt, raising total concentration of solids in your solution. Diluting everything enough lowers the unwanted co-precipitation and clumping. I tried once precip. THH from a concentrated solution and it formed hard sticky mess.

Quote:
it had turned into a very coarse powder and even containing porous clumps like pumice stone.


This always happens with my zinc. I poked it with a rod and it was loose - i thing the fine powder just clumped together but it did its work anyway.
 
Jagube
#5 Posted : 5/3/2019 2:55:11 PM

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blue.magic wrote:
The problem might be the zinc because it oxidizes over time.

Zinc oxide is supposed to be white, my zinc looks metallic.

I don't think the water is a problem either, I've always used tap water with success until this time.

I'm thinking that maybe my purported harmaline has a lot of harmine in it, because it has a harmala feel, although there must be some THH in the mix too. I bioassayed 200 mg of the result of Attempt 3 and 200 mg harmine with some ACRB tea last night and got very strong harmala effects with heavy tracers. I didn't get much of the harmaline lightheadedness, but it lasted very long and made the DMT effects seem disproportionately short-lived.

Yes, I've learned now that lower concentrations work better for basing; at lower concentrations the magnetic stir bar gets stuck in the sticky mess. But for the reaction perhaps a higher concentration will result in a quicker completion of the reaction?

Update: it looks like the result of Attempt 3 is THH in the end. I did another bioassay with 100g harmine, 300g of said product and ACRB tea. Very little of the DMT got activated and what did get activated could have been solely due to the 100g harmine, so I conclude that the product contained no significant amounts of either harmine or DHH. It did have THH effects, which may have been dulled due to tolerance as I was drinking back-to-back.
 
 
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