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Reduction with HCl. Why is the liquid so clear? Options
 
Jagube
#1 Posted : 8/7/2018 11:24:16 PM

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I got mesh 350+ zinc and it's orders of magnitude finer than the one I used previously. It's really dust.

I then proceeded to reduce my harmaline with the fine zinc, and the green UV glow diminished greatly, but I wasn't sure if the reduction was complete (it didn't have a vinegar smell, it was bitter and the zinc may have contributed to that). So I added some HCl. This brought the pH down to 1-ish.

After a few hours of magnetic stirring, I turned the stirrer off and after settling, the liquid was very clear. Much clearer and lighter colored than the original harmaline acetate solution. What happened? Is it because the alks converted from acetates to hydrochlorides and those are lighter-colored?

Also the zinc seems to have disappeared. Did the HCl eat it?

I've now added a bit more zinc and it turned metallic-colored again. I guess in a couple of hours it will be clear again.
 

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Jees
#2 Posted : 8/8/2018 2:57:35 PM

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I've never used HCL for that job, can't say Embarrased
 
Elrik
#3 Posted : 8/9/2018 8:13:53 PM

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I believe the reduction decolorizes alkaloid contaminants, thats why the color lightened up so much. I dont know, I just enjoy my white THH and faintly yellow harmine Pleased
So how did your second phase of the reduction go? Did it turn clearly blue under blacklight?
The neon green of harmaline is much more powerful than the blue of THH so even if the green doesnt fully vanish you may have gone nearly to completion.
 
Jagube
#4 Posted : 8/9/2018 10:31:21 PM

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It didn't turn blue. It just became less green, like the faint green you get when a glass of water is *contaminated* with a drop of harmine or harmaline.

All the zinc dissolved - see my post here.

I've precipitated the alks and they're drying now. What didn't precipitate will be re-acidified, reduced and mansked.
 
Elrik
#5 Posted : 8/9/2018 11:43:14 PM

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The zinc is supposed to dissolve, any that doesnt is saved for next time.
I just had an interesting idea relevant to partial reduction runs.
- The solid harmala freebases pretty much dont fluoresce under blacklight, I think that also applies to harmaline. Its the dissolved alkaloid salts that glow.
- Even a little harmaline will give a greenish color, blue means essentially pure harmine, THH, or harmine + THH.
- Ammonia is a good base for selectively basing out alkaloids one at a time because theres at least a little of an equilibrium in the reaction [lye would be too clumsy for this].

So, if you would like to be a stickler for purity, you could dissolve your alkaloid bases in just enough dilute vinegar, turn on a blacklight, and with lots of stirring slowly drip in ammonia until the glow turns from green to blue and stays there. The harmaline could then be filtered out, then A) an excess of ammonia could be added and the THH base filtered out or B) a teaspoon of vinegar and then an equal volume of saturated salt water could be added and the THH•HCl would be mansked out.
Theoretically it should work.
 
Jagube
#6 Posted : 8/10/2018 11:30:59 AM

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Thanks Elrik, but I believe the harmala alkaloids glow even in freebase form when dissolved in water. They're not very soluble, but the little that does dissolve, glows. Or could it be salts that didn't convert to freebase? (you never get 100% conversion, but you can get infinitely close to it) I guess an easy test would be to re-dissolve some fb in 1% ammonia and see if it glows.

All the wash water I've discarded after basing in my harmala extractions has fluoresced.
And I have only ever seen a green glow, never a blue one.

Also from what I understand, harmaline and THH precipitate at similar pH points, which makes them hard to separate.

My dried alks post-reduction alks weigh 1270mg, down from the original 1500mg, so I abandoned the idea of manske-ing the supernatant: it was thick (it must have had a lot of ions floating about as I had taken it to pH 1 with HCl, then to pH 10 with ammonia, and back to pH 4 with vinegar, and added NaCl on top of that; not to mention the zinc salts), had a strong apple-like odor while reducing, and after reducing to 100ml nothing mansked out. I've discarded it now.

I've tasted my presumed THH freebase and it still had a strong, bitter taste, which may be a sign it's harmaline. I always dry my alks in a heated propagator (the kind you use to germinate seeds and raise seedlings) and I wonder if the heat from it may have converted any THH I may have produced back to harmaline?

I might bioassay the freebase tonight.
 
Elrik
#7 Posted : 8/10/2018 7:45:41 PM

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Your right, I forgot about that little bit that never precipitates and glows like a college student at a rave. Its a shame that idea wont work though Laughing

If you ate up lots of zinc with acid then your reduction must have gone pretty far, even if not to completion. Take 150 mg of your product an hour before harmine+DMT and I doubt you'll be disappointed. To be safe use a moderate DMT dose the first time, if your not used to the combination. It kicked my ass the first time I mixed them Wink
THH alone, in moderate dose, seems to act as an antidepressant mood enhancer for me. Subtle, but I really like it.
 
Jagube
#8 Posted : 8/10/2018 9:45:46 PM

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Elrik wrote:
I believe the reduction decolorizes alkaloid contaminants, thats why the color lightened up so much.

Another explanation is that THH salts in solution are lighter colored than harmaline salts. I've seen off-white freebase harmine/harmaline mixes take on a Coca Cola appearance when dissolved in vinegar.

I took 50mg of the freebase sublingually, actually it wasn't that bitter, so maybe it is THH after all.
 
 
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