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Is that freebase? It looks pretty clean - good job
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Purification after manske
- Thread starter Loveall
- Start date
Is that freebase? It looks pretty clean - good job
Kalitechnik
Established member
Yes that is freebase.Is that freebase? It looks pretty clean - good job
If i understand correctly i did four cycles of acidify - filter - base.
and at the last base i washed it (settle - decant - fill with water) 4 times, than dried.
Awesome - it sounds like it became a meditation for you
What volumes of water did you use throughout the process, particularly the first brew? I've struggled with a rue basification before because of using too much rue and not enough water. Concentrated, first-brew rue tea forms unfilterable sludge on addition of base, so consider yourself lucky
Had I known this I would have waited and mixed it with the later brews to thin it down some more, but I guess that's what often comes of too much making it up as you go along.
Kalitechnik
Established member
Yes it was like a meditation, and oh boy how excited it was when i first aded base and see how the harmalas are crashing out, pure beauty.Awesome - it sounds like it became a meditation for you
What volumes of water did you use throughout the process, particularly the first brew? I've struggled with a rue basification before because of using too much rue and not enough water. Concentrated, first-brew rue tea forms unfilterable sludge on addition of base, so consider yourself lucky
Had I known this I would have waited and mixed it with the later brews to thin it down some more, but I guess that's what often comes of too much making it up as you go along.
As i remember i was boiling 100g od seeds in two cups of water, which during boiling possible reduced half. So i had 3 brews that summed up with around a liter of liquid. I put all seed in a tshirt and sqeezed all drop into it. And yes the first brew had a lot of gunk, so as i remeber i did 3 cycles of settle/decant and getting rid of the sludge.
Than i proceded with basyfing. Once i tried to filter the base but it was nearly imposible, so i realized that i will just pour of the liquid and acidify the frebase remains.
I realized that when acidified and warm the liquid is easier to filter so the second acid phase went through a coffe filter leaving not so much of a sludge.
So that was my thought that in the future i will settle/decant the base phase and filter acid phase.
And i just ordered buchner setup so the hopefully filtering part will be easier.
And next step in my journey will be to learn how to get THH from my harmalas
Yeah, the decant is really the only way to go with the first brew. On the Buchner it foamed so much the filtrate receiving flask overflowed, so be forewarned and use an extra flask as a trap before the pump. I was using a repurposed tyre pump so I didn't really careYes it was like a meditation, and oh boy how excited it was when i first aded base and see how the harmalas are crashing out, pure beauty.
As i remember i was boiling 100g od seeds in two cups of water, which during boiling possible reduced half. So i had 3 brews that summed up with around a liter of liquid. I put all seed in a tshirt and sqeezed all drop into it. And yes the first brew had a lot of gunk, so as i remeber i did 3 cycles of settle/decant and getting rid of the sludge.
Than i proceded with basyfing. Once i tried to filter the base but it was nearly imposible, so i realized that i will just pour of the liquid and acidify the frebase remains.
I realized that when acidified and warm the liquid is easier to filter so the second acid phase went through a coffe filter leaving not so much of a sludge.
So that was my thought that in the future i will settle/decant the base phase and filter acid phase.
And i just ordered buchner setup so the hopefully filtering part will be easier.
And next step in my journey will be to learn how to get THH from my harmalas
We'll be looking forward to hearing reports of your journey towards THH - do you have a specific method in mind?
Of course, you may want to try separating the harmine and harmaline before the reduction - although I could make the possibly arcane observation that if you were to use magnesium dissolving in phosphoric acid as the reductant on a harmine/harmaline mix, you can both precipitate harmine quite neatly and then cleanly separate the magnesium as highly insoluble magnesium ammonium phosphate with (meticulously) careful addition of ammonia.
One more thing we've never confirmed is whether ascorbic acid somehow - directly or indirectly - reduces harmaline to THH. It would be good to either confirm this or debunk it as another potential piece of 69ron misinformation.
Most sensible people just use zinc dust to reduce the harmaline, so if you prefer a documented and proven method you should stick to that one before getting all experimental (because at least you'd then have a reference standard for THH).
Kalitechnik
Established member
Right now i think i will like to follo the path that has been described by Van Der Sypt.
Although i am open for some noveltys if you have something good and proven.
Will definetely ask you for some other aproaches, soon i will start new extractions and i would like to have all three (harmine, harmaline and thh) nicely separated.
Thats what i would like to do. Follow some proven method and if anyone around Nexus can guide me i will be very grateful. See you soon in my new thread when i will get all the goods needed for new extraction.
I'd say VDS protocol counts as the gold standard here, so that's a good decision.
The descriptions of the zinc reduction process found on here should be sufficiently detailed. The only real disadvantage is the mildly toxic zinc waste that's left over afterwards.
doubledog
Established member
There is another option how to use a Manske NaCl salting step.
If salt and alkaloids concentrations are high enough, harmalas hcl will precipitate instead of producing typical brown crystals. This precipitated material is cleaner and contains less gunk than normal Manske crystals.
So, after first basing, dissolve the sediment in acidic water, but use less amount of it to keep alkaloid concentration higher. After filtration, keep it in a hot water bath and add salt slowly until over 20% concentration (or more) is achieved.
This works quite good, but I think that Loveall's method from starting post works better.
If salt and alkaloids concentrations are high enough, harmalas hcl will precipitate instead of producing typical brown crystals. This precipitated material is cleaner and contains less gunk than normal Manske crystals.
So, after first basing, dissolve the sediment in acidic water, but use less amount of it to keep alkaloid concentration higher. After filtration, keep it in a hot water bath and add salt slowly until over 20% concentration (or more) is achieved.
This works quite good, but I think that Loveall's method from starting post works better.
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Kalitechnik
Established member
hmm.
But Loveall starts allready with HCL, and what you propose is to take the acidic solution saturated with harmalas and start to super saturate it with NaCl?
And then the harmalas should start to crash out as HCL salts?
That would be quite interesting. Also it would be the way to change my freebase into HCL form for easier oral administration?
doubledog
Established member
It's basically just adding more salt than you would normally use for typical Manske. But it still depends on low solubility of harmalas hcl in salt solution. So yes, hcl salts of harmala precipitate in golden yellow grainy amorphous sediment.
I've never tried harmala hcl orally, but would expect it to work fine that way.
I've never tried harmala hcl orally, but would expect it to work fine that way.
Keyword (OK, phrase) here is "common ion effect"