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Heat and Zinc Options
 
MachineElf88
#1 Posted : 12/24/2014 6:36:11 PM

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Hey guys, a couple of extraction questions -

1. Whats the optimum temperature for heating your brew when extracting to maximise yield without destroying any product?

After a low yield extraction on some old MHRB I've been reading about adding zinc to the brew to stop getting oxide in your result - https://www.dmt-nexus.me....aspx?g=posts&t=1553

2. Would standard zinc metal powder be appropriate?

3. How much should I be adding per litre of solution?

Thanks
 

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arcologist
#2 Posted : 12/24/2014 7:45:17 PM

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1. Light boiling should be fine, the DMT is safe. Just make sure to always have enough water so that it doesn't evaporate and then burn the bark. Water keeps it at a max of ~100C, which is less than the vaporization temperature (~160C).

2. It needs to be zinc metal, not any oxide or compound of zinc. It should be a medium grey color, white is oxidized. Very fine powder will work the best because of the large surface area.

3. Something around a spoonful, it doesn't really matter as long as there is an excess. You should do the zinc reduction in smaller vessel (500ml) so that the reduction more easily occurs. The zinc needs to touch every part of the solution for a complete reaction. If the powder is fine enough, it will "cloud" the solution at first and take 30 minutes to settle and coalesce into bigger pieces. At this point you will probably notice a color change (from yellowish to clear). I recommend doing the reduction after freeze precipitation (redissolve freebase goo in vinegar), then base and re-pull after reducing. It seems to go better this way than to do it directly after boiling the bark, there's a lot of garbage in the initial brew that might interfere with the reaction efficiency.

Don't cover the reduction vessel, lots of H2 is produced and could cause an explosion.
 
MachineElf88
#3 Posted : 12/26/2014 12:19:50 PM

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Thanks very much arcologist. So to recap-

Do extraction as normal.
Dissolve total precipitate in small amount of vinegar.
Add zinc, mix and allow to settle.
Colour will change from yellow to clear.
Add sodium hydroxide and then do multiple pulls with solvent.

A few more questions-

Why not just dissolve the precipitate in solvent instead of vinegar and add the zinc to that, then just siphon of the clear result and freeze or evap.

Should I heat the solution during the zinc reduction?
 
endlessness
#4 Posted : 12/26/2014 12:32:41 PM

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I think there's no need at all for zinc, there is no evidence that there's any n-oxide formed in extractions.

DMT itself can be yellow even pure, it is polymorphic.

Please check the FAQ for 'is my dmt ok to smoke?' question since it goes over the different colors and possible content.

If you do this, I strongly suggest you have a control group (in other words, part of your stash you dissolve in vinegar, base and re-extract, without adding zinc), otherwise you will have no clue if you're actually doing anything there, or if the results are simply a result of the redissolving and recrystallization.

And no you cannot add zinc to your solvent since it wont dissolve in that. And no need to heat the zinc.
 
Orion
#5 Posted : 12/26/2014 5:03:02 PM

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endlessness wrote:


DMT itself can be yellow even pure, it is polymorphic.



Besides polymorphism, any info on this? I've never seen really clean spice turn yellow after cleaning unless dirty solvent was used to re-x. And Mini a/b has removed yellow into the aqueous phase every time. To help confirm that pure DMT can be yellow, have we ever seen said pure yellow DMT redissolved into minimal non-polar solvent ? If I'm not mistaken, the solvent should go clear since the molecules are no longer in any kind of lattice which could affect light and give a yellow colour.

As for Oxides... well yeah, if they are yellow then can be removed by mini a/b, I've never seen a case where they couldn't be. Which leads me to think that they aren't oxides in the first place.

A lot of people claim to have removed oxides with zinc, but the other processes needed to clean up impure DMT are usually happening along with this so-called reduction, hence if someone's DMT comes out clear, they consider the experiment a success and sing it's praise, which misleads more people into doing the same when really all you did was clean off some crap the usual way.

As for the adding zinc to vinegar and DMT and having the solution clear up, this is interesting. I can't explain it. But isn't n-oxide insoluble in naphtha? How could it have ever been extracted that way in the first place? Very confusing. Perhaps zinc attracts some crap from the solution, stuff that isn't necessarily n-oxide ? It DOES remove colour from solution after all: https://www.dmt-nexus.me...aspx?g=posts&t=61970
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arcologist
#6 Posted : 12/26/2014 9:17:13 PM

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Orion wrote:

As for the adding zinc to vinegar and DMT and having the solution clear up, this is interesting. I can't explain it. But isn't n-oxide insoluble in naphtha? How could it have ever been extracted that way in the first place? Very confusing. Perhaps zinc attracts some crap from the solution, stuff that isn't necessarily n-oxide ? It DOES remove colour from solution after all: https://www.dmt-nexus.me...aspx?g=posts&t=61970


I use xylene to extract from the bark on the first go, so I regularly pull a lot of yellow goo, especially with ACRB. I can't say for sure whether or not this is N-oxide but it seems likely based on its characteristics (yellow, insoluble in naphtha, won't crystalize, slightly water soluble). It's not NMT either, because I have previously removed it. Upon doing the zinc reduction to this material, the result is a roughly equal amount of pure white DMT that is soluble in naphtha.

My process to replicate these results:
1. Extract powdered ACRB with vinegar, 4x 3 hour boils.
2. Reduce extract down to a manageable amount (<1L).
3. Base/pull with NaOH/xylene, 6+ pulls.
4. Use dry ice to remove NMT.
5. FASA precipitate out DMT alkaloids from xylene.
6. Dissolve result in vinegar, add zinc powder to perform reduction. Turns yellow to clear solution.
7. Base/pull with NaOH/naphtha, 6+ pulls. Leaves behind totally clear solution. If there is any yellow goo left, it will form a layer on top of the water and is barely soluble in naphtha, use xylene to recover goo and reduce again.
8. Freeze precipitate white DMT, results in mimosa-like DMT.
 
Jees
#7 Posted : 12/26/2014 10:59:18 PM

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arcologist wrote:
...I use xylene to extract from the bark on the first go, so I regularly pull a lot of yellow goo,...

In the same spirit of that, since working with mini a/b, I noticed swims pulls (on STB MHRB) are with toluene, it seems not to pull any reds-in-NPsolution (naphta pulls red easily), even in a heat bath 40 deg C or 100 deg F, for easy layer separation, even after vigorous shaking at that temp. Only some green/yellow comes along in the toluene, as you say Arcologist about xylene.

On a side note: second advantage of toluene pulls: freezing the bottle (leave enough space so it doesn't break), simply poring of the toluene instead of fiddle-bastering top layer (the actives stay liquid in NPsolution that cold). It just takes more time freezing/thawing between the pulls, but that in itself is a nice practice of wear on the bark. Plus the freezing forces a near perfect separation. Toluene is sold in any DIY here as Synthetic Thinner, but check MSDS always.

The green-yellow goes partly/mainly into the salting (some stay in the toluene for some ? reason), and some move into the naphta pulls later. This suggest these naphta-green-yellow are no N-oxides. These yellow-green does not really crystallize when the naphta get frozen, it makes the crystals white to colored high-bright yellow and little more fatty/oily though, and give them considerable more weight than white-of crystals.

This thread wondered swim if it's worth doing a zinc game on the salting-liquid before basing/pulling with naphta. This looks promising:
arcologist wrote:
...6. Dissolve result in vinegar, add zinc powder to perform reduction. Turns yellow to clear solution...

Edit: it should work: in wiki:
Quote:
DMT N-Oxide
Dmtnoxide.jpg

Appearance: Basic oil (Weak base. Weaker than DMT, NMT or tryptamine.) Fish et al. 1956. Hygroscopic solid Banerjee & Ghosal 1969
XLogP3: 2
Colorimetric reagent results: Here
Solubility:

Soluble in Xylene, Toluene, Limonene (?) .....
 
 
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