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Super Direct Dry Tek? (Initial Results & Fixes) Options
 
Wanderer
#21 Posted : 1/22/2011 10:06:35 PM

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Ah, that makes more sense. I suppose sealed cavities in the lattice could definitely store small amounts of acetone, but as dg pointed out, crushing, washing, and cleaning with water (or freebasing) should eliminate these.

Yeah, as far as the volume of acetone is concerned, the goal was to completely cover the basified powder and have a good amount of acetone above that. It would have been fine to mix less with the powder and then pour and filter, but dealing with the filtering is always a pain. Acetone has a very low viscosity (about 3x less viscous than water), so "racking" it for a day or so causes any particulate matter (even highly microscopic bits) to completely settle. This creates a highly "filtered" fraction above the particulate layer, which can be siphoned off without requiring filtration.

The plan is to recycle the acetone after precipitation (it's kind of expensive), but SWIM needs to find a way to clean any remaining fumaric acid from solution (does anyone know of any other insoluble fumaric salts?)

More to come from SWIM!

-- Wanderer
Wandering back to the home I never left.

All posts made by this member (Wanderer) should be read and interpreted solely as fictional accounts of fantasy, and in no way represent or depict real events or the life of any living or deceased persons.
 

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Metanoia
#22 Posted : 1/27/2011 1:22:27 AM

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Any news Wanderer? Any news, even if it's bad? Pleased Smile
 
Wanderer
#23 Posted : 1/28/2011 3:50:26 AM

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Indeed! SWIM just finished a test of the acetone with FASA.

The results are ambiguous, but clearly show something is amiss. FASA was added dropwise (at first) to the MHRB acetone (which has been sitting for about a week). All the particulate matter had settled to the bottom, so the MHRB acetone was carefully poured into a separate jar. It was perfectly clear but had a yellow hue.

After about 10 drops of FASA was added and no visible clouding or precipitation was formed, SWIM thought to set it aside for a while to see if there were any changes. An hour later, no changes. The air temperature is 58 F, but b/c fumarate salts are insoluble, it was expected to see something precipitate out regardless of temperature.

So then a ton of fumaric acid was added. Probably close to a gram, which all dissolved into the MHRB acetone. Nothing but a few gains of something precipitated out to the bottom with no clouding (probably 20-50mg worth), which SWIM expects to be excess fumaric acid.

Does anyone have any idea what could have gone wrong? Is it possible acetone precipitation takes some time? The clouding should of been immediate, or so SWIM thought. Absolutely no clouding was witnessed. SWIM thought at least something should have come out.

There is still acetone left in the MHRB jar, settled down with all the MHRB itself. Is it possible for solutes to "settle"? SWIM didn't think this is possible for soluble compounds in solution, but perhaps a gravitational solute gradient was formed? SWIM will have to perform more tests after he filters the remaining acetone.

-- Wanderer
Wandering back to the home I never left.

All posts made by this member (Wanderer) should be read and interpreted solely as fictional accounts of fantasy, and in no way represent or depict real events or the life of any living or deceased persons.
 
Metanoia
#24 Posted : 1/28/2011 7:41:25 AM

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Well at least there's some news.

I was thinking, as I read this thread over again, that perhaps sodium carbonate is too weak? Perhaps the DMT wasn't fully based before drying? I really do not have the expertise to give anything more than an estimate, a rather uneducated estimate at that.

If I try this method, I will probably use calcium hydroxide instead of sodium carbonate to basify the MHRB. I'm still hoping we can come up with a sound drytek that utilizes acetone eventually.

Let us know of any new developments!
 
Wanderer
#25 Posted : 1/29/2011 2:02:47 AM

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Will do! I have a feeling the basicity was too weak to fully freebase the alkaloids. I know the pH of freebase n,n-DMT is around 8.7, but because the natural salts are probably bonded ionically to some natural acid (tannic, oxalic, etc), a pretty strong base would be needed to overcome the bond.

But judging by the fact that there are no precipitates in pretty anhydrous acetone, I fortunately haven't lost any of the tasty bits in the powder, and ended up just doing a really complex defatting process.

The only downside is I added considerable amounts of MgSO4, which reacts with OH- ions to form Mg(OH)2 and Na2SO4 (or CaSO4 or K2SO4, depending on the hydroxide salt), etc. So I'm going to need to add considerable amounts of a soluble hydroxide salt to rebasify the solution sufficiently.

I suppose I'll just do a non-polar pull with d-limonene on this instead of using up all the acetone, and try again with a fresh batch but use a stronger base.

But now we now Na2CO3 isn't basic enough!

-- Wanderer
Wandering back to the home I never left.

All posts made by this member (Wanderer) should be read and interpreted solely as fictional accounts of fantasy, and in no way represent or depict real events or the life of any living or deceased persons.
 
endlessness
#26 Posted : 1/29/2011 2:27:52 AM

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CaCO3 ?

You mean Na2CO3 ?
 
Metanoia
#27 Posted : 1/29/2011 4:11:53 AM

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I had a feeling sodium carbonate would be too weak, but I wasn't sure, as I haven't experimented for myself. I'm still glad someone made a thread about this acetone drytek. I feel there needs to be more discussion and experimentation with acetone teks.
 
Wanderer
#28 Posted : 1/29/2011 7:13:19 PM

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Indeed, I'm happy to make any contributions I can. And you're correct endlessness, good catch! I made the edit. I had been reading about carbonic ocean acidification affecting the CaCO3 shells of plankton and zooplankton before posting -- must have still been on the brain.

-- Wanderer
Wandering back to the home I never left.

All posts made by this member (Wanderer) should be read and interpreted solely as fictional accounts of fantasy, and in no way represent or depict real events or the life of any living or deceased persons.
 
Wanderer
#29 Posted : 1/30/2011 7:42:39 PM

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Thanks for the tip elru! Finding Na2CO3 wasn't the issue, though. I managed to produce it by dehydrating sodium bicarbonate, or more commonly known as baking soda (2 * NaHCO3 + Heat => NaCO3 + H2O + CO2). In this way it was completely anhydrous; any water left in the final acetone solution would have pulled the fumarate precipitates into solution.

I'll look for some more basic salts soon -- if I can't find any in stores, I'll make some potassium hydroxide from wood ash.

-- Wanderer
Wandering back to the home I never left.

All posts made by this member (Wanderer) should be read and interpreted solely as fictional accounts of fantasy, and in no way represent or depict real events or the life of any living or deceased persons.
 
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