Cleaning calcium acetate from jim-jam acetate

[VoyagerGrey]

Recently did my first extraction of MHRB, using Q2121 tek. I would say partial success- I have useablr product and a decent yield, but its contaminated with what another member here has helped point out is likely calcium acetate, the result of not letting settle/filtering excess lime from the limonene before salting with vinegar. The result is difficulty fully evaporating off the vinegar to prepare a dose and when it is, failure to achieve complete vaporization in 2-3 drags or at all, because the product is closer to a solid than a goo, and as the DMT vaporizes the residue left behind becomes more and more of a solid, and it's hard to maintain contact with the heated surface of the vape crucible. This might be less of a problem with a convection type device, but I'm trying to figure out using a handheld dab vape. Yes I know, get a GVG... I've been served with one, by someone else, and it was great, but to me trying to handle torch flames and hot glass while trying to remember which side of my face my mouth is on is just craziness. I think without this impurity it would actually work quite well. But I stray. Then there's also how calcium acetate breaks down with heat and releases acetone. Not great - so much for using a food grade tek. It's kind like how they add amylase to "unsweetened" drinks...or celery culture to "preservative free" jerky :?:

I will be starting another extraction soon, and hopefully now that I know I can avoid this pitfall. For now, the member who helped me figure this out on another thread has agreed to suggest some possibilities to clean up what I have if I share some information, so here is all the relevant stuff:

I have maybe 15 ml of vinegar tincture with an estimated (actual, after accounting for impurity weight) concentration of roughly 100mg/ml jimjam if my math is correct (2.5 mg per drop, a drop from this particular dripper being 0.025 ml. Roughly equal amount (by weight) of impurities, measured by weighing the chalky residue left behind after complete vaporization.

Solvents/supplies I have/can easily get around here:
Naptha
Acetone
99% IPA
Lime
90% Ethanol

One interesting to note, which may be helpfull- The tincture out of the dropper is clear translucent red. When evaporating off the vinegar in my e-vape at 220f^, a residue starts to form- little chunks that sink to the bottom, and perhaps could be filtered. No idea what those are or whether there's any of the good stuff in them.

I can't figure out how to tag another member (if that's even possible?) but I'll shoot a DM and hopefully they'll chime in. Any other advice from knowledgeable

 

[downwardsfromzero]

You might as well just mix your impure acetate into a paste with sodium carbonate (washing soda). Let this dry completely, then pull the freebase with naphtha, acetone or IPA. These latter two ought to be as dry as possible - dissolved/absorbed water should be removed using a dehydrating agent before use.

When it comes to recovering the freebase, in the case of naphtha, you have freeze precipitation as an option, otherwise evaporation should do the job just fine although there may be traces of sodium acetate if you use acetone or IPA and they were too moist.

Another route would be conversion back to salts. Naphtha is in a way the most convenient solvent here since you can recover the DMT with a little vinegar. A solution of any other edible acid should do the job too; in the case of acetone or IPA this solution would have to be made with the respective solvent. You could also try dumping in crystals of citric acid (but not in the naphtha though) which should yield a goo suitable for dissolving in PG for making e-juice.

 

[VoyagerGrey]

Ok I have an update.

Let's say one has 7.5ml of vinegar tincture containing an estimated 600 mg of spice...But also unwanted calcium acetate to be removed...

And followed this procedure:

*Add 3 tsp calcium carbonate (Correction: sodium carbonate) and 2ml water. Mix/crush thoroughly
*Let air dry overnight
*Finish to bone-dry for 1hr @ 104F in food dehydrator
*Crush and crumble to as fine a powder as possible
*Add 45ml warm naphtha and keep in a hot water bath for ~60 minutes
*Pour of naphtha trough coffee filter, then let cool to room temp, then an hour in the fridge, then move to freezer for 24hrs to precipitate.
*Carefully pour off remaining naphtha, recovering ~ 25ml
*Put dish off to the side to finish evaporating at room temp and at the same time:
* 2nd pull with recovered solvent +15ml fresh solvent. Same procedure.
*Repeat for a total of X3 pulls.

Decant and store remaining solvent, let the dishes all evaporate until dry.

At this point one might find the crystal is formed atop a layer of yellowish/ brown residue. Impossible to separate when scraping the dish, resulting in an orange/ brownish powder. perhaps some recrystallization is in order?

*If so, one might redisolve the yield in some of the warmed recovered naphtha, just the minimal amount that will dissolve everything.

*This time fats and other non soluble goop readily clump and are easily filtered through a coffee filter.


*Re precipitate- cool gradually, first to room temp, then fridge, then freezer.
Decant and store naphtha.

If someone did all this, well they might end up with something like this:

The bottom dish being the recovered spice from the cleanup/freebase conversion, the top being the yield from a Q21Q21 style lime/vinegar extraction of 100g MHRB pulled X4 with warm naphtha and likewise re-x'd and cleaned of oils and plant residue that made it through.

576mg and 800mg respectively.

That's pretty good on the conversion IMO, given that the amount of spice in the tincture was only an estimate... Less than stellar for the fresh extraction. Given a result like this one might think first extraction with Limonene/vinegar, then conversion with naphtha may be the way to go in the future.

 

[downwardsfromzero]

Very nice! :thumb_up:

*Add 3 tsp calcium carbonate and 2ml water. Mix/crush thoroughly

Did you perchance mean sodium carbonate? While calcium carbonate does occasionally get used as a (very mild) base, this would be something of a first for DMT extraction.

 

[VoyagerGrey]

Very nice! :thumb_up:

*Add 3 tsp calcium carbonate and 2ml water. Mix/crush thoroughly

Did you perchance mean sodium carbonate? While calcium carbonate does occasionally get used as a (very mild) base, this would be something of a first for DMT extraction.

:roll: Yes I did. Sodium carbonate. Corrected.

 

[VoyagerGrey]

Some dried goop seperated in re-x'ing. Looks like a mix of fine plant matter dust and oils to the naked eye. One might try smoking it to find out if there's anything active in it.

 

[VoyagerGrey]

Some dried goop seperated in re-x'ing. Looks like a mix of fine plant matter dust and oils to the naked eye. One might try smoking it to find out if there's anything active in it.

The answer is yes, very much so. It produced harsh smoke and a terrible taste, but was fully active. There is a chance that my vaporizer is set to a too-high temperature, based on previous experimenting with the much less pure acetate goop, and that this stuff might have vaporized at a much lower temperature and been less harsh as a result. There's a chance, but I don't have any more of it on hand to test that theory.

 

[downwardsfromzero]

Hypothesis :lol:

Your experiment shows that the dark goop (if it was isolated during naphtha re-x) largely consists of polymerised DMT. It's not clear to me where this goop appeared in your re-x, however.

Then there's also how calcium acetate breaks down with heat and releases acetone. Not great - so much for using a food grade tek.

Small amounts of acetone are produced in the body as a metabolic byproduct through the decomposition of acetoacetic acid, which is a crucial component of the citric acid (Krebs) cycle at the epicentre of aerobic energy production in cells. Thermal decomposition of calcium acetate can/does produce some nasty, stinky impurities of course.

 

[VoyagerGrey]

Hypothesis :lol:

Your experiment shows that the dark goop (if it was isolated during naphtha re-x) largely consists of polymerised DMT. It's not clear to me where this goop appeared in your re-x, however.

Could very well be. How it formed was as a film on the glass dish on the initial evaporation. Inevitably got scraped up and mixed with the crystal.
When I added warm naphtha for re-x, the reddish brown stuff mostly stayed in easily separated clumps, i.e. did not dissolve. Polymerized DMT should have dissolved, shouldn't it?
I discarded some of it but then decided to save the rest for testing.
Interesting to note that after vaporizing it there was a little bit of the same chalky residue left in the bowl, like when vaporizing the impure acetate.

It could have been:
A. Unreacted DMT acetate? (doubtful)
B. Polimerized DMT
C. Some impurity, perhaps calcium acetate
D. All of the above?

 

[downwardsfromzero]

IME, polymerised - or perhaps, more correctly, oligomerised - DMT only starts dissolving at above 60°C. The higher the temperature, the more of it dissolves and the darker the undissolved residue. Orange-brown oil separates out again on cooling. This is the stuff that has been referred to as "plant fats" and "DMT-N-oxide" but work by Benzyme in particular indicates that it consists of various short-chain aggregations of DMT molecules that are partially oxidised by loss of an electron from the pyrrole ring.

Recrystallisation of DMT can be a bit weird because of this, and is also compounded by its polymorphic behavior, along with its limited solubility in naphtha at temperatures above the melting point of at least one of the polymorphs, so we're also dealing with liquid DMT being partially dissolved in the oily oligomer - or vice versa.

Work by others including Loveall has shown that acidification appears to break down most of these oligomers and this observation was itself a spinoff from investigations of using zinc and acid to reduce (remove oxygen from) the aforementioned so-called DMT oxide.

It seems we've missed a bit of a trick here now that the bulk of your polymeric goo has been discarded. In future you'll know to save it for recovery of further freebase through acid treatment, possibly with the help of zinc.

EDIT: I see you mentioned a chalky residue, for which small amounts of calcium- or sodium-bearing particulates making their way through the re-x process seems to be the most likely explanation.

 

[VoyagerGrey]

downwardfromzero-

Putting the spesifics of chemistry aside, (it's way over my level of understanding) here's my takeaway from your last reply:

*The gooey residue is likely polymerized DMT
I've done a bunch of reading around the forum and it seems like several people have run lab tests on various substances previously hypothesized as "jungle DMT"/DMT n-oxide/"yellow DMT" and so on only to find...DMT. No other alkaloids in any significant quantity.

And that the variations in appearance and physical characteristics seem to be due to how the individual molecules arrange themselves as the DMT comes out of solution, be it by evaporation, precipitation, or chemical reaction. Single molecules form pure white crystals, various bonded chains of molecules form various types of wax/goop

And that how the molecules arrange themselves depends very much in conditions during the final step of isolation.

Did I get that right? And is this pretty much consensus now? i.e. has the whole "jungle"/"red"/"yellow"/"full spectrum" etc debate been put to rest?

The most convincing /comprehensive on this that I have seen is here:
Chilled Acetone with IPA and Naphtha contains the following quote:

Q: What is the difference between DMT polymers, oligomers, aggregates, and aromatic pi-pi stacking?

A: None, all names are equivalent and refer to the same thing: weakly bonded groups of DMT molecules that form goo instead of crystals.

Having said that, in my non-chemist, non-pharmacologist mind, even if all of these are chemically speaking, more or less pure DMT freebase, isn't it plausible that oligomerized/polymerized DMT might have some variations in felt effects, on account that a polymer might react differently to the heat of vaporization, affecting efficincy/speed of absorption, and furthermore, might react differently once in the body?

Essentially, isn't it possible that polymerized forms of DMT in effect function as a different ROA, which could in turn have significant impact on effects?

Work by others including Loveall has shown that acidification appears to break down most of these oligomers and this observation was itself a spinoff from investigations of using zinc and acid to reduce (remove oxygen from) the aforementioned so-called DMT oxide.

wouldn't acidification return the DMT to acetate form, requiring aditionl subsequent basification back to freebase?

Just curious about all that. Again, I don't have the training to understand the chemistry beyond a very superficial level.

I think that goop was mostly DMT. It looked like oil, but couldn't have been, because I was to mix (not dissolve) it in water.
I had 40mg of it, and I'd say it hit like 30. It had a bit of residue, be it some form of calcium/sodium or even just plant dust. In the future I will favour washing the filter media (coffee filter/cotton ball) with additional clean solvent rather than squeezing it dry, which seems to let some particulate into the collection vessel.

Pragmatically speaking, is there a reason why I should give a hoot? I suppose from the chemist's perspective, if your goal is to produce pure white monomer crystals, you would aspire to maximize that outcome. Being a perfectionist in other things I am much more skilled at, I get it.
From the psychonaut's perspective, if it vaporizes all the same and sends you into hyperspace, why bother? It had a bit of a foul taste (but not like VOC), but 40mg out of 800 or so, evenly distributed, probably wouldn't have been noticeable.

 

[alchemizt]

Just dissolve the DMT acetate in acetone and filter out the insoluble calcium acetate. Then evaporate the acetone. You can drop some anhydrous magnesium sulfate in the acetone to make sure its dry.

Another way would be to add food grade phosphoric acid, filter out the calcium phosphate, then use sodium carbonate to precipitate the freebase.

Another idea. Put the spice in a test tube and heat with a heat gun. The DMT acetate will melt. Decant the liquid.