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*PROOF* Freebasing acetates with only heat (to white crystals *pic*)

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SWIM's been doing somewhat extensive work with this, and he ran into a little snag. While one can clearly obtain a smokable product free of acetic acid taste when vaporized, presumably freebase, vinegar itself (yes, even distilled white vinegar) contains a fair amount of impurities that can not only throw off one's weight but also clog a smoking device (not a huge problem if one's sure to cash each time), and make for a strange, almost sickeningly sweet taste to the vapor, proportional to the concentration of impurities and how heated they are allowed to get).

Anyway, this is what he's been reporting:

Veggie Oil Extraction Log - Eco friendly extraction teks - Welcome to the DMT-Nexus
amor_fati said:
SWIM's had some trifling results from vinegar evaporations. Something seems to be gumming up his product and almost seems like a sugar, as it has a sweet smell and seems to caramelize when an attempt to vaporize is made. He believes it to originate in the vinegar itself since evaporating straight vinegar left a powder and he had the same impurity when salting from straight limonene as well as veggie oil. This may be unique to the particular generic brand of vinegar, so he'll try evaporating some heinz distilled white vinegar and see what comes of it. Kind of unexpected and troublesome...he'll get to the bottom of it.
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Veggie Oil Extraction Log - Eco friendly extraction teks - Welcome to the DMT-Nexus
amor_fati said:
SWIM's decided to elaborate on the impurities he's finding when evaping vinegar:

The first photo is of the precipitates after evaping vinegar used in salting, diluted at ~1:2 with water. This after an IPA wash to remove residual oil and a bit air-drying. The precipitates are bone dry in this photo.

resource.ashx


The second photo is of the precipitates having been scraped up. The consistency is waxy but doesn't adhere easily to itself, as it's quite flaky and could probably only be compressed into a resin to achieve a solid chunk.

resource.ashx


The third is the remnants of vaporization. It's a dry powder and gives the vapor a sweet taste, as if caramelizing (as has been mentioned previously). Apart from throwing off the weight of the product, this powder will clog air passage if allowed to accumulate in a smoking device. SWIM still isn't sure whether this impurity originates in the vinegar or is carried over from oil and limonene, but he doesn't think it's anything that could dissolve in oil of any kind. Again, he's only seen this substance after evaping vinegar no matter what he's used it to salt from.

resource.ashx
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Veggie Oil Extraction Log - Eco friendly extraction teks - Welcome to the DMT-Nexus
amor_fati said:
Well, no luck with Heinz distilled white vinegar. The photo is what it looks like when one evaporates it straight from the store. This has not been used in any part of an extraction.

resource.ashx


For SWIM, that largely puts to rest the possibility of utilizing acetate's beneficial properties. He is, however, experimenting with IPA and vinegar, so we'll see where that goes.
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Anyway, more work needs to be done before this could be considered viable.
 
Maybe tommorow I'll test my vinegar.
I think it might leave a little residue, like 0.5-1mg/mg just by past experiences I always seem to get about that or MUCH MUCH more when they extraction works.
 
Off topic but could impurites in the vinegar cause initially white fluffy spice to turn a semi-sticky yellow/orange color? This is using your tek 2. I mentioned this in another thread a while back for the record. Also this hasn't caused any change in purity or potency when smoked. Actually I kind of think I'm pulling a little jungle spice when this happens. But after evapping the spice is a beautiful white fluff but after a couple days it turns color and gets a little sticky. Puzzling! Of course it could be naptha I reckon.
 
I dont see why not. To reduce volume of liquid and time could cleaning vinegar be used? It can be bought from eco shops or even supermarkets, sold as cleaning vinegar at a concentration of 10% acetic acid.
 
So I told a freind about this and he tried it and said it produced brown oil from clear dmt acetate and is uncertain whether it transfers over manufacturing impurities that may start off inert but be converted to a toxic compound when heated.
The equipment used probably needs to be accurate and the experimenter skilled , it shows promise but Im told its unstealthy and has a small margin for error..
 
Interesting that this topic has limped back to life relatively recently. My 2 currency-subunits' worth:

Several brands of white vinegar contain sodium sulphite, which would leave a residue on evaporation, probably sodium acetate. It's clearly just as valuable to do an evap test on your vinegar as your naphtha, it seems. For those so inclined and possessing the right equipment, redistilling the vinegar would be an option.

Why not go on a shopping trip to Germany? 25% acetic acid is sold in German supermarkets as "essig essenz" - vinegar essence. This probably doesn't need any sulphites...
 
why not just convert with sodium carb instead of wasting time/effort/yield etc evaporating acetates to that point. Converting it is faster/easier.
 
jamie said:
why not just convert with sodium carb instead of wasting time/effort/yield etc evaporating acetates to that point. Converting it is faster/easier.
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It might still be useful if your only solvent is impure naphtha (ie leaves an oily residue) and you have no freezer (or vacuum sublimator:D)
 
So I just had this idea: I have read that DMT freebase prepared from thermal decomposition of the acetate has been successfully recrystallised in naphtha. Now, the boiling point of acetic acid is 118 to 119 °C; 244 to 246 °F; 391 to 392 K; surely if one were to heat the DMT acetate in higher boiling naphtha, e.g. >140 °C, the acetic acid would boil off and the naphtha could then be cooled judiciously to obtain (one would hope) some nice white crystals of freebase?

Some examples are the boiling point of octane is 125.1 to 126.1 °C (257.1 to 258.9 °F; 398.2 to 399.2 K), that of nonane 150.4 to 151.0 °C (302.6 to 303.7 °F; 423.5 to 424.1 K) and decane, 173.8 to 174.4 °C (344.7 to 345.8 °F; 446.9 to 447.5 K). One would have to use a fractionating column to achieve successful separation of the acetic acid which kind of defies the point of the acetate decomposition method a bit. It might be a fun experiment, though.

Overall, it's probably better to just heat the DMT acetate in plenty of water, the more volatile acetic acid will distil out with the water.

So why should this latter process work? DMT and acetic acid are both moderately weak in their respective basicity and acidity. This means that in solution, DMT acetate is always partly decomposed into acetic acid and DMT freebase. (The equilibrium for this can be worked out using pKa and pKb values.)

In a way it's fortunate here that DMT freebase is not steam-volatile, even if some had hoped that the steam distillation of DMT might be a viable process.

Distilling out acetic acid from the solution causes an equilibrium to be re-established, forming more acetic acid from the acetate ions. This will distil out until there is virtually no acetic acid left and DMT freebase and water remain in the flask (if it hasn't boiled dry, I suppose), perhaps in solution, as an emulsion or an oily layer on top. Then all that remains is to collect the freebase.

Is anyone doing any of this already? Or have we possibly concluded that it's simply not effective or worthwhile?
 
downwardsfromzero said:
Interesting that this topic has limped back to life relatively recently. My 2 currency-subunits' worth:

Several brands of white vinegar contain sodium sulphite, which would leave a residue on evaporation, probably sodium acetate. It's clearly just as valuable to do an evap test on your vinegar as your naphtha, it seems. For those so inclined and possessing the right equipment, redistilling the vinegar would be an option.

Why not go on a shopping trip to Germany? 25% acetic acid is sold in German supermarkets as "essig essenz" - vinegar essence. This probably doesn't need any sulphites...
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Could you elaborate on this a little further? Is sodium sulphate labelled when present in vinegar & what brands are free of it?

I am a stickler for purity when it comes to extraction ingredients & finding a food grade acid that is pure & free of preservatives & things like this is proving difficult. Even online shops i am weary of because they seem to know little about what may or may not be mixed into citric or ascorbic acid powder.
Take ball for instance. Their canning acids are available in chain stores but are not pure. Very weary of ordering from anywhere involving lab supply because I tend to be a little paranoid.

I know canning salt is free of iodide & anti-caking agents, there has to be a similar product when it comes to acids where additives cause problems & are left out.
 
I'm pretty disappointed in your claims of 'proof'. Here are my reasons why:

The bp of DMT last I checked was recorded at an incredibly strong vacuum, nowhere near the BP of water. (<.1mmHg?)

It us suggested acetic may not have even formed an acetate salt of DMT, and therefore you only removed excess water/acetic acid.

The acetic acid may have simply created other salts, trapping DMT salts in the formation.

I use temperatures ~bp of water just to dissolve DMT into heptane, with no loss of product recorded by measuring combined weight. I use this weight as a reference point to calculate how much material came from approx how much solvent.

You have no analytical data: rf values, chromatagrams, mp, bp, etc.

All you have is empty claims and a diminished yield, with no actual proof.
 
concombres said:
downwardsfromzero said:
[...]Several brands of white vinegar contain sodium sulphite[...]
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Could you elaborate on this a little further? Is sodium sulphate labelled when present in vinegar & what brands are free of it?

I am a stickler for purity when it comes to extraction ingredients & finding a food grade acid that is pure & free of preservatives & things like this is proving difficult. Even online shops i am weary of because they seem to know little about what may or may not be mixed into citric or ascorbic acid powder.
Take ball for instance. Their canning acids are available in chain stores but are not pure. Very weary of ordering from anywhere involving lab supply because I tend to be a little paranoid.

I know canning salt is free of iodide & anti-caking agents, there has to be a similar product when it comes to acids where additives cause problems & are left out.
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I'm a bit wary of commenting outside my remit here; it makes me weary ;)

The trouble is in part, it seems, that I'm commenting from the other side of the Atlantic. E.g., this is the first time I've even heard of "canning salt". Thus, it would be difficult for me to comment on your local brands of vinegar. What I've done is read the label and avoid ones that mention sodium bisulphite (bisulfite your side of the pond). (EDIT: sometimes there will be an E-number - in this case, E223 - instead, but that's a European thing.)

[Please note that sulfate/sulphate and sulfite/sulphite are two different things and difference of even one letter in chemistry can make a huge, even fatal difference. Fortunately not fatally so in this specific case, though.]

Where I am the strongest vinegar is generally the stuff from Poland, so learning enough Polish to read labels comes in handy. Sometimes there's Czech or Slovak stuff as well but you kinda get used to Eastern European languages.

Fortunately I'm able to be food grade citric acid monohydrate in huge bags from my local Asian grocers, and, e.g., department stores also carry anhydrous citric acid for descaling which - I trust at least - is almost certainly food grade.

Basically I'm always on the lookout for OTC items which may be re-purposed for the laboratory so I don't end up running around with my extraction tek shopping list like some headless chicken. And tbh several decades of chemistry experience helps rather a lot as well.

Sorry I don't think I can be of any more help than that!
 
pitubo said:
downwardsfromzero said:
Fortunately I'm able to be food grade citric acid monohydrate in huge bags from my local Asian grocers,
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Don't forget the 25 kilogram bags of MSG!! (gaaack!)
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Ssssh! You'll give away my secret freebasing tek I've been working on!

1ce, congratulations on reaching your eleven-eleven'th post!
 
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