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..

why has no one dissolved a bit of the final product in water and checked the pH?

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.

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)

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?

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.

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!

Don't forget the 25 kilogram bags of MSG!! (gaaack!)

Ssssh! You'll give away my secret freebasing tek I've been working on!

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