Yes, even though when SWIM was working on this method he was a bit lazy and he was not decanting off all the water and he was not filtering properly etc. For these reasons his precipitated freebases had a fair amount of residual water and thus sodium fumarate and sodium carbonate. But if one filters properly as endlessness did then there should be no significant amount of neither sodium fumarate nor sodium carbonate.

The latter is important to those who want to keep on the food-safe path for as much as possible and do not want to mess with potentially non-food safe acetone. If one has enough acetone then he may as well go for the paste method instead of the water precipitation.

So he has to use ACE to clean his crystals from impurities ?

He will loose the food-safe quality of his initial product or did I understood wrong ?

Sounds to me like Vacuum Filtration with the basified water precipitation is the way to go.
IF the minimum amount of saturated Sodium Carbonate solution is used -- which I am trying to figure out -- then contamination should be at a minimum.
Unless one really enjoys working with acetone.
Besides, look at those pictures, that is amazing, pure spice with ALL food grade processes!

Plumsmoth, I don't enjoy a lot working with acetone, just when there is no way around (looking at the solvents available).
When I see these picture, I think the same as you, both the SWIM speak about use limteks for the reasons of staying food safe whenver it's possible.
What is vaccum filtration ? Do you mean sucking out the basified water to leave crystals behind ? If so, why was it discussed here the residue could be wash (actually maybe in traces amount the bases and acid are not toxic to vape...

I think acetone is a very nice solvent to work with actually, but I get it food/USP grade.. I dont know about hardware store acetone, thats always very uncertain, I would be wary of trusting that....

In any case if you just read the thread again you'll see that acetone is not really necessary to clean up. As infundibulum said, when he tried this method he wasnt so careful in his separation of the crystals from the water it crystalized in, so he had some impurities (sodium carbonate and sodium fumarate).

Nevertheless, the amount of these impurities present in the final product is negligible if you just filter it till dry. Vacuum is useful but not necessary. r0m, if you dont understand the process of vacuum filtration I suggest you look it up, its very simple.

and yeah, in any case, trace amounts of sodium fumarate and sodium carbonate are not really gonna hurt you

really?! very interesting, I tried it twice and it didnt work, once nothing precipitated, the second time it was a small goo on the bottom.. It was with vinegar though, not glacial acetic acid, maybe that makes a difference.

What was the yield like, in terms of weight and looks?

by the way, this was added to the wiki:

https://wiki.dmt-nexus.m..._Freebase_Conversion_TEK

Maybe the sodium hydroxide made the difference here? Endlessness, did you try the basification with NaOH or sodium carbonate?

hmmmmm.. the sodium carbonate basing of the vinegar pull was the one with no yield, while the one with small amount of goo, I had used NaOH... though to be honest its possible in this second one that I had first tried to precipitate with sodium carb and then added NaOH later, I dont remember much, so that also might have made it screw up.

So would be interesting to make tests with:

1- Vinegar salting vs dilute glacial acetic acid salting.
2- Sodium carb precipitation vs NaOH precipitation

I just started this last night.

I only used 2.5 oz of water to dissolve 1.91 grams of DmtFum. And then added the carbonate solution slowly which was only around an oz of liquid all together.
I have this mixture sitting in a pyrex measuring cup in the fridge and I'm worried that the 3oz of liquid in there is too little for whatever reason.
I never have much confidence in any new procedures even though I essentially have a 100% success rate with everything I've tried.
12 hours later and I do see some particulate settling on the bottom but nothing yet stuck to the glass.

When I dissolved the DmtFum there was a bit of particulate that wouldn't dissolve. Just a few off color specs of stuff that definitely came from the Dmtfum. I was going to decant the Dfum solution but somehow forgot. Is there any chance that this foreign material, little as it may be, could effect the outcome?

there is no reason I can think of why 'too little' water would make it a problem. Dont be affraid of things just because. If all is done right, it will work fine, and if something doesnt go as expected, just dont throw it away an it can always be saved. 12 hours is not enough, wait 3-5 days, the more the better.

As for the particulate that didnt dissolve, did you use warm water? Can you show some picture? maybe it was just a bit of dense dmt crystals.. you should give it enough time and stir to dissolve all.. Maybe,though, its some dust or whatever that came in and it wont dissolve. .This you could just decant or filter to remove it. Dont throw it away just in case there is some actives there, it can be recovered (though I guess its just dust or something). But if you dont want to do anything there, just leave it and it will be small contaminant in your final product, maybe you can even remove it manually once your freebase dmt has formed

You are probably doing just fine. good luck!

Thank you for that encouragement. I'm just a worrier. Something I'm constantly trying to correct.

I think that which didn't dissolve, which was given ample stirring, time and proper water temp, was just some dust or something else that, for the most part, is insignificant. Of the 1.91g of DmtFum it was probably .001% that didn't dissolve.

Thanks also for all your work and documentation.

I agree. Acetone is easily one of the safer solvents people can use. Check out these LD50 numbers.

RTECS#:
CAS# 67-64-1: AL3150000
LD50/LC50:
CAS# 67-64-1:
Dermal, guinea pig: LD50 = >9400 uL/kg;
Draize test, rabbit, eye: 20 mg Severe;
Draize test, rabbit, eye: 20 mg/24H Moderate;
Draize test, rabbit, eye: 10 uL Mild;
Draize test, rabbit, skin: 500 mg/24H Mild;
Inhalation, mouse: LC50 = 44 gm/m3/4H;
Inhalation, rat: LC50 = 50100 mg/m3/8H;
Oral, mouse: LD50 = 3 gm/kg;
Oral, rabbit: LD50 = 5340 mg/kg;
Oral, rat: LD50 = 5800 mg/kg;

The source for that is here: http://fscimage.fishersci.com/msds/00140.htm

I also agree that hardware bought Acetone in a metal can likely has some sort of anti rust additive in it....not positive here...and probably not that big of a deal.

I still say that from the home hobbiest perspective re-crystallization is going to be the purest form people can obtain. Vacume dry if you want, but I'd vacume dry after a recrystallization step. I say this NOT having done every tech out there...nor do I even plan to. I may try a straight to base route if I do this again in the future, but maybe not. I like the control an A/B affords me.

BTW one can find nice hand held vacumme pumps that can be connected to Erlynmeyer flasks that work quite well for separating crystals from solvent in a filtration step...this however is NOT the same as vaccume drying. For that you will need an electric vacumme pump...and a few other pieces of lab equipment to do it effectively...a rotovap would be ideal.

Starting to look like cottage cheese at 48 hours in. I fucking love cottage cheese.

36 hours in and its looking good but I'm noticing that the crystals don't seem to be sticking to the sides of the jar as they do in the pictures. Instead they are just floating on the top of the solution.

I wish I had a camera.

EDIT 1: I've now pulled it and it's drying. It still has a tan color to it and I'm wondering if it's possible that it's somehow still fumarate. Once dry I'll weigh it to see what was lost and I've put the left over solution back in the fridge to see what comes of it.
EDIT 2:I mean...if it was still a fumarate it wouldn't have precipitated out of the SodiumCarb/water solution right?

EDIT 3: Well it's not soluble in water whatsoever so it surely isn't fumarate. I guess my freebase just didn't turn out to be white is all.

EDIT 4: Mine came out to look more like the acetone tek but after vaping it I'm happy to see it burns away clean.

Hmm, well this is bit confusing. SWIM used Amor Fati's non toxic tek for full range spice and decided to convert his fumarate to freebase using the sodium carbonate saturated solution method. On day 3 the jar was pulled from the fridge with stalagmite-esque crystal growth and tannish chunks floating at the top. SWIM filtered off the solution and set the tannish chunks aside believing them to possibly still be DMT-fumarate. After air drying the crystals, beyond a tiny bit of sodium carbonate visible on the top layer, the crystals were completely clear--but the quantity was far too large to be DMT freebase.

3.5 grams of DMT-fumarate were used for the conversion, yet these crystalline flakes weighed in at over 20 grams. The taste was slightly bitter and of course the crystals were completely inactive smoked. SWIM decided to weigh out the tannish chunks pulled from the solution, which was approximately 1.3 grams. The color was slightly lighter than the original fumarate and glistened some in the light. 50 mg were melted (fairly quickly, I might add) onto copper mesh and vaporized, and proved to be very active (no complete breakthrough, but wonderful closed eye fractals and spicy headspace/dimension distortion).

Is it possible that the crystals that precipitated were actually salt by-product (possibly sodium fumarate?) and the tannish chunks are in fact freebase spice? If so, any ideas on why SWIM's crystallization turned out crystal clear chunks of salt rather than spice?

SWIM has dissolved the crystals in distilled water and is planning on putting them in the fridge to see if they recrystallize. If they do, SWIM is going to attempt to pull any freebase out of the crystals using IPA.

Anyone have any ideas? Any help is greatly appreciated, slowly but surely SWIM's knowledge of the chemistry will improve.

Friend of mine done the old CaC03 saturated Water method of converting DMT-fumarates twice.
Once it yielded some slightly pinkish / off white freebase crystal DMT.

The second time yielded some tan goopy substance, with a light dusting of white crystalline. Once dried and chopped it resulted in a sand/tan colored freebase.

Any reason for the differences in color? Apparently the second batch was pulled over a period of two weeks. Perhaps there was more there to begin with.

Is Acetone is the only recommended solvent for cleaning these full-range freebase molecules, without loosing the full-range goodness?
Righto.

This thread seems like the right place for some questions SWIM has. He seems to be having the same thing going on as shiznackazane did. He did an all natural tek with Calcium Hydroxide and FASW to get the fumarates. He thinks everything went within normal expectations up to then. After doing a wash he ended up with ~.75g of fumarates from 50g of MHRB.

SWIM ended up using the conversion tech 1 leaving in the fridge for 5 total days with .5g of the fumarates. Within the first day or so he could see crystals starting to form and float on the top. At then end of day 5 it looked like the 2 pics attached in the shot glasses.

He then used some tongs to pull out what he could at first and placed in a petri dish. Then poured the shot glass through a coffee filter and spooned up the rest of the stuff at the bottom of the glass. There was some water left attached to the crystals which explains why he saw a bunch of white powdering looking stuff (assuming sodium carbonate that was dissolved in the water) on top of his crystals. The crystals that were floating on top of the liquid were a little more orangish as well as some of the loose floating ones in the glass. But there were a bunch of larger crystals that were pretty much see through. You can see two of them growing from the bottom of the shot glass.

As with shiznackazane, SWIM ended up with crystals weighing in well over what would be possilbe (SWIMS were close to 5g from the .5g of fumarates he attempted to convert to freebase.

Does anyone know what exactly happened here and what those extra crystals are? Where do you think SWIM possibly went wrong here? He notes a couple of things he wasn't fully comfortable with.

1) He couldn't get all his Fumarate to dissolve in warm water even though he had way more than enough and stirred. So end result was there was a lot more water than needed.
2) It was hard for him to tell how saturated the sodium carbonate water wash. It didn't settle nicely visible to the bottom as when saturating water with Fumaric acid. So he kind of eyeballed it to match the cloudiness in the pictures. Could have been oversaturated.
3) The shot glass was just put in the fridge w/o a cover.

So SWIM is wondering what his next steps should be. He would like to keep it food grade if possible, but if there is no option he could try and recrystallize as per the wiki with some naptha.

For endlessness: When you are collecting the freebase from conversion tech 1 do the crystals totally stick to the glass like in the pick, or is that dumped back in from what was collected in the coffee filter?

My guess is the sodium carb solution was over-saturated and the particles hadnt settled yet, and then with the cold of the fridge, appart from DMT a lot of sodium carbonate crashed. Ideally you can just leave the sodium carb solution standing for a while to decant before using, maybe I should edit the wiki to explain this better?

Anyways what you could do now is simply wash this with water, which should dissolve the sodium carb but not the freebase dmt. Just dont throw anything away until you have your final yield, because it can always be recovered if something doesnt go as expected. Dont worry for sure you can keep it food-safe. let us know how it goes with the water wash!

Not sure if you need to update the wiki or not. I think SWIM's problem was that it took so little fumaric acid before it settled that he expected the same of the sodium carbonate. This was his first extraction after all . Next time he will wait for it to settle a little. Perhaps to be safe he could just pour the Sodium Carbonate solution through a coffee filter before adding it into the FASW.

He was confused by the results cause there was a slight amount of water on the petri dish along with the clear crystals and the orangish crystals and he assumed all the carbonate would be in the water and not crystalize. He thought it looked like a bit much, but it's hard to eyeball in such small amounts. When he put it on the scale it it was about 5g he knew something was amiss or he stumbled upon a miracle

Will update with SWIM's results.

Why do you do a lengthy freeze-precip? To get larger x-tals? To remove excess sodium carbonate? After precipitation occurs, why not just evap away the liquid?