Is this the right way?

[HippyDippy]

So on re-crystallization... How many times does one have to go through the process? SWIM started with a couple of pretty dark paste like materials. SWIM likes to evap the whole run rather than freezer precipitate because they are very impatient. They are working on this though, and have questions...


So the 2 papers on the right are runs that had a lot of goo in them to begin with. They were washed with sodium carbonate water and then 3 batches of clean water, which removed most of the goo. But then SWIM got impatient and just evapped the washed solutions instead of freezer precipitating.


Now, both of the 2 papers on the right were scrapped into a jar for re-crystallization using heptane. After sitting in the freezer for 48 hours, the jar had 3 substances in it. It had some stuff that looks sorta like salt, some silty tan solution, and yellow heptane. The yellow heptane, and as much of the tan silt that could be had was pipetted out of the jar. This left a sandy brown salt that was scrapped from the jar and went into the vacuum chamber to finish drying out.




Should this be continued to be recrystallized, and if so, how many more times will it take to make shards or white powder?

 

[Toshido]

I would invest in at least three 100mL beakers. You can find them on amazon. It makes it much easier to decant the dmt heptane concentrate from the dark goo.

The key is to let the heptane cool to the point the goo solidifies on the bottom (usually room temp is the right time to decant) and then decant from one 100mL beaker to another. I'm actually doing a re-x right now. Notice how on my first round of decanting, some goo is left behind, then I waited for it to cool down some more and then did round 2 of decanting which left behind the remainder of the goo.

We'll find out in a few hours how well this crystallizes.

The spouts on the 100mL beakers are key to decanting properly, would highly advise getting a few of them. Also, the dish washer is the best way to clean out the goo unless you want to wash the beakers with heptane and then decant into a larger crystallization dish if you wanna scrape all the goo up and save it.

 

[Jees]

I would invest in at least three 100mL beakers. You can find them on amazon. It makes it much easier to decant the dmt heptane concentrate from the dark goo...

I very much like decanting with these things. I don't care carrying over some caustic in the first round, after 3 decants all is clean of caustic. Usually using 250ml beakers.
Hopefully you're aware the goo is not to throw away, some people think it's impurities to discard, there is a hoax out there, it's very much very active dmt in oily form. If you're sure all caustic was out, it's blazingly usable.

To make the oil manageable one can freeze with oily layer still at the bottom. After freezing & poring the deems-depleted naphtha off and beaker evaporating is done, scraping off the whites for vaping, then scraping off the yellow layer that gives one solid chunks, no more dripping oil. Good for weighting and storing with convenience, for pharmahuasca or changa...
I think a flat wide glass pan is not ideal for this style of the oil-hardening. I use a narrow beaker to freez in, gives a thicker layer of whites to scrape off the bottom yellow layer and the bottom yellow layer is really hard. What makes the oil hard? I suppose it absorbs 'whites' just enough to loose it's goo-ness.

If the yellow bottom layer is too much intertwined with the above whites, I suppose too fast freezing occurred, better to let it first cool of as in your picture, let the bottom layer form sufficiently before freezing, can be done in fridge too. Or do a second re-X, the separation will be even better.

HippyDippy, I've no experience with evaping solvents fully instead of freezing.

Happy trials...

 

[Toshido]

Yeah I got rid of it. Was too hard to collect out of the beaker. Next time, after I do a re-x after a bunch of extractions, I'll transfer the goo to a larger flat dish that's more easy to scrape. Re-x came out great though.

 

[ABe©eDarian]

Beautiful.

 

[HippyDippy]

OK, Apparently SWIM didnt wait long enough for the stuff to separate before placing it in the fridge or freezer. This time SWIM fully dissolved about 1.3g of gross looking very dark red goo(the 2 papers on the right in the OP) in about 5ml of hot heptane. They let this sit for about an hour, until the layers were more separated than your picture Widderic. The layer of heptane that SWIM sucked off was nearly completely clear. This liquid was placed in the fridge over night about 8 hours, then placed in the freezer for a full 24 hours. The crystals that formed were amazing! SWIM sucked all of the liquid off, scrapped the crystals onto a paper and placed them into the vacuum chamber to evap the rest of the heptane that remained. What came out of the vacuum chamber was almost pure white fluff!!!! SWIM didnt think it was possible!!!! SWIM was sure they kept doing something wrong, but they just had to be patient!!!!

SWIM forgot to take pictures while the crystals were still in the jar, but this is the powder that came from the vacuum chamber...
Before...


and after...

this only ended up being about .24g
BUT, SWIM started with way icky stuff. Soooo, they arent too surprised. And they are trying to recrystallize the leftovers to see if there is anything left behind... Will keep you all updated.

 

[HippyDippy]

So after trying to glean more molecule out of the slurry that was left, they are now getting a jelly like substance. The oils are not settling down to the bottom of the jar when the solution cools off like it did last time. Can heptane be washed with water like Naptha? SWIM knows this will remove a good portion of the fats if it works...

look at how the stuff is floating on top now...

 

[HippyDippy]

Just wanted to say this morning, you can do a water wash with heptane! The solution was much cleaned up. It was left in the fridge over night, and just transferred to the freezer this morning. Did not see any crystal formation though. May have to evap by half and try again...

 

[HippyDippy]

The solution has set in the fridge for over 8 hours and the freezer for over 8 hours. There is still no crystal formation beginning. There is just a layer of tan silt at the bottom of the jar. The last time there was silt, it formed prior to going into the fridge. The liquid was sucked off leaving the silt behind. The liquid was then precipitated in the freezer, making the glorious pile of white powder. So should SWIM try this method again? Currently the jar is sitting out to reach room temp. If the silt is still present, then the liquid will be sucked up and transferred to another jar again. At this point its just trial and error.


I do have a question though... If so much settled out of the solution to be silt in the bottom, why is the solution still so yellow?

 

[HippyDippy]

After the jar sat for several hours and came back to room temp, there was still a layer of silt on the bottom. I used a pipette to suck up all the liquid leaving the silt behind and transferred it to a clean jar. This jar was then placed in the freezer over night, and this morning I found growth!!!!

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From what I have read, the yellowing is from using heat while I processed and during re-xing. Is this correct?

I am going to alternate this jar from fridge to freezer, in an effort to grow some big crystals. How long should I expect this to take to precipitate all of the DMT? How do I know when all that will precip has done so already?

 

[Timmyt]

You know I did some mhrb and it was white crystals I used lab grade naphtha but the secound and third pull were yellowish and I had heated it up in the pool by heating up the whole batch but the first one was no heat added. It's funny you say it turns yellow with heat caus4 I figured it was the lessor of the pulls but know I think back I didn't put the flask into boiling water until pulled 2 and three and they were yellow. But when they dried it was more Caucasian kinda

 

[HippyDippy]

So I realized that I never posted my results from this re-x. It turned out ok. I still have not vaped any of the crystals yet, but they look nice.




I went after trying to glean any more spice out of the sediment, and ultimately it has not worked out for me. First, I placed 10ml of naptha into my jar of sediment.


I then heated it again with an electric tea kettle until it was fully dissolved. Once it cooled to the point sediment should have started to settle out, it had become jelly.


So once again I thought, "well, a water wash worked last time...", but this time I turned it into an emulsion that does not want to separate... So eventually, i will just put the whole jar into my vacuum chamber, and boil off both the water and the naptha leaving whatever is left. Once I get to this point again, I am going to mix it with some herbs and smoke it.