Oversaturated naptha/DMT extraction, evaporation is not the only answer

[Dev84]

A week ago I did my first STB MHRB extraction. I did the extraction in a gallon glass jug, with a half pound of MHRB, all at once. I know smaller batches pull better quantities. But for my first extraction I just wanted to do one jar, so I did. After I soaked the MHRB in the Ph 13 base, I added naptha to the very top of the gallon jar. So that there were minimal air bubbles when flipping the jar upside down and back. After doing several extractions this way, with fresh naptha filled to the top of the jar, and collecting all the DMT/naptha extractions in a separate jar, I ended up with a 13 x 9in deep glass casserole dish, a little over half full. After doing an unsuccessful 24hr precipitate/freeze/pour-off and then some online searching, I found out the naptha/DMT solution I had was way over saturated. The oversaturation wasn't letting the precipitate properly. So after more online searching the one and only solution I could find was to evaporate off the excess naptha.

Well, I didn't have a good way to evaporate the naptha right away. I ordered an electric plug-in flat top warmer/burner online. So that I would be able to evaporate my solution outside. But that was going to take a week or so to come in the mail. So, while I was waiting on that to come in the mail, I just left the oversaturated naptha solution in the covered glass casserole dish, in the freezer. It was in the freezer, set on maximum coldness, for a full 5 days. When I went to check it, the dish had roughly the same amount of naptha, but it was full of big chunky DMT crystals at the bottom of the dish. I quickly and carefully poured off the naptha. None of the chunks of DMT floated. All the DMT crystals chunks stuck to the bottom very nicely.

Even though I had a way oversaturated extraction, with enough time in a cold freezer (roughly 5 days for me), it still precipitated nicely. So evaporation is not the ONLY answer to an oversaturated extraction. It has me wondering, if I left it for more days would the crystals have continued to grow? I will do more experimentation in the future, to see if larger crystals in fact do continue to grow further. I bought a mini fridge/freezer with a now dedicated freezer section.

So anyways, I decided I'd spend the time to write and post my accidental success. To maybe help someone else in the future that has the same problem. Because when searching for an answer to my oversaturation problem last week, the only sole answer I found was to evaporate. That was it, period, there was no other answer. Well, evaporation is not the only answer. You can just leave it covered, in a cold freezer, and your DMT will still slowly precipitate into crystals.

 

[Bas Sarkin]

I am confused about your using 'oversaturated'. I think oversaturated means there is like 30mg/ml dmt in the naptha. Which would not be a problem, since it would precipitate out just fine.

Did you mean 'undersaturated' (I dont know if thats a term): less then 1mg/ml, which would make it not precipitate (as it all stays dissolved)? Thats why evaporation works: if you have say 100mg of DMT in 200ml of solvent, none will precipitate out. But if you reduce that solvent to 50ml, 50mg would precipitate.

Perhaps your freezer just touched the temperature that made the first dmt precipitate out, but there is some more to get: if you evaporate.
I estimate the depth of your solvent to be 2 inch? then you would have about 3 liter of solvent, which should hold about 3grams of DMT (as it just starts to precipitate out when really cold and with much time).

Now you could evaporate, but I was thinking you could also try to do a mini a/b on it (not sure if that would work, never done it, but it might just be an idea)
put the solvent together with water, acidify, to make the dmt go back into the water. Then remove the solvent, and add 150 ml of solvent, then basify again, and pull the dmt to the solvent. In 150ml at room temperature, you should be able to dissolve the 3 grams just fine (rule of thumb is about 30mg/ml at room temperature, 1mg/ml at -20C).

Put that in the freezer, and you should get 2.850 gram out via precipitation.

But I am not sure. Perhaps someone can weigh in with more experience doing mini-a/b's?

 

[Dev84]

Thanks for the response. Ya, it was just too much naptha used in the extractions. In my mind, for some reason I just think of it being oversaturated with naptha. But yes, undersaturated may be the proper terminology. Making it so it does not precipitate properly in the freezer after 12-24hrs.

All it took was more time in the freezer (5 more days), to precipitate into these crystals. An evaporation step to remove the excess naptha is not the only answer to get it to precipitate. Which from hours of online research is the only answer I was able to find. I will still evaporate further and freeze, but I wanted to post that. Because its clearly not the only answer. I was still able to get a fair amount of usable crystals without stinking up my kitchen using the stove to evaporate off excess naptha. Freezing for a longer period of time is a successful alternative solution, that allows your DMT suspended in excess naptha to still freeze precipitate.

 

[fractals4life]

How about "over diluted"

 

[acacian]

Hey @Dev84 .. being that your naptha was very undersaturated, there might still be quite a bit of DMT left in it. You could evaporate it down further and then try freeze precip again. I bet you have more to come

For doing larger scale extractions like this you'd be much better off just doing 1 or 2 pulls with something like xylene. Back salting your alkaloids out of the xylene into an acidic solution, rebasing with lye and pulling with the minimum amount of naptha needed. In fact, you might even try combining the rest of your naptha, and salting out of that.. then just using the minimum required amount to retrieve your alkaloids.

 

[Soberdelic]

Thanks for posting! It gives me a lot to think about as I struggled with floaters either because I used too much naptha in my soup or because my freezer might not be cold enough.
My first 2 pulls I removed from freezer
i combined them and placed in front of fan
I evaporated 40% then put back into freezer for 24 hours then I removed and dried in front of fan because I was interested. Then to prevent floaters it was recommended after water wash, to bring naptha to room temperature then place in refrigerator for an hour, before freezer.
What exactly is floaters?
thanks in advance