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(nice) DMT Oil -> Petroleum ether -> (nice) crystals Options
 
Levanah
#1 Posted : 9/20/2016 4:19:36 PM
Inspired by endlessness eco-friendly tek and q21q21 tek I recently did an IPA-Lime extraction and ended up (after further IPA cleaning) with very active brown goo. It's very nice on its own and I had one of my most intense experiences with 25mg of this brown material.

However I finally got my hands on some petroleum ether 40-65 and want to do a further purification step to get an easier to handle product. I don't aim for the whitest of the whitest crystals but want to get rid of the oil.

From this thread I understand so far:

- room temperature solubility of spice in naphta should be around = 2.04081633 mg/ml

- endlessness uses 30ml of warm naphta (at maybe 50c) to pick up 1g impure dmt


I also understand:

- The more warm the naphta / petroleum ether the more impurities are pulled

So if I use room temperature petro ether I need about 250l to dissolve 500mg spice.

If I would use such a vast amount of petro ether to dissolve 500mg brown goo, would freeze precip still work? (Solvent availability is not the problem + I can re-use solvent)

In theory 15ml of warm petro ether (50C) would be enough to dissolve the goo, however a) maybe the end-product will be a goo again and b) I have no thermometer to measure the temperature.

What's your advice? How would you convert this goo in crystals?

What ratio of petro-ether:goo would be your advice? Warm petro-ether or room temperature?

Thanks alot! Smile



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1ce
#2 Posted : 9/20/2016 4:32:13 PM
Depemds. Purity can cost you yield. I'd dissolve in some solvent, add some carbon, filter until clear. Then evap sovent off. I'd then prewarm the dmt oil near the bp of my crystallizing solvent, and add it dropwise until dmt was dissolved.

Then I'd decant it into a crystallizing dish and allow it to cool down SLOWLY. Crystallization, like any other from of separation/purification enjoys its time rather well. The longer, the better. Usually.
 
Levanah
#3 Posted : 9/21/2016 5:47:25 PM
1ce wrote:
Depemds. Purity can cost you yield. I'd dissolve in some solvent, add some carbon, filter until clear. Then evap sovent off. I'd then prewarm the dmt oil near the bp of my crystallizing solvent, and add it dropwise until dmt was dissolved.

Then I'd decant it into a crystallizing dish and allow it to cool down SLOWLY. Crystallization, like any other from of separation/purification enjoys its time rather well. The longer, the better. Usually.


Hi 1ce and thanks for ya time Smile

As my english is not the best I don't understand the chronological order of your steps.

1. I dissolve my oil in pet ether
2. I add some carbon (would like to skip this step, as I don't have carbon at hand and prefer a more easy approach this time, until i'm more expert).
3. I filter this until clear

How can I prewarm the dmt oil in the next step if it's already dissolved? Or should I prewarm the entire oil-pet-eher solution? But where to add it dropwise then? Sorry please talk to me as if I am a completely retard Smile . I'll profit from of your advice and will keep the carbon step in my mind for the future.

Yesterday I just did an easy experiment:

1. Dissolved 200mg DMT-Oil in 30ml warm Pet-Ether which was warmed by a warm water bath (at some point the Pet-Ether even seems to be boiling a bit)
2. Stirred and Stirred and squeezed the DMT Oil with a little spoon - the DMT-Oil is kind of resistant to be dissolved because the DMT seems to be very protected by the oil. (In comparison: Hot IPA dissolves the OIL very fast!)

When I thought that it's done, I decanted the Pet-Ether on my evap dish and just evaped it completely. Had still enough goo(oil)-residue at the bottom, so just a part of it was dissolved in peth-ether.

It was evapped within nothing more than 2 hours.

Yielded 50mg of brown-waxy solid material which looks exactly like my freebase yield from my limonene-pulls.

The end-product was nice and I'm satisfied with the purity.

However the yield was low! Just a small amount of my DMT was dissolved.

Safed the left brown residue which will be recycled and re-converted in another pull from an IPA extraction.

I think the (nice) Jungle OIL wants to stay as (nice) Jungle OIL.

Yeah, that's what my intuition and my angelic elf are telling me.

But they are also telling me, that I should use the petro-ether for future pulls of fresh 250g MHRB and will get nothing but nice and delicious results.






 
Levanah
#4 Posted : 9/21/2016 6:05:49 PM
Two more ideas:

As I said I'm mainly interested to get a better to handle, more solid product.

I'm guessing two things should work:

1. Dissolve 1g DMT-Oil in 30ml hot IPA
2. Let it dissolve SLOWLY in a small glass (no evap dish!) -> should possibly yield brown needles or a more solid brown stuff

______

And then a completly other thing came to my mind.

I couldn't find anything in the nexus about it.

Shouldn't it be possible to dissolve the DMT-Oil in 30ml hot IPA, cool this down (put it in the freezer) and then slowly add FASI to get Fumarates?

We give always FASI / FASA in our limonene-pulls, but shouln't it work with IPA-pulls likewise?

This morning I did my last (fourth) pull from a IPA-Lime tek. As I already yielded about 1,2g DMT-Oil the fourth pull always yield very less. Maybe 200mg more is in there if i'm lucky.

Then I just tested it and put some drops of FASI in the IPA saturated solution and got clouding...


I stopped after some drops, because I'm not sure yet, if I will do this experiment with this last pull or just convert it to the good old dmt-oil ...





 
 
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