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Total re-x FAIL using naphtha

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hexagonal

hexagonal

Rising Star
Hey guys, please help me understand what went wrong here.

I took one gram of slightly yellow fluff xtals and dissolved it in about 15ml (x2) warm/hot (~45C)
clean naptha. I noticed right away the xtals didn't dissolve easily and that the naph got very yellow . After the 2nd 'pull' there was the expected layer of orange crap, but not much.

I let the solvent cool at room temp, then a couple of hours fridge, and overnight in the freezer.


I had 2 petri dishes in the freezer and found both containing completely dispersed and totally yellow micro xtals. It looks like I lost a LOT of material and furthermore it's now more yellow than before.

Thankfully there are 2 more grams to re-x and I've ordered Heptane but before I even attempt using that for the first time there must be something to learn from this.

edit: possibly of importance: my 'naphta' may be petroleum ether, though from what I understand that shouldn't matter. It certainly did a decent job of pulling roughly 3 grams out of 200gr of mimosa.

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What it do is to do several small "pulls" on the orange residue. The residue still contains lots of material.

Maybe use more solvent. It looks like your was too saturated and everything dropped out too quickly. I use like 30-40 ml per gram of DMT extract. You can always evaporate and re-freeze it to push more alkaloids out of solution. Leaving the solvent at room temp, then few hours in fridge, then freezer is also beneficial to crystal forming.

One final trick I use is to heat the solvent to dissolve micro-crystal seeds. Then slowly cool as described above. This will give you larger crystals.

I would definitely tried different solvent. Heptane and Zippo lighter fluid are great. I like n-heptane the most. BTW most of the product crystallized right in the fridge with heptane - the freezer pushes the rest out.

Some plant oils still precipitate in my case even if heptane is used. Sometimes full re-A/B is necessary to get pure product. But yours look great and using proper solvent and proper washing will solve the problem.
 
Then I'll try it with 40ml of Heptane. Is it true that this has a higher boiling point? Can you say anything about how hot it needs to be for it to dissolve the DMT?

Thanks a lot for your helpful reply!
 
Then I'll try it with 40ml of Heptane. Is it true that this has a higher boiling point?
Click to expand...
Well, n-heptane boils at 98°C but you'd have to look at the label on your naphtha/pet ether to compare. As a mixed hydrocarbon solvent it will have a boiling range according with its composition.


Allowing your recrystallisation to cool (yet) more slowly will result in larger crystals forming. This would include using pre-warmed petri dishes, and insulation to slow the cooling. I see that you are otherwise on point with the slow cooling method.

You could even save a couple of your current batch to act as seed crystals.
 
hexagonal said:
Then I'll try it with 40ml of Heptane. Is it true that this has a higher boiling point? Can you say anything about how hot it needs to be for it to dissolve the DMT?
Click to expand...

Please do the reasearch, you can find basic physical properties on the Wikipedia :) Yes the BP is 98° C.

You don't have to boil heptane, I usually immerse a beaker in a hot water bath (80° C) while mixing with a rod, then decant the liquid in a Pyrex dish. When pouring/decanting, the solvent usually gets milky immediately so I can see it is supersaturated. After few pulls, it does not get milky and the total amount of solvent is some 40 ml per 1-2 grams of DMT.

Pre warmed dish is good so the product does not crash out too soon. I don't mind since I warm the dish a bit on a hotplate, then let cool slowly.
 
blue.magic said:
hexagonal said:
Then I'll try it with 40ml of Heptane. Is it true that this has a higher boiling point? Can you say anything about how hot it needs to be for it to dissolve the DMT?
Click to expand...

Please do the reasearch, you can find basic physical properties on the Wikipedia :) Yes the BP is 98° C.
Click to expand...

I don't know why I phrased the question like that. I had already read that very thing on wiki. I asked in relation to recrystalising, and whether it needs to be boiling hot, which you now answered :)

Great idea to pre-heat the dishes. I'll do that and place a seed crystal. This is gonna a take a few days but i'll report back. Thanks again!
 
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