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Is it possible to purify dirty industrial solvent?

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iyiyandiyiy

Rising Star
Hello!
Where I am located, xylene and toluene are relatively easy to obtain. I've read around here they're pretty good for a full spectrum extraction of MHRB. Now, I did an evaporation test and at least the xylene leaves an oily gasoline-smelling residue behind.

I guess this could be an azeotrope of some heavier HC from the rough industrial production process. Now, would it be possible to further purify this in a kitchen lab distilling it through a reflux column? Even if the yield was relatively low?

EDIT:
I found a vendor selling imported ExpertQ brand petroleum ether for analysis TDS reports 0.0005% residue on evaporation (that'd mean 50mg per 100g). No total purity stated.
And n-hexane, also analytical, which reports 0,001 % residue on evaporation. 96% purity stated.
Since the nature of the "residue on evaporation" in both cases is unknown I suppose these solvents would not be safe for food-grade procedures such as freebases. No?

Would slowly boiling the freebase in excess methanol (for example) for a relatively long period until all ethanol has evaporated help remove the possible contaminants for either the dirty xylene above, the petroleum ether and the hexane? Funily enough it's remarcaby easier to find these chemicals here rather than, for example, limonene.
 
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Well, the residue isn't an azeotrope, and you'd need a fractionation column rather than reflux - but it is in principle possible to do so if you have the relevant equipment and are competent enough to perform the procedure safely.

Instead of evaporating the toluene/xylene to recover the freebase, you could instead use vinegar to recover the DMT from the NPS as the acetate, and then add a base such as sodium carbonate or calcium hydroxide to the acetate goo to freebase it again. The DMT freebase can be recovered after allowing this mixture to dry, with the help of some acetone, IPA or ethanol.

Using this so-called mini A/B method you can purify the product and leave the oily contaminants behind without resorting to a stinky, dangerous distillation.
 
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Ok, ok. I see... So I'd not use the xylene FB directly. Makes total sense now. And I corrected it now, I meant distilling the xylene under reflux (like using a vigreaux column). My idea was roughly along the lines of "heavy reflux at minimum temperature required for xylene boiling"... (I'm still interested in stuff like refining chemicals and solvents).

I did some years of chemistry and was fairly competent in the lab :D. Unfortunately forgot all my theory (trying to quickly get it back though).
 
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iyiyandiyiy said:
gonna get off-topic now, but may I inquire on the nature of your avatar? Have you met a clown in hyperspace? (not joking)
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More like I was an actual clown in real life. I tend to meet arthropods with DMT if anything, and have far more experience with mushrooms in terms of actual psychedelic mileage.


While you can recover crude DMT FB from evaporation of the xylene, it seems a shame to waste solvent (not to mention its penetrating odour). Glad to hear you've some chemistry background - it's good to polish off the rusty spots and, in my case, the Nexus really helped incentivise me in this. Have a good browse of the resources on this site and you'll find DMT extraction to be about as hard as baking a cake.

Also, as a fellow chem nerd you might just want to distill your solvents for the fun of it as well as it being sensible to avoid unnecessarily introducing impurities. Just so long as you have a safe heat source - no naked flames or incandescent material.
 
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Interesting. I don't have a particular relationship with clowns. Neither negative nor positive. And the first entities I came across were actually clowns haha. Never came across entities with either mushrooms or mescaline.
I'm actually in the process of designing a resistive heating mantle ;) I intend to use refractory cement and some temperature controller. Might upload it here when (or IF) it works fine.
 
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Looking forward to hearing of progress on your heating mantle here. I have some heating tape that's been waiting basically forever for me to build it into some kind of custom heating mantle; I could really do with some inspiration there - not to mention some recommendations for a heating controller.

Posting about your heating mantle will bring major kudos for you (hint, hint... :lol: )
 
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Slowly moving forward with the design haha. My limiting factor at the moment is finding a thermocouple that can be immersed in solvent. I'll try to perhaps use a glass tube with the thermocouple inside thermally coupled with conductive grease. My idea is to be able to boil things like HCL solutions too which would damage the stainless steel housing of the thermocouple, while solvents on the other hand would dissolve the wire insulation. Worse case I'll just use a PWM controller and a manual thermometer the old way ... at least I already got the materials. Nichrom wire, refractory cement, glass fibre rope...

On the topic of extraction. Should the ethanol/isopropyl be anhydrous or a 95% ethanol (the one readily available) would be ok? Will the 0.5% water draw a tiny amount of the resulting Ca-acetate and Ca(OH)2, perhaps? On the other hand, ISO is not rated at purity % where I encounter myself at the moment so not even sure how much water there will be in there and AFAIK ISO's very hygroscopic.
 
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iyiyandiyiy said:
On the topic of extraction. Should the ethanol/isopropyl be anhydrous or a 95% ethanol (the one readily available) would be ok? Will the 0.5% water draw a tiny amount of the resulting Ca-acetate and Ca(OH)2, perhaps? On the other hand, ISO is not rated at purity % where I encounter myself at the moment so not even sure how much water there will be in there and AFAIK ISO's very hygroscopic.
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Calcium acetate will form a gel with ethanol or isopropanol, so it's probably better to use acetone for pulling from the lime paste.
 
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