Did a two pull STB extraction on 50g of MHRB. Yielded just under .5g clear and white xtals with a little bit of yellow goo. I decided to see how a re-x would help, so I dissolved entire yield into about 50ml of heptane using a double boiler type set up. Once xtals were dissolved poured off heptane into a shallow dish and started CFC. After about an hour the amount of xtals in the dish are quite disheartening. Just moved to freezer so I'll so how that goes.
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Re-X issues.
- Thread starter sinner_di
- Start date
- Merits
- 117
take a look at the FAQ for instructions on recrystallization. You used too much heptane, the ratio should be about 30ml per gram of impure product, you used 50ml per half g.. This means first of all that you wont be really cleaning much (because with so much heptane, you will also dissolving all the impurities), and it also might mean that its not saturated enough so not all dmt will crash out at freezer. If nothing or not much crashes after 12 hours, evap half of the volume and stick in freezer again.
Next time remember to use less solvent and to decant away the solvent layer (with dmt) on top away from the undissolved goo (mostly impurities) on the bototm
Next time remember to use less solvent and to decant away the solvent layer (with dmt) on top away from the undissolved goo (mostly impurities) on the bototm
Phantastica
Rising Star
- Merits
- 42
do similar spice to solvent proportions also apply when doing a re-x with Naptha instead of Heptane, or does it not matter in the case of Naptha? would 50ml/half g spice be too much Naptha in the case of naptha re-x as well?endlessness said:
are these not active spice oxides, mixed with plant fats? would you suggest saving it, or throwing these away in the case of Naptha re-x? and what about in the case of Heptane re-x, and acetone re-x? since these impurities would vary in their content depending on the solvent..endlessness said:
Thanks in advance
- Merits
- 117
Naphtha should generally be equivalent to heptane. When we commonly talk about naphtha here, take in account that naphtha is meant as a mixture of aliphatic hydrocarbons, (pentane, hexane, heptane, octane, etc). In this case you can consider naphtha equivalent so measures are around the same.
At times, it can happen that a product sold as naphtha (this is the case in parts of europe for example) but it has some aromatic hydrocarbons (such as xylene) also mixed in, which would either change the numbers or even make it unusable for recrystalization (because impurities can also be very soluble in xylene). So make sure your naphtha is aliphatic hydrocarbons, and then yes keep around same ratio for recrystallization.
Regarding the undissolved goo, yeah its possibly active oxides (though Ive never heard of anybody actually chemically analyzing that goo to know for sure, so I guess its only educated guesses at most at this point), plus other impurities. Actually I've noticed there might be even some normal dmt still there, so I recommend doing a second small wash (like lets say another 10ml warm naphtha), and freezing that separately, as it will likely have some dmt but also a bit more impurities than the first wash.
As for acetone re-x, what do you mean? How could you re-x dmt with acetone? Acetone dissolves too easily all impurities and it wont freeze precipitate... Acetone re-x can work with dmt fumarate, but thats a different story
At times, it can happen that a product sold as naphtha (this is the case in parts of europe for example) but it has some aromatic hydrocarbons (such as xylene) also mixed in, which would either change the numbers or even make it unusable for recrystalization (because impurities can also be very soluble in xylene). So make sure your naphtha is aliphatic hydrocarbons, and then yes keep around same ratio for recrystallization.
Regarding the undissolved goo, yeah its possibly active oxides (though Ive never heard of anybody actually chemically analyzing that goo to know for sure, so I guess its only educated guesses at most at this point), plus other impurities. Actually I've noticed there might be even some normal dmt still there, so I recommend doing a second small wash (like lets say another 10ml warm naphtha), and freezing that separately, as it will likely have some dmt but also a bit more impurities than the first wash.
As for acetone re-x, what do you mean? How could you re-x dmt with acetone? Acetone dissolves too easily all impurities and it wont freeze precipitate... Acetone re-x can work with dmt fumarate, but thats a different story
Thanks for the info Endlessness. I'm working with quite a minimal set up and wasn't able to slowly add in the heptane. After the CFC I decided to just evap off what was left and got about a .40g yield, so not too much loss. Guess next time I should read over what I'm doing a bit more thoroughly.
Phantastica
Rising Star
- Merits
- 42
Ok, thanks a lot endless!! you're right, acetone re-x doesn't apply in this case. for some reason, i confused the crystal growing with a re-x that would leave behind impurities..makes sense now
