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The Big & Dandy N,N-DMT Extraction Thread - Elves are watching

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Would Koh be a better way to basify over NaOH?
How much mimosa/lye per 250ml jar is normal
 
KOH and NaOH is practically the same in this context. I think they have nearly the same solubility. I use 110 g lye/150 g bark/1800 ml water. Dont ask me how I came up with this stoichiometry, it just works best for the bark/tek Im using =D
 
Im unsure how big an extraction to try first time. I have 10 - 8 oz jars to use, and have about 500g of MHRB.
 
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You'd be better getting a stainless steel stockpot and doing an extraction in that rather than working with lots of little jars.
 
I was going to use a 1litre Pyrex separatory funnel to do the pulls (is this ok for an exothermic reaction?
Mimosa, basified water and naptha all mixed in the funnel. Then seperate out into some glass jars. Seems like it should be fine.

I was going to prepare the correct amounts of materials per pull based on what i could fit, by volume into the jars.

Is that not a good way to work? If so why not.
Id rather use a separatory funnel then a large metal jar as its easier to separate the layers using that then use a crappy turkey squirt-er.
 
Definitely use the sep funnel, that's what I use when I can. Though you most likely won't be able to use the actual funneling action because of all the chunky stuff.

But yea pyrex is especially what you wanna use for hot conditions.
 
For 50g bark, 50g KoH, and naptha at the rate of 0.4ml per g of bark, 50 times 0.4 millilitres = 20ml
750ml of water.

So my total volume will be 770ml in total, 20ml solvent layer and 750ml aqueous layer.
Plus x amount of volume of the mhrb.

This seems like a manageable size extraction. Would anyone disagree with these numbers?
Wont well ground bark aqueous solution be to thick the pass through a 1000ml Sep funnel?
 
That's what I was saying, You will need to pipette the nonpolar layer off the top. Most likely you will need more than 20 mL in order to have a thick enough layer to pipette from.


Seems like a reasonable extraction setup though.
 
Or i could use a narrow tall mixing container right? That would make using the pipette work better.
Or else id have to do a larger extraction. Id rather keep to .4ml per g of bark for a few reasons.
 
After doing several pulls and filling some jars
with naptha, letting them cool, the putting lids on
and freeze precipitating it...
take it out
How do i avoid the crystals redissolving into the solvent as i pour the crystal/solvent through the filter.

This is the only thing im unsure about. Seems like a really frustrating thing to happen and i want to make sure it doesnt.
 
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given the idea that crystals are forming in the solvent you have more disolved in the solvent than it likes to have at a given temperature....

if you warmed it up it would dissolve as completely as it was before.... so filter before it fully warms up.... but as long as it is cold not much will be redisolved....

you can always just evaporate leftover solvent and have whatever was held in it....
 
^good answer right thar

And if you are having trouble getting crystals to precipitate, try letting some of the solvent evaporate away before putting in freezer.
 
Ahh! Supersaturation, Ill go learn a bit more about solubility & solvents.

Can anyone explain in which order i should perform cleaning the result of a naptha pull...

Extract naptha
>
Freeze precip
>
Pour off solvent & save for later (maybe refreeze if looking for max yield)
>
Sodium Carbonate*** wash + 2x distilled water wash
>
Recrystallization
>
Throw crystals in garbage and go play sports.

Is this good order. Im starting to feel like a further solvent wash might not be needed. If recrystallization removes any remaining lye and a sodium carbonate wash does too... then after the above process, i should be left with some lye free clean xtals, right?

Im just looking to get clarified that this is a decent process before i go ahead.
That i wont loose too much yield using these steps, and that this procedure will not leave any unhealthy levels of lye or anything else in the product.

I dont want to make any mistakes.
 
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Sodium Carbonate wash ought to be enough.

And yes that's both a safe and correct procedure, though I never do sodium carbonate wash..only recrystallization.
 
Can chemist comment on HDPE containers and NaOH. I was going to basify my water in a large HDPE bottle then transfer it to a seperatory funnel.

But im not sure if adding NaOH to water in a HDPE container is going to cause any reactions with the plastic. It should be ok to store as pellets in HDPE, but adding it to water is a high energy reaction... just wondering if its Kosher.

http://avogadro.chem.iastate.edu/MSDS/NaOH.htm
 
It is not too difficult at all to get lye free crystals really, no need to overdo the washes and stuff. But anyway, that order is good (though instead of sodium chloride you want sodium carbonate heh) if you're wanting to be extra thorough with your crystal cleaning. Though I prefer to bury my crystals.
 
Hoping for a White xmas, thanks Adrian. Though you prefer to bury your crystals? Instead of throwing them in the garden? I might just do one SC wash then.

Woo wish me luck.
 
HDPE is fine in alkaline conditions e.g. NaOH.

HDPE is a saturated linear hydrocarbon and, for this reason, exhibits very low chemical reactivity. The most
reactive parts of HDPE molecules are the double bonds at chain ends and tertiary CH bonds at branching points
in polymer chains. Because its reactivity to most chemicals is reduced by high crystallinity and low permeability,
HDPE does not react with organic acids or most inorganic acids such as HCl and HF. Concentrated solutions of
H2SO4 (>70% ) at elevated temperatures slowly react with HDPE with the formation of sulfo-derivatives. HDPE
can be nitrated at room temperature with concentrated HNO3 (approx 50% ) and its mixtures with H2SO4. Under
more severe conditions, at 100-150oC, these acids decompose the polymer and produce mixtures of organic
acids. HDPE is also stable in alkaline solutions of any concentration as well as in solutions of all salts, including
oxidising agents such as KMnO4 and K2Cr2O7. At room temperature, HDPE is not soluble in any known solvent,
but at a temperature above 80-100 oC, most HDPE resins dissolve in some aromatic, aliphatic and halogenated
hydrocarbons [4, 10, 12, 13].

4. Encyclopaedia of chemical technology (4th edition), 1996, 17, p724-32
10. Encyclopaedia of chemical technology (4th edition), 1996, 17, p81-87, p414, 425-8, 440-2,
12. Polymer Degradation and Stability, 1997, 57, p381
13. Seymour Carrahers, Polymer Chemistry: an introduction (4th edition), 1996, 451, p471-2, 525
Click to expand...
 
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