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Precipn with Sodium Carb?(acetic dont work) Options
 
killuminati420
#1 Posted : 3/14/2011 6:45:08 AM

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I found an old STB jar thats been sitting around for months actually...and i pulled the naphtha that was in there and added some vinegar to the naphtha and shook the hell out of it.

There is some emulsion but it is slowly settling out and the vinegar went kinda cloudy and a tiny yellowish and made the naphtha a bit more translucent yellow color.

My question is...instead of evaporating the vinegar for acetate, can a solution of sodium carbonate water be added to the vinegar instead to precipitate freebase? Im about to try it right now as a test.

It'd be nice if someone could tell me it doesn't work before i try it.
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killuminati420
#2 Posted : 3/14/2011 9:12:47 AM

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Damn this forums real slow...so i seperated the vinegar from the naphtha. And right now i have the option to evap the vinegar or to precipitate it out by adding a base to the vinegar. In this case i am asking...which base should i use for precipitating freebase from vinegar?

I am thinking of using sodium carbonate water with ph10-11 or would i need a higher ph than 10 or 11 to precipitate DMT? Could someone plz give some advice that'd be nice. Im about to just go ahead and use sodium carbonate water to see if it precips it out.
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endlessness
#3 Posted : 3/14/2011 9:46:09 AM

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lye, and if you want, wash/purify later to remove lye traces, but dont use sodium carb now (or do it and confirm/disconfirm my experience)

Ive already tried precipitating like this with sodium carb and it doesnt work. It works with FASW water but not with vinegar, at least in my experience, I tried twice.. With lye people had success..

Let us know how it goes.

Btw, you want pH higher than 10, yeah.. at least 11.
 
killuminati420
#4 Posted : 3/14/2011 6:30:10 PM

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I added sodium carb water to the vinegar and nothing happened. So i added a solution of NaOH and it instantly went cloudy and precipitated..Its been "precipitating" in the fridge over night. But i added the NaOH along with some sodium carb...what does that do?

I went for a 2nd pull on the same STB jar and did a 2nd vinegar salt and the 2nd time i used only NaOH water to precip and that one precipitated real good. So i got the 1st pull with hella sodium carb in it along with precipitate from the NaOH water. And the 2nd vinegar pull just had only NaOH solution added to it and that one is precipitating nicely.

Shouldn't there be no lye traces now that i neutralized it with vinegar? I read that when sodium hydroxide and acetic acid is mixed it produces "Sodium Acetate"...so is there really actual lye traces in the precipitate? Or is there just sodium acetete, H2O, and freebase dmt.

I'll still do a wash on the end product but im pretty sure there is only sodium acetate impurities in there and not just lye or just acetic acid.


...Im going to leave both pulls in the fridge for as long as i can. Is 2-3 days good?
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Entropymancer
#5 Posted : 3/14/2011 6:42:05 PM

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Stoichiometry is crucial. There is no lye left if you neutralized it with an equimolar amount of vinegar... but in that case the pH of the solution would be neutral, not alkaline, so you wouldn't see any precipitation of DMT. Also be aware that sodium acetate can precipitate if you exceed its solubility limit (a bit less than half a gram per milliliter).

Out of curiosity, why are you salting your pulls with vinegar? Why not just evap the naphtha to saturation and freeze-precip?
 
killuminati420
#6 Posted : 3/14/2011 6:59:20 PM

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LoL dont ask me that now...this was more of a test than trying to get yield...next time i will use FASW and precip with sodium carbonate

I know that on the the 2nd vinegar pull, the one without the sodium carb in it,...i only added a tiny splash of NaOH water and it precipd immediately. There is way more vinegar then there is lye since i only added a tiny splash and it instantly worked.

No matter what, im still doing a re-xstal on all of it in the end so it doesn't really matter. Its just cool that i found an OLD stb jar and did a little experiment on it and actually yielded some D from it.

Next time i will use FASW to salt and sodium carb to precip. Since both fumaric acid and sodium carb are more environment/food safe that'd be a nice experiment.
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Entropymancer
#7 Posted : 3/14/2011 7:03:42 PM

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killuminati420 wrote:
I know that on the the 2nd vinegar pull, the one without the sodium carb in it,...i only added a tiny splash of NaOH water and it precipd immediately. There is way more vinegar then there is lye since i only added a tiny splash and it instantly worked.


It sounds to me like what you're saying here is that something precipitated after you added the lye while the solution was still acidic. If that's the case, then the precipitate wasn't DMT; the solution would have to be alkaline for DMT to precipitate. Do you have litmus papers or a pH meter to confirm the pH of the solution?
 
killuminati420
#8 Posted : 3/14/2011 7:23:29 PM

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Well when i added the lye water to the saturated vinegar it instantly turned cloudy and started precipitating crystals in the bottom of the jar it was in. Right now i got it draining through a coffee filter to catch all the precipitate.

After its done filtering i will test the PH of the solution it crashed out from. It should be alkaline or how else could it have precipd? It smells real fishy just like freebased alkaloids.
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killuminati420
#9 Posted : 3/14/2011 10:38:42 PM

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The precip came out to be a shitty brown goo that im going to put back in my exhausted stb jar to go for a 3rd pull to do a normal evap. And a couple sodium carb water washes before the evap to get rid of any impurities.

This was just a test to see if sodium carb would precip from vinegar...it does not. Like Entropymancer said, it cant be done. Next time i will try with fumaric acid and sodium carb and see what happens. I need to order some MHRB to do some tests
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endlessness
#10 Posted : 3/14/2011 10:50:13 PM

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Yes as I said before this has been tested, both that the vinegar doesnt work but that using fumaric acid solution it does. Doing FASW pulls and adding sodium carb to that to precipitate crystallize dmt freebase out of water is known to work, check BLAB last conversion steps for pics and instructions.
 
killuminati420
#11 Posted : 3/15/2011 2:21:45 AM

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Well i cant wait to order some MHRB to try that FASW and sodium carb extraction
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killuminati420
#12 Posted : 3/15/2011 8:11:00 PM

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Will sodium carb work to precipitate freebase from a DMT citrate solution in lets say grape or lemon juice? Would that work?...Im just trying to think ways to get freebase but with food safe chems.

Fumaric acid is pretty food safe so im not trippin. Where do i get it? Its in some grape drinks and such so if its drinkable its food safe and i'll use it to salt my food safe solvent.

But will sodium carb work with citric acid solution? Can sodium BI-carb be used to precip from FASW or does it have to be sodium carb?
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endlessness
#13 Posted : 3/15/2011 8:54:48 PM

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You know you can make sodium carbonate from bicarbonate? It wont have any non-foodsafe impurities, if you start with foodsafe sodium bicarb.

I dont know about precipitating dmt from citric acid solution, but if its something as impure as grape/lemon juice that is used to salt, even if with the pure acid it could work, it could be that with the juice impurities it interferes with crystallization.

Fumaric acid can be gotten foodsafe, check suppliers section

So can lye, by the way, be gotten as foodsafe, but its still gonna be caustic.
 
killuminati420
#14 Posted : 3/15/2011 8:59:57 PM

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Ya thats how i make my sodium carb by heating Baking Soda in the oven at 300F for 2 hours. Forget about the citric acid idea...i'd rather go with fumaric. And yes i have pounds of 100% food grade lye that i ordered awhile back.

I ordered a shit ton so i wouldn't have to order it again.
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Apoc
#15 Posted : 3/23/2011 6:58:12 AM

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hmmm, so killuminati says that adding lai to acidified water results in preciptation? So then, what if you're doing an A B? Wouldn't stuff precip just from adding the base part to the tea?
 
alzabo
#16 Posted : 3/23/2011 7:55:41 PM

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^I think that's the theory behind wanderer's experimental method;
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Quote:
Yes as I said before this has been tested, both that the vinegar doesnt work but that using fumaric acid solution it does. Doing FASW pulls and adding sodium carb to that to precipitate crystallize dmt freebase out of water is known to work, check BLAB last conversion steps for pics and instructions.


Is there a theory on why precipitation happens from a solution with fumaric but not acetic acid?
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Apoc
#17 Posted : 3/24/2011 4:47:51 PM

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alzabo wrote:
^I think that's the theory behind wanderer's experimental method;
*Water Only* Tek -- Successful! And Super-Duper Easy Smile No Acids or Solvents w/ Pic


I see. Upon further reading, I learned that the solution has to be quite pure for any significant amount to precip (ie: just water + dmt. It won't work well with a tea), and also it takes days for good amounts of precip to form, where the usual thing in most extractions is to add the solvent shortly after basing the liquid.
 
 
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