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acid/base tek + fumarate end product Options
 
tspirit
#1 Posted : 9/4/2008 4:23:01 AM
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hi all, i was looking for comments on a combination of techniques aiming directly for dmt-fumarate end product (no smoking here):

- cover mhrb powder with distilled water + HCl at ph 2, stir well
- let sit 20 mins, filter water, repeat water extraction 2 more times
- boil water down to 1/3 or 1/4 of original volume
- basify water with NaOH to ph 12, add naphtha
- mix, let sit until separation, remove dmt-laden naphtha to container
- add fumaric-acid-saturated anhydrous acetone (FASA) to naphtha, dmt-fumarate will (eventually) precipitate, collect crystals
- wash naphtha with water to remove fasa
- re-add naphtha back to basified water to extract then precipitate more dmt as many times as desired

here are some positives i've thought of concerning this tek:
- much lower chemical requirements - water + concentrated acid are cheap 1st steps, then boiling down reduces base + naphtha requirements
- neither naphtha nor acetone will dissolve dmt-fumarate, so fats/impurities that are pulled into naphtha from the basified water aren't much of an issue
- nice and fast! all you're waiting for is the water to extract dmt, the naphtha/water to separate, and the dmt-fumarate to precipitate - no evaporation! each pull of water could be boiled down and naphtha-ized concurrently also (pipelined)

negatives:
- any other alkaloids that form fumarate salts will end up precipitating out with the dmt into the final product. some people may like this, some may wish to basify, extract as freebase and freeze-crystallize for purity
- we can't easily reclaim the acetone. oh well? and we'll have to use more acetone to wash our fumarate crystals too

unknowns:
- how long should the acid extraction stage take? how ph-sensitive is it? does it matter as long as it's anywhere from 1 to 3?
- dmt-hcl's melting point is around 167 degrees C i believe, so there's no harm in simmering the water to speed evaporation, right?
- how much crap is likely to precipitate out of the naphtha + fats + acetone + fumaric acid combination in addition to our dmt? how washable is dmt-fumarate of these impurities?
- how readily will the acetone and naphtha keep the extra un-needed fumaric acid dissolved? if the dmt ends up with too much dried fumaric acid, it could easily be washed away with acetone washes, right?

i know i'm probably missing a lot of things here, my main reasons for writing out a tek were to minimize cost (the smaller the chemical amounts the better), eliminate evaporation steps, and get long shelf-lifes (fumarate). yield can be increased by repeating the most important step, which is also luckily the cheapest, the acid-water extraction.

i know it's hardly a newbie's place to start rattling off like this, but i really really love having theories torn apart, it's definitely the fastest way i've found to learn. so please, have at it Smile
 

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amor_fati
#2 Posted : 9/4/2008 4:59:08 AM

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Well, I'm not sure how important or useful the HCl evap step is. Is it even safe to evaporate HCl?

I would imagine that the acetone used for washing could be reused as FASA.

I'd throw in a xylene/toulene pull for good measure though. Hell, if you don't mind jungle-spice in your product, use xylene/toulene for all your pulls; you could easily separate it later if you ever freebase it. Save your naphtha for crystallizing freebase.

Seems valid overall. This is pretty much how I was planning to do future extractions.
 
tspirit
#3 Posted : 9/4/2008 5:35:01 AM
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yeah evaporating hcl, especially starting with such a low ph, does worry me somewhat. if not done outside, the acidic fumes may damage whatever vent is being used. though i suppose having more water really only means we have to use more lye to basify it, the volume of toluene/xylene/naphtha needed doesn't really change much since we're just re-using it via washings. i just don't like dealing with any quantity of lye, quite honestly. i suppose a higher-molecular-weight acid could be used, like citric or just fumaric since we'll have plenty of it regardless. they won't evaporate off, and will be filtered out by the naphtha wash of the base. fumaric and citric acid are, best of all, CHEAP.

nice catch on the acetone wash being used for fasa! i didn't think of that at all, what a waste that would have been.

i'm very very new to dmt. is there any reference for the different focuses of toluene/xylene/naphtha? i assume naphtha is more selective when it comes to dissolving actives, with xylene/toluene pulling additional stuff out (i remember reading that toluene extracted jungle spice from supposedly-dmt-exhausted mhrb). for some reason i'm having a lot of trouble finding toluene in the south, xylene and naphtha are quite easy to come by. also, are we sure that xylene/toluene won't dissolve our dmt-fumarate at all?
 
tspirit
#4 Posted : 9/4/2008 7:48:11 AM
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is the mhrb just an incredibly strong buffering agent? the 'BATE' chemistry calculator gives me (for 1 liter of water), 0.35 grams of fumaric acid (0.03 mol at pka1 3.03, pka2 4.44) to reach ph 2.88, and then 1.0 grams of NaOH (0.02 mol at pkb 0.2) to raise it up from acidic to ph 12.26.

if that's accurate, the amount of lye people are using is just staggering..
 
DarkShaman
#5 Posted : 1/15/2009 9:10:33 AM

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tspirit wrote:
is the mhrb just an incredibly strong buffering agent? the 'BATE' chemistry calculator gives me (for 1 liter of water), 0.35 grams of fumaric acid (0.03 mol at pka1 3.03, pka2 4.44) to reach ph 2.88, and then 1.0 grams of NaOH (0.02 mol at pkb 0.2) to raise it up from acidic to ph 12.26.

if that's accurate, the amount of lye people are using is just staggering..


No doubt the truth. As someone who prefers STB extractions, SWIM is astounded when reading extraction tek suggestions that, for example, call for up to 1g NaOH per gram of MHRB used. Unless I missed something, it seems that perhaps some take the term "...to a pH of 12 or higher..." to astronomical extremes!
 
Infundibulum
#6 Posted : 1/15/2009 10:40:00 AM

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Hi tspirit,

tspirit wrote:

- cover mhrb powder with distilled water + HCl at ph 2, stir well
- let sit 20 mins, filter water, repeat water extraction 2 more times

First off, one does not need such a low pH. 4-5 will do equally well if not better. And one will get far superior results if the acidic MHRB solution is shimmered/boiled instead of just letting it sit for some time. Do not believe the QT tek.
tspirit wrote:
- basify water with NaOH to ph 12, add naphtha

OK, if one has NaOH, why not go go STB?

tspirit wrote:
- add fumaric-acid-saturated anhydrous acetone (FASA) to naphtha, dmt-fumarate will (eventually) precipitate, collect crystals

Addition of FASA in the naphtha will most likely result in precipitation of the fumaric acid itself. This does not happen when xylene (in place of naphtha) is used. so, it is very likely that one may be collecting fumaric acid crystals, not dmt-fumarate crystals. One should try it for himself; i.e. get some unused naphtha, drop some FASA in it, see what happens.

Quote:
negatives:
- any other alkaloids that form fumarate salts will end up precipitating out with the dmt into the final product. some people may like this, some may wish to basify, extract as freebase and freeze-crystallize for purity
- we can't easily reclaim the acetone. oh well? and we'll have to use more acetone to wash our fumarate crystals too

"any other alkaloids is not a problem; they all add to the experience. If naphtha is used however, there's not much chance for "other alkaloids" to be pulled with naphtha.

Acetone that has been used to wash the dmt-fumarate salts can be reclaimed and used to make more FASA.

tspirit wrote:
unknowns:
- how long should the acid extraction stage take? how ph-sensitive is it? does it matter as long as it's anywhere from 1 to 3?

See above
Quote:
- dmt-hcl's melting point is around 167 degrees C i believe, so there's no harm in simmering the water to speed evaporation, right?

Aye, but do not boil hard, dmt can still get degraded by strong heat.
tspirit wrote:
- how much crap is likely to precipitate out of the naphtha + fats + acetone + fumaric acid combination in addition to our dmt? how washable is dmt-fumarate of these impurities?

Almost none. But there's gonna be residual impurities on the dmt-fumarate precipitates just like residual NP solvent. Acetone washes take care of these pretty well.
Quote:
- how readily will the acetone and naphtha keep the extra un-needed fumaric acid dissolved? if the dmt ends up with too much dried fumaric acid, it could easily be washed away with acetone washes, right?

Yes

good luck with everything!

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