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where did SWIM go wrong, which approach would you suggest for SWIM's next extraction Options
 
dziga
#1 Posted : 8/8/2013 6:17:43 PM
Hello dear DMT-Nexus community.

SWIM has done a lot of research on this web page in order to achieve his own MHRB DMT extraction.

Nevertheless, after three failed attempts he can not figure out where the problem lies.



So SWIM decided to share his experience (hopefully not annoying the more experienced users asking for what could be an obvious explanation) in order to gain further insight and some possible ideas for an alternative approach for his 4th extraction.

So. The first two extractions were STB extractions using: MHRB, Distilled Water & Hexane.
At that point SWIM did not own a PHmeter and followed instructions on ratios posted on several websites.

FIRST EXTRACTION

After a week of letting the MHRB soak in basified water, he pulled with hexane and then let it evaporate. The result was yellow goo and absolutely no crystals. For this extraction no heat was used. Since SWIM didn't like the result and was worried of impurities, he decided to dispose the resulting goo and did not try it.

SECOND EXTRACTION

Followed Norman's Tek. Did three heated pulls with hexane and tried to freeze precipitate.
Nothing precipitated... Due to external circumstances SWIM had to dispose of the solvent and could not see what resulted when evaporated.

THIRD EXTERACTION

Did an A/B extraction. And probably did several things wrong, and here is where many questions arise, to which he has no answers:

For starters, when heated the 200g MHRB in a crockpot, he only added Vinegar, and no water. (What could this have as a consequence?)

He let his three Vinegar extractions sit overnight and decanted carefully, altough a minimal amount of sludge did make its way through to the next step.
(What could this have as a consequence?)

He then proceeded to defat with three Hexane pulls. One of the problems is that SWIM's separatory funnel has a capacity of only 250ml. So he divided his aqueos (sorry for the spelling) solution into four equal amounts, and for every 200ml of solution he did three times 50ml hexane pulls (which ended in a lot of Hexane being used, almos 1 liter). Now SWIM realizes that Hexane might not be adequate for defatting. Is this true? Would Naphta or Toluene be better instead, if yes, which one of both would be better?

After defatting he proceeded to basify with LYE. The solution turned black and measured 12.9 PH.

He then proceeded to do three warm Hexane pulls. Since SWIM had heard about Warm pulls resulting in a bigger yield, he did not only heat the Hexane, but also the basified MHRB solution before performing each pull.

This procedure took a lot of time, again the small separatory funnel being the main problem. Dividing his solution into four and making three Hexane pulls for each, resulted in twelve heated hexane pulls and a lot of work (about 8 hours).

Afterwards SWIM proceeded to do 1 sodium carbonate (PH9) and 2 tap water washes of his solvent. He then dried it with Epsom salts. At this point the Hexane was completely transparent.

He combined all his pulls and tried to freeze precipitate them, with no results. So he then decided to do a partial evaporation, which took really really long. So he decided to heat the solvent in a hot water bath to speed it up until it turned cloudy.

At that point he attempted another freeze precipitation (-23 C), which precipitated one extremely tiny crystal, but expecting to see about 2grams of spice, SWIM decided this was not how it was supposed to be.

So SWIM evaporated the Hexane (for over a week) and got a yellow goo with some brown residue, smelling a lot like DMT.

After reading a thread on yellow goo he noticed a comment by "halcyon" that suggests this might be the result of heating the MHRB basified solution and afterwards heating the Hexane pulls to speed up the evaporation. So the yellow goo could be DMT Oxide. SWIM was able to dissolve the yellow goo in alcohol and is preparing changa (which has not completely dried yet). Altough the brown residues did not dissolve in alcohol at all ( and are odorless, have no dmt smell at all).

So SWIM would like to post a few questions that may give him more confidence towards his fourth extraction attempt:

- Not having added water to the vinegar solution, what consequences could there be?

- What consequences could the minimal amount of sludge that made it thorugh the initiall decanting of the acidic solution have?

- For SWIM's next extraction he would like to boil his acidic solution down before defatting. Is there a limit to how much one can boil his solution down? Should the solvent be still measured in terms o how much MHRB was used?

- Is hexane suitable for defatting, does it work at all for this purpose?

- Even tough SWIM could have converted the DMT to DMT Oxide by heating his solvent, could it not also be that his MHRB was too old and already contained mostly DMT OXIDE from the beginning on? This could explain why SWIM's first two STB extractions turned out so poorly, since Hexane would not be able to extract the DMT oxide from the MHRB. Should SWIM try an extraction with toluene instead?

- {Mod Edit:} Please DO NOT ask for supplier information regarding MHRB see HERE

- SWIM has seen a lot of threads on salting the DMT out of Limonene and Xylene with FASW. Would this also work with any other solvent (Toluene, Hexane, Naphta)?

SWIM appreciates all your commitment to this community, and would particularly like to thank endlessness for his posts which have helped provide SWIM with a great amount of understanding.


 
olympus mon
Moderator | Skills: Tattooist specialized in indigenous art, Fine art, medium ink and pen.
#2 Posted : 8/8/2013 8:08:03 PM
O boy.
For starters I would recommend stop throwing out perfectly good dmt! Everyone often feels if it aint purty perfect crystals then they must have this or that oxide ext. Its often not the case and they have perfectly good dmt that simply contains fats which personally I much more prefer.

Back in the early days dmt wasn't such a pretty thing. It was gooey, red or brown, yellow beige, waxy, sticky and sometimes sand like. Its all the same dmt. Especially considering your making changa from your extracted spice don't worry about how it looks other than heavy impurities but your description doesn't sound that bad at all. Yellow, imo never a problem, brown to dark brown, well yea you probably have a bunch of bark powder in there that should come out in a clean up re X. What matters is does it work or not and id bet my right arm the dmt you tossed was perfectly fine.

Acidify, basify, pull. Keep it simple the more steps and you add the more things that can go wrong but NEVER...NEVER discard your materials until the cows come home every last one. Dmt doesn't just vanish into the ether its in there somewhere and as long as you don't throw things out you can always extract it. I have never once done any thing other than acidify, basify, pull. No de fatting is needed unless your really wanting freebase white crystals and even then just do the q21 tek since that has never made me anything but perfectly white crystals and imo is the easiest extraction. It seems to have a lower yield than a/b teks but can be tweaked to get more outta it for sure.

I may not address every question you have but will throw you some pointers that I think can solve your riddle.

Is there a reason your working from just a vinegar solution? Why not use acid soaked bark? Add enough vinegar to make a mud like mush and let sit for a day or 2 then add your lye and water to that. I use .75-1g lye per g of mhrb. 800ml is a LOT more vinegar than you would ever need to use and can make it harder to get your ph up to 14 which by the way is optimum for converting dmt to freebase form. It needs to be at 14 to convert all the dmt to freebase and be pulled into the solvent. So because your using so much vinegar you need to use more lye to adjust the ph to 14.

Your using entirely too much hexane and this is making it impossible for it to freeze precip for sure. I'm surprised you even got the one crystal you did with that much solvent. If I understand you correctly your working with 800ml of vinegar and 600ml heptane. That is not necessary but don't not despair you can get this extraction back on track.

If your not wanting jungle alks and fats in your dmt then stop using heat period till maybe the last final pull. Time trumps heat every time and heat pulls far more fats and jungle alkaloids so don't make your life harder than need be. Also the brown stuff you speak of, was your solvent tinted? Did it look like tea or black coffee? If so its probably ultra fine particulates from vendors overly powderizing their bark. This has been driving me crazy lately since the stuff is too baby fine and gets into the solvent causing brown dmt that needs to be cleaned up. Sounds like you got some bark particles when you decanted and then into the heptane so when evaporating it was left behind in the dmt. Just Re-x it.

Mate I highly doubt you have dmt oxide. That gets thrown around too much IMO and its never been the case for me and I have extracted kilos and kilos of bark. You probably have dmt, fats from using heat, and some bark sediment from improper separation. Next time do a re x and get the dirty stuff out before you make changa.

Next time keep it simple. Add vinegar to your bark and make a mud then leave to sit for a day or 2. Add lye water solution to mud. Pull with solvent. For 200g bark Id say max 100ml per pull. Evap with a fan partially then put in freezer. Claim your Xtals and re use the solvent. Evap all solvent when done with all pulls. The end.

Hope that helps. Sitting here waiting for a train this gave me something to do so thanks.

I am not gonna lie, shits gonna get weird!
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endlessness
#3 Posted : 8/14/2013 10:29:06 PM
Oly mon already said a lot of good things.

Indeed please don't throw away goo. When you get goo next time, just recrystallize it by adding small amount of warm solvent to dissolve most of the go, maybe leaving a little bit darker undisslved stuff, and then freeze precipitating it.

As for using vinegar only, that wouldn't prevent you from having good yields, but its just wasteful. Vinegar is already somewhat dilute acetic acid, but to not waste that much vinegar (and lye to neutralize it later), better just use a dash of vinegar to your water solution.

Forget defat, even if you want white crystals, defatting is completely unnecessary specially in the case of mimosa.

You need to adjust your amount of hexane per pull for your mimosa. The ratios are written in the FAQ

Also maybe get a bigger separatory funnel (I say go for 2l already, or at least 1l), because otherwise I think it might be even easier to just use a pipette to pull your solvent layer up instead of using the small sep funnel.

Personally I like working with A/Bs, but STB is fine too, whatever you preffer. A bit of sludge coming into the A/B wont have much consequence at all, at most it will be something that blocks your separatory funnel...

As oly said, I doubt there was any n-oxide there, probably just DMT goo that needed to be recrystallized or at least moved around, scrapped and rescrapped till it dried properly into a wax.

By the way, if you're using hexane, I recommend turning pH a little bit higher, like 13.5-14, it will help increasing yields and diminishing chances of emulsion.

Oh and, how well did you mix each pull to the basified solution? Sometimes low yields are result of improper mixing of solvent with polar layer.

Hope that helps a bit more.. If there are any further questions, let us know.
 
 
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