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q21 failure - help find the error Options
 
Enoon
#1 Posted : 8/22/2010 10:40:48 PM

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So SWIM tried a q21 extraction.
Materials were as follows: ~150 g MHRB, Vinegar, lime, limonene (95%) / pure orange oil from orange peels, Fumaric acid, IPA, sodium carbonate (washing soda)

Followed the tek as written, I think. Shredded bark, added vinegar, added hot water, added lime until consistency was like thick mud, pretty chunky, like in the pics.
Put the limo in, stirred, pulled after ~ 1h.

Limo was kind of opaque which SWIM didn't really notice at first. SWIM put in the FASI and nothing happened. At least SWIM couldn't see anything happening. SWIM added about 150ml of FASI to maybe 250ml of limo and let it sit for some 20 hours or so.
The limo cleared and there was a rather fluffy emulsion layer, but no crystals. SWIM took off most of the clear stuff and checked to see if anything would precipitate out of it if more FASI was added - nothing.
SWIM let the fluffy stuff sit for a while longer, tried freezing it, but nothing had any effect on it.
SWIM decided to filter it and got as a result what looked like brown mud in the filter and beautifully clear limo/FASI mix.

SWIM didn't think this looked anything like what it should look like. Rather it looked like lumps of MHRB powder stuck together. SWIM tried redissolving the stuff in water, but it would not dissolve. SWIM filtered the water off again, thinking if there were any fumarates in the mud, then they must have gone into solution, so SWIM tried to freebase them using sodium carbonate, but again there was no clouding, nothing precipitated.

Yield = 0...

So - where did SWIM go wrong?

Honestly, the quality of the bark is questionable, since SWIM got it from shayana, and has heard of no one ever buying it from them. Also at least 1/3rd of it couldn't be properly powdered because SWIM's blender died. SWIM cut it up by hand (resulting in many blisters) and tried grinding it with a mortar, but this didn't work very well, meaning the powder was fairly coarse.
Otherwise the chemicals are what they say they are, I would guess. SWIM even tried a second pull and tried filtering the opaque limo that came from the pull. No precipitation whatsoever. No clouding when FASI was added.

Can anything be done with the brown mud that SWIM still has lying around?

Would appreciate some insight so SWIM's next run won't go quite as south as this one... Smile
Thanks
Buon viso a cattivo gioco!
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mushroom-grow-help ::: energy conserving caapi extraction
 

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dreamer042
#2 Posted : 8/23/2010 12:11:08 AM

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ok lets see if I can outline this here and make some kind of semblance of sense:

first you shredded the bark
then you added vinegar to the bark (this was the mistake you can't acidify for semi-dry tek)
then you added water (this step was too soon)
then you added lime to make a thick muddy goop
then you pulled with limonine and attempted to salt out with fasi

this is how the process should be done:
shred the bark
*completely eliminate the acidification step its unnecessary*
mix ground dry bark with lime
add water to make a thick goopy mud and give an hour or a few so the lime can react with the bark and freebase the molecule.
pull from the mud several times with limonine and combine pulls
salt out from limonine with fasi and collect dmt precipitate

When you added the vinegar to the bark the molecule was converted to an acetate salt
when you added the lime after said conversion the extra water and vinegar kept the molecule as a salt and prevented the lime from raising the ph of the goop high enough to freebase the molecule, thus when you added the limonine it collected only the plant fats and oils and things that were soluble in a non polar solvent while in the acid state leaving behind the acid salted molecule in the bark mud/goop.

I hope that makes sense

now I'd say your best course of action is to mix the goop with water until a liquid consistancy and no longer goop if possible, then add sodium carbonate (less preferred) or lye (much more reliable) to the goopy water and pull again with your limonine then you can salt with your fasi and enjoy your goodies
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Enoon
#3 Posted : 8/23/2010 12:47:39 AM

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thanks so much, SWIM's on it and I will report, though somehow I have my doubts (not concerning your proposition but SWIM's barks capacity to yield...). What you say seems plausible, meaning SWIM should have had to add much more lime to get it to work properly?
Anyway, NaOH is added and doing it's warming up thing as I type this and SWIM will see what limo can do in the morning.

cheers and good night.
Buon viso a cattivo gioco!
---
The Open Hyperspace Traveler Handbook - A handbook for the safe and responsible use of entheogens.
---
mushroom-grow-help ::: energy conserving caapi extraction
 
ragabr
#4 Posted : 8/23/2010 1:30:00 AM

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dreamer042 wrote:

then you added vinegar to the bark (this was the mistake you can't acidify for semi-dry tek)
then you added water (this step was too soon)

Incorrect, read the tek.

SWIM had a similar issue, she added too much water in acidification and didn't have enough lime on hand to thicken the solution up. Somewhere else in the forums, she read that too much water actually allows lime to move into the d-limo. This was probably the cloudiness you noted before. Since she had no more lime, she based further with lye, but normally it wouldn't have been necessary. Someone more familiar with Q21Q21's tek could probably provide further information.
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Enoon
#5 Posted : 8/28/2010 2:28:32 PM

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So.. in order to save her stuff SWIM followed dreamer's (and others-from-the-chat's) advice and tried to make it into a jorke's limo tek by adding massive amounts of lye and doing a few limo pulls. After the mixture got really warm and then cooled down again SWIM added some limo and let it sit for a few days (was busy with work etc.), pulled, added more limo and pulled after another day or so.

SWIM followed jorke's tek using FASW instead of FASI this time, gathered the watery layer as best she could using a pipette, and finally evaporated the gathered water (after one short filtering step to get the residual limo out). Yield: ~380 mg DMT-Fumerate.
Given the fact that SWIM had done lots of other stuff to the poor bark first, and that probably only around 70g of it was actually powdered, SWIM's satisfied. She is going to try and convert it to free base now.

So why didn't q21q21's tek work? I'm guessing the ratio of acid/base after the first few steps wasn't right, meaning it was not basified enough to get the goodies out of the bark. SWIM might have added the limo too soon as well, though she doesn't think that was the main problem. The mix was also a bit too liquidy for the tek. But then I'm really just guessing.

SWIM hopes the conversion will go well but in case it doesn't she will only use half of it at first.

Breathe well
Buon viso a cattivo gioco!
---
The Open Hyperspace Traveler Handbook - A handbook for the safe and responsible use of entheogens.
---
mushroom-grow-help ::: energy conserving caapi extraction
 
ayahuascan
#6 Posted : 8/29/2010 1:00:35 AM

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sorry to hijack,
swim has two related question.

would mixing mhrb powder with lime in the blender, then adding water work?
and how long would it take for say a 100g stash to freebase with stirring?

thankyou
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ubu
#7 Posted : 9/10/2010 5:23:32 PM

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ayahuascan wrote:

would mixing MHRB powder with lime in the blender, then adding water work?


Well, q21 is an A/B tek and it is pretty clear about the acidification being done prior to basification step. So, I believe q21 tek already answered your question:

q21q21 wrote:

-Take 10g-200g or more powdered MHRB and place in your container.

-Add vinegar to the bark and stir until the bark starts forming clumps. Add enough so most of the bark is wet, red and clumpy.
Then add near-boiling water and stir it around until it is wet enough to flow when you tip the container to one side or the other. (Aproximately: 100ml vinegar and 100ml near-boiling water for 100g MHRB)

-Stir several times as the bark is let to sit for 20-40 minutes. (Longer won't hurt though)


But why not give a try? Mix MHRB powder with lime and tell us what happens. There is an interesting discussion about mixing lime with the powder versus mixing lime with the aqueous acid solution.

ayahuascan wrote:

how long would it take for say a 100g stash to freebase with stirring?


q21 tek doesn't suggest an exact time for stirring but it is clear about the consistency to be obtained. So, just give a try and soon you will discover:

q21q21 wrote:

Start stirring and it might get a little dry, stir very well first, if it is still dry add some boiling or hot water a TINY TINY splash at a time, stir well and repeat adding until it is moistened throughout
The ideal consistency is moistened throughout but thick enough to make a hole in the middle.


In Ubu experience just a few minutes stirring are necessary to obtain the suggested consistency.
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