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Complete extraction (Q21Q21) with sunflower oil and vinegar (pics and description) Options
 
smuggelr
#1 Posted : 1/23/2014 11:43:56 AM
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SWIM used Q21Q21 Vinegar/Lime A/B Extraction Tek no.1 with slight modifications. Instead of d-limonene SWIM used sunflower Oil and did a sodium carbonate wash prior to the Acid wash/Salting.

Special thanks go out to Parshvik Chintan, who patiently answered all of my noob-questions.

Ignore the dates on the pics. Solvent means oil.

Step 1 (Acidification)
-Pour Mimosa hostilis root bark powder (50g) in glass container
-Add about 50g of Vinegar till wet red and clumpy
-Add about 50ml of near boiling Water, till it can flow when you tip the container to one side or the other.

-Let sit for an hour with stirring every 5 Minutes

Step 2 (Basification)
-Add lime bit-by-bit with mixing in 3 to 4 ratio (37,5g)
-Add teaspoons (5 in my case) of water to reach thick oatmeal consistency

-Let sit for 24 hours

Step 3 (Non-polar Wash)
SWIM did three pulls, the first after 24 hours, the second after 48 and the last after 7 days.
For every pull:
-Added 100 ml of sunflower oil mixed periodically for 20 minutes.
-Poured out the solvent

First Pull:


After Last pull:


SWIM noticed, he had to much residue, so he filtered the solvent, using a piece of cotton in a big (100ml) syringe. SWIM would not recommend it, the cotton absorbed part of the solvent and didn´t filter very good after it absorbed it.

Without the residue (sorry for the quality):


Step 4 (Sodium Carbonate wash)
-Take lukewarm water in 1 to 4 ratio to the solvent (In SWIM´s case about 40 ml Water to 160 ml solvent)
-Add half a teaspoon of sodium carbonate (washing soda)
-Add the solution to the solvent and mix vigorously for 5-10 seconds

At this point the solvent became cloudy and only a very little part of the sodium carbonate solution was at the bottom, so SWIM added a few pinches of normal kitchen/table salt. The layers separated a little bit.

-Pour of solvent

This is how the solvent looked after being poured of:


Step 5 (Acid wash/Salting)

Repeated 3 times:
-Add a shot-glass-full of vinegar
-Agitate the container
-Wait 4-8 minutes
It looked like this:

-Suck out layer of vinegar
-Added shot or two of hot tap water and agitate it for a minute
-Suck out layer of water and add to the vinegar

SWIM added the pulled of vinegar and water straight to a pot

Step 6 (Evaporation)
-After adding the results of the salting to a pot, SWIM just boiled it in a pot, till there was a dmt-crust and scratched it off.

This is the result:



SWIM appreciates every comment, critique and so on and has one question (as a beginner): Was the sodium carbonate washing really necessary? What did it do?

EDIT: SWIM just noticed, is his product smokable DMT? Because it isn´t hard and looks more like DMT Fumarate:

(this is not SWIM´s result, this is a pic of DMT-Fumerate from the wiki)

Would you recommend doing this Conversion with half of everything, since SWIM has about 2grams?
 

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Mimosa_Man
#2 Posted : 1/23/2014 11:50:06 AM

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Sodium Carbonate washes are commonly used to make sure your spice is free of whatever base you added to the mixture.

As for the necessity it depends on each individual batch that is made.
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Parshvik Chintan
#3 Posted : 1/23/2014 5:46:01 PM

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Thumbs up
looks good.

one thing i have noticed is that if you put the oil in the fridge during the sodium carbonate wash, the layers will separate a lot faster.
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CHANGA IN THE BONGA!
 
smuggelr
#4 Posted : 1/24/2014 11:05:20 AM
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I did this conversion exactly as described, only with half of everything, since I only had half of the fumarate.
After 5 minutes in the freezer the DMT still didn´t crystallize. After half an hour in the freezer it looked like this:

The darker liquid seems to float on top and on the rim, not like a full layer and it is very liquid.

By now it is more or less frozen and looks like this:

I assume the sodium carbonate and a little of the dmt-fumarate-water soultion froze, but there is still liquid on top, that should have formed crystals.

What should I do?

I know I´m getting on your nerves, but I finally got the fumarate and now now it seems like I wasted it.
 
YargPirate
#5 Posted : 1/24/2014 8:27:01 PM
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I don't think you are wasting anyone's time, you are working with a -very- uncommon method. So don't worry.

I know that I am glad to see and read about your workings with sunflower oil. I think your write-ups will help a lot of new people to try out this method.

I don't think you had dmt fumarate though, unless you used fumaric acid instead of acetic acid(vinegar).

I can't be of much help with your freebasing step, but as long as you keep your material, you won't ruin anything. Hopefully someone can chime in on how to help you.Razz
 
dreamer042
#6 Posted : 1/24/2014 9:29:58 PM

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After doing the q21 tek with the vinegar you final product should have been a freebase or at least a partially freebased mixture of DMT acetate and impurities that may have been present in your vinegar. It may look like DMT fumerate, but it's not and that is why the conversion tek for fumerates didn't work as expected. That's gonna be kinda tough to recover you may just wanna thaw it out and pull it back into a nonpolar solvent and salt it out again.

With the other half you want to mix it with just a tiny bit of sodium carbonate and moisten it up with some water to make a paste, allow it dry and powder it then pull it into alcohol, decant and filter the alcohol really well and you'll have pretty pure dmt freebase.
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smuggelr
#7 Posted : 1/25/2014 1:20:46 AM
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@YargPirate
thanks for the kind words, I hope my experiences will help others, too. But I ask questions at literally every step of the tek, so I felt a bit like a little child trying to do something it doesn´t understand.

@dreamer042
Thank you, you´re a savior. I will do that and report back with the results. But it may be a while (I wait for the alcohol to be delivered).
 
Parshvik Chintan
#8 Posted : 1/25/2014 6:20:52 AM

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dreamer042 wrote:
After doing the q21 tek with the vinegar you final product should have been a freebase or at least a partially freebased mixture of DMT acetate and impurities that may have been present in your vinegar.

i believe benzyme mentioned something about q21q21's method of freebasing as not actually converting it to freebase.
im not sure how positive he was that it was ineffective, i think that would be best answered by the man himself, but i always noticed a differenced after doing the paste-n-pull freebase conversion.

also i noticed my jim-jam from q21q21 was water soluble, so that seems to indicate it wasn't freebased prior to conversion.
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CHANGA IN THE BONGA!
 
DreaMTripper
#9 Posted : 1/25/2014 8:50:11 AM

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The sodium carb wash will have dragged out some of the gunk from the oil back into the water section as the idea is to clean the solvent and separate it from the freebase so if youre going to salt out then the oil is a good place to leave behind any impurities. You then rebase in a now clean solution and pull again resulting in only the alkaloids being present in the solvent.
Freezing is a good way to get rid of the last bit of oil but other than that will just cause complications as I believe sodium carbonate will precipitate out and crystallize around the dmt.
If you have patience you could let it thaw out slowly in the fridge allowing the sodium carbonate to eventually redisolve in the water then leave it in the fridge and see if the dmt precipitates. But if theres a layer of oil that could stop it hardening into a wax on the surface.
I dont see why the dmt wouldnt be in freebase form if the solution has a pH of 11+ but im no expert.
Its a good salvage to repull in a nps then salt out again then evaporate to a goo and paste and pull or alternatively try a slow water crystallization.
If you paste and pull watch you dont burn it when reducing the liquid the less volume of water the better as it means less sodium carbonate (when its dry a hammer is a good way to powderise it) Consequently less IPA and therefore a much more condensed extract rather than just a microscopic layer spread across the dish.
Im sure you will have a very clean product after the steps you've done it may take a bit longer yet but Im sure youll be proud of the result!
 
smuggelr
#10 Posted : 1/25/2014 11:26:17 AM
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I am going to do what dreamer042 said. I pour off the top, make a paste and dry it and with the rest I will pull it back into a nonpolar solvent and salt it out again. I like to have two options, so when one fails, the other might work.

For the next time. Would it be better to put the results of the q21 tek in IPA, filter and let it evaporate? Would it then be freebase?
 
endlessness
#11 Posted : 1/25/2014 12:44:32 PM

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if you mix the acetates from vinegar salting evap, and mix with sodium carbonate and a bit water to make paste, let dry, and pull with IPA, then you`ll have freebase.
 
smuggelr
#12 Posted : 1/25/2014 4:52:06 PM
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So,
I poured of the top, made a paste and let it dry. It looks wet, but it will be dry by tomorrow.
(I coulnd´t get a good picture, but I figure that should be enough)


I thawed the rest, added about 100 ml of sunflower oil, let it sit for about 15 minutes.
(cloudy) Oil on the left, thawed sodium solution on the right:


Then did the salting. Just for the protocol:
Repeated two times:
-Added 20 ml of vinegar, agitated, waited 7 minutes, sucked out vinegar with turkey baster, added to pot
-Added 20 ml of hot tap water, agitated for a minute, then sucked off and also added to pot

Then boiled pot contents:


After a short while:


Result (about 4 grams, but mostly not DMT I would say):


So my next step for both is to pull with IPA?
Does Pull mean mix IPA (how much?) with both powders, wait (how long), pour IPA off and let evaporate?
 
Parshvik Chintan
#13 Posted : 1/25/2014 5:45:37 PM

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yea, the sodium carbonate is insoluble in IPA (unless there is water in the alcohol, as it would be soluble in water), but dmt is, so you are dissolving the dmt into the alcohol, separating it from the sodium carbonate, and evaporating the alcohol; leaving you with dmt.
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smuggelr
#14 Posted : 1/25/2014 8:39:31 PM
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I will have 99,5% isopropanol, so I also will have 0,5% water and 0,5% sodium carbonate in my final product. Could these 0,5% of sodium carbonate damage something, when smoked?
 
DreaMTripper
#15 Posted : 1/26/2014 6:27:12 AM

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You can dry the IPA first by pouring it into a glass jar addding sodium carbonate to absorb the water then decant the IPA away.
Or you could dropper wash the final extract with cold distilled water to remove the sodium carb although it may well have hardened and co-crystalized with the extract by then rendering it unvapeable.
Burn some see what happens it just blackens and turns to soot (carbon?). Not good for an extract or your lungs.
I recommend pulverising that now dry paste it looks very flakey.
 
smuggelr
#16 Posted : 1/26/2014 10:13:22 PM
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I will probably have the IPA in two days, I will report back.

I´m just curious, why does my acetate looks this:


If I would have stopped cooking earlier it would not be gooey at all. The transition was like immediately liquid to pulver.
 
smuggelr
#17 Posted : 1/29/2014 9:57:17 AM
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So,
the dried up top liquid looked like this:


The dried up result of the salting of the rest like this:


Mixed with 99,5% IPA:
top


rest


Poured off through coffee filter:


I poured the IPA in two plates and left them on a radiator.
After a 20 hours it looked like this:



and this:



It was very gooey and wet. I noticed, that everytime I heat something in a pot, it results in powder (more or less). So I mixed the gooey stuff with IPA and poured in in a pot. I let it simmer on the lowest heat:


But the results were goo again:


Can I smoke it this way? And if not, how do I get it into a smokable form?
 
DreaMTripper
#18 Posted : 1/29/2014 10:26:54 AM

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Did you disolve the result of the salting into IPA and evap? Its still in a salt form so isntin the best form to be smoked. Although some people have said they've had success smoking dmt acetate..
The way to do paste and pull is to mix the goo into sodium carbonatate before the IPA youve missed out a major step that is the freebasing.
See the wiki ....
https://wiki.dmt-nexus.m...p_6-Acetates_conversion

and Type 3 - Sodium Carbonate Paste and Pull method

https://wiki.dmt-nexus.m...Freebase_Conversion_TEK

Good photos by the way and your extract now looks nice and clean just the freebasing to do.



 
smuggelr
#19 Posted : 1/29/2014 10:32:07 AM
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I am 100% sure I did the freebasing step with the top one, I just forgot to mention it, because I did it some days ago. But the results of the pulling and evaping with IPA looked the same, so I think I did the freebase step with the rest too.

Should I repeat it maybe?
 
DreaMTripper
#20 Posted : 1/29/2014 11:28:34 AM

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Im confused your picture sais
" The dried up result of the salting of the rest like this:"
Then you say you dissolved that in IPA.

If it has been mixed with sodium carbonate before dissolving in IPA then its now in a smokeable form and if you evapped on a radiatior it results in goo and may not crystalize.
You would have to freezeprecip to get crystals or a slow water precipitation with minimal distilled water.
 
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