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expanding
#861 Posted : 3/30/2010 11:12:35 PM

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halten wrote:
gammagore wrote:
halten wrote:
SWIM was wondering what to do with leftover naptha after most has evaporated and crystals have formed. They tell me there is maybe 100ml total naptha left, with some crystals still floating in it. Should they just throw it back in the freezer and wait for it to evap some more?

SWIM used q21q21's tech, with what appears to be beautiful results! (no weight, but shiny white crystals!Cool )


I hope your naptha isnt evaping in the freezer?

Anyway, if there are a few floaters in there, filter it through a coffee filter and keep the naptha for next extraction.


It was SWIM's understanding that you to a freezer precip...is that not the same as evaporating?

Thanks for the help!


evaporate = allow liquid to turn to gas (usually under a fan, this is not done in a freezer)

freeze precip = place solvent in freezer so the lowered temperature pushs dmt out of solution forming crystals.
 

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halten
#862 Posted : 3/30/2010 11:54:06 PM

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Thanks for clearing that up!

The dish is out of the freezer EVAPORATING! Laughing
 
ztz
#863 Posted : 4/8/2010 7:40:54 AM
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Hello, this is my first post here although I've been lurking for a while. I'd like to get some input about what could have possibly went horribly wrong in an extraction using Lazy Man's tek (I feel like a complete idiot for screwing up what is supposed to be the easiest extraction method and have no good excuse :oopsSmile

200g 100% NaOH was added to 2000mL H2O and stirred. While still hot, the solution was poured onto approx. 500g prepowdered MHRB in a glass 1-gal. mixing container and was left to sit for a few hours. 300mL room temperature 100% VM&P Naphtha was added and mixed with a wooden stirring rod until the naphtha took color, and was decanted immediately and fanned to evaporate, resulting in a slightly off-white and very waxy substance. Another 500mL H20 and 100g NaOH were added to the MHRB solution at this point and it was left to sit overnight. 300mL of naphtha was heated in a hot (max. faucet temperature, not boiling) water bath and added to the MHRB. MHRB and naphtha were rolled in jug for 15 minutes and then stirred for 30 minutes. Separation between the two layers occurred nicely. Naphtha was then decanted and had a much darker than usual color. Absolutely none of the MHRB layer got into this naphtha. Naphtha was fanned to evaporate and a brown coating formed on the bottom of the evaporating dish. Upon collection this material is extremely dark and sticky. Since none of the MHRB mix got in the naphtha there was definitely SOMETHING extracted although not the target chemical. Odor has resemblance of pure white DMT.

This method has been used before with good results. I'd like to know what went wrong. I am inclined to believe that it may be that not enough NaOH was added, however previous trials yielded a more pure product with similar quantities. An attempt will be made to recrystallize the black product in hopes of purifying it. The yield from the first pull, while not pure white, was acceptable.

Picture shows the yields from the two pulls- left is the first and right is the second.

Thank you in advance.

 
endlessness
#864 Posted : 4/8/2010 9:23:12 AM

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strange.. your naphtha evaps clean by itself, I suppose, right? anyways, def recrystalize it
 
cellux
#865 Posted : 4/8/2010 12:10:44 PM

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(I posted this to another topic but didn't get any answers. Perhaps I will be luckier this time.)

I'm planning on doing an A/B extraction and would like to have a grasp on the entire process so that I can discern the important variables from the unimportant ones.

Here is how I understand it at the moment:

MHRB contains the salt form of DMT. If one pours a nonpolar solvent (like naphtha) onto the (powdered) bark, nothing happens, because DMT in its salt form doesn't dissolve in nonpolar solvents. However, if one puts the bark into water, then the DMT salt would dissolve in the water (because salts dissolve in polar solvents and water is one such solvent). But this doesn't happen automatically, because the DMT is "locked up" in the bark (inside the cells perhaps?). Therefore one must find a way to break those cell walls, so that the DMT can come out into the water. And that's the reason for the "acid bath": one puts the bark into water + acid (I will use vinegar), the acid breaks the cell walls, then the DMT salt comes out and gets dissolved in the water.

* Question 1: how can one ensure that all (or most) of the DMT gets dissolved in the water (and nothing gets back to the bark again, if that is possible)?

When this is done, one puts enough base (I will use pickling lime) into the water + acid + DMT salt mix, so that its pH reaches around 9. At this point, the DMT salt gets converted into DMT freebase.

* Question 2: how can I ensure that all (or most) of the DMT gets converted to freebase and stays so?

After this happens, one puts the non-polar solvent (I will use naphtha) into the mix and the DMT freebase "moves from the water layer into the nonpolar solvent layer".

* Question 3: Why does this happen? (What force makes the DMT "move" from the water to the naphtha?)

* Question 4: What variables control the amount of the DMT "pulled" by the solvent?

* Question 5: Do I have to stir the solution for this (water -> naphtha migration) to happen?

Anyways, let's say it happens. Then the solvent - which now contains the DMT freebase and forms a well separated layer on top of the water + acid + base mix - is somehow decanted (removed) from the mixing bowl, poured into a separate dish and put into the freezer for "freeze precipitation". This takes 24-48 hours, after which DMT crystals will show up in the solvent. Then the fridge is opened, the solvent poured through a coffee filter (back into its own container so it can be reused later), then the coffee filter is put to a dry place, the DMT crystals are dried (excess solvent on them is evaporated) and then the crystals are scraped off with a razor blade or something into a vial.

The teks say that after this the recycled solvent should be mixed back into the water + acid + base solution and another "pull" should be made (mix, remove solvent, put into freezer for precip). I suspect that this is necessary because the naphtha cannot pull all of the DMT at the first time.

* Question 6: How do I know that I'm ready (don't have to make any more pulls because I managed to pull all of the DMT)?

Thank you for your time.
 
endlessness
#866 Posted : 4/8/2010 1:29:22 PM

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cellux wrote:

However, if one puts the bark into water, then the DMT salt would dissolve in the water (because salts dissolve in polar solvents and water is one such solvent). But this doesn't happen automatically, because the DMT is "locked up" in the bark (inside the cells perhaps?)


not really true.. if the bark is powdered, most of it will go to the water 'automatically'... but yeah if one wants to just be 100% sure (as well as to guarantee the water is not too basic, in case of some places where tap water is basic), then adding acid is recommended

cellux wrote:

* Question 1: how can one ensure that all (or most) of the DMT gets dissolved in the water (and nothing gets back to the bark again, if that is possible)?


bark being powdered and doing 4 or 5 long acidic simmers (couple of hours each) will get nearly all your alkaloids. Even the first 3 simmers would probably be enough but SWIM likes to do 5 just in case (since this first step will basically limit everything else later on..) . Other option is doing a BLAB (or an STB), in which case you wont be straining and throwing the bark out, so all your alkaloids will be there

cellux wrote:

When this is done, one puts enough base (I will use pickling lime) into the water + acid + DMT salt mix, so that its pH reaches around 9. At this point, the DMT salt gets converted into DMT freebase.


bad idea, calcium hydroxide is poorly soluble in water, its not a good base for doing basifying an acqueous solution.. it is used only in 'dry teks'... So either find some lye or KOH or do a dry tek....

cellux wrote:


* Question 2: how can I ensure that all (or most) of the DMT gets converted to freebase and stays so?


just having enough calcium hydroxide in a dry tek and mixing well, or having the high pH (in other words, when the solution is completely black) will guarantee to make the dmt be a freebase

cellux wrote:

* Question 3: Why does this happen? (What force makes the DMT "move" from the water to the naphtha?)


it lost the proton from the salt, so because of its charge it is soluble in non-polar and not soluble in the polar acqueous solution, therefore when you mix it will go to the non polar solvent.

cellux wrote:


* Question 4: What variables control the amount of the DMT "pulled" by the solvent?


the solvent (for example, heptane wont pull so much, toluene/xylene/limonene will pull more), the temperature of the solvent, the time of contact... Therefore making many cycles of mixing and letting stand before pulling the solvent, and warming it in water bath, will improve yields.

cellux wrote:

* Question 5: Do I have to stir the solution for this (water -> naphtha migration) to happen?


for sure some migration will happen even if you dont stir much but obviously stiring will improve yields, because more dmt will get in contact with your solvent and since it 'preffers' it, it will go to it.

cellux wrote:


* Question 6: How do I know that I'm ready (don't have to make any more pulls because I managed to pull all of the DMT)?


if you freeze precipitate each pull when using naphtha, or if you make FASI on limonene, you can see the crystals being formed, so just keep pulling until no more crystals come out with the pull.. SWIM goes for around 6 or so pulls, and his last one he always leaves for days and days and days..

hope that helped
 
TryptoFiend
#867 Posted : 4/9/2010 4:36:43 AM
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Hi everyone
I attempted Q21Q21 tek recently and was surprised to get very low yields and no white crystals barley any brown stuff. I did only do two pulls with naphtha and one with xylene..
The bark is a few months old but has not been exposed to air, was atleast hopping for alot of jungle spice +dmt n oxide if that was the case.

Id like for anyone to give me some tips on how to perfect on Q21Q21 tek or any other way to do an extract with Pickling Lime as I bought alot of it not knowing that I even bought wayy more than id need.
It be great if I could do something with all the Lime I got instead of going to buy some lye. Id like a tek were I can let the bark marinate in a jar possibly for extended periods of time.Anything to get the most yield would be nice.
 
cellux
#868 Posted : 4/9/2010 7:41:02 AM

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Thank you for your kind answers, endlessness!

Quote:
Other option is doing a BLAB (or an STB), in which case you wont be straining and throwing the bark out, so all your alkaloids will be there


Hmm, I didn't know that one should strain and throw the bark out. So after those couple of "acidic simmers" (provided I'm doing a non-dry tek) I should pour the liquid through a strainer (metal mesh? cloth?) and work only with the filtered solution from there?

Quote:
bad idea, calcium hydroxide is poorly soluble in water, its not a good base for doing basifying an acqueous solution.. it is used only in 'dry teks'... So either find some lye or KOH or do a dry tek....


I may seriously misunderstand something then. In the q21q21 tek (which I think is a dry tek), the author recommends the use of vinegar. But food-grade vinegar (as I know it - as it is sold in the grocery store) is a solution (vinegar+water). If I poured that vinegar onto the bark (as the q21q21 tek would advise me to do), I'd get an aqueous solution. Then how come q21q21's tek (which uses lime to basify later) works? May the secret be in the proper amount of vinegar (his tek uses 2ml vinegar for 1g of bark) so that the bark "soaks up" the vinegar+water therefore it remains relatively dry? Or perhaps by "vinegar" the tek means some undiluted form (which contains no water)?
 
endlessness
#869 Posted : 4/9/2010 9:39:09 AM

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TryptoFiend, where was your bark from? maybe it was bad bark? How long did you let it react with the lime for freebasing before adding sovlent? Did you mix the solvent well before pulling it out? did you try freeze precip or evap the solvent?

cellux: yeah with A/Bs usually bark is trained but you dont have to, as I said, if you chose to go BLAB/STB way. But yeah in an A/B, you simmer, strain, add fresh water, simmer, strain, do this at least 3x, put the liquid togethr, throw the solids away. But if you are using q21 tek, that is different, and yeah it is a dry tek, and yeah you are right that the amount of vinegar is low and the bark soaks it up so it will be still reasonably dry (it just wont be a dilute solution with the bark in it, but rather a thicker moist solution, kinda lake a paste). I havent done q21 tek, btw, im just saying from what I understand when reading it..

good luck all
 
TryptoFiend
#870 Posted : 4/9/2010 6:23:27 PM
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I got my bark off ebay powdered, cant recall the seller right now. Ive made pretty potent aya before but I have serious problems with nausea and projectile vomit too soon.
For each step I took an hour thinking that be enough for everything react. I stirred every 10 minutes and had an electric kettle near to change the water bath very often.
The naphtha was left in for 15-30 minutes.
The consistency was a bit too dry but mixable I'm thinking a bit more vinegar or water should have been used.

Next time ill do it all in a jar with a water bath and extened each step for much longer and leave the first naphtha pull over night.
^^^^^
Sound good?
 
ztz
#871 Posted : 4/10/2010 1:48:38 AM
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I'm having some quite strange results here, the recrystallization from the previous pull isn't looking too good (it's going to require multiple recrystallizations and most of the mass is likely to be lost, not sure if it's worth it) but even stranger is that after leaving the jar overnight without anything added, a layer of naphtha formed on the top. This layer was also extremely brown and very hard to tell from the MHRB layer. This naphtha layer was decanted (volume was approx. 150mL) and then washed multiple times with sodium carbonate and then washed multiple times with water. Much of the brown color was removed but it was still yellow and washing wasn't doing anything more. The naphtha was evaporated, this time leaving a very nice and large yield which will still need to be recrystallized but isn't an awful brown/black tar like the last one.



Another layer of naphtha has separated out overnight again. So, a total of 300mL of naphtha was added only once, and it has separated over multiple nights with a very dark color. I think that further extractions from this bark will require a defat step before anything more is extracted.

 
astroNOMADical
#872 Posted : 4/10/2010 6:34:00 AM
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SWIM created a separate thread for this question before he realized hes retarded for not seeing this thread and posting here originally. But here goes:

Ok- so SWIM tried another pull after 48 hrs from his first couple pulls, which were mildly successful. The first couple pulls SWIM did not freeze precip, he just evapp'd in dish with fan blowing. This time he wanted to freeze precip to see if he could get a cleaner looking spice- he put the glass dish with the naphtha (200ml) in the freezer about 36 hrs ago. A signifigant amount of the nap has evappd and he is very excited to see that this pull seems to have a large amount of spice in it. His question/concern is, there is still a bunch of liquid with spice floating in it (as well as some stuck to the bottom)...but what does SWIM do from here? Is it normal for it to take this long for the naphtha to evap? Should he leave it in the freezer till all fluid is gone or is there a way to strain it without loosing all the spice floating around? SWIM feels like if he uses a coffee filter he might lose some of the spice? Maybe not...dunno. I used the lazymans STB tek (which doesnt really talk about freeze precip), very new to any kind of extraction process, and def not a chemistry whiz here. I think all seems to be going ok, just wanted to make sure I dont eff it up after being this close to having some very pretty white crystal spice :-D Thanks for the help!
 
kkem
#873 Posted : 4/20/2010 1:43:54 AM
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So, SWIM just finished his first DMT extraction!

The whole process was a lot of fun, and SWIM looks forward to learning more as he go.

Currently, SWIM has a bunch of DMT, which is quite yellow.

SWIM used whatchamacallits tek, and everything went quite well. During freeze precip there was the crystals which formed seemed to be much whiter than they ended up. The last bit of the naptha was evaporated under a fan, and that's when it seems to have gone yellower, ending up with what I have in the pic.

Should SWIM rex this before smoking? From what SWIM understands, there is a good chance that the yellow is just fatty oils and plant matter, which some people seem to prefer.

SWIM is interested in trying different ways of using the DMT. Would his current batch be more useful if used in a specific way? Currently SWIM is looking at making a machine and trying to smoke it, making enhanced leaves (when the herbs arrive), and attempting pharmahuasca as he currently has 100g of syrian rue sitting around.

Any advice would be appreciated.
kkem attached the following image(s):
dm.jpg (37kb) downloaded 100 time(s).
 
HyperD
#874 Posted : 4/22/2010 1:53:01 PM

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Just to share my exerience with S/B extraction is that
use Epsom salt!
Removes all the water before freezer for much better resultSmile




Remember that when you walk through the door you just opened the experience can be compared to flip a coin
But the coin can have more than two sides
 
neverwas
#875 Posted : 4/27/2010 3:50:15 AM

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I have short question about STB.

Where can I find ph paper locally? I tried the pet store but they only go up to 8.5 and I need ph 14?
Alternatively, is it ok to just leave the vineger in longer just to be sure or do Is that a no no? I also have muriatic acid to use if that will work with q21q21 STB tek.

Any answers are good answers Smile
My name is love, for I am without fear
 
GirlsHateMe
#876 Posted : 4/29/2010 6:15:14 AM

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My unicorn found full range litmus paper at a school supply store. It was a pain to find, but well worth it due to peace of mind.
For we wrestle not against flesh and blood, but against principalities, against powers, against the rulers of the darkness of this world, against spiritual wickedness in high places. Wherefore take unto you the whole Armour of God, that ye may be able to withstand in the evil day, and having done all, to stand. - Ephesians 6:12-13

GHM is an internet handle, a fictional one at that, the person I portray in no way depicts real life actions and or opinions. After all, whats the internet for besides pretending to be someone you arent! Also, no girls do not really hate me.
 
HyperD
#877 Posted : 5/4/2010 7:07:55 PM

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Morbiddoctor wrote:
I have short question about STB.

Where can I find ph paper locally? I tried the pet store but they only go up to 8.5 and I need ph 14?
Alternatively, is it ok to just leave the vineger in longer just to be sure or do Is that a no no? I also have muriatic acid to use if that will work with q21q21 STB tek.

Any answers are good answers Smile


Where you buy aqarium fishes




Remember that when you walk through the door you just opened the experience can be compared to flip a coin
But the coin can have more than two sides
 
jabberwocky
#878 Posted : 5/17/2010 2:11:06 AM
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Can heptane be safely used with HDPE containers?

[edit] To answer my own question: It appears heptane damages HDPE slightly, especially at higher temps and after longer durations. It should be okay to use for a short period of time.

n-Heptane in HDPE: Reference 1
Quote:
G โ€“ Little or no damage after 30 days of constant exposure to the reagent
F โ€“ Some effect after 7 days exposure to the reagent. Solvents may cause swelling and
permeation losses


n-Heptane in HDPE: Reference 2
Quote:
70°F "Some attack"
140°F "Unsatisfactory"
 
Daydreamer
#879 Posted : 5/26/2010 7:07:06 PM

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SWIM was doing the Poor Mans Tek (https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=9372) with 100g of MHRB.

The Text says:
Quote:
For every gallon of water add 1.5 cups of vinegar or 1 cup lemon juice per gallon and measure out an equal amount of this acidic water for the amount of oil that you have. (If you have 2.5 cups oil , you'll need 2.5 cups acidic water


1 US gallon = 3.78541178 liters

So for each of the 3 pulls he mixed about 2 litres of water with 1 cup of vinegar (because he has 1 cup of sun flower oil)
Then he mixed the oil with the acidic water filtered out the oil pured it back in the pot simmered for 1,5 hours and repeated this procedure twice after this.

Now he is left with about 4 litres of water that he made basic with washing soda (to get the freebase DMT+washing soda)

Main Questions: 1. Is it normal that one must evaporate ~4 litres of basified water using this tek?
2. If yes is it more efficient to pour the liquid in one big container or is it more efficient to pour it in several smaller container in order to evaporate it using a small desk fan?
3. How long will it take to evaporate this water?
 
cyberelf
#880 Posted : 5/27/2010 9:08:39 AM
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Hey everyone

SWIM performed his first extraction following the Lazy tek with MHRB (approx 50g) and Shellite as solvent. As the solvent has taken a long time to evaporate, he decided to freeze the solvent in a glass jar (first pull, of course). After a few hours he could see a few "snow cones" forming at the bottom of the jar. He waited another 6 hours or so and the number or size of the "snow cones" didn't seem to change.

So at this point he really did'nt understand what to do next. So he scrapped the snow cones off using a knife. The snowcones were just running free in the solvent. Then he filtered (using 100% cotton tshirt) the solvent into another glass jar. The remaining "snow cones" really looked more like ice or crystals. After a few minutes THEY DISSAPPEARED! They melted or something...

What happened? Please help! What could he do to successfully extract the spice? What could those crystals be? SWIM thought the spice would only melt at high temperatures. The whole thing was done at average room temperature.

Cheers

 
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