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No naptha tek Options
 
neuro_rocket
#1 Posted : 8/15/2009 6:45:44 PM

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SWIM is running low on naptha (and doesn't have access to other non-polar solvents) and was trying to come up with an extraction method that doesn't require any non-polar solvent.

His tek goes like this, any questions or comments are appreciated.
THIS TEK WILL NOT WORK

1- Grind up plant matter (SWIM is using phalaris grass) with acidified alcohol (SWIM is thinking of dissolving citric acid in alcohol until it reaches pH 4).

2- Strain and discard the plant matter.

3- Evaporate the alcohol solution.

4- Mix the residue with basified alcohol (SWIM will dissolve sodium carbonate in alcohol until it reaches pH 10 or 11)

5- Evaporate approximately half of the alcohol

6- Stick in the freezer, freebase DMT will precipitate. Filter and collect the spice.

The advantages of this tek are that it only uses one solvent, it doesn't require a seperatory funnel and it is simpler than an A/B extraction.

Notes
-SWIM is using rubbing alcohol but ethanol or acetone should also work (acetone would probably be the best since it is the most polar).

-The reason SWIM is using alcohol is because it is very polar and very volatile.

-SWIM will distill the alcohol when evaporating so he can reuse it.

-SWIM stumbled upon this tek, which is a bit like SWIM's http://www.thenook.org/a...lfspice_dual_solvent.htm

-Using dry alcohol or acetone would probably work better.

-If any nexians would like to try this with something known to consistently contain DMT (like MHRB) and report there results and yield SWIM would greatly appreciate it.

-Neurorocket
I'm mad as a hatter and a compulsive liar.
Nothing I say is true or should be mistaken for the truth.
 

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endlessness
#2 Posted : 8/15/2009 8:20:55 PM

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at least one thing I can tell you, is that freeze wont work neither with alcohol neither with acetone, as dmt is too soluble in it even at freeze temperatures.

I dont know about the solubility of different bases, acids and impurities in alcohol so someone else will have to comment on that part. In any case you can straight ahead just look at the dry teks.. check the wiki also... People dont report too good results it seems, but I havent done myself so cant really say.
 
neuro_rocket
#3 Posted : 8/15/2009 8:27:50 PM

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I was under the impression that freebase DMT was insoluble in alcohol and acetone.
Whereas DMT salts are very soluble.

Otherwise it would be helpful to know the solubility of plant fats and oils in alcohol and acetone, so that SWIM could find a way to defat.

SWIM will also check out the dry teks.

What about vegetable oil, could SWIM use vegetable oil to defat and then separate? (This is either a really good idea or a really stupid one, SWIM's just not sure which yet).
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Infundibulum
#4 Posted : 8/15/2009 9:12:58 PM

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neuro_rocket wrote:
I was under the impression that freebase DMT was insoluble in alcohol and acetone.
Whereas DMT salts are very soluble.

On the contrary, SWIM tells me that the freebases are soluble in alcohol and acetone.

The tek, as it is written, has some flaws and it may not work.
Quote:

1- Grind up plant matter (SWIM is using phalaris grass) with acidified alcohol (SWIM is thinking of dissolving citric acid in alcohol until it reaches pH 4).

Acids do not usually dissociate (even though they can dissolve) in alcohols or acetone so the notion of pH of an acid dissolved in absolute alcohol/acetone does not exist. pH can be increased/decreased as a result of water reacting with an acid or base.

But things will be fine if there is water present in the alcohol. Using acidified 50-70% alcohol sounds totally fine and people have been using this solvent for the acidic extraction,
Quote:

4- Mix the residue with basified alcohol (SWIM will dissolve sodium carbonate in alcohol until it reaches pH 10 or 11)

Sodium carbonate does not dissolve in alcohol, so you'll have problem doing that step. But if water is present in the solution then things will be fine.

Quote:
5- Evaporate approximately half of the alcohol

6- Stick in the freezer, freebase DMT will precipitate. Filter and collect the spice.

These won't work that well either, even if you use water:alcohol solutions for the acidification and basification. Basically, in steps 1-3 you'll get salted alkaloids and tons of fats. In steps 5-6 the fats will also precipitate as alcohol evaporates and/or becomes colder.

Hope that helps!

Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
neuro_rocket
#5 Posted : 8/15/2009 9:25:33 PM

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Thanks for the input.

SWIM thinks that he may make a mix of 70% alcohol and 30% water and substitute that for the alcohol. He'll then complete the tek as written and during the freeze-precipitation step he'll pour off and then evaporate the alcohol. (The idea being that the oils would migrate to the water [since it is less polar] and the alcohol would have the DMT).

Mineral oil cannot be used for defatting, SWIM just checked with some phalaris juice.

Would freebase DMT precipitate out of water?

Thanks again for the input,
SWIM hopes that with other nexians help he will be able to develop a naptha free tek.
I'm mad as a hatter and a compulsive liar.
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Infundibulum
#6 Posted : 8/15/2009 9:55:22 PM

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neuro_rocket wrote:
SWIM thinks that he may make a mix of 70% alcohol and 30% water and substitute that for the alcohol. He'll then complete the tek as written and during the freeze-precipitation step he'll pour off the alcohol and keep the frozen water, then melt the water and either evaporate or (though this kind of defeats the purpose of the tek) use naptha to extract the spice and fats and clean it up with a recrystallization.
SWIY would have also trouble doing the thing in bold. It is not the same as freezing a mixture of water and xylene or water and naphtha. Alcohol is miscible with water and water will not freeze if it is mixed in alcohol. Just like good vodka or other strong spirits.


Quote:
SWIM hopes that with other nexians help he will be able to develop a naptha free tek.

One of the best ways to go with phalaris is to use xylene instead of naphtha and go FASA.

Other teks that do not use naphtha or other petrochemicals are the dryteks.

Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
neuro_rocket
#7 Posted : 8/15/2009 10:17:37 PM

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Alright,
SWIM has a new idea based on the dryteks, it depends on whether or not freebase DMT is soluble in basic water.

1A (if using phalaris)-Grind grass with basified water then filter and discard the water

1B (if using MHRB)-Grind plant material and add lime then mix with water to make it pasty.

2-Add to the herbal percolator and pour basic water over it. Discard the basic water.

(if using phalaris repeat step 2 until all the fats are out)

3-Pour acetone over the plant material, repeat 4-5 times with the same acetone.

4-Evaporate acetone to yield freebase DMT.


The main idea is that the basic water does not dissolve the DMT but does dissolve the fats. The fats are then discarded and the DMT is dissolved with the acetone (or anything else that dissolve freebase DMT).

SWIM would love to try FASA but he doesn't have access to fumaric acid. Would tartaric acid work?
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Infundibulum
#8 Posted : 8/15/2009 10:54:19 PM

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neuro_rocket wrote:

1-Grind plant material and add lime then mix with water to make it pasty.

2-Add to the herbal percolator and pour basic water over it. Discard the basic water.

3-Pour acetone over the plant material, repeat 4-5 times with the same acetone.

4-Evaporate acetone to yield freebase DMT.

In step, the basic water will not carry away the spice ( it is very marginally soluble in water, but it won't carry away the fats either. SWIM does not know whether step 1 will work either. It has a so-so success for MHRB, great success for cactus and anadenanthera seeds but SWIM does not know whether it would work with phalaris. Let us not assume beforehand that it works!

In SWIM's opinion, the following may work;

1. Use preferably fresh material or freshly cut and frozen. SWIM has had minimal success with fresh phalaris grasses and no success with dried. It is possible that while the plants dry they also degrade their alkaloids. Not all the plants are like that (chacruna and chaliponga are supposedly fine but in practise we do not know how much is lost due to cell death). Allowing the grass to freeze-thawing some times will help burst the cells and release the goodies.

2. Soak in acidified 70% alcohol+strain. Repeat 2 more times.

3. Let everything dry totally. It will leave a gooey mass which contains the dmt in salt form and other crap and oils and fats.

4. Wash the gooey mass with water a few times. dmt will be picked up by the water and fats will be left behind.

5. take this water that contains dmt and basify it. the dmt freebase precipitates out of aqueous basified solutions.

6. Presto!


Quote:
SWIM would love to try FASA but he doesn't have access to fumaric acid. Would tartaric acid work?
Tartaric acid won't work as well. Plus, dmt tartrate is a pain in the ass to work with.

Hope that helps!

Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
neuro_rocket
#9 Posted : 8/15/2009 11:28:54 PM

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Thanks for the tips and tek.

Infundibulum wrote:

1. Use preferably fresh material or freshly cut and frozen. SWIM has had minimal success with fresh phalaris grasses and no success with dried. It is possible that while the plants dry they also degrade their alkaloids. Not all the plants are like that (chacruna and chaliponga are supposedly fine but in practise we do not know how much is lost due to cell death). Allowing the grass to freeze-thawing some times will help burst the cells and release the goodies.

SWIM read something in Trout's notes on phalaris that said the dried material contains significantly less alkaloids than the fresh material.

Would SWIM also receive results if he used acetone instead of alcohol?

SWIM will try out this method and report back if he gets any results (although all results or lack thereof from phalaris are sketchy because phalaris itself is very inconsistent in alkaloid content). He plans to use phalaris picked from numerous locations and environments to see what causes the best alkaloid concentration in wild phalaris grass.
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neuro_rocket
#10 Posted : 8/17/2009 4:01:41 PM

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SWIM just used the last of his alcohol so he is going to modify the tek to use just water.

1- Blend Grass with pH 4 or 5 water. Allow to sit for an hour or so and strain, discarding the grass.
2- Add basic water (pH 10) and evaporate to a goo.
3- Wash the goo with basic water to remove the fats, discard the water.
4- Spice and other alks are left in the evaporation dish.
(optional) 5- Clean up with a hexane recrystallization.

Any water or alcohol extraction of phalaris grass seems to seperate into 2 layers, one being a dark brown/red thin liquid layer on top and the other being a dark green thick layer on bottom.
SWIM thinks that the green layer is the fats, because the green layer tends to go to the top when naptha is added. But he was under the impression that fat floats, is it possible that the fats could sink under the water layer?
SWIM also read that the fatty layer traps most of the spice. So he may try evaporating the green layer and the red layer separately and see which yields the most.
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Infundibulum
#11 Posted : 8/17/2009 4:29:35 PM

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neuro_rocket wrote:
SWIM just used the last of his alcohol so he is going to modify the tek to use just water.

1- Blend Grass with pH 4 or 5 water. Allow to sit for an hour or so and strain, discarding the grass.
2- Add basic water (pH 10) and evaporate to a goo.
3- Wash the goo with basic water to remove the fats, discard the water.

4- Spice and other alks are left in the evaporation dish.
(optional) 5- Clean up with a hexane recrystallization.

SWIM does not really like SWIY's extraction strategy, it is dodgy and very prone to fail. for instance in step 1, why not slow boil the plant material for like 3 times for 20min each?

And re to 2; why not use higher pH just to be sure? Underbasification is often an issue with extractions. One can go up to pH 14 with not real problems. The way you wrote it gives the impression that SWIY will not raise the pH to 10 but rather will pre-make basified water and add it to the acidic solution. Tell SWIY to forget all those dodgy QT-style extraction rubbish! QT tek sucks ass!

Finally, re to 3; Why think that washing teh goo with basic water will remove the fats?!?!? Do not do this step.

SWIM thinks that SWIY is working with a difficult material of very questionable success and on top of that he tries to use unorthodox, unreliable and not that satisfactory techniques. This is a recipe for sure waste of time. If SWIY wants to do things correctly then tell him to find some solvent (naphtha, xylene, toluene, DCM) and do things properlyWink

Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
Infundibulum
#12 Posted : 8/17/2009 4:35:51 PM

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neuro_rocket wrote:
Any water or alcohol extraction of phalaris grass seems to seperate into 2 layers, one being a dark brown/red thin liquid layer on top and the other being a dark green thick layer on bottom.
SWIM thinks that the green layer is the fats, because the green layer tends to go to the top when naptha is added. But he was under the impression that fat floats, is it possible that the fats could sink under the water layer?
SWIM also read that the fatty layer traps most of the spice. So he may try evaporating the green layer and the red layer separately and see which yields the most.

Fats float if they are less dense than water. Fats sink they are more dense than water. chlorophylls are very fatty substances, phalaris is full of them and they tend to sink.

As far as the green layer trapping most of the spice, this is also questionable. where did SWIY read that?

Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
neuro_rocket
#13 Posted : 8/17/2009 11:36:15 PM

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Infundibulum wrote:


And re to 2; why not use higher pH just to be sure? Underbasification is often an issue with extractions. One can go up to pH 14 with not real problems. The way you wrote it gives the impression that SWIY will not raise the pH to 10 but rather will pre-make basified water and add it to the acidic solution. Tell SWIY to forget all those dodgy QT-style extraction rubbish! QT tek sucks ass!



SWIM always checks the pH of the sol't (he does use water basified to 14 to make his sol't basic)


Infundibulum wrote:


As far as the green layer trapping most of the spice, this is also questionable. where did SWIY read that?



SWIM is using phalaris-oid's post as a reference for that
http://forums.mycotopia....s-canary-reed-grass.html

SWIM is going to boil his grass with acidic water, strain, basify, evaporate then clean it up with naptha or heptane.

Infundibulum wrote:


SWIM thinks that SWIY is working with a difficult material of very questionable success and on top of that he tries to use unorthodox, unreliable and not that satisfactory techniques. This is a recipe for sure waste of time. If SWIY wants to do things correctly then tell him to find some solvent (naphtha, xylene, toluene, DCM) and do things properlyWink



SWIM knows that what he is trying to do probably won't work out, he's pretty much just doing it for the practice and to satisfy his curiosity (although it would be great if he could develop an simple tek for phalaris).
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jamie
#14 Posted : 8/18/2009 2:02:53 AM

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[quote=InfundibulumIn SWIM's opinion, the following may work;

1. Use preferably fresh material or freshly cut and frozen. SWIM has had minimal success with fresh phalaris grasses and no success with dried. It is possible that while the plants dry they also degrade their alkaloids. Not all the plants are like that (chacruna and chaliponga are supposedly fine but in practise we do not know how much is lost due to cell death). Allowing the grass to freeze-thawing some times will help burst the cells and release the goodies.

2. Soak in acidified 70% alcohol+strain. Repeat 2 more times.

3. Let everything dry totally. It will leave a gooey mass which contains the dmt in salt form and other crap and oils and fats.

4. Wash the gooey mass with water a few times. dmt will be picked up by the water and fats will be left behind.

5. take this water that contains dmt and basify it. the dmt freebase precipitates out of aqueous basified solutions.

6. Presto!

[/quote]

Interesting tek..I have access to tons of this grass so might try this tek out of curiosity..one question though..durring the water wash on the goo to retrive the spice, is cold or warm water ideal, and how long of a wash is best?..or should I just run the water over the goo with a filter as in percolation? I would think that hot water would pick up some fats?
Long live the unwoke.
 
 
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