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Non toxic food safe extraction of mescaline using d-limonene (orange oil) Options
 
floatingwater
#1061 Posted : 4/5/2011 5:22:09 AM
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A friend of mine wanted to relay the following information:

Limonene from GT took two weeks to arrive. No chance at customer service but it did make it there. Made the mistake of only ordering a 16 oz bottle (500 mL).

300 mL of limonene was used for each extraction round from the CaOH2 basified cactus mix. Each successive round needed to include larger amounts of re-used limonene. By 3 or 4 rounds it was all recycled limonene being used to extract materials from the cactus mix. 5 Rounds were performed.

Each round of limonene was washed with HCl solution with a concentration of 4 to 5 drops of 10% HCL v/v per 100 mL of water. The salting solutions came out to be about a pH of 2 - 3 before mixing with limonene (thanks to futura for the excellent advice!) 4 to 5 washes of 100 mL HCl solution were done and pooled per limonene extraction round.

Evaporated at room temp with air blowing
Round 1 -> Very White but only a yield of about 200 mg
Round 2 -> white but slightly yellow/tan and a yield of about 200 to 250 mg
Round 3 -> Whiter again and a yield of 300mg
Round 4 -> Getting a little tan, slight reddish now, maybe 150 to 200 mg yield
Round 5 -> tan colored maybe 50 mg yield



Other notes: Cactus mix swallowed about 100 mL of limonene by the 4th round.
 

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mew
#1062 Posted : 3/24/2012 6:32:23 AM

huachumancer


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3 hours, some improvising:
stir bassified pulp through limo, let settle pour off, repeat (400 ml limo)
salted once with 100 ml vinegar (5%)
22g flesh yielded, 766mg, 34.5%
amber/orange wax, a drop of undriable fluid (suspected limo contam.)

previously same strain from same source was used with hcl salting, hcl salting after 2x dry acetone washes yielded 7%, however much more energy went into salting and pulling due to using more plant matter.

was the potency issue ever figured out (acetate vs hcl)
 
quetzalcoatl42
#1063 Posted : 3/27/2012 8:53:55 PM

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Hi,

so I tried this tek now 3 times and I have a few questions.

I've read a couple of times ppl are worried about getting every last drop of limo. I have successfully used a juicemaker, filled with the pulp. The juicemaker is basically a centrifuge with a fine metal strainer, spinning the pulp to separate the juice (limo) by means of the occuring centripal-force. The only downside is the limited space, so you'll need to refill it a couple of times, but it works great, as long as you dont over water and avoid having a slimey mix. I guess a somewhat modified salad spinner will also work very well with bigger quantities.

What I consitently failed, is getting more than 1% crude material, light amber, from dried fine powder and trying more than 3 times, I badly failed in purification.

I dont have MEK, so I used acetone, fresh and lab grade, and it seemed either I have hardly any mesc but only other alks or the acetone was not dry. That was my first attempt.

So Magnesium sulfate was purchased, not powdered but in small pearls. The epsom salt was dried in the oven and added to a huge jar of acetone which then went to freezer. So materials aquired the wash was tried again, the excess Magnesium sulfate was at the bottom, the acetone was ice cold. With a spoon 2-3 Tsp were added into a small bowl together with the amber mesc. The mesc. was then crushed with the flat side of a chopstick and the color of the acetone was getting red-amber-ish. The top layer was then carefully sucked up (making sure not to suck up any mesc) with a big rubber ball pipette. Acetone was added twice more, mixed and mesc was washed again. The color was nearly transparent when the remaining acetone together with the remaining mesc was poured on a glass plate. The acetone was evapped completely. Nearly boiling hot water was then added to the dish and the the washed reamining mesc. redissolved. It didnt look good again, from 0.2 it went to not measurable, and after the water was evapped, the color was even more dark and it wouldnt crystalize anymore. Sad

So I'm adding a few pictures now, and I'm curious if anyone thinks it might be possible to guess the concentration of mesc from the pictures alone, because it looks very well, but washing it, really doesnt work, and I'm not sure what is going wrong.

P.S. Is it possible to re-use the limo ? I found that boiling any remaining vinegar away, it gets clear again, but its still green-yellowish. Its really expensives stuff where I'm from.


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SKA
#1064 Posted : 4/14/2012 9:07:03 PM
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It's a shame that so often soap forms and makes layers hard to separate.
Obviously mixing dry cactus powder with Lye and then mixing in water
doesn't seem a good idea either.(Reaction heat could break down Mescaline?)

Maybe someone here could revise this method.
As long as the solvents, acids & bases used
are easily obtainable.

Nexus Wiki sais that Mescaline is:
wrote:
Soluble in: alcohol, chloroform, benzene, xylene, toluene, acetone, dichloromethane, highly soluble in isopropyl alcohol, soluble in d-limonene
Moderately soluble in: water
Insoluble in: practically insoluble in ether or petroleum ether


Perhaps dried san pedro powder could be washed with Petroleum Ether first
(or another solvent in which Mescaline is insoluble)
You just soak the SP-powder in Petroleum Ether for 30 mins & then filter off
the plant-oil-saturated Petroleum Ether through a coffee filter. Repeat 3 to 4 times.
After a couple of Petroleum Ether washes the Mescaline in the SP-powder could
perhaps be extracted with several portions of Ethanol.
This Ethanol can either be evaporated on a baking dish to leave a Mescaline residue
or put in the freezer untill the Mescaline crystals precipitate out & then filter out the crystals.

Just a quick sketch based on the Solubility characteristics of Mescaline.
If anyone has a better idea, please share it with us.


 
quetzalcoatl42
#1065 Posted : 4/14/2012 11:39:22 PM

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I wrote in my mesc extraction help thread that I had the feeling the mentioned 3 layer problem I encountered was due to over-basing and saponification. Then and there I used NaOH AND KOH (which is really nasty and probably a very bad idea). I have absolutely no idea if that theory that I concluded bears any reality, it was merely a theory, I dont even know if cactus powder contains any oils. No oils no saponification.
Using too much base, however, I have seen the same phenomenon when trying a freestyle phalaris extraction, not really following any specific tek.

And back to 69's tek which uses CaOH (which is really mild compared to...^), I have never run into any trouble except in purification, but there I used acetone instead of MEK, so that might have been the culprit.

Just trying to un-confuse any confusion I might have created, this tek really works, from my experience all the way to light amber crude mesc.

And yet another edit:
Trying 250 mg of the produced uncleaned full spectrum amber "stuff" which imo actually looked really pretty (see pictures) had a profound effect on me.
Lasting about 6-8 hours I remember sinking into myself emotionally, re-visiting many many awkward situations of my life, looking at them from a totally new perspective, forgiving myself for many wrong doings and even understanding why they were, not as previously thought embarassments, but stepping stones on a path that led to where I am now. No mistakes no learning.
I also remember accidentally breaking a fossilized moss bathroom stone plate from japan, which my wife bought (sucks up water really good) and carefully picking up the pieces and fixing it with glue. During that process, playing with, very old organic substances that were enclosed within, my mind spaced off quite hard on 145 million years old looking like hair or fibre substances, catapulting myself to the Cretaceous period of Pachamama's long history...

Very long talk, and a lot of bla, short version,
I can confirm it works.
 
The Day Tripper
#1066 Posted : 4/15/2012 4:05:23 AM

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SKA wrote:
It's a shame that so often soap forms and makes layers hard to separate.
Obviously mixing dry cactus powder with Lye and then mixing in water
doesn't seem a good idea either.(Reaction heat could break down Mescaline?)

Maybe someone here could revise this method.
As long as the solvents, acids & bases used
are easily obtainable.

Nexus Wiki sais that Mescaline is:
wrote:
Soluble in: alcohol, chloroform, benzene, xylene, toluene, acetone, dichloromethane, highly soluble in isopropyl alcohol, soluble in d-limonene
Moderately soluble in: water
Insoluble in: practically insoluble in ether or petroleum ether


Perhaps dried san pedro powder could be washed with Petroleum Ether first
(or another solvent in which Mescaline is insoluble)
You just soak the SP-powder in Petroleum Ether for 30 mins & then filter off
the plant-oil-saturated Petroleum Ether through a coffee filter. Repeat 3 to 4 times.
After a couple of Petroleum Ether washes the Mescaline in the SP-powder could
perhaps be extracted with several portions of Ethanol.
This Ethanol can either be evaporated on a baking dish to leave a Mescaline residue
or put in the freezer untill the Mescaline crystals precipitate out & then filter out the crystals.

Just a quick sketch based on the Solubility characteristics of Mescaline.
If anyone has a better idea, please share it with us.




As far as mesc breaking down due to naoh reaction heat, i highly doubt thats possible. Mesc, like other phens is pretty damn stable, and it would take temps far exceeding the boiling point of water to break it down, but it would prob just evaporate before it decomposed. And with freebase thats like 350f or something if i remember right.

And for using pet. ether, or other np's to wash the dry powder, instead, i'd consider making a tea/alcohol (etoh, iso) tar, then washing the resin with a much smaller amount of warm NP and keeping the insolubles. I also feel this should be how np washes on lsa extractions should go. Much less solvent waste, and much quicker.

Another method i like, is since mesc fb is very soluble in iso, make a lime/cactus powder paste, add water, mix and let it sit for a day or so, dry it and powderize, then add to a narrow glass container. Pull with DRY isopropyl, 3x, should not require day long pulls, but to be safe i would, plus it gives time for it to decant.

Then collect, filter, and evap that iso, adding distilled vinegar, or dilute hcl water before or after evapping. As long as you salt all the freebase in the dry iso, then wash with a small volume of warm np 2-3x, you should be able to fully dry what remains, wash with cold dry acetone/iso and get xtyals. Acetates might be an issue here as they are more soluble in alcohols vs. hcl, but not impossible from what I've read.

Redissolve hcls in a minimal amount of distilled water, or hot iso, and evap. Iso works better as crystals form sooner and the impurities are less concentrated/get caught up in the precipitates vs. using water, where it crystallizes only at the very end as its so damn soluble. Scrape up, Crush and wash with cold dry iso/tone once more, and you should have almost white, near odorless very sparkly pure mescaline hcls. Acetates work, just make sure you aren't losing product in the cold acetone/iso washes.
"let those who have talked to the elves, find each other and band together" -TMK

In a society in which nearly everybody is dominated by somebody else's mind or by a disembodied mind, it becomes increasingly difficult to learn the truth about the activities of governments and corporations, about the quality or value of products, or about the health of one's own place and economy.
In such a society, also, our private economies will depend less upon the private ownership of real, usable property, and more upon property that is institutional and abstract, beyond individual control, such as money, insurance policies, certificates of deposit, stocks, etc. And as our private economies become more abstract, the mutual, free helps and pleasures of family and community life will be supplanted by a kind of displaced citizenship and by commerce with impersonal and self-interested suppliers...
The great enemy of freedom is the alignment of political power with wealth. This alignment destroys the commonwealth - that is, the natural wealth of localities and the local economies of household, neighborhood, and community - and so destroys democracy, of which the commonwealth is the foundation and practical means.โ€ - Wendell Berry
 
Once
#1067 Posted : 4/15/2012 2:32:23 PM

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Hey guys,

I am doing Rons tek using HCL. I have performed this Tek many times with consistent results, both the Acetate and HCL teks. I the pastI have either skipped the wash step, or have washed with dry 99% Iso. Is there a problem with skipping the Acetone wash and just doing a wash with Iso? I don't have Acetone at the momen and have plenty of Iso.
Logically, I told myself that if Iso was the final step then it should leave me with pure mesc hcl. Wasnt sure if there maybe some impurites that the Acetone will remove that the Iso will not?
My unclean HCL has always been strong, but this time I am really trying to shoot for purtity!

Thanks All,
Once
All statements made by Once have no basis in reality, if reality even exists.
 
biopsylo
#1068 Posted : 4/15/2012 3:29:02 PM

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Quote:
Another method i like, is since mesc fb is very soluble in iso, make a lime/cactus powder paste, add water, mix and let it sit for a day or so, dry it and powderize, then add to a narrow glass container. Pull with DRY isopropyl, 3x, should not require day long pulls, but to be safe i would, plus it gives time for it to decant.

Then collect, filter, and evap that iso, adding distilled vinegar, or dilute hcl water before or after evapping. As long as you salt all the freebase in the dry iso, then wash with a small volume of warm np 2-3x, you should be able to fully dry what remains, wash with cold dry acetone/iso and get xtyals. Acetates might be an issue here as they are more soluble in alcohols vs. hcl, but not impossible from what I've read.

Redissolve hcls in a minimal amount of distilled water, or hot iso, and evap. Iso works better as crystals form sooner and the impurities are less concentrated/get caught up in the precipitates vs. using water, where it crystallizes only at the very end as its so damn soluble. Scrape up, Crush and wash with cold dry iso/tone once more, and you should have almost white, near odorless very sparkly pure mescaline hcls. Acetates work, just make sure you aren't losing product in the cold acetone/iso washes.


this sounds nice, have you gotten good results? i tried a dry tek where the lime paste was dried to powder, and pulled with limonene. this tek failed/ contaminated with salts.

I follow you on this tek until you say "then wash with a small volume of warm np 2-3x" could you explain this step a bit--what np is used, what is it doing, etc..

thanks

 
The Day Tripper
#1069 Posted : 4/15/2012 10:12:50 PM

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I've done a drytek like that with limo, it used far too much limo to make it worthwhile though. Worked great though, just had to filter decant it well, and it turned the limo dark green. That's where alcohols have an advantage, much cheaper and should get the job done in a fully drytek. Never tried it with alcohols, but i am fairly sure its a sound tek in theory. Mesc freebase should be very soluble in dry iso/meoh/etoh.

As far as the NP wash, basically your washing the resin with a Non-polar solvent that the mesc salts should be insoluble in. There should be a couple of np's you can use here, naptha, and heptane are safe bets, prob limo, etc. Anything that won't mix with water, or have any solubility towards mesc salts is what you are looking for.

The warm NP washes off fats/oils/chlorophyll/etc that was pulled by the alcohol, since alcohols will pull polar/non polar stuff. thats Why you get goo resin from alcohols, compared to a much cleaner product from a evaporated tea resin, since water is much more polar and won't pull oils/np molecules like alcohols. You do it after evaporating and salting your resin, since you'll be washing 10x+ less volume than dry powder, and use a fraction of what you would use to wash the powder with a NP beforehand.

Just remember to add an acid to salt the freebase mesc after evaping the iso pulls, otherwise the mesc fb will dissolve if you use limo/tolulene/xylene to wash it.

"let those who have talked to the elves, find each other and band together" -TMK

In a society in which nearly everybody is dominated by somebody else's mind or by a disembodied mind, it becomes increasingly difficult to learn the truth about the activities of governments and corporations, about the quality or value of products, or about the health of one's own place and economy.
In such a society, also, our private economies will depend less upon the private ownership of real, usable property, and more upon property that is institutional and abstract, beyond individual control, such as money, insurance policies, certificates of deposit, stocks, etc. And as our private economies become more abstract, the mutual, free helps and pleasures of family and community life will be supplanted by a kind of displaced citizenship and by commerce with impersonal and self-interested suppliers...
The great enemy of freedom is the alignment of political power with wealth. This alignment destroys the commonwealth - that is, the natural wealth of localities and the local economies of household, neighborhood, and community - and so destroys democracy, of which the commonwealth is the foundation and practical means.โ€ - Wendell Berry
 
Kash
#1070 Posted : 8/16/2012 7:06:53 AM

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So I have a question about this tech, anyone who has better experience with d-limonene feel free to answer...

I am guessing that mescaline hcl is not soluble in d-limonene. Therefore, instead of doing an aqueous acid extract, would it not be possible to precipitate mescaline hcl straight out of the d-limonene by bubbling in hcl gas?

I have done this with some other techs and it can save on hours of evaporation and yeild instant beautiful crystals. Anyone know if you can precip hcl salt out of d- limonene?
--------------------------------------------------*Kash's LSA Extraction* * Kash's Mescaline Extraction*------------------------------------------------------
All things I say are complete and utter ramblings of nonsense. Do not consider taking anything iterated from the depths of my subconsciousness rationally and/or seriously.
 
Kash
#1071 Posted : 8/22/2012 11:42:46 PM

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Kash wrote:
I am guessing that mescaline hcl is not soluble in d-limonene. Therefore, instead of doing an aqueous acid extract, would it not be possible to precipitate mescaline hcl straight out of the d-limonene by bubbling in hcl gas?

Swim tried this and HCl gassing out mesc from the d-limo did work, however the precip was an impure light blue/green likely due to impuirites, and the precipitate was too fine for the filter paper on hand. Thumbs down So, it was not an effective extraction method and swim had to improvise and pull with 1% HCl/H2O.
--------------------------------------------------*Kash's LSA Extraction* * Kash's Mescaline Extraction*------------------------------------------------------
All things I say are complete and utter ramblings of nonsense. Do not consider taking anything iterated from the depths of my subconsciousness rationally and/or seriously.
 
The Traveler
#1072 Posted : 8/23/2012 12:34:18 PM

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One other tek is to salt out the Mescaline by the use of adding FASA to the d-limo, that way the mescaline will drop out in the form of mescaline-fumarate. Infundibulum tought me that.


Kind regards,

The Traveler
 
biopsylo
#1073 Posted : 8/23/2012 10:16:29 PM

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~~Traveler::

does fasa precipitate better than fasipa? fasipa worked well with fresh cooked cactus, but not so well with san pedro powder. dont know why. it is very hard to separate from the dlimo because it is too whispy, and does not hold together to decant. also, it will go thru a coffee filter. this was not the case with cooked fresh cactus that clumped nicely with fasipa, and formed a cake on the filter.
 
mew
#1074 Posted : 8/24/2012 2:46:04 AM

huachumancer


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from my understanding (not experience, as i use an aqueous phase for salting)

fasipa works best with limo and fasa works best with xylene

in regards to powder vs fresh id say the fresh was more potent offering more salts to clump together or try using less limo to saturate it further... 2 cents


i use hcl solution at 1.5-2% evap in dehydrator and wash repeativiely with dry acetone, save washes for later to retrieve lost alks. this yields a brownish tan powder that has yet to fail to impress
 
mew
#1075 Posted : 8/24/2012 2:48:03 AM

huachumancer


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SKA wrote:
It's a shame that so often soap forms and makes layers hard to separate.
Obviously mixing dry cactus powder with Lye and then mixing in water
doesn't seem a good idea either.(Reaction heat could break down Mescaline?)



i always add lye to cacti powder then mix water in, never had a problem with saponification/ separation of layers
 
Kash
#1076 Posted : 9/2/2012 8:19:35 AM

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The Traveler wrote:
One other tek is to salt out the Mescaline by the use of adding FASA to the d-limo, that way the mescaline will drop out in the form of mescaline-fumarate. Infundibulum tought me that.


Kind regards,

The Traveler

Has SWYM tried this and the precipitate been collectable? Its one thing to form a salt and a whole other thing to collect it lol. This would be very ideal if the crystals were actually large enough to filter.
--------------------------------------------------*Kash's LSA Extraction* * Kash's Mescaline Extraction*------------------------------------------------------
All things I say are complete and utter ramblings of nonsense. Do not consider taking anything iterated from the depths of my subconsciousness rationally and/or seriously.
 
Mr. Kush
#1077 Posted : 9/4/2012 7:58:07 PM

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My FOAF is in the middle of this...

He is having a hard time seperating the d-limo from the cactus sludge. When he tries to filter it with either papers or wire mesh the sludge clogs up the pores and doesn't allow any of the d-limo to pass through. He's not able to decant it off the top either...

has anyone come up with a good way to seperate the two?

Sorry for asking, I tried my best to read through the 54 pages, but only had time to scan and couldn't find anything.

My foaf did this a couple years ago with success, but at the time had a buchner funnel he poored it into, the vacuum helped the liquid(NP) come through. He no longer has one...


Foaf was also wondering if seperating isn't doable if he could add more water and NaOH and turn it into a stb. Does D-limo seperate easy or does it form nasty emulsions?

Any advice would be greatly appreciated, thanks!

 
Dante
#1078 Posted : 9/4/2012 8:10:31 PM

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Mr. Kush use the search engine, there are few threads about this same issue.

I remember someone saying that using a white cloth to squeeze all the limo out is very effective.
Listen to a man of experience: thou wilt learn more in the woods than in books. Trees and stones will teach thee more than thou canst acquire from the mouth of a master. St. Bernard
 
mew
#1079 Posted : 9/13/2012 12:59:13 AM

huachumancer


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biopsylo wrote:
~~Traveler::

does fasa precipitate better than fasipa? fasipa worked well with fresh cooked cactus, but not so well with san pedro powder. dont know why. it is very hard to separate from the dlimo because it is too whispy, and does not hold together to decant. also, it will go thru a coffee filter. this was not the case with cooked fresh cactus that clumped nicely with fasipa, and formed a cake on the filter.



couldnt you wait for precips to stop then just add water and let it be separated as an aqueous phase, then evap the water? or would the ipa mess up this theory
 
mew
#1080 Posted : 9/13/2012 1:03:04 AM

huachumancer


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@ mr kush

tell your foaf to use the least amount of water as possible when extracting mesc (especially when your bassifying the powder)

roll basic powder around in a vessel, this separates the dlimo out

try using a caserole dish (the big square pyrex), the more surface area exposed the easier the separation, unless your basic cacti is more of aslurry, if thats the case, well idk man, id add more cacti till it gets clumpy
 
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