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Offlinesancho
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what went wrong with my mescaline extraction?
    #3872263 - 03/05/05 10:46 AM (12 years, 2 months ago)

so here is what i did, step by step.

-first i took the cactus and stuck it in a blender
-heated with a cooking stove 3 times for an hour, each time adding new distilled water and filtered through coffee filter (no acid added).
-combined all three water/mescaline washes and boiled down to half volume.
-placed the not quite syrup (more like dirty brown water) into two half gallon mason jars.
-did about 6 defats with naptha per jar and then gave up trying to remove fats!
-added basic solution (each jar about 2 cups from a quart of water with around 20 spoonfulls of NaOH added).
-did 4 washes on basic water solution with 1-1.5 cups of naptha each time. after each wash added more base.
-combined naptha/basic mescaline solution and did a polar wash- added few grains of NaOH to distilled water. three polar washes.
-added my acid. on accident used way to much. distilled water and HCL in ratio of 1:10 or 15. used about a cup of this for my first wash. did four distilled water washes on non polar. each time added a tad more acid.
-evaporated with fan and heat pad.

what went wrong? at the end, i noticed that i had a bunch of salt remaining, and that is about it. some fine cactus particles as well. i noticed during my extraction that when i did the naptha wash, a bunch of fats came along with it. i mean a bunch. but as a few minutes past when sitting in with so much NaOh, the fats began to disappear. when i added the acid, all the fat was gone and i had two perfect layers. is that normal?

should i use xylene instead?

could it be too much acid? or should i start differently/ add acid when boiling? i have no idea what temp. i let the solution boil at. it was a rolling boil for the hour.

any help would be awesome. im quite bumed out that this did not work.


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OfflineGNIOM1498
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Re: what went wrong with my mescaline extraction? [Re: sancho]
    #3872317 - 03/05/05 11:10 AM (12 years, 2 months ago)

-did about 6 defats with naptha per jar and then gave up trying to remove fats!

skip that step its useless
u got salt because of HCL + NAOH = NACL (salt) im curious did u use a seperatory funnel?


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OfflineGNIOM1498
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Re: what went wrong with my mescaline extraction? [Re: GNIOM1498]
    #3872322 - 03/05/05 11:14 AM (12 years, 2 months ago)

I'm guessing there is mescaline in there but there is a lot of salt in there so u can't tell.  also how long was the wait until u pulled the alkaloids out of the basic solution with naphtha.  Xylene and Naphtha are the same but xylene i found to be cheaper.
how basic is the solution?  the reason i ask this is because i read and it makes sense that a highly basic solution would begin to break down mesc.  Man i know that feeling ending up with nothing.  happened to me my first 2 runs. there shouldn't have been any fats or needles or NaOH.  But ya u got that from erowid so did i waste of time doing that defat.  I did outside hovering around 10 no seperatory funnel just droppers.  Took me over a week to complete 18 hrs to finish with the water ready to evaporate.
-boil cactus
-make basic
-pull with ur naphtha i used xylene
-then add HCl to the naphtha
-evaporate
so i figured u got mesc in there but just a lot of salt so u can't dose correctly.  Man that sucks i hope u didn't do a lot of cactus.  If neuro or Ekstaza come on they would probably know for sure what went wrong.  I feel ur pain man ive been there. :frown:


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Edited by GNIOM1498 (03/05/05 11:33 AM)


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Offlineesin
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Re: what went wrong with my mescaline extraction? [Re: sancho]
    #3872418 - 03/05/05 12:03 PM (12 years, 2 months ago)

I dunno why you failed.
There's lots of shroomerites failing and i can't really understand why. Especially in a mescaline extraction which is quite forgiving, compared to say growing shrooms or extracting pure enough DMT.


Your specific case:
-I see you boiled the cactus for only one hour each time: Well i had to boil for a total of 8h in two passes to get all the mescaline taste out of the cactus pulp.

-I also see you added a lye solution instead of straight lye: you used 2 cups per jar which increased your volume quite a lot - this can lower your efficiency.

-You experimented instead of following a specific tek. Which is something that most people who failed did.


So what i can say to people considering attempting this extraction is: FOLLOW THIS DAMN TEK exactly as it says, no experimenting on the first time.

If you start with fresh cactus, make a tea or syrup like mjshroomer recommends, but instead of boiling only once, boil twice for 4h each boil - until no bitter taste remains on the pulp.

Than reduce to a practical volume, basify with quite a lot of STRAIGHT LYE, add xylene/toluene, stir for 10-20mins, let stand one day, and follow foaf's tek EXACTLY like he says, from the "Syphoning" step forward. I must repeat: exactly like the tek says (separate xylene, recover mesc with dilute HCl, return xylene into the cactus soup, let stand one day, separate, recover mesc again, and repeat until the cactus soup is spent).

If you start with potent cactus and do this there is no chance of failing, really.

Defatting isn't necessary because the alkaloids end in an aqueous solution, and fats aren't water soluble.

(Keep in mind that the measurements in foaf's tek are for 1kg of dried cactus - which usually yields 10-12g of mescaline. Reduce/increase amounts appropriately)


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Invisiblemoecat
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Re: what went wrong with my mescaline extraction? [Re: esin]
    #3872493 - 03/05/05 12:35 PM (12 years, 2 months ago)

.


Edited by moecat (10/17/05 09:05 PM)


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OfflineAuroricDistortions
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Re: what went wrong with my mescaline extraction? [Re: moecat]
    #3872567 - 03/05/05 12:54 PM (12 years, 2 months ago)

Both are standard acid/base extractions on plant matter. It helps to use slightly acidified water to boil the cactus for the first step; it will salt the mescaline, and increase efficiency.


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Invisiblemoecat
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Re: what went wrong with my mescaline extraction? [Re: AuroricDistortions]
    #3872708 - 03/05/05 01:50 PM (12 years, 2 months ago)

.


Edited by moecat (10/17/05 09:04 PM)


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Offlinesancho
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Re: what went wrong with my mescaline extraction? [Re: moecat]
    #3872997 - 03/05/05 03:20 PM (12 years, 2 months ago)

no, i did not use a sep. funnel.

see, i thought i could deviate from the teks a little because many a times (around 5) i have extracted dmt not really following a specific tek and have had GREAT results every time. well, not the first time. it seems i always mess up the first time, but then i learn from my mistakes. the second time is the charm! it is not that i am experimenting, im just modifying a tek slightly for a different situation.


thanks all.

so you time that boiling for a longer time, not using base+water, only base would most likely help? and skip the defat?

but other than that, does the process seem fine?


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Offlineneuro
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Re: what went wrong with my mescaline extraction? [Re: sancho]
    #3873258 - 03/05/05 04:34 PM (12 years, 2 months ago)

Quote:

-heated with a cooking stove 3 times for an hour, each time adding new distilled water and filtered through coffee filter (no acid added).
-combined all three water/mescaline washes and boiled down to half volume.
-placed the not quite syrup (more like dirty brown water) into two half gallon mason jars.




You should have added acid. The reason for starting your acid base extraction with aqueous acid is to protonate the alkaloids making them more soluble in water. When you've not added acid you're not going to get very much of the alkaloid base into solution.

You can set it up as an equilibrium equation, where you'll have a very small Ksp value (ie very close to zero) since the alkaloid doesn't have appreciable solubility in water, though it has some due to interactive hydrogen bonding. But that's simply not enough to get an decent yield.

Alkaloid-NH2 <---(H2O)---> Alkaloid-NH2 Ksp <<< 1


basically you'll have more of what's on the left side of the arrows than the right

When you add acid you shift the equilibrium

Alkaloid-NH2 + H+ <----> Alkaloid-NH3+ (aq)

Ksp ~>> 1

Protonation makes the alkaloid more soluble. Thus you'll have it in your solution and not bound up in the plant matter.



Here's where your problem is.


>>-did about 6 defats with naptha per jar and then gave up trying to remove fats!

This was probably over kill but not a source of problem unless you lost stuff in emulsions and never waited or tried to settle out the emulsions.


>>added basic solution (each jar about 2 cups from a quart of water with around 20 spoonfulls of NaOH added).

Again this is why i stress creating standardized solutions.



>>-did 4 washes on basic water solution with 1-1.5 cups of naptha each time. after each wash added more base.

I don't understand this. Please describe your procedure here. Washing what with basic solution and naptha.


The rest i'm not realling following.


Naptha is fine over xylene.


As for your basic procedure it should be

Heat plant matter in acid maybe a few times, strain and collect all water.

Add naptha to remove fats and oils. Becareful of emulsions. If you get emulsions heat your vessel to separate it out.

To the aqeuous acid solution add your base from your standardized base solution. To titrate excess acid and protonated alkaloids Check pH.

To that add naptha again, remove aqeuous layer keep naptha.

You can now do two things migrate to aqeuous phase again (addition of H+ and then OH) and recrystallize with a solvent mix don't worry about NaCl it'll stay in solution while Alkaloid crystallizes out. Or leave it in Naptha and evaporate off the naptha and collect crystals, wash and dry and do whatever else you want.

To naptha layer add some grains of CaCl2 to dry naptha solution.


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Offlinesancho
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Re: what went wrong with my mescaline extraction? [Re: neuro]
    #3873807 - 03/05/05 07:18 PM (12 years, 2 months ago)

neuro- basically, after i add the base, it will be soluable in naptha. then i add acid/polar (water) to naptha, so alkaloids migrate to water. i evaporate the water and what remains is a mescaline salt.

you always speak of standardized solutions. in my last post you said you would elaborate, but i guess you never got around to it. i would really appreciate it if you explained what you mean by that. i really am no chemist.

thanks!


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OfflineCatalysis
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Re: what went wrong with my mescaline extraction? [Re: sancho]
    #3874849 - 03/05/05 11:07 PM (12 years, 2 months ago)

Quote:

neuro- basically, after i add the base, it will be soluable in naptha. then i add acid/polar (water) to naptha, so alkaloids migrate to water. i evaporate the water and what remains is a mescaline salt.





No, if it is soluable in naptha that means it will dissolve in naptha and not water. NaCl dissolves in water and if you got salt, it means you evaporated water instead of the naptha and there is zero mescaline in your product.


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Offlineneuro
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Re: what went wrong with my mescaline extraction? [Re: sancho]
    #3874945 - 03/05/05 11:23 PM (12 years, 2 months ago)

>>neuro- basically, after i add the base, it will be soluable in naptha. then i add acid/polar (water) to naptha, so alkaloids migrate to water. i evaporate the water and what remains is a mescaline salt.

Correct, but i'd probably do this. Add naptha, stir it in good, then separate off the aqueous layer. Take that aqueous layer and add more naptha and separate off the aqueous layer and discard it. Combine the naptha layers. Dry it with pellets of CaCl2 and remove the resulting water that layers out (you'll probably have to use a pipette to get it out).

Now depending on the acid you use you can evaporate off the aqueous layer but i wouldn't reccomend doing that. I'd work on an isolation technique and recrystallize. So you could depending on the acid evaporate it off and have somewhat pure mescaline salt with some residues but that can be cleared up with recrystallizing what's left from the evaporate in a solvent mix. But don't ever consume what's left from an evaporated aqueous layer without recrystallizing it.



On the standardized slutions some people answered it so i didn't think it was necessary to reiterate it. But it's basically done by creating solutions of known amounts of base and known amounts of acid in it so you don't have to do a guess and check type thing.

Since 1 equivalent of HCl neutralizes the same equivalent of NaOH 1 mole (which is 6.022x10^23 particles) of HCl neutralizes 1 mole of NaOH, and 1 mole is simply the atomic weight of the molecule. Thus we take 1 mole of HCl and put it in water, and 1 mole of NaOH and put it in water.

That way we know that 250ml of acid solution contains the same equivalents as 250ml of base solution that way you don't have to be guessing with how much acid to add or not. You added 250ml of acid so you add 250ml of base + some extra to titrate the protonated alkaloids too.

You can think of it like this

1HCl + XAlkaloids-NH2 --> Xalkaloids-NH3(+)(aq) + 1-XH(+)(aq) + 1Cl-(aq)


Thus we know we have 1 equivalent of Acid to neutralize plus the alkaloid, and that can be determined by the original amount of acid we added plus the unknown amount of alkaloid. Takes the guess work out of things.


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Offlineneuro
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Re: what went wrong with my mescaline extraction? [Re: Catalysis]
    #3874965 - 03/05/05 11:27 PM (12 years, 2 months ago)

Quote:

Catalysis said:
Quote:

neuro- basically, after i add the base, it will be soluable in naptha. then i add acid/polar (water) to naptha, so alkaloids migrate to water. i evaporate the water and what remains is a mescaline salt.





No, if it is soluable in naptha that means it will dissolve in naptha and not water. NaCl dissolves in water and if you got salt, it means you evaporated water instead of the naptha and there is zero mescaline in your product.




I think what was implied here was that naptha would be added. As i elaborated in my post

And what he's saying about mescaline salt is mesacline-hcl which is considered a salt, salt does not just mean NaCl.

And if only aqueous acid was added to a naptha layer and no base was added afterwards before the evaporation of the water then no NaCl would be created.


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Offlinesancho
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Re: what went wrong with my mescaline extraction? [Re: neuro]
    #3877528 - 03/06/05 04:05 PM (12 years, 2 months ago)

>I'd work on an isolation technique and recrystallize

what do you mean by isolation? by that you mean doing something like taking the naptha/basic/mescaline solution and adding hcl until all the mescaline percipitates out? if i do that, will it have to be neutral, or will a ph of 5 or so work?

but for the first time, i would like to make it as easy as possible. so if i just add water+acid and evaporate and then recrystalize, i should be fine, right?

so do you see any other major problems with my procedure other than not boiling longer and with acid water?

thanks.


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Invisiblephalloidin

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Re: what went wrong with my mescaline extraction? [Re: neuro]
    #3878511 - 03/06/05 06:35 PM (12 years, 2 months ago)

would you just use water for recrystallizing mescaline?


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InvisiblelIllIIIllIlIIlIlIIllIllIIl
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Re: what went wrong with my mescaline extraction? [Re: phalloidin]
    #3881859 - 03/07/05 10:23 AM (12 years, 2 months ago)

This is a bit off topic but here goes...

Could you use one of new and more efficient spice teks on mescaline cactus (instead of MHRB) without changing any of the steps? Why or why not?


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Invisiblephalloidin

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Re: what went wrong with my mescaline extraction? [Re: lIllIIIllIlIIlIlIIllIllIIl]
    #3881971 - 03/07/05 11:27 AM (12 years, 2 months ago)

the spice teks are for extracting freebase, so you would need to add another step to convert the mescaline back into a salt. I don't think those teks would be as efficient though, because they are designed specifically for the delicate nature of DMT. Mescaline is a lot more stable and can take all kinds of abuse.


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Re: what went wrong with my mescaline extraction? [Re: phalloidin]
    #3883346 - 03/07/05 05:52 PM (12 years, 2 months ago)

How much do you pay a bottle of Xylene ? and what kind of shop !
In France it is very difficult to find this ! i just saw by web shop at 35 dollars the bottle !
but naphta is only 3 dollars ! naphta is better or not to use in the extraction ?

i find this extraction method :is there somebody who use this method ? without xyl?ne but with chlorogforme :

EXTRACTING MESCALINE FROM PEYOTE IN THE KITCHEN

1. Obtain 50g of dried ground peyote and put in a 500 ml Erlenmeyer flask.

2. Add 250cc of wood alcohol, cover the flask tightly, and let cactus powder oak it up for one day, with occasional stirring.

3. Pour off the wood-alcohol solution into a 500 ml beaker, filter properly, and place in a well ventilated place to evaporate.

4. Again soak the plant powder in the flask fo two hours, but in 100cc of 1- normal hydrochloric acid.

5. Filter, discard the mush, and combine the filtered HCL solution with the residue from the evaporated wood alcohol solution. Filter again.

6. To the solution add enough 2-normal potassium hydroxide until the solution is normal.(Turns pH paper beige.)

7. Add 100cc of chloroform, stir, and let the mixture stand until it separates into two layers,

8. Separate the two layers, using a separatory funnel and discard the water(top) layer.

9. Add 40 cc. of water to the chloroform, shake, and separate the layers again, Discard the top layer.

10. Filter the chloroform, evaporate, and dissolve the gummy residue in 20cc of wate. Refilter it. Makes about one dose.

CAUTION: Although this method is suppose to reduce the foul taste and smell of peyote, it still might make you nauseated. Vomit, puke, etc., but you'll get VERY stoned. The nausea will pass.


Edited by mezkal (03/07/05 05:53 PM)


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Invisiblemoecat
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Re: what went wrong with my mescaline extraction? [Re: mezkal]
    #3883405 - 03/07/05 06:06 PM (12 years, 2 months ago)

.


Edited by moecat (10/17/05 09:02 PM)


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OfflineEkstaza
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Re: what went wrong with my mescaline extraction? [Re: moecat]
    #3883844 - 03/07/05 08:05 PM (12 years, 2 months ago)

You are all trying to use overly difficult techniques to do something that others have found simpler ways to do.

So, go ahead and continue to chip away at your stone wheels or get going with this simple extraction technique written up by a master at TheNook.


Posted by: ion Feb 17 04, 05:52 PM GMT
Finally!! Cactus extraction made easy!

I'd like to thank foaf and owen for their contributions to this technique. Thank you both for sharing your hard-earned knowledge with the rest of us!

Also, thanks to droop23 for the suggestions on clarifying some things. : )

OK!
Here's what you need:


Materials:
I am listing more materials than are necessary... this should encourage you to read the instructions carefully... or at least get some extra stuff!

500 g of dried cactus chips (home-made or purchased)

2 or 3 plastic cans of Red Devil lye (find this brand... go to less popular stores if you must)

1 gallon of Kleen-strip brand xylene (the can says "Xylol")
-OR-
1 gallon of Kleen-Strip brand toluene (the can says "Toluol")
The word "xylene" will be used in the instructions, but may be substituted with toluene if that is the solvent you choose to use.

1 bottle (pint or quart) of acetone (right next to the xylene)

1 bottle (pint or quart) of sulfuric acid (available as Dr. Wellfish [Aquarium Pharmaceuticals] brand "pH Down" @ Petco or online)
-OR-
1 bottle of muriatic (HCl) acid (at hardware store, used for cleaning concrete. try Lowes)

2 or 3 gallons distilled water (if you can't find this... you might have a problem tongue.gif )

Optional: 1 bottle of grain alcohol (95% ethanol)


Equipment:

For safety:
Neoprene chemical-handling gloves (in the solvents section, usually)

Safety goggles or glasses

Box of baking soda

Bottle of vinegar

Large glass or HDPE turkey baster, 1" piece of clear tubing, and a disposable pipette tip
(walmart, lowes, and online or lab buddy, respectively)
-OR-
Siphon pump and tubing, and a disposable pipette tip
(maybe hardware)

Masking tape, grease pencil or something else that can impermanantly mark plastic or glass.

Wide spout plastic funnel (used for canning... so look around the PC's and jars in the store)

Normal spout glass or metal funnel (listed in order of preference, no plastic unless you can be sure it is HDPE or LDPE. )

Cotton balls (100% cotton... each one looks like a tiny "roll" of stuff)

Large HDPE plastic jar (carbuoy) or jars (enough to hold 1.5 gallons of liquid) with HDPE lids. Glass jars can be used, but there have been many problems with the bottoms of the jars breaking due to etching from the lye. If you decide to use glass, be extremely careful! See "Tips" section.

2 of ~one pint glass bottles with a small necks and tight-fitting, solid lids. (this lid can be made of HDPE or metal... whatever it is, just make sure that xylene or toluene will not soften it!)

Glass dish (for evaporating)

Blender (preferably industrial metal, but glass works)

Freezer (set as cold as possible)

1/4 inch steel rod, non-threaded, preferably stainless... the length depends on how tall your tallest jar is... you want it to be long enough so that at least 6 inches stick out from the jar. (available at hardware store)



Here's what ya do:

Step 1-- GRINDING
Place both hands into the bag of cactus and grab a 5-6" diameter "ball" of chips. Put this into the blender and grind it to dust. Pour the dust into the extraction jar.

DO NOT use any water or be in a humid environment!! I'm quite serious about this. nono.gif
Also, do not try to grind more than one scoop of chips at a time... otherwise you will end up with a lot of un-ground material at the top.

Repeat the ball-grinding step until all cactus is pulverized and in your jar.



Step 2-- MIXING

PUT YOUR GLOVES AND GOGGLES ON!!

You will need approximately 3/4 to 1 gallon of water for every 500 grams of cactus... however many jars that will take. Save the water jug(s)!

You will need 1 full can of lye for every gallon of water used... so if you used 3/4 gallon of water, you need 3/4 can of lye.

Order of mixing:
Mix 3/4 to 1 can of lye per 500 grams of cactus powder. Just mix the dry lye into the dry cactus powder. This mixture will warm up a bit because there is always some water present in the plant material.

Level off this mixture in the jar by shaking it down. Allow the mixture to sit for one hour, uncovered.

Pour xylene (or toluene) into the jar. Pour just enough to match the level of the powder in the jar... all the powder should be saturated, in other words.

Slowly pour water into this mixture while stirring with the steel rod. Fill the jar only to the base of its shoulder.

Heat will be generated, so beware of vapors from the xylene or toluene... toluene will make more vapor, but both require decent ventilation. NO SPARKS OR FLAME IN THE VICINITY!!
Let the solution cool before proceeding.

Now pour a small layer of xylene over the top of the slurry.

MARK A LINE on the outside of the jar with some masking tape, grease pencil, or whatever, exactly at the level of green goo in the jar (the base of the xylene layer). You can use a rubberband, but be aware that solvent vapors (and the likely small spills) will eventually destroy the thing. This demarcates the level that the xylene layer should reach in the future, before you remove it.

If filled properly, this layer of xylene is only about an inch or two high... it should only be maybe 1/8th the volume of the cactus water mix.



Step 3-- EXTRACTION

Cap the jars tightly and shake the hell out of them... invert, roll, shake, whatever. Just mix it all up until you can no longer see a xylene layer at the top... it should just look like a green speckly mass in the jar. Tighten the lid periodically, just in case! ohmy.gif

NOW WAIT. I mean it. You may see separation of the layers begin in a few minutes, and it may even look completely finished in a few hours (according to your mark)... but it's not. The xylene contains very tiny cell fragments that must have time to settle. Wait at least a full day.






Are you waiting? I sure hope so...



Alright. Now the xylene layer should be colored anywhere from yellow to green to orange, depending on your particular cactus. In all cases, it should be totally clear... no cloudiness at all. If there is still cloudiness, put the jar in the fridge for a few hours and see if it clears up. Hopefully so...

Assemble your baster: Push the peice of tubing onto the end of the glass baster and then push the pipette tip over or into the tube... just make sure everything fits tightly.

-OR-

Assemble your siphon: Just push the pipette tip into or onto the siphon tube.

You need the pipette tip to keep the baster from dribbling, and it aids precision when sucking up the xylene layer with either the baster or the siphon... However, if you are unable to find a pipette tip, you will just have to practice your precision.

Well... now ya gotta suck up the xylene. Be careful not to get any of the fine white "dust" on the top of the goo layer... and be careful not to disturb it. It may take a little finesse (especially without the pipette tip), but you'll figure it out.

Squirt or siphon all of this xylene into your smaller bottle. If you don't have a pipette tip, you can hold your finger over the end of the baster to keep it from dribbling as you move from extraction jar to the bottle. You will have to leave some of the xylene behind to avoid sucking up the dust... don't worry, you won't miss anything by doing this. ; )

Thus far, this is all quite similar to foaf's tek: http://forum.thenook.org/index.php?showtopic=13271&hl=extract

However, this is where it gets a little different...

You will only need to use the same xylene over and over. You'll see.



Step 4-- SALTING
Now comes the best part.

This first part is OPTIONAL... it is only listed here for the particularly anal (like me : P ).

Pour about 1/6th the volume of xylene as distilled water into the bottle. IOW, if you have 60mL of xylene, you only need to add 10mL of water.

Add a few granules of lye to the bottle. An approximate measure is this: for every 10mL of water, add 1 granule of lye. Use a pencil or something... just stick it into the lye and a few granules will stick to it... scrape the granules into the bottle with your fingernail.
-Alternately-
You can mix this weak lye-water before adding it to the bottle.

Cap the bottle tightly and shake it up well.

You will likely see some discoloration of the water. This is good.

Siphon or separate this water from the xylene in some way. It can be added to your extraction jar, so don't worry if you suck up a little xylene (you'll get it back, later)... just get all that lye-water out of there!

If there are droplets on the walls of the glass, you can either leave them there, or empty the jar, rinse with a bit of fresh xylene, and wash the jar out.

-end optional portion-


At any rate, when the xylene is back in the bottle and the water is gone, it's time to add acid.

The Aquarium Pharmaceuticals pH down is a decent dilution of sulfuric acid... you will probably not need to dilute it further, but doing so won't hurt.

However, if you have stock sulfuric acid (~18M), then the dilution ratio is about 2mL acid per 100mL water.
If you have muriatic (HCl) from the hardware store, the dilution ratio is about 3 or 4mL per 100mL water.
These ratios are approximate... it is not necessary to measure these things precisely. You do not need to dilute the acid, yet. Read further...

If you have access to concentrated acid (18M sulfuric from chem supply or muriatic from hardware), you can drop the acid into the xylene directly, then dilute it with water, later.
You will see the acid droplet suddenly turn into tiny crystal powder as it falls through the xylene. Add one drop at a time. The powder will be white, but eventually you will see a drop that turns black or dark green for a second... swirl the xylene and see if the dark area becomes light again... if so, add another drop of acid.
Repeat this process of addition and swirling until you get a drop that stays dark... it will likely leave a sort of greasy smudge on the glass. If it remains darkly colored, you are finished adding acid. Technically, you should finish on the drop before it stays dark... but you will only be able to find that drop with practice. wink.gif
This method will get you the most crystal with the least excess acid at the end.

So... dilute your acid/powder at the bottom of the xylene with some distilled water. About 1/6th the volume of xylene should be your acid water volume... same amount as the "cleaning" lye-water in the optional step. Cap tightly, and shake it up, baby!

Let it stand upright for about a minute, and loosen the cap. Now screw the cap down only just enough so that it is slightly past the point where the cap stops with gentle pressure. Not too tight, but not too loose... you need it on to keep xylene from evaporating out, so don't just leave it off.

Now here's where owen's tek comes in... Stick the bottle in the freezer. biggrin.gif

See more about this process here: http://forum.thenook.org/index.php?showtopic=16130

I have modified this a little to avoid "ice droplets"
This is my version:

1. Let the acid water freeze solid.

2. Take it back out of the freezer and let the water (the ice plug on the bottom) thaw back to a liquid. (all ice droplets will be at the surface of the bottom ice, and will thaw and mix with it)

3. Put it back into the freezer again.


Once it's frozen solid again and you remove it from the freezer, you will need to do the next few things rather quickly...

Open the cap... this may be tough, unless you left it properly loose. You are just "pre-opening" the bottle to make sure you can do it easily when you need to.

Once it's open, tighten it back down well, and swirl the xylene around a bit. You may see fluffy stuff floating around in it... this is just some sort of fatty or proteinous material (and probably a little mescaline salt)... you just don't want it sitting on top of your ice plug.

While it's swirling, open the cap and pour the xylene into the other salting bottle.

Add a little room temp distilled water to the ice plug and swirl it around for a few seconds. This will melt the top layer and clean the ice plug. Pour this sludgy water into the other salting bottle with the xylene. Repeat if necessary, but don't melt the whole ice plug with it.

Set aside the iceplug to melt.

Now add some pure water to the xylene bottle (to make 1/6th volume, again), shake, let settle a bit, and repeat the double freezing step.

When finished freezing, swirl the xylene and pour it back into the extracting jar(s)*. You can rinse the iceplug as before, but you will pour the sludgy water into the extraction jar.

*You can repeat the salt-washing step more than once if you like, but returns are minimal.

Let the ice plug in the bottom of this jar melt and combine it with the water from the first ice plug.

Repeat the EXTRACTION and SALTING steps another 3 to 5 times. You will probably be able to use the same xylene for most or all of the passes.




Step 5-- PURIFICATION
Pour all of the acid-salt-water (from the ice plugs) into the evaporating dish. Rinse the bottle with a bit of fresh distilled, and pour this into the dish, too.

The fastest way to evaporate the water is to set up the dish on a heat pad, in front of the outlet air of a dehumidifier... but it's not necessary. You can use a fan to speed it up, also.

However, the slower the water evaporates, the more perfect the crystals grow. This is especially pertinent when working with HCl.

Once the crystals have formed and all the water appears to be gone, you're ready to purify and clean the crystal.

Notes on specific salts:

If you used sulfuric acid: There may be a small amount of brown liquid leftover with the crystal... this is acid and it will never evaporate. If you see this, then just evap with heat until you see no further reduction in liquid volume.

If you used HCl: There will be residual HCl gas trapped inside the crystals. The best way to remove this is to finely grind the crystals and heat them in an oven at 200?F for about half an hour.

When finished evaporating, pour a thin layer of acetone over the crystal. This loosens it from the dish, as well as sucks up any leftover water... it can also suspend any excess acid.


The filter funnel:

Take a cotton ball and look at it. You will see that it is cylindrical... each end of the cylinder looks "twirled". This is because the "ball" is actually a thin sheet of cotton that has been rolled up into a cylinder shape.

Now, you want a cylinder of cotton that is about 1.5 times the diameter of the spout of your normal funnel (the glass or metal one). Simply unwrap the "roll" until you reach the desired diameter. You can make a larger ball if necessary by unwrapping a second cotton ball and then wrapping the strip around the first ball... wrap in the opposite direction that the first ball is wound.

Gently push the end of this cotton cylinder into the receiving end of the spout of your funnel (iow, from the top of the funnel). Make sure it is snug but not too tight in the hole. Push it down until the top of the cotton is still about the original diameter, but the lower portion of the cylinder is well in the funnel spout.
When all is done, the cotton "cylinder" will be slightly mushroom-shaped. You'll figure it out.

Set up the filter funnel over a jar... be sure there is airspace around the rim.

If you used sulfuric, simply pour/scoop the crystals and acetone into the filter.

If you used muriatic (HCl), then you need to grind the crystals up in the acetone. They should already be ground from the "baking" step, anyway. In this case, you may also need a more tightly-packed cotton ball to keep from losing the fine powder.

Rinse the crystals with a gentle stream of acetone. Rinse until the drips from the bottom of the filter are clear.

Allow the funnel to drain and dry completely... there should be no more acetone smell emanating from the funnel when it is done.

*Optional (higher purity, but may result in loss of product) : Freeze the dried funnel, crystals, and a clean jar. Place some grain alcohol (sealed) in the freezer, also, until it is as cold as it can be. Set the funnel on the clean jar (all still in the freezer), and pour a small amount of the cold alcohol over the crystals in the funnel (just enough to cover them). If it is draining swiftly, just leave it in the freezer. If it is slow, move the setup to the fridge.

Take the funnel and hold it over a clean evaporating dish. Pour hot, warm, or room temperature distilled water over the crystals in the funnel and swirl gently. The water temperature is determined by the size of your dish... the smaller the dish, the hotter you want the water (just so you don't have to use as much water).

As a general rule, the cooler the water, the less crud will be flushed through the cotton... but if you were clean about your processing up to this point, then you can use as hot of water as you wish!

Allow the water in the dish to evaporate, leaving large beautiful crystals of mescaline salt.


That's it! Weigh and enjoy!


Tips:

Plastic vs. Glass-- It is best to use HDPE (high density polyethylene) for containing strongly basic solutions (lye water). Glass will etch and eventually crack in the presence of such a solution. Glass is okay if you can do everything within a week, but life generally keeps that from happening tongue.gif ...also, re-use of that glass vessel for any future extraction is not recommended.
HDPE is not as clear as glass, but that is its only drawback here. The safety it provides far outweighs the slight inconvienience of reduced visibility.
HDPE can be identified by the triangle of arrows imprinted on the plastic... this triangle should contain a numeral 2, often with the letters HDPE under it, aptly enough. Most plastics that look similar to a translucent milk jug are HDPE... the stuff is everywhere.

Pouring solvents-- place the steel rod over the mouth of the solvent container and point the end of it into whatever container you wish to pour into. Pour slowly and the solvent will travel along the rod, instead of creeping back and getting all over the place. *This is especially helpful when pouring the acetone/crystals out of the evaporating dish into the filter funnel... since the evap dish is not likely to have a spout.

Drying acetone-- in order to keep from dissolving any of your alkaloid salts while cleaning, you may want to dry the acetone. This is easily accomplished by a few grains of dry magnesium sulfate (oven-dried epsom salt) to the acetone. Just be careful not to pour any of this drying salt into your alkaloid.

Washing crystals-- sulfuric is not exactly soluble in acetone, just suspendable. So, you may need to crush up the crystals a little bit to get into the pockets of excess sulfuric between them, so that the acetone can rinse them out mechanically.
As mentioned, this crushing is inherently necessary with HCl salts of mescaline.

Heating HCl salts-- Once this is done, acetone is only necessary if you wish to clean up the colored impurities... in other words, you don't need to use the acetone as long as you don't mind a little crud.

Extra basification-- you will notice that the cactus material begins to get less and less gooey and more like a liquid as time passes. This is due to the lye (most likely).
So, before re-adding the xylene from the salting step, you can plunk in and stir a little extra lye into each jar. This will help keep it nice and basic. Lye becomes baking soda after a while, which is only a weak base... so adding a few tablespoons of lye before re-extraction will push the pH back up to where it needs to be. Just be careful not to put so much lye in that the liquid level gets too high!

Recovery-- there may be some mescaline salt that gets washed through the cotton ball during purification with acetone (or the optional cold ethanol wash). It won't be much, but for purists, I am including an easy remedy:
Evaporate off the liquids in the funnel collection jar (some may remain if sulfuric was used) until there is very little left. This jar is then covered and placed in the freezer for a week or two. When the time comes, add a little cold acetone to the jar, swirl, and pour the liquid through a clean filter funnel setup. The sulfate salts will look like little white BBs in the funnel... (I haven't tried this with HCl salts, though).

Recrystallization (a method of further purification)-- This can be done as long as you have access to some kind of 95% alcohol (usually ethanol, but possibly isopropanol [strong rubbing alcohol]) AND some way to safely heat it (sparkless hotplate and blowing air ventilation). You also need a beaker and a thin, straight, colorless glass vessel (look for plain vases in the craft store). One last item you'll require is oven mitts... practice holding and pouring the beaker (full of water) with the oven mitts to avoid any mishaps later!
-Put the mescaline salt into the beaker and pour about ten times that powder volume as alcohol over it.
-Heat and stir the liquid till boiling. Dissolve all of the mescaline salt in the alcohol. Add more alcohol if necessary.
-Place the thin glass vessel near the hotplate, but not touching it. This should somewhat preheat the glass to avoid shocking it, later.
-When all is dissolved, continue boiling to evaporate the alcohol, stirring occasionally, until you see a tiny amount of solids begin to form. This means that the solution has reached a supersaturated point and can no longer "hold onto" the mescaline salt. DO NOT look over top of the boiling solution!! The vapors can hurt your eyes and nasal passages! Watch for solids through the side of the beaker, only.
-*When you see solids, turn off the heat and put on your oven mitts. Pick up the beaker with both hands, spout facing outward, and pour the hot alcohol solution into your thin glass vessel. The alcohol will be hot enough to burn you, but probably not hot enough to shock the glass and break it... no guarantees, though... anything can happen.
-You will probably see crystals begin to grow immediately. It's really cool to watch! 8D
-Place some plastic wrap over the top of the vessel and put it in the freezer. Let it sit overnight.
-In the morning, pour the crystal wad and liquid through a cotton ball filter and rinse with freezing cold alcohol... this is similar to the optional ethanol rinse mentioned earlier.
-To recover more crystal, you may reheat the alcohol and evaporate it until you see solids form again... just start at the * step and follow the process down.

One jar or many? --
One large jar has the advantage of being very easy to manage... but it takes longer to extract all the goodies... in other words, it takes more passes with xylene.
Many smaller jars have the advantage of speed (fewer passes on each jar, and all are processed at the same time)... but they are difficult to manage.
Just decide what is more important to you... ease or speed?
...and, no, adding a larger xylene layer to the big jar will not help... use only small xylene layers in any jar.

A note about impurities --
-As far as we are concerned, there are two things in the xylene after using it to extract the cactus... mescaline and impurities.
-There are two kinds of impurities in the xylene... non-extractable and extractable.
-There are also 2 kinds of extractable impurities... those which are affected by acid, and those which are unaffected by acid.
-When we add acid to the xylene, 2 things are extracted (salted out)... mescaline and extractable impurities (both acid-affected and not).
-Now, mescaline is much more "attractive" to the acid than the impurity is.
This means that mescaline is going to be salted out first, more or less.
The impurities will also come out of the xylene... but only after the mescaline.
*This means that you will only get a lot of color if you add too much acid.*


--------------------
YOUR EXPERIENCE WITH ANY GIVEN DRUG ISN'T THE DEFINITIVE MEASURE OF THE DRUGS EFFECTS.


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