Author Topic: mescaline extraction  (Read 2187 times)

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GOD

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mescaline extraction
« on: March 25, 2002, 10:55:00 PM »
greetings my children.
i'll bet you never imagined to bee hearing from me over the WWW! at the HIVE no less?
well, actually I have a question for YOU!
it seems GOD was attempting to extract mescaline out of San Pedro cactus, and he/she/it encountered a little problem.  He (there you have it folks! difinative proof that GOD is a male entity!) first soaked dried/powdered cactus in methanol then filtered a few times followed by evaporation of said MeOH.  To the resultant crud was added a bunch of dh2o pH ~1 to 2.  This crud was again filtered (to remove the gummy tar that occampanied the mix) and then dcm was added in order to defat.  Here is where the problem lies.  The combined contents in GOD's separatory funnel have been sitting for over 24 hours and it is extremely difficult to differentiate the two layers.  GOD knows that under normal circumstances, dcm will sink and form the bottom layer within the separatory funnel.  It appears as if GOD didnt filter the acidified gunk enough, there doesnt seem to be a clear layer between np layer, emulsion and aqueous layer (that combined with the fact that everything is so increadibly dark- even if the layers were clearly distinct, it'd bee rather difficult to see).
GOD fears that there is so much heavy stuff within the aqueous layer, that it approaches similar density to the dcm layer thus confusing GOD as to what should bee collected/discarded in order to save aqueous layer.
Another factor which has added confusion is that GOD continued to add more and more dcm in hopes of diluting dcm layer so as to make things more visable.  This created extra confusion as both layers appeared to gain size as the extra dcm was added! There is the faintest of lines between the dcm layer and emulsion, but no distinct layer visable between aqueous layer and emulsion.  Another added factor that confuses GOD: when he has tried to drain off some of the bottom layer and smell, there is only a slight smell of dcm and a fair amount of the smell of his origional aqueous solution. And likewise, when he opens the sep. funnel and smells inside through the stopper, he smells strong dcm vapors (however, this may bee just because the dcm was added last, and there is/was a bunch along the sides of the sep. funnel)

so here are GOD's questions:
1. is it possible that the aqueous layer has gained so much crud from the cactus that it would actually bee more or equally dense as the dcm?
2. seeing that there is a strong probability that GOD didnt filter the initial aqueous solution as good as he should have, would it bee smart for him to do this now?

GOD is open to any flames, advise, questions or opinions.
Prayers however, will not bee listened to, as it is part of my cosmic plan to allow you folk to suffer without reprive in order for you to remain utterly dependant on me and my so-called "priests" and churches.  enjoy.

aquagirl

  • Guest
salts
« Reply #1 on: March 26, 2002, 12:48:00 AM »
I've seen an extraction posted where the non-h2o-soluble sulfate salt was simply precipitated out.   somewhere in general forum along time ago
 

(retired)
She Who Dances With Hampsters

GOD

  • Guest
sep and filter more
« Reply #2 on: March 26, 2002, 01:59:00 AM »
yes, GOD did add aprox 2.5 times (pH ~1.5 dh2o) the volume of the gunk left after evaporation, he also heated it up to near boiling to try and make the insoluble tars fall into solution.
He has tried the flashlight thing and still cannot see past the liquid!(way too dark/thick!) only the bottom inches of the sep funnel are able to allow light to pass.

BEND OVER AND PROSTRATE YOURSELVES BEFORE ME!

paranoid

  • Guest
Seems to me the simple solution would bee to add ...
« Reply #3 on: March 26, 2002, 06:47:00 AM »
Seems to me the simple solution would bee to add more water (and HCl to acidify along the way, don't want the mescaline jumping ship to the DCM).  Your post is a little confusing (not a place to take shortcuts now), but I gather you did this.  Would adding a bright food coloring help (red)?  Would it stay in the aqueous phase?

Also, maybe just filter the whole damn mess as it is for now, try to get most of the crud out.  Then check out your solvent mix and attempt separation again.  Adding salt may help break the emulsion.  Maybe boiling with charcoal might help clear things up.

Mescaline is quite heat tolerant, so heating and distilling the DCM should not be a problem.  If you've got distillation equipment, this might be your best go at it.

monkpea

  • Guest
Can the damn stuff just be steam distilled out of ...
« Reply #4 on: March 26, 2002, 07:46:00 PM »
Can the damn stuff just be steam distilled out of a basic solution of pulverised plant material???

GOD

  • Guest
with all of the tars and fats contained within ...
« Reply #5 on: March 26, 2002, 09:06:00 PM »
with all of the tars and fats contained within cactus, GOD believes (with his limited chemistry know-how) that the product would bee quite impure

BEND OVER AND PROSTRATE YOURSELVES BEFORE ME!

ClearLight

  • Guest
Use kitty litter!
« Reply #6 on: March 26, 2002, 11:02:00 PM »
ClearLight ( an emanation from GOD  :)  ) had a similar problem trying to extract the goodies from the peganum harmala seeds purchase for $2.50 a pound at the local arab market under the name "esphand". Even though an acidic solution was used, WWAAAAAYYY too much fatty material came over in the mix... more dcm added more acidification and the next thing you know I'm sitting there with 2 liters of dcm extract, an unbreakable emulsion in my 2l flask all for 250 ml's of peg seeds!!!
  So, I noticed this stuff glowed under U.V. and grabbed one of the handy chromo columns about 3 feet long and 1/2" diameter and packed it with unscented kitty litter! Washed it down with dcm until clean and then ran all the dcm/fat stuff through the column. Watched the fat glom onto the kitty litter and then the yellow florescent goodies peel off and flow into the beaker... vac distill under reduced to strip and then the usual b/a/b gas operation.

  Got to make sure you kitty litter is the cheap stuff and does not come with additives...makes a very nice chromo clay...

Infinite Radiant Light - THKRA

GOD

  • Guest
mescaline extraction emulsion dcm
« Reply #7 on: March 27, 2002, 06:38:00 AM »
ahhhhh
GOD thanks fellow bee's for their helpful advise.
the problem was that the aqueous layer was brought down to a pH of ~3, when an ~2 is needed.
GOD carefully separated both layers and found that the top layer had a pH of ~3 so he knew which layer was which.
He distilled the dcm layer (reclaimed the solvent, no need for waste!) and added some dh20 ph ~1 and brought that to a near boil to try and dissolve the tarry gunk.  Meanwhile, he put the aqueous layer through another filtering (with cotton balls).
Once the aq. layer made it through the filter, GOD dumped the pipeing hot tar-water through the filter.  The reclaimed dcm was added to the funnel, and then the aq. layer was added (not before verifying w/ph paper that the pH was below 2).
This time, the layers separated nicely and GOD could see the tars and fats migrating through the emulsion layer and into the clear dcm layer on the bottom.
The initial problem was definatly caused by too high of a pH (poor technique on GOD's part not checking with pH papers!)


BEND OVER AND PROSTRATE YOURSELVES BEFORE ME!

GOD

  • Guest
damnit!!!!
« Reply #8 on: April 07, 2002, 07:28:00 AM »
GOD dreamed that he had completed the above extraction and was left with a red, tar-like substance (as opposed to the crystals he was looking for)
He now understands that the reason he didnt get crystals is because he didnt defat enough!
evidently, one needs to defat until the np one is defatting with shows up clear when mixed with the (acidic) aqueous solution.
so GOD tries his hand again, round number two, this time GOD goes out of his way to defat the hell out of the acidic solution in hopes of obtaining a clean product.  He starts off with aproximatly 800 grams of dried, ground peruvanis cactus.  3 X MeOH soak/reflux.  Evap/recover meoh.  Add near boiling acidic dh2o (pH ~2, maybee a little under).  Filter several times to remove sediment/undissolved tar.  DEFAT.
ok, here is where the new problem lies.  working with about 2.5-3 liters of aqueous solution in a four liter separatory funnel, GOD goes through about 1/2 to 3/4 of a gallon of dcm.  The non polar layer gets clearer and clearer with each new addition of dcm.  Hardly any emulsions are (seemingly) formed because for the first few washes, GOD very carefully adds the non-polar and is also careful not to agitate, he just gently swirls.  Once the washes appear to start getting lighter and lighter (indicating that the aqueous layer is not as saturated with dcm soluble fats, tannins and whatnot)  GOD starts to agitate the mixture progressivly harder as he notices that the emulsions that do form are rather thin and whispy and settle out within 10-15 minutes if GOD buggers with the sep funnel (he likes to use an electric massager to vibrate the sep funnel which helps speed the breaking up of the emulsion layer).  The last wash GOD did with dcm, he noticed that he was just about run out of dcm.  So he decides to shake the living shit out of his funnel in hopes of getting one last really good, clean wash.  He figures that his aq layer is almost all clean now, so no big emulsions should form. WRONG.
He is left with a huge, spongey emulsion and very little non polar settling out.  shit, theres hardly any dcm left and GOD isnt going to the chem supply store again -no way, no sir, no how.  He's gotta go find someone to do it for him, but until he does (or until he gets off his ass and distils some from some stripper) he's gonna do some 'speramentin', well its experimenting for him anyway.  He realizes that although dcm is what he's going to end up using for his final extraction (of freebase mescaline) he can still use any other non polar solvent to continue pulling fat from his aqueous solution.  Maybee he thinks to himself, that by adding more non-polar, hell help make the nonpolar more nonpolar (the same way brine or salt can bee added to emulsions to make the polar layer more polar- his chemistry knowledge isnt that technically sound, but he says fuck it and gives it a try anyways).
He adds some xylene (straight outta the can from his local hardware shop). Fuck! GOD forgot that some solvents will float, and some will sink.  He knows that dcm sinks (thats what hes been using up to this point) but now hes looking at a clear puddle sitting on TOP of the aqueous layer and his emulsion is on the bottom.  Anyways, with just a little movement of the funnel, GOD watches the xylene drop through and pulverise the emulsion on the bottom! It didnt completly destroy it, but he noticed that it made the once geletanous emulsion now become thinner, and lighter.  So GOD shakes (swirls) the shit out of the funnel and notices the emulsion continues to break even more.  A few more of these xylene washes, and the emulsions almost completly gone!  But now theres another problem- after the xylene has been removed, so now just the aqueous layer remains, GOD notices that the aqueous solution has gained considerable volume! He hadnt noticed this before (while he was using dcm) but it possibly could have been a gradual buildup while he was uding the dcm (his guess) OR it could have gained volume when he used the xylene, he isnt sure when it happened.
what the fuck?
there is no visable emulsion layer...
???
GOD is confused.
a few other tid-bits-
When GOD looks into his aq. layer, he see's tiny little specs and tiny little flakes floating around.  He assumes the flakes may be fats that have settled out of solution..? They are really "light" and never really seem to settle ( theyre real small and move around like snow does in those glass christmas thingys you shake to make it look like its snowing)
also, the aqueous layer smells strongly of dcm (or so he thinks, it could bee xylene smell, theyre kinda close, and GOD really hasnt taken the time to become a conniseur of carsinogenic solvent vapors so he has a hard time differentiating the two).
and when the aq. is left to sit for a long time, the thinnest layer of those little spec's will settle to the bottom and take on the appearance of a thin (aprox 1 millimeter) emulsion layer.
---------
not knowing what to do, GOD empties his separatory funnel and puts his aq. solution into a bunch of canning jars (he is considering gently heating some of his solution in a distillation setup to see if dcm comes over, he'll record temperatures as shit comes over) in this way, he hopes to determine if the added volume is just unseparated dcm (which he hopes, but doubts because there doesnt seem to bee ANY form of an emulsion left)
he doesnt really know what else the problem could bee.
He aquired the dcm from a friend, maybee his friend accidentally added some h2o to the dcm? dunno, GOD has to wait for his friend to come back from vacation.
Do any bees think any kind of azeotrope may have formed?
any thoughts or ideas for GOD?
GOD is also considering just saying fuck it and continuing on with a little more defatting when he gets more solvent and then basifying and going on with the extraction- but he knows that it'd probably bee wise to wait and get opinions.
any help is appreciated


BEND OVER AND PROSTRATE YOURSELVES BEFORE ME!

uemura

  • Guest
Confirm bad news
« Reply #9 on: April 07, 2002, 10:06:00 AM »
Just for confirmation, even it doesn't help much. Extraction of Trichocereus spec. material with chloroform didn't work either for Uemura because of all these troublesome emulsions. Ever thought about soxhleting dried plant stuff? Works nice for Psilocybe cubensis!
Carpe Diem

bujinkan

  • Guest
wow god
« Reply #10 on: April 07, 2002, 01:45:00 PM »
thanks for the worthless news...(god)


ie..fuck off.

GOD

  • Guest
where the hell did that come from?
« Reply #11 on: April 07, 2002, 08:49:00 PM »
re-read asswipe, that was a question, not news.  There was alot of detail given so's that possibly someone in the know might bee able see what I did wrong so as to help me.

fuck you too.

uremura, pulling with methanol alleviates the emulsion problem.  Just keep soaking with methanol 'till the pulls start getting a lighter and lighter color.
Then evaporate the methanol until your left with a tar-like liquid.  Go on and perform a regualr acid/base work-up.  Also note, that when you initially acidify the tar, it helps to use near boiling hot h3o+, then filter the fuck out of it (youll have to use cotton balls, filter paper will get clogged) and move on to defat (several times till the np - which you should use dcm- is absolutly clear) then basify, extract w/dcm, backwash with slightly basic dh2o then evap or collect solvent. walla!

BEND OVER AND PROSTRATE YOURSELVES BEFORE ME!

metwurst

  • Guest
Alternative San Pedro extraction.
« Reply #12 on: April 23, 2002, 03:43:00 PM »
Excuse me GOD, but you might wish to consider this method

Post 263746

(cornelius: "novel mescaline extraction", Methods Discourse)
for extraction from San Pedro. It is reasonably quick, and much less messy than extraction from dried cactus.  It uses only DCM as a solvent, and starts with fresh cactus. It has been tried here, and verified to work. It's feasible that with some extra cleanup, gassing with HCl might yield crystals, though no-one here has felt the need to go any further than the resultant oil.
If you need to store the oil in capsules for any length of time, you'll need to remove any water with vacuum.