Mescaline extraction (salting) problem

[Bosper]

Hi there
I recently started an extraction with the help of this (acid-base extraction of Peruvian incense (by Litmus)) tek. The Xylene layer did seperate quite well, so i took it off and put it into a separatory funnel. Then about 200ml distilled water were added and about 30drops of Hcl (not diluted, i know that was way to much..). The point is now, that the result was .. well.. not expected. The pic shows what i'm talking about.

thats the bottom layer directly out of the sep. funnel. The Layers in there seperated quickly as they should but this is far far away from the clear solution i expected. Anyone knows what this is? I used about 580g cacti powder (from whole, dryed cati-slices), 3L distilled water about 500g NaOH and 1L Xylene.
Now another problem is, that i thought this happend because of the acid, so i put everything back into the big jar and added another 200ml distiled water and 200g NaOH. But now the layers wont even start to seperate... Is there anything how i could save the project?
While writing this i remember something about defatting the soloution... any connections with that maybe?
Thankfull for everyone who has an idea

[sagiboy]

-=welcome to mycotopia Bosper!=-

enjoy your time here, youll get answers soon.

meanwhile, please upload pics to mycotopia using the "Manage Attachments" at the Attach File section while writing a post.

the extraction looking good but im not the man with the answers.

welcome to the best place i know on the net.

[Bosper]

Ah thanks for the hint (and the welcome ^^).
Looked for that option but didnt find it in first place. i'll edit that

[EmmisonJ]

30 drops of concentrated hcl? yeah that's overkill many times over. so you had xylene with an emulsion in the sep funnel. the emulsion consisting of xylene and basic water/ cactus sludge-crap. then you added dh2o to it and acidified as a means of fighting the emulsion? if that is true, then your aqueous layer is a combination of sludge, NaCl (NaOH from the emulsified dh2o neutralized with HCl), and your goods.

what you should have done was this:
separate the xylene from the basic water, entirely, leave no basic water with the xylene. if you're dealing with an emulsion then try to use temp changes (heat works well)/agitation/patience to break the emulsion, sometimes extra NaOH helps, just depends. wash the xylene once with just plain neutral dh2o and then once with saturated brine. if separated well enough there should be close to no water soluble impurities in the xylene, but the washes are quick/easy wash and so i recommend doing them to be sure. the dh2o wash will remove any residual NaOH and water soluble impurities and the brine wash to help dry the organic layer. now you have your relatively clean xylene with the crude freebase and plant oils. now... go ahead and salt it by whatever method you prefer. i recommend for you get some ph strips, they help a lot and are absolutely necessary if you're wanting to do sulfate.

i think your problem was that you jumped the gun and salted it when you should have dealt with the emulsion and cleaned up the xylene first. for dealing with the problem at hand - re-a/b the water layer and reuse the same xylene.

[Bosper]

Actually there was no basic water in the sep funnel. It was only filled with the Xylene from the big jar (like in the 6th step of the extraction guide) and dh2o. Then added 30 drops of Hcl. Normally this should produce a layer of xylene and a layer of clear acidic water or am i missing something here? I have never read that the xylene must be cleaned first? I have some Ph stripes here (1-14) should be ok i think.
But anyway thanks for the advise. As i have put everything back together, this may help me when i start the next try.. I placed the jar in a box with hot water to help the separation, seems to work so far..

hell i wrote all that and forgot to click the post button xD. The 2 Layers are now nearly completly separated. Seperated 10ml Xylene from the Jar and tested with dh2o + hcl. result is as it should be... i have absolutly no idea why this did not work the first time..

[dimension traveler]

Hi bosper and welcome to mycotopia.

sorry I didn't have time to go over the tek u posted but let's see if we can sum some things up here!

Hmmm well in the first picture it looks to me like u seperated the emulsion, meaning you didn't let it seperate all the way. (30 drops hci is way to much).

you say that you added everything back together again, well first did you add more lye and check the ph ( would have changed being 30 hci drops were put in) You only need to hit a ph of 10 to get the alks out but imo going up to 13 is alot better cause it makes seperation alot easier, can't hurt to go over but wont get anywhere if you under base it. Oh I don't believe this was said but did you let the cuctus powder sit in the basified water for a while before attempting to do xylene pull? it needs some time to let it break down, some people say 24 hours I do half of that.

as far as salting goes what I like to do is say take 130ml of dh20 and add 3 drops of hci to it mix with xylene gentlyy swirel around, let seperate give it a minute then seperate it and check the ph of the dh20 if it comes out neutral or acidic then it's good if it comes out basic then I add another drop then mix again with the xylene untill I get it to be as close to neutral as I can without it being on the basic side. (for me it's usually always in the 2 to 5 drop zone but this is for the material I was useing)

Hope this helps, sorry if I worder it shitty let me know if you need me to explain something different/better or if you have anymore questions.

[Bosper]

Hi
Yes i added another 200g NaOH to the mix. The pH is about 13-14.
Well i planed to let it sit but as i was a little excited, i just forgot about it. I added the xylene right after the lye was well shook up with the powder. But after all i think things could turn out well. I evaporated the small test amount pictured above and there was already some result (not measurable with my 0.01g scale but hey it is something ).
Thanks for the tip, i will do it like you said, maybe tomorrow if i can find the time to do it (my cubensis are soooo eager to get into their casings ). But there is yet one question i would like to ask. Which pH value is prefered: more to an acid (4-5) or more neutral (around 7), and why?

[dimension traveler]

IN the end when your salting your doing just that converting the molecule to it's salt form ( was a freebase) using hci acid.
7 is neutral, anything in the solution below that is it's salt form and anything in a solution that's above 7 is in it's freebase form.

So the reason you want to make sure that water comes as close to neutral but a little bit below (6 at the lowest, aim between 6.5-6.9) is so that it will solute into the water(if you dont add enough the mesc will still be in the xylene), altho the more under seven you go the more impurities your going to pull, imo it's very wise to take your time salting because washing a salt is no fun

[Bosper]

Wow thanks thats exactly what i was looking for! So i think i need some more accurate pH sticks now ^^.
I know why i choosed this forum to ask my questions . Even while just reading it is simply -great-!

[EmmisonJ]

glad to hear you got it worked out. you don't read about the xylene washes in other teks because they're not in there, but they're a good idea. i got the idea from ion who uses a very dilute, mildly basic NaOH wash. i just changed it to dh2o and tossed in a brine wash for good measure. halfway stolen from ion and halfway stolen from the workup in some mdma synths.

another thing one could do for really pure crystals is to isolate the freebase by distilling or vac distilling off the solvent leaving the crude freebase. quickly dissolve the freebase (quickly so that the carbonate does not form) in an equal volume of anhydrous IPA and titrate. slowly and very carefully evaporate off the IPA which will evaporate off azeotropically, removing the water present from the hcl drops. once you get a gummy mass then pour enough dry freezer chilled acetone over the gummy mass until it dissolves in the acetone and beautiful crystals will burst into existence. vac filter the crystals and wash with a little more freezer chilled anhydrous acetone. beautiful white crystals. stole that procedure from spiceboy who uses it for mdma crystallization. works f**king awesome just be careful evaporating the bulk of the IPA as to not scorch the goods or evaporate it down too much, you don't want it to solidify or scorch the goods. yeah it sounds like a lot of work but the result is beautiful and you don't have to wait for water to evaporate. i'd only recommend doing this crystallization procedure for an expected 2+ grams of goods though because it's really hard to work with such small amounts. gassing is another option.

[Ferretious]

When using a sep funnel for the acid pull, sit down and lay the sep funnel on your thigh. Then roll it gently back and forward. The way you mix the xylene acid is directly related to how much emulsion you will end up with.Nice and gently, less emulsion. Vigorious shaking and airation and it will emulse.

[Mushroom Kingdom]

I work in an organic chemistry lab and we always shake the crap out of everything we are separating. The reason is, if you don't you're not thoroughly cleaning your solution! Like the past 5 other people have said, you got an emulsion, easiest thing to do is separate it with tons of water (little bit of solution and more water). that way (and be patient) you will have two completely separate layers (orgo layer on bottom, water/brine on top, usually). I get shitty stuff to separate that turn the water dark brown and my shit is a darker brown... You just gotta be patient, and wait for it to completely stop separating ( or at least see a defined line where its separated from the emulsion). Idk if you got one, but if you plan on doing this a lot you should buy a separation funnel, stopcock, and a cap. this will make your life a whole lot easier and they are only like 30$ depending on how big a one you buy. good luck! its kool to see you're getting results!

[whatchamacallit]

SWIM has washed his xylene before salting with dilute lye solution, but he noticed no impurities or color being pulled from the solvent, so he stopped bothering with it. It can help, but usually it's not necessary.

[dimension traveler]

Originally Posted by Mushroom Kingdom

I work in an organic chemistry lab and we always shake the crap out of everything we are separating. The reason is, if you don't you're not thoroughly cleaning your solution! Like the past 5 other people have said, you got an emulsion, easiest thing to do is separate it with tons of water (little bit of solution and more water). that way (and be patient) you will have two completely separate layers (orgo layer on bottom, water/brine on top, usually). I get shitty stuff to separate that turn the water dark brown and my shit is a darker brown... You just gotta be patient, and wait for it to completely stop separating ( or at least see a defined line where its separated from the emulsion). Idk if you got one, but if you plan on doing this a lot you should buy a separation funnel, stopcock, and a cap. this will make your life a whole lot easier and they are only like 30$ depending on how big a one you buy. good luck! its kool to see you're getting results!

I'm at the moment doing a spice a/b, and this is the first time I have ever shooken the crap out of it and all I got to say is that I will always do this from now on.

normally you would have to heat the naptha up to concentrate it but in return you also pull more impurities.

this way I dont have to use heat and it completely concentrates it (when I seperate it it's super cloudy and it started to precip just from the little bittle of coldness that took place from night time.

oH and if you basify it heavily it seperates just fine like in 10 minutes and I mean I really shook the crap out of it for like 5 min.

[Bosper]

OK i'm back ^^.
I tried to wash my xylene with some water/salted water (probably not enough) which helped a bit with that emulsion layer problem. But as i got the water with the goodies out without a loss before, i dont care about that point to much. What i do not understand is, that it seems, like i'm loosing xylene! I started with 1l at the beginning. With the first pull it shrinked down to about 750ml. ok it did not separate well so some might be in the snooze i thought. Now i just pulled out the xylene the second time and there was only 400ml to get out! Both times i used a hot water bath to help it separate, than let it sit for at least 12 hours. May this has something to do with the dark layer which build up on the bottom of my jar? Does anyone have any idea what this is all about?

Another question is about the water i used to wash the xylene with. The first (acidified) water was the normal salting-thing. Because the emulsion was so heavy, i tried to wash it with dh2o and dh2o + nacl. Visually helped a little bit but i would like to know if there could be some goodies in that water too. Or did the majority of the goodies came out with the acidfied water?