Troubleshooting/Questions about mescaline extractoion(2nd attempt)

[Shambalaa]

So last time swim did extraction and it was this Erowid Cacti Vault : San Pedro Alkaloid Extraction type of a extraction tek.

So there was some issues with emulsions when added xylene with basic water, so this took around a week to clear up, would of been faster if swim would of had some knowledge how to help it to clear out.

There was also a little bit emulsion when de-fatting too, but this was pretty minor and swim just discarded that emulsion.

Problem there is that swim used 100g of san pedro powder what is full plant blend most likely, so it wont be so high on alks, but should be higer than swim was able to take out. 100g used, gave around 200mg of very impure acetate goo, so that would be like 0.02% yelid, so swim thinks that there must be a mistake made in process.

Swim boiled cacti powder in distilled water, where was citric acid added PH 3 measured, 3x boiled for 20min. All liquids added together and let sit for almost a week to get some solids to the bottom and this way making liquid more clear. Then de-fatted 3x, but xylene what came of was pretty clear. Then waited few days to get that emulsion cleared, didint work well so discarder all that emulsion, just a tiny bit. Then making fb mescaline with lye water added to the acidic water, PH almost 14. Then added xylene 100ml and swirled around and turned upside down and all that, gigan emulsion problem, added more lye and salt to help that emulsion to clear, did take that almost week to clear. Added more xylene another 200ml, worth of 3 pulls, but end up doing only one pull with that 300ml. After seperating layers after long wait, did 3x pulls with vinegar, used mainyl pure 5% vinegar with it. And evaporated in oven 100-125c and end up with that ~200mg of mescaline acetate goo..

So few things that swim can think that went wrong is that mescaline got destroyed by that strong base liquid. Or some how using to acids was not good idea, should of use citric acid all the way or vinegar all the way. Or didint do enough pulling with xylene from that base water, but that 300ml xylene was there almost one week,everything should transfer there faster than that? Or oven evaporated or destroyed that mescaline. Or the final reason, swims cacti is really weak..

Swim did try that mescaline acetat, but it was so mild, just treshold level, maybe just a bit over, felt stimulated and funny, some nice glimmer, but thats all. But it sure is mescaline!! :d

Does somebody have any idea what might of gone wrong? Need some help with this before attempting another 100g.

 

[Shambalaa]

Btw,

Swim is planing maybe to switch aceitc acid to phosphorica acid, not sure, but it would be easier to clean, but if swim keeps yeliding 200mg, there is no point to wash is away. Also swim has been thinking if there would be better solvent option too instead of xylene.

Psychedelic Compounds Chemical and Physical Properties - DMT-Nexus Wiki

wiki.dmt-nexus.me

wiki lists soluable stuff there and gives acetone and touluene, would those work instead of xylene? And is there some properties that would be better or wors than xylene?

 

[endlessness]

Several things to comment there.

1- Your cactus may be weak to begin with, its impossible to know beforehand.
2- Boil for more than 3x20min, try 3x 40mins or first 20 min, then 40 min, then 60 mins boil. Also try pressure cooker if you have access to one.
3- Citric acid works fine but you can just use vinegar since its cheap and easy to find and proven to work just fine
4- No need to defat
5- If there's emulsions, dont add just a bit of salt, add loads of it, and lye, and vibrations (like on top of speakers or washing machine) also help clearing it up. It should clear up in a matter of minutes, not days.
6- 3x xylene pulls are not enough, and specially 1 big pull is not enough. Read our FAQ why 1 pull is not enough. Also mescaline freebase is somewhat soluble in water so you need to do more pulls to get it all out. Do 5 or 6 pulls or something, and make sure to separate most of the layer before adding the next, so that its really 5-6 pulls and not one big one.
7- Extract more than 100g, otherwise its too much trouble for too little results, try 2 or 300g.

Also, dont use phosphoric acid, stay with acetic acid or use HCl or sulphuric acid.

Toluene works equivalent to xylene, and acetone cant be used because it mixes with water.

 

[El Mescalero]

ENDLESSNESS WROTE: Several things to comment there.

1- Your cactus may be weak to begin with, its impossible to know beforehand.
---True

2- Boil for more than 3x20min, try 3x 40mins or first 20 min, then 40 min, then 60 mins boil. Also try pressure cooker if you have access to one.
---I agree. This is the most important part of doing an acid extraction. You should boil it long enough so that it strains easily through T-shirt material. I would boil the first time for an hour with constant stirring to prevent scorching and addtion of extra water if the level gets too low. Subsequent boils don't need to be that long to make it easily strainable. You can boil down the combined pulls later to get a manageable amount to work with. What you want is liquid with minimal solid material. Pressure cooking at 15psi for 30 minutes works for sure.

3- Citric acid works fine but you can just use vinegar since its cheap and easy to find and proven to work just fine
---Go with vinegar or hydrochloric acid. Given the availability of vinegar and how safe it is to work with, I'd choose vinegar.

4- No need to defat
---If you boil or pressure cook adequately, you don't need to defat. Emulsions are common with defatting.

5- If there's emulsions, dont add just a bit of salt, add loads of it, and lye, and vibrations (like on top of speakers or washing machine) also help clearing it up. It should clear up in a matter of minutes, not days.
---As long as you suction only xylene and avoid the bottom layer it doesn't matter what's in the aqueous layer. Salt and lye are cheap. You can add so much that it lies on the bottom of the container because no more will dissolve and you won't hurt anything.

6- 3x xylene pulls are not enough, and specially 1 big pull is not enough. Read our FAQ why 1 pull is not enough. Also mescaline freebase is somewhat soluble in water so you need to do more pulls to get it all out. Do 5 or 6 pulls or something, and make sure to separate most of the layer before adding the next, so that its really 5-6 pulls and not one big one.
---The real pearl of wisdom here is that several small pulls are superior to one larger one. It has to do with what is called the partition coefficient.

7- Extract more than 100g, otherwise its too much trouble for too little results, try 2 or 300g.
---Working with 100 grams will work if everything is done correctly, but if you're doing it right in the first place, why not start with more and end up with more? That said, while you're working out the kinks, a smaller amount can keep you from wasting starting material.

Also, dont use phosphoric acid, stay with acetic acid or use HCl or sulphuric acid.

Toluene works equivalent to xylene, and acetone cant be used because it mixes with water.

The only thing I would add to the great advice Endlessness has given you is that you really need to write everything down so you end up with a clear record of what works and what doesn't, since you want to perpetuate success not failure. Also, you should consider using sulfuric acid to salt with. The sulfate form has to be the easiest to completely purify since you can do a recrystallization with boiling distilled water and acetone to get very, very pure product. Washing the hydrochloride form with acetone and IPA just isn't the same as recrystallizing.

 

[Shambalaa]

So big thanks for both of you guys!

Next extraction will be done with 150g of san pedro, just dont wanna waste it if it goes wrong again, if it will be succes then there will be a reason to move for bigger quantities. So swim luckly owns a pressure cooker, so that will be coming handy again for acid pulls that will be done 3x 40-60min, maybe that first one just for an 20min, not sure if there is any difference really.

No defatting was totaly new thing, that will be intresting, so cacti is not so fatty or is there other reason for not doing defatting?

Most likely there will be vinegar used for this whole process, not sure if there will be sulpuhric acid envolved yet, gotta think about this, just it would be easier to clean than acetate and there is no MEK around, only MEK(p), but swim dont know enought about chemistry to say that would work too, so acetate sounds safer and easier.

And xylene pulls will be done 5-6x with smaller amount of xylene, maybe 100ml.

That re-X from sulfuric acid sounds good, but swim gotta ask that with what porporcion there will be water and acetone added together? And how safe that is to boil?

And last question, what do you guys think, is there any good reason to let those first acidic water pull to settle down that all solids will fall of and that water becomes cleaner, ofcourse there would be filtering done with this before with coffee filters, but to get those smallest particles out to the bottom, is that really necessary? It will take almost a week to get all those out by just waiting gravity to pull them down.

 

[Shambalaa]

What would you guys think about this simple titration, and dual solvent crystalization - Preparation - Welcome to the DMT-Nexus

Would that be wise to do after acid pulls from xylene? To get pure product, sounds easy and simple, ofcource it requires use of sulphuric acid, but that would not be a problem..

 

[Shambalaa]

So swim started second attempt with extracting mescaline from san pedro.

-150g san pedro powder is added to pressure cooker
-4l of ph 3 water is made(used citric acid)
-1l of water is added to pressure cooker and boiled under 12psi for 40minutes and this is repeated 4x and after every pull ph is confirmed and shows ph 5, so it has come up from ph 3 to 5, it seems that alkaloids are still moving to acidic water. So swim decides to taste that san pedro and it tastes very slightly like alkaloids, but way less than in begining and that extracted water taste like alkaloids big time, so if there is anything left in that powder its something very small amout. But incase swim puts that left over cactus material on pyrex and let's it to dry if there is something in it for future.

- ~4l of slightly acidic water is reduced to 2.5l and stored in two tall bottles for next step. So now is time to wait that most of those solids are falling out to the bottom to those bottles, they have been filtered before adding them to the bottles with t-shirt and after that with coffee filters, there is nothing in those coffee filters so its pretty clean already.

So question is how important is to let all those solids to fall to the bottom of these bottles? Swim thinks that if those small particles fall out that might reduce emulison risk in future and thinks that one week should be enought to get most of them to fall to the bottom. Is there risks that mescaline might start to break down in one week in that acidic water and is there any point on in this waiting?

Next step would be to reduce that water to 250ml and make it basic and start to pull with xylene.

Swim has also played with idea that what if that mescaline should become mescaline citrate when its pulled out in xylene, rather than acetate. Swim know that it's not easy to make good citrate, but by titrating it should work right? It would be easier to clean than acetate.

Thanks for help!

 

[Shambalaa]

edited topic from(before 2nd attempt) to second attempt.:thumb_up:

 

[dg]

the link above is good
if you want a pure material to work with some type of crystallization is advised

that said 200mg from 100g cactus is .2%- Sounds about right for the average PC san pedro

 

[Shambalaa]

Okay dg, Swim is not sure how to proceed that crystallization yet, not sure witch point it is to be done, but swim hopefully will figure that out. Soon will be the day to take this project to the end, but still waiting gravity to pull all the solids to the bottom. Swim did filter everything with thick t-shirt and after that with coffee filters, but nothing really stayed in those coffee filters, but now swim waited almost a week and there is some sediment at the bottom, hopefully that helps with emulsion problems, this time swim will take that shaking easier anyways!

 

[Shambalaa]

Okay,

Yesterday swim had change to continue this extraction process and next things followed.

After one week waiting for all solids to fall down, looked pretty good and clear. Reduced that 2l of water to 200ml of water. Next is adding lye to the water slowly to gain ph 13-14. Then swim did 5x xylene pull for this base liquid(and saved it in case). Then swim did citric acid water and pulled 5x from xylene, last one out of those five was probably too much, because PH did not go up at all. Well then all that water was reduced in oven on pyrexpan, it looked really bad for a moment, but hey, mescaline is quite soluble for water, so even tiny bit of water holds loads of it. So now swim has X-amount mescaline citrate, looks to me 5x more than from first attempt, so swim was soooo happy. It looks amber colored and when scraped of from that pan, it had spiny crystal shapes on it, most likely from that oven drying came that color, next time swim will use fan!

Well, swim learned quite a lot from this.

-No de-fat needed when doing A/B
-Do small pulls, but more
-Use proper gear and know when and how to use them

Swim is not chemist so this has been miss and trial type of journey.

Cant wait to measure my final product!

Not sure if there is any ways to clean mescaline citrate, but swim is just fine with this!

Next time swim will try to pull more stuff from that base mescaline liquid after that swim will use much more cacti for this.

So thanks for everybody for supporting me!

 

[Shambalaa]

Okay, swim had chance to measure the weight of final product and it is 309mg mescaline citrate out of 150g of san pedro cactus, so its not so good ratio, but swim has still quite a lot of this stuff still and its not only skin like most of you use.

Today swim will try to pull more stuff out of this base mixture and see if there is still something left, because swim did only 5x pulls with xylene and this mixture was only swirled around to prevent emulsion. So swim thinks there might still be much more, this time swim will give more shake. :twisted:

 

[Shambalaa]

Swim had some luck and did 4x xylene pull and used vinegar instead of citrate this time and gain 200mg mescaline acetate. Swim thinks that there will be more in, so swim is going to do one more and see again, till nothing comes out. Maybe swim should use HCL so all these could be purified. It should still work if swim would just dissolve that citrate and acetate to water and add some hcl in it, that should make it mescaline hcl right?

Swim has been drying all these products in oven around 125celcius so its all brown gunk and does not look very pretty, but this is just because these are just practices, so next time there will be fan+air drying to get nicer product. How you guys keep all the dust out when you air dry your stuff?