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PH when salting mescaline and emulsion question? Options
 
Shambalaa
#1 Posted : 10/17/2012 1:34:57 PM
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Swim feels that it is hard to find detailed instructions for extracting mescaline and that has raised a question that what should be PH when salting mescaline from basic solution? Swim is gonna use acetic acid, just normal vinegar 5% acetic acid.

And last thing is that swim has wondered that how long it takes to get layers from xylene and cactus water when de-fatting the solution, so how long swim should wait that all that xylene has come to the surface?Love

So swim wants to find right PH for salting mostly pure mescaline out from xylene, just because swim wont be able to clean mescaline acetate after its done. Swim is not able to get MEK for cleaning and not sure if there is way to re-X mescaline acetate without having to use some crazy chemicals.. Confused
 

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El Mescalero
#2 Posted : 10/18/2012 3:40:59 AM

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Are you asking what the pH of the acetic acid should be before adding it to the xylene, or are you asking what the pH of the water layer should be after mixing it with the xylene?

The pH of 5% acetic acid would be around 2.5. If you are trying to titrate the amount of acid added to keep the pH of the water layer after mixing at the optimal level, I would say a pH of 7 is adequate. The problem with driving the pH to low is that you will pull more unwanted substances along with the mescaline.

I'm not sure exactly what you mean by the second question. If defatting is done at all it's done to the acid-water layer gotten from soaking/boiling the cacus in acid-water. In some extractions the cactus is boiled or soaked in an acid/water mixture to turn the mescaline into a salt that is soluble in water. While in its salt form, the mescaline won't dissolve in xylene, but unwanted fats will and can be separated and discarded. Many extractions go straight to basifying the cactus/water material. Then the mescaline is taken out of its salt form and into its free base form that soluble in xylene and not water. The time for the layers to separate varies for several reasons. What you look for is the water layer to be clear and not cloudy. It can be clear and yellow colored, but it shouldn't be cloudy since that indicates that there is xylene still suspended in the water layer. And then there are emulsions which is whole different conversation.

You likely knew much of this already, but I hope this helps in some way. Good luck.

Shambalaa wrote:
Swim feels that it is hard to find detailed instructions for extracting mescaline and that has raised a question that what should be PH when salting mescaline from basic solution? Swim is gonna use acetic acid, just normal vinegar 5% acetic acid.

And last thing is that swim has wondered that how long it takes to get layers from xylene and cactus water when de-fatting the solution, so how long swim should wait that all that xylene has come to the surface?Love

So swim wants to find right PH for salting mostly pure mescaline out from xylene, just because swim wont be able to clean mescaline acetate after its done. Swim is not able to get MEK for cleaning and not sure if there is way to re-X mescaline acetate without having to use some crazy chemicals.. Confused

I am El Mescalero and I demand Mescaline for the Masses!
 
Shambalaa
#3 Posted : 10/18/2012 8:46:15 AM
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Right on! That actually answered swims question perfectly, nice!

Gotta admit that swim did not write so clear questioning, but hey, you got the point.

So now swim has whole new 'problem' with emulsions, like you said it is whole new conversation too, so here is the problem.

-Swim used 100g of san pedro cacti powder, did 3x~30min boils with distilled water and added citric acid that Ph would be around 4. So far good.

-Swim did let the solution wait 2 days to get more solids out from the water and then used siphoning to take good water to new container. so far good.

-Then swim did de-fatting with xylene 3x and did give swirling and turning upside down bottle for around 50-100 times, stopped counting after 50. Got some really minor emulsion here, but still everything ok. Then swim left de-fatted solution to stand another day, to get more plant material out.

-Then next step was to add some basic water(lye+water) Ph was set to 12(for the final solution). Then swim added xylene for the solution and swirls it around gently and turns it upside down gently as well, but swim finds out that lot of emulsion starts to form up, so now all the xylene is trap with the water and it wont separate nicely at all. So swim goes google and finds out that salt would help to remove emulsion and separate layers nicely, well swim makes the solution saturated with salt, then it start to look like it is separating from not only from xylene but from other stuff too, it looks like it has more than two layers coming up. So swim decides to read more and finds out that hot bath would help, tries that, it wont do a thing, so swim reads more and adds more lye to make it more basic again, nothing happens still. So swim ends up putting the bottle away and wait another day or two to get the emulsion to separated and hopefully to see if there is more than two layers of stuff.

So here is few question what needs to be cleared from swims mind..

-Is there a way to avoid formation of emulsion or is there reliable why to make it happen faster?

-Swim has about 300ml of basic cacti water and swim added around 200ml of xylene to that to pull mescaline FB, but now swim has run out of xylene and wonders if that amount would be enough or should swim buy more xylene and do two more pulls?

-Swim is wondering if adding salt is good idea, swim does not know what salt actually will do for that basic cacti water at all, but it looked to swim that it started to separate other stuff too, so question is what it could be, it looks like solids almost, like adding vinegar to milk type of a thing going on?

-And is there any way that salt in lye water would form something with that solution?

-How long it takes to lye to start to break up mescaline, swim don't wanna let it destroy just because of emulsion?

-And finally if you guys know any good way to clean that final product, assuming that swim gets anything out from it, so it would be in mescaline acetate form? Is re-x possible, if it is how swim can do it?

Well this is swims first time with extracting mescaline and not sure witch tek is best, but this was what swim decide to do first, next time it might be something else. Swim wont do extraction with d-limonene, because its way too hard to find anything from here, so xylene is only option?. There is also no way to get Hcl or other acids than citric acid and acetic acid. Only chemicals swim is able to get hands on are lye,xylene and acetone.

Oh, and final question for now is, is there good way to dispose xylene? or just gassing? Swim read from internet that some people discard their xylene right down from toilet, this sounds wrong to swims ears, could some one confirm swim what to do with it? Swims common sense says that it should be gassed out. Or is there way to clean it from fats and other stuff, other that distilling?

Smile yahoo!
 
dg
#4 Posted : 10/18/2012 2:53:56 PM
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using swim in every sentence is annoying, hard to read your post

use the search engine, tons of threads on breaking emulsions Smile
 
El Mescalero
#5 Posted : 10/20/2012 2:25:47 AM

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DG is correct, there are lots of threads about emulsions, but let's just agree that emulsions are a BITCH!

First off, I think it's best to do everything possible to avoid creating an emulsion in the first place. I see in several places that people say add the non polar and "shake the hell out of it." That's a mistake. If you look at an organic chemistry lab manual the usual procedure is to gently shake the separatory funnel upside down then back right side up 10 times then let the layers separate. After they have mostly separated it can be done a couple more times. If you are doing three pulls on the material that's plenty of mixing to get all the product.

Let's say you did this and you still got an emulsion, and that happens because, as I said, emulsions are a BITCH and they can happen no matter what.

My first step is to warm the container in a hot water bath. Patience is the key because it should stay in the bath a couple hours. If the emulsion is layered out so that it lies between the top and bottom layer, gently stirring the emulsion layer with a stirring rod can help as can tapping on the container.

If that doesn't work then adding more lye is the next reasonable step. You really can't add too much. If you do the only thing that's going to happen is that no more will dissolve in the water layer and it will settle on the bottom. You can start by adding the same amount of lye you originally added then agitate 10 times and let it sit.

If you still have an emulsion you can add salt. What adding salt does is that it makes the water layer even more polar, and that should squeeze out the nonpolar mescaline into the xylene layer.

I do these things in the order above with the reasoning that warming the solution adds nothing to the container, adding lye is adding something that's in the bottle already, and finally using salt which does add to the solution.

So if you do all of this and you still have an emulsion then more drastic measures can be taken.

If the emulsion is layered out you can siphon off the xylene plus the emulsion layer being careful not to get any of the water layer then transfer to a separate container. Add anhydrous magnesium sulfate and shake several different times. The mag sulfate will absorb the water in the emulsion and hopefully render an all nonpolar layer. Then use a fine filter to filter out the mag sulfate. Make anhydrous mag sulfate by baking Epsom salts at 400F in the oven for an hour. The granules should coalesce into large chalky pieces.

If you have one big emulsion with no layers there are two choices I know of. Using a centrifuge will work almost no matter what. Problem is that not too many people have a centrifuge, especially one with 50 ml buckets. Second is to cool the emulsion and put it in an ultrasound bath. You can pick one up fairly cheaply on eBay.

That about exhausts my knowlege on emulsions.

Adding salt to lye doesn't create any new problematic compound.

In my experience lye won't damage mescaline for a long time. Several days to weeks, if at all.

Do a search here for cleaning up mescaline acetate. PM me for more info.

Good luck.


Shambalaa wrote:

-Then swim did de-fatting with xylene 3x and did give swirling and turning upside down bottle for around 50-100 times, stopped counting after 50. Got some really minor emulsion here, but still everything ok. Then swim left de-fatted solution to stand another day, to get more plant material out.

-Then next step was to add some basic water(lye+water) Ph was set to 12(for the final solution). Then swim added xylene for the solution and swirls it around gently and turns it upside down gently as well, but swim finds out that lot of emulsion starts to form up, so now all the xylene is trap with the water and it wont separate nicely at all. So swim goes google and finds out that salt would help to remove emulsion and separate layers nicely, well swim makes the solution saturated with salt, then it start to look like it is separating from not only from xylene but from other stuff too, it looks like it has more than two layers coming up. So swim decides to read more and finds out that hot bath would help, tries that, it wont do a thing, so swim reads more and adds more lye to make it more basic again, nothing happens still. So swim ends up putting the bottle away and wait another day or two to get the emulsion to separated and hopefully to see if there is more than two layers of stuff.

So here is few question what needs to be cleared from swims mind..

-Is there a way to avoid formation of emulsion or is there reliable why to make it happen faster?

-Swim has about 300ml of basic cacti water and swim added around 200ml of xylene to that to pull mescaline FB, but now swim has run out of xylene and wonders if that amount would be enough or should swim buy more xylene and do two more pulls?

-Swim is wondering if adding salt is good idea, swim does not know what salt actually will do for that basic cacti water at all, but it looked to swim that it started to separate other stuff too, so question is what it could be, it looks like solids almost, like adding vinegar to milk type of a thing going on?

-And is there any way that salt in lye water would form something with that solution?

-How long it takes to lye to start to break up mescaline, swim don't wanna let it destroy just because of emulsion?

-And finally if you guys know any good way to clean that final product, assuming that swim gets anything out from it, so it would be in mescaline acetate form? Is re-x possible, if it is how swim can do it?

Well this is swims first time with extracting mescaline and not sure witch tek is best, but this was what swim decide to do first, next time it might be something else. Swim wont do extraction with d-limonene, because its way too hard to find anything from here, so xylene is only option?. There is also no way to get Hcl or other acids than citric acid and acetic acid. Only chemicals swim is able to get hands on are lye,xylene and acetone.

Oh, and final question for now is, is there good way to dispose xylene? or just gassing? Swim read from internet that some people discard their xylene right down from toilet, this sounds wrong to swims ears, could some one confirm swim what to do with it? Swims common sense says that it should be gassed out. Or is there way to clean it from fats and other stuff, other that distilling?

Smile yahoo!

I am El Mescalero and I demand Mescaline for the Masses!
 
Shambalaa
#6 Posted : 10/26/2012 8:41:31 AM
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Thanks again El Mescalero!

So swim end up adding salt and lye, in wrong order, because lack of knowledge, but what happend was that all that emulsion moved on top and then waiting started, swim waited for one week. Yesterday when inspected that bottle there was clearish xylene layer, some emulsion layer and water layer, so waiting helped, but did not clear all the emulsion. Took stirring rod and stirred and poked that emulsion layer would mix back to that water layer gently and would let leftover xylene to come to the surface.

So swim feels hope again, this is just waiting game and there is no hurry.

Found a lot help from search, but it's scattered all over and it is hard to relay on that kind of information, so thanks again from really informative posting! Thumbs up

Didin't find any information yet about how much mescaline freebase could xylene hold inside in theory? Confused ..just trying to figure out how much xylene is really needed pulling out mescaline fb. Final from will be acetate..
 
El Mescalero
#7 Posted : 10/27/2012 1:40:24 AM

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Shambalaa:

No mistake in the order. That's just the order I do it in. Nice that you finally got some xylene on top.

So how soluble is freebase mescaline in xylene? It is most likely similar to benzene in which it is soluble. A definition of soluble is one part mescaline to 10-30 parts solvent. Freely soluble would be one part mescaline to 1-10 parts solvent and highly soluble would be 1:1 or less. So if we were talking about water that would be one gram of mescaline to 10 to 30 grams of water which would be the same as 10 to 30 milliliters since the density of water is 1 gram/ml. Since the density of xylene is about .87 grams/ml it would be that one gram of mescaline would dissolve in 11.5 to 34.5 milliliters of xylene. (10 gr xylene/.87 = 11.5 ml) So you can see that you're using a large excess of solvent to pull the mescaline from the basified mixture, which makes sense because there's always an equilibrium between what's in the basified mixture and what dissolves in the xylene.

I'd like to change your mind about the acetate salt. You should consider using sulfuric acid to get the sulfate salt. It's easy to clean and gives beautiful, pure crystals when recrystallized. Also, doing a titration instead of adding a fixed amount of acid will give you a cleaner product which is easier to recrystallize. You can always PM me with questions.

Peace.

Shambalaa wrote:
Thanks again El Mescalero!

So swim end up adding salt and lye, in wrong order, because lack of knowledge, but what happend was that all that emulsion moved on top and then waiting started, swim waited for one week. Yesterday when inspected that bottle there was clearish xylene layer, some emulsion layer and water layer, so waiting helped, but did not clear all the emulsion. Took stirring rod and stirred and poked that emulsion layer would mix back to that water layer gently and would let leftover xylene to come to the surface.

So swim feels hope again, this is just waiting game and there is no hurry.

Found a lot help from search, but it's scattered all over and it is hard to relay on that kind of information, so thanks again from really informative posting! Thumbs up

Didin't find any information yet about how much mescaline freebase could xylene hold inside in theory? Confused ..just trying to figure out how much xylene is really needed pulling out mescaline fb. Final from will be acetate..

I am El Mescalero and I demand Mescaline for the Masses!
 
Shambalaa
#8 Posted : 10/28/2012 7:42:24 AM
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So swim did salting yesterday, with vinegar dialuded with water and there was few unexpected things happend, first when viegarwater was added to xylene, that xylene turned cloudy, dont know if this is normal or what it means? Second was that when swim was drying that vinegarwater total yelid was tiny amount of this brownish goo with redis tint on it, so really impure, this impurity was what swim was expecting, but that yelid was too little. Swim dont have scale yet, but has pretty good eye on things like this, would say that its around 200mg not much more, could be even less, but you get the idea. So it is hard to belive that 100g of san pedro cacti would only include that little, its possible, but swim thinks there would of been mistake on the extraction process.

So, what swim thinks could of gone wrong is, keeping that mescaline too long in base liquids, it was there one week or just over a week, it was strong base liquid because of that emulsion problem. Or its still trapped in base liquids, its hard to belive tough, because there was xylene in whole week too, so there would of been time for mescaline move from basewater to the xylene. One thing what always makes swim nervous and thinks that is where it could of been gone wrong is the very fist acid extraction, swim used PH 3 citric acid water, did 3x25min boils and boiled it down to manageable size, so maybe that 3x25min was too short time.

Swim did A/B extraction using xylene, lye and vinegar.

Oh, and found MEK(P) methyl ethyl ketone peroxide from one store, but not sure if that would do, but it gave hope that there is MEK around too, but not sure where to get it. Anyone here have any idea if that would work, not gonna try if there is no real knowledge going around about it. Next time would be time to try that sufuric acid, thats easy to get too, just worried that using too much easily, because it wont evaporate. And not fully understanding that titration, kind of an idea how it works, but not fully sure how it worksConfused

So swim will try to play with some of the leftover liquids and try to find where all the mescaline went, or is this cacti so unpotent, what would be really really sad because swim was really looking into mescaline, well there is still 10x more stuff to play with Big grin

Well, swim gotta use scale for that goo first and then put it inside the capsule and try how it feels, had some previous experiences with cacti, lots of light nice enegizing experiences when its nice to walk and bicycle around places, but no visuals, just glow, that is fun, mini doses work fine. One experience was full blown universal brainfuck for 15h strait, where swim realized that how strong mescaline/san pedro can be, much much stronger than DMT/Ayahuasca, only lenght wise, visual/psychedelic qualities where same level, but that lenght makes some difference there.


SWIM would really like to know why that xylene turned so cloudy after adding vinegar in it?
 
 
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