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simple titration, and dual solvent crystalization Options
 
Precog
#61 Posted : 2/27/2013 10:21:05 PM

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Kash wrote:
Precog wrote:
dg wrote:
i dont recomend using d-limo. but it will likely work (as long as the acid you are salting with is very dilute-)


Having only performed 69ron's d-limo extraction thus far, d-limo is the only NP I have available. I am guessing this incompatibility is due to the reactivity of the alkenes in limonene with strong acid?

Correct. If you over-titrate your saltings then the excess acid will pull garbage from the d-limonene.


Wouldn't that be the case with any other non-polar?
"The peak experience might be likened to a spot on a mountain top from which the surrounding panorama may be viewed; yet being on the top of the mountain does not supply more than the possibility of seeing, whereas this process of observation is different from that of mountain climbing[...]insight is distinct from the mental state from which it originates, and constitutes the result of a creative act in which consciousness at a certain height is directed toward what lies below."
--Claudio Naranjo

There is no becoming, no revolution, no struggle, no path.
Already you are the monarch of your own skin.
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Trippy glass for trippy people.
 
Kash
#62 Posted : 2/27/2013 11:51:27 PM

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Not necessarily. I believe that d-limonene can be protonated by excess acid and form gunk that contaminates end product, where other solvents do not behave the same.
--------------------------------------------------*Kash's LSA Extraction* * Kash's Mescaline Extraction*------------------------------------------------------
All things I say are complete and utter ramblings of nonsense. Do not consider taking anything iterated from the depths of my subconsciousness rationally and/or seriously.
 
dg
#63 Posted : 2/28/2013 12:14:44 AM
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^ afaik that is correct. use dilute acid w/dlimo
but dilute acid is always best imo- much harder to overshoot the desired ph
 
Precog
#64 Posted : 2/28/2013 3:59:54 AM

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Kash wrote:
Not necessarily. I believe that d-limonene can be protonated by excess acid and form gunk that contaminates end product, where other solvents do not behave the same.


Coolio- I was just confused when Kash said 'pull' garbage. Regardless, the world's obsession with oil makes petrochemical solvents cheap and abundant so I think I will get myself some of that stuff to avoid potential risks. Thanks for the responses and the tek!
"The peak experience might be likened to a spot on a mountain top from which the surrounding panorama may be viewed; yet being on the top of the mountain does not supply more than the possibility of seeing, whereas this process of observation is different from that of mountain climbing[...]insight is distinct from the mental state from which it originates, and constitutes the result of a creative act in which consciousness at a certain height is directed toward what lies below."
--Claudio Naranjo

There is no becoming, no revolution, no struggle, no path.
Already you are the monarch of your own skin.
--Hakim Bey
 
Loveall
#65 Posted : 1/23/2020 4:28:33 AM

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Has anyone tried to go straight to acetone and skip the NP step here?

- Etract with water/filter/reduce/filter
- Add same volume of acetone and cool. Expect Proteins to crash here (if so decant/filter). Expect mescaline to remain soluble here (but not sure).
- Add dilute drops of dilute sulfuric acid to cold solution (until cloudiness stops?). Mescaline sulfate should crash out (?).


Someone must have tried this, right? What happened? Or does anyone see an obvious issue with this a priori? Why would this not work? Thanks!
“... (a) psychedelic substance occasionally causes psychotic behaviour in people who have not taken it.”
Excerpt from a McKenna talk transcript / audio.
 
Loveall
#66 Posted : 1/27/2020 5:37:45 PM

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dg wrote:
add water to glass or stainless steel pan, fast boil it down.
notes: you want to remove as much water as possible w/o scorching product, i like medium heat on an average gas range.
as the concentration of the solution increases the sound the boiling makes changes, and it sounds syrupy. you may also notice the solution get cloudy(a sure sign you have gone far enough.

Has anyone measured the pH of the reduced water before adding acetone? I wonder what it is because mescaline (bi)sulfite precipitation may depend on the availability of HSO4+ ions which could depend on the starting water pH and how much acetone is added.

This is just speculation on my part, but curious on any data for the pH of the reduced water pH. Thanks.
“... (a) psychedelic substance occasionally causes psychotic behaviour in people who have not taken it.”
Excerpt from a McKenna talk transcript / audio.
 
Loveall
#67 Posted : 1/29/2020 12:25:58 PM

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Loveall wrote:
Has anyone tried to go straight to acetone and skip the NP step here?

- Etract with water/filter/reduce/filter
- Add same volume of acetone and cool. Expect Proteins to crash here (if so decant/filter). Expect mescaline to remain soluble here (but not sure).
- Add dilute drops of dilute sulfuric acid to cold solution (until cloudiness stops?). Mescaline sulfate should crash out (?).


Someone must have tried this, right? What happened? Or does anyone see an obvious issue with this a priori? Why would this not work? Thanks!


To answer my own question, I went ahead and tried this. Interestingly when I added acetone a clumpy snot formed (see first picture). The snot is very easily separated (see second picture) from solution by decanting (most sticks to the glass wall) and filtering (for the little bit that pours out). To the filtered water + acetone sulfuric acid was added, and more acetone until cloudy, then that was put in the freezer overnight. This morning loose white particles are crashing out of solution. Can't say for sure it's mescaline sulfate (or how pure it is), but definitely want to investigate more.

To recap: hot water extract (I used fresh cacti I had chopped and frozen) filter/decant/reduce (final pH was 5.1), acetone crash of gunk, sulfuric acid crash of potential product and/or other stuff.

Seems to good to be true, more tests will tell. I'm keeping the snot too incase the Mescaline went there.

Loveall attached the following image(s):
IMG_20200128_230441793.jpg (5,554kb) downloaded 174 time(s).
IMG_20200128_231041500.jpg (2,843kb) downloaded 171 time(s).
“... (a) psychedelic substance occasionally causes psychotic behaviour in people who have not taken it.”
Excerpt from a McKenna talk transcript / audio.
 
Loveall
#68 Posted : 1/31/2020 5:26:49 AM

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Looks like the shortcut may have worked (but not 100% sure yet). I'll get a separate thread going for it since it's diverging from dg's original process.

Edit: it did not work - FYI
“... (a) psychedelic substance occasionally causes psychotic behaviour in people who have not taken it.”
Excerpt from a McKenna talk transcript / audio.
 
Loveall
#69 Posted : 6/4/2020 8:53:31 PM

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This works with HCl salting (and probably other acids in general I imagine). I used minimal diluted HCl to just titrate. Maybe more acetone is needed vs. sulfuric before cloudiness shows up. The brown/tan color stays in the acetone/water and the crystals come out pretty white. Below is the result after decanting, one acetone wash, dissolving in water and drying slowly. Positive for Marquis 🙂

Here is the general technique as explained by Mindlusion if one wants to try other acids.
Loveall attached the following image(s):
IMG_20200603_225008361.jpg (2,272kb) downloaded 114 time(s).
“... (a) psychedelic substance occasionally causes psychotic behaviour in people who have not taken it.”
Excerpt from a McKenna talk transcript / audio.
 
doubledog
#70 Posted : 6/4/2020 9:42:00 PM

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Could I ask what ratio of acetone/water ratio did you use for HCL?
What it could be for, let say, ascorbic?

IME, with sulphate, even IPA could be used for dual solvent crystalization.
 
Loveall
#71 Posted : 6/5/2020 12:20:42 AM

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doubledog wrote:
Could I ask what ratio of acetone/water ratio did you use for HCL?
What it could be for, let say, ascorbic?

IME, with sulphate, even IPA could be used for dual solvent crystalization.


Of course 🙂

I used a small mason jar on a scale and had 3g of brown water after reducing. I noticed clouding after adding 8g of acetone at room temp. I added more acetone to be extra sure everything crashed (probably not needed though, just paranoia on my part) and let it rest on the fridge. After the acetone was clear, I added more with no clouding which I think means mescaline crashing was done.

One interesting thing about the HCl salt, it bubbled with Marquis. The fumarate salt does not do that for me 🤷‍♂️

Not sure about ascorbic salt acetone ratio. It has low solubility in acetone, so excess ascorbic precipitation may be a concern. I think fumaric and malic acids have good acetone solubility (and even citric) so they should not crash with the salts, those may be good ones to try on principle. Also, they wouldn't have the low pH issues in Limonene (more contaminants) so careful titration is not as important. That's all in theory, we'd need to test to know.
“... (a) psychedelic substance occasionally causes psychotic behaviour in people who have not taken it.”
Excerpt from a McKenna talk transcript / audio.
 
Loveall
#72 Posted : 6/5/2020 3:01:53 AM

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Loveall wrote:
dg wrote:
add water to glass or stainless steel pan, fast boil it down.
notes: you want to remove as much water as possible w/o scorching product, i like medium heat on an average gas range.
as the concentration of the solution increases the sound the boiling makes changes, and it sounds syrupy. you may also notice the solution get cloudy(a sure sign you have gone far enough.

Has anyone measured the pH of the reduced water before adding acetone? I wonder what it is because mescaline (bi)sulfite precipitation may depend on the availability of HSO4+ ions which could depend on the starting water pH and how much acetone is added.

This is just speculation on my part, but curious on any data for the pH of the reduced water pH. Thanks.


I went ahead and checked. Not much pH change during reduction of a sulfuric salting (6.5 to 6.1).

I think think it is important to have this kind of pH because any excess sulfuric acid can react with metal.

Next, I might check the xtalizatiom with organic acids that have some solubility in both acetone and water (eg, fumaric, malic, citric). Anyone try this already? If some of these work, that process could have a wider window (no issues with over titration and no chances of having a very acidic pH). Also, when the pH is slightly acidic emulsions seem to break up faster from what I have seen.
“... (a) psychedelic substance occasionally causes psychotic behaviour in people who have not taken it.”
Excerpt from a McKenna talk transcript / audio.
 
doubledog
#73 Posted : 6/5/2020 11:02:24 AM

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Once I overused sulphuric acid and had a huge excess of it in crude mescaline sulphate. After redissolving in small amount of warm water (in salt:water 1:4 ratio) , it had pH 2.
Then added 10x volume of warm Ipa.
Crystals started to crash almost immediately and were quite nice, different structure than in acetone. Quite nice visually, recommend just for aesthetic experience Smile
Product was again dried and redissolved in water, pH about 6.
 
Woolmer
#74 Posted : 6/5/2020 11:45:45 AM

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Loveall wrote:
This works with HCl salting (and probably other acids in general I imagine). I used minimal diluted HCl to just titrate. Maybe more acetone is needed vs. sulfuric before cloudiness shows up. The brown/tan color stays in the acetone/water and the crystals come out pretty white. Below is the result after decanting, one acetone wash, dissolving in water and drying slowly. Positive for Marquis 🙂

Here is the general technique as explained by Mindlusion if one wants to try other acids.


Very nice Loveall!

So this is as simple as what you wrote earlier in the thread, just using HCL instead of sulfuric acid?

The process being:

Reduced tea
Acetone to crash gunk
HCL to crash mescaline

Do you think this could be done with acetic acid?
 
Loveall
#75 Posted : 6/5/2020 2:31:42 PM

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Woolmer wrote:
Loveall wrote:
This works with HCl salting (and probably other acids in general I imagine). I used minimal diluted HCl to just titrate. Maybe more acetone is needed vs. sulfuric before cloudiness shows up. The brown/tan color stays in the acetone/water and the crystals come out pretty white. Below is the result after decanting, one acetone wash, dissolving in water and drying slowly. Positive for Marquis 🙂

Here is the general technique as explained by Mindlusion if one wants to try other acids.


Very nice Loveall!

So this is as simple as what you wrote earlier in the thread, just using HCL instead of sulfuric acid?

The process being:

Reduced tea
Acetone to crash gunk
HCL to crash mescaline

Do you think this could be done with acetic acid?


Unfortunately, probably not (but go ahead and try if you want). I tried this exact thing using sulfuric acid but it did not work 🙃. However, sulfuric has the problem of forming HSO4- at low pH which may stop precipitation. HCl does not have that possibility.

It works here after getting to very clean and concentratedwater/mescaline thanks to the limonene step.

What you are saying could work in principle, but like I said, I've run into issues with it, maybe because of too much plant junk. Stuff does precipitate and in one case it was even positive for Marquis, but bioassay and MS analysis by Benz showed no mescaline. After drying what didn't precipitate and doing a standard extraction on that, the mescaline was recovered. Doubledog said the plant stuff from the water extract gets in the way of precipitation, and so far that is what I have found.

I haven't completely given up yet. Maybe I just needed to keep on adding acetone 🤷‍♂️ and gave up to soon. Also, 70% ethanol tinctures of dry powder are said to be clean and active. 70% IPA too, which makes me wonder about 70% acetone. That kind of extract could be reduced in volume, decanted from any junk that crashes during reduction, and then add acetone to see what happens. There may be several clouding/precipitation events at different acetone/extract ratios, one of them hopefully mescaline. Adding an acid (e.g. sulfuric) could change how early mescaline precipitates from the acetone/tincture like you say.

Also, it looks like the natural mescaline salt is not soluble in acetone. So starting with a water extract and increasing acetone % should make it crash, no? We could start with a cacti water extract, then,

1) Add 50% acetone. We know I'm this condition junk precipitates because of phlux's and other confirmation work.
2) Reduce to say 10ml, and add more acetone (usay up to 200ml). This may have to be done in steps (less aggressive reductions and acetone additions) because if there is a lot of junk, a small water volume is not possible without being overwhelmed by junk.
3) Hang dry epson salt (say ~15g) wrapped in a filter and tied to a thread into the top of the solution to suck up all the water that was left in 2)

After 3) (or before?) the mescaline should have crashed somewhere - I hope.
“... (a) psychedelic substance occasionally causes psychotic behaviour in people who have not taken it.”
Excerpt from a McKenna talk transcript / audio.
 
Loveall
#76 Posted : 6/5/2020 6:01:22 PM

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doubledog wrote:
Once I overused sulphuric acid and had a huge excess of it in crude mescaline sulphate. After redissolving in small amount of warm water (in salt:water 1:4 ratio) , it had pH 2.
Then added 10x volume of warm Ipa.
Crystals start to crash almost immediately and were quite nice, different structure than in acetone. Quite nice visually, recommend just for aesthetic experience Smile
Product was again dried and redissolved in water, pH about 6.


This is great info. Thank you!
“... (a) psychedelic substance occasionally causes psychotic behaviour in people who have not taken it.”
Excerpt from a McKenna talk transcript / audio.
 
Loveall
#77 Posted : 6/6/2020 1:08:14 AM

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doubledog wrote:
Once I overused sulphuric acid and had a huge excess of it in crude mescaline sulphate. After redissolving in small amount of warm water (in salt:water 1:4 ratio) , it had pH 2.
Then added 10x volume of warm Ipa.
Crystals started to crash almost immediately and were quite nice, different structure than in acetone. Quite nice visually, recommend just for aesthetic experience Smile
Product was again dried and redissolved in water, pH about 6.


Guys, how about extracting cacti powder in 70% IPA (I read claims that it works to pull the natural mescaline salts but haven't tested), them reduce that, then add sulfuric, then maybe 99% IPA too. Stuff will be crashing during this, I wonder if the sulfate crystals mentioned above would fall out at some point (?)
“... (a) psychedelic substance occasionally causes psychotic behaviour in people who have not taken it.”
Excerpt from a McKenna talk transcript / audio.
 
doubledog
#78 Posted : 6/6/2020 7:56:08 AM

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Problem to solve is still the same with similar approaches:
30% of water will extract some gunk, which will crash when 99% IPA is added, so outcome will be still resinous.
It is possible that you can somehow separate components with different concentration of added Ipa or acetone, but doubt that outcome would be worth the effort.

I do not think that good crystals and yields are possible without playing with pH.
So maybe something like this:
-Start with dry water extract or 70% ethanol extract
-dissolve it in small amount of water and add base, let react
-add acetone, mix it, separate acetone
-reduce, add sulphuric
-hopefully some crystals appear.

 
Loveall
#79 Posted : 6/6/2020 1:08:54 PM

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Yeah, you are probably right doubledog.

Looking into it a little more, there are people that seem to be using 91% IPA to extract cacti powder. That can be reduced and the azeotrope concentration would stay ~ 91%.

I really wonder what would happen if sulfuric is added to that kind of extract. And/or also 99% IPA. I tried a 99% IPA extraction and got trace amount of mescaline. Maybe exploring the sulfuric vs IPA concentration space for different precipitates turns out to be interesting.

I'm out of cacti material now and can't try this. The cacti are outside happily growing 🙂 After the growing season I can try this stuff again. Cheers.

“... (a) psychedelic substance occasionally causes psychotic behaviour in people who have not taken it.”
Excerpt from a McKenna talk transcript / audio.
 
Woolmer
#80 Posted : 6/6/2020 7:06:32 PM

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I'd like to add that a knowledgable Nexus member has stated that the natural mescaline salts are not very soluble in alcohol.

drnocturne wrote:

Alcohols are not good solvents to use to pull M-malate out of the cactus, as M-malate is not very soluble in alcohols... I think the only reason they're getting any yields is most likely due to the water content in the vodka or whatever they are using.


 
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