-
Members of the previous forum can retrieve their temporary password here, (login and check your PM).
simple titration, and dual solvent crystalization
- Thread starter dg
- Start date
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.
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!
- 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!
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.dg said:
This is just speculation on my part, but curious on any data for the pH of the reduced water pH. Thanks.
Loveall said:
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.
Attachments
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
Edit: it did not work - FYI
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.
Here is the general technique as explained by Mindlusion if one wants to try other acids.
Attachments
doubledog said:
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.
Loveall said:
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.
doubledog
Titanium Teammate
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
Product was again dried and redissolved in water, pH about 6.
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
Product was again dried and redissolved in water, pH about 6.
Woolmer
Established member
Loveall said: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?
Woolmer said:Loveall said: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.
doubledog said: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
Product was again dried and redissolved in water, pH about 6.
This is great info. Thank you!
doubledog said: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
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 (?)
doubledog
Titanium Teammate
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.
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.
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.
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.
Woolmer
Established member
I'd like to add that a knowledgable Nexus member has stated that the natural mescaline salts are not very soluble in alcohol.
drnocturne said: