Musings on crashing mescaline salts

[Woolmer]

1) Concentrated cacti tea
2) Add acetone slowly until crashing stops
3) Remove gunk.
4) Add MgSO4 slowly, at some point it stops dissolving we want to avoid that.
5) Stuff should crash at room temp, collect, dry and wash with acetone.
6) Where is the product? If it is in what crashes out of 5 would be interesting to see what we have at that point. If it does not crash in 5) you can try to freeze it (may have MgSO4 crash too). If it doesn't crash at all, you would need to evap, base in new water, and pull with a solvent to separate the mescaline from the MgSO4 salt.

I tried out the procedure labeled above and something ended up precipitating after MgSO4 was added. Unfortunately, and with short notice, I am forced to move countries so I have handed over all of my extraction material to a good friend who will hopefully clean up the precipitate and maybe bioassay the product.

 

[Woolmer]

Here is a pic of some of the precip that was left when pouring it into a different container. Looks very similar to the precip from the first acetone wash.

 

[Loveall]

Many thanks for the testing. I wonder where the mescaline is now. Quick questions for the record (if you have the info)

- Ammount of starting material and type (fresh/powder)
- Volume of extract before adding acetone
- How much acetone was added?
- How much MgSO4 was added? Was it dried in the oven or straight from the package?
- Cou can taste a tiny amount the MgSO4 precipitate. If you do, is it bitter?

Note: It would make sense to put in the freezer next and get a second precipitate to test.

Best of luck on your move and thanks again.

 

[Woolmer]

- Ammount of starting material and type (fresh/powder):
40 cm fresh (not sure diameter)

- Volume of extract before adding acetone:
Initially only dissolved in a tiny bit of water, but this was not sufficient to dissolve acetone and precipitate anything, so more water was added in total around 30 ml.

- How much acetone was added?
Approx 40-45 ml

- How much MgSO4 was added? Was it dried in the oven or straight from the package?
Straight from the package less than 3 grams. I figured it would not make much sense to dry as it would be added to a water mix anyways. Also, considering the solubility of MgSO4 and the amount of water used this probably dissolved fine, right?

- Can you taste a tiny amount the MgSO4 precipitate. If you do, is it bitter?
My friend says it tastes bitter and slightly salty. I also had a tiny bit left that I did not give away which tasted bitter and slightly salty but I am not sure if the saltiness is placebo. Smell is also lovely and sweet.

- Note: It would make sense to put in the freezer next and get a second precipitate to test.
After first adding the MgSO4 and witnessing the precipitate, I placed it in the freezer for the night but when I tried pouring off the solution it seemed some bits of water had frozen so I let it heat to room temperature again.

Below is a pic of the dried precipitate.

 

[Loveall]

Thank you so much for the experiment and the details. Yes, straight undried MgSO4 should be equivalent to (~50/50) dried MgSO4 + water (by weight). I wonder if the mescaline crashed after adding MgSO4 along with other things. I would hope all the epson salt dissolved, but can't say for sure (we could test with pure water/acetone mix).

Would be interested to hear about the bioassay of the precipitate and of whatever dries from the un-crashed acetone/water/Epson. The mescaline has to be somewhere. I don't think laxative effects from epson start until ~10g, so there shouldn't be any issues taking it.

I'm going to do some tests to and compare notes. I have Marquis which may help keep track of where the mescaline is.

Thanks again

 

[Loveall]

I did some tests, starting with mescaline from a standard extraction.

Dissolved 50mg in water and added ammonium sulfate up to 60% by weight of water. Although the solution became cloudy, nothing precipitated. I had similar results with MgSO4.

It seems that mescaline precipitation using salts is difficult. In theory the low solubility of mescaline sulfate in cold water should help out, but I can't get it to work beyond clouding up . I have a cheap centrifuge I'm going to try to see what happens to the cloudiness.

Woolmer, I think the mescaline may still be in the acetone/water/epson liquid because of what I'm seeing. Would be interesting to hear what you find, cheers.

 

[Woolmer]

Unfortunately, I tossed out the acetone/water/MgSO4 mix because I was in a hurry and it was difficult to get to my friend before moving. A decent amount precipitated from not much resin so I think it would have made a fairly potent resin had I evaporated it.

 

[Loveall]

Unfortunately, I tossed out the acetone/water/MgSO4 mix because I was in a hurry and it was difficult to get to my friend before moving. A decent amount precipitated from not much resin so I think it would have made a fairly potent resin had I evaporated it.

It happens, the risk of experiments. I've done it too many times .

 

[Loveall]

Here is another system of possible interest in our musings: IPA and NaSO4.

It could be worth a look for mescaline. Anyone try it yet?

Water/NaOH/IPA could be used to extract from cacti powder. IPA would hopefully separate from the NaOH/water/cacti paste by simply pouring it out, carrying the FB and a small ammount of NaOH I think. Titrating with 10% sulfuric may not crash Na2SO4, mescaline sulfate, and along other stuff - layers could also form.

As with many ideas so far, probably will run into an issue in practice - but who knows. Looks somewhat interesting on paper.

 

[Loveall]

Here is another system of possible interest in our musings: IPA and NaSO4.

It could be worth a look for mescaline. Anyone try it yet?

Water/NaOH/IPA could be used to extract from cacti powder. IPA would hopefully separate from the NaOH/water/cacti paste by simply pouring it out, carrying the FB and a small ammount of NaOH I think. Titrating with 10% sulfuric may not crash Na2SO4, mescaline sulfate, and along other stuff - layers could also form.

As with many ideas so far, probably will run into an issue in practice - but who knows. Looks somewhat interesting on paper.

I did some practical tests on this kind of system (IPA and NaSO4 from NaOH and sulfuric). It looks promising. For the record, IPA/NaOH use has been brought up as a question at least once before. Seems like the suggestion was brushed aside, but there may be something to it.

Started with some crude (slightly pink) mescaline fumarate. Separately, NaOH was added to 91% IPA to saturation (6% was more than enough). Two layers formed the top IPA rich layer was kept. This layer had a high pH as expected. The mescaline fumarate was mixed in, hoping for the following kind of reaction (assuming fumarates are formed with two mescaline molecules which is a guess),

2(MescalineH)Fumarate + 2NaOH -> 2Mescaline (free base)+ 2H2O + Na2Fumarate (possibly only partially soluble in IPA rich environment)

Some solids remained: could be plant stuff or Na2Fumarate salt (or worst case unteracted 2(MescalineH)Fumarate). The IPA was decanted off, it was still alkaline with pH meter.

The decanted IPA was titrated down. What I think are Na2SO4 salts precipitate first (confirmed with a separate experiment with pure IPA/NaOH/sulfuric only). Once the pH reached 11.5, the IPA was decanted again to remove the bulk of Na2SO4 (more keeps on precipitating, but a lot less at lower pH).

Here is the cool part: At lower pH what looks like shiny sulfate xtals formed .

To remove the last of the Na2SO4 salts one could try to dry the precipitate, dissolve in a small amount of water, and add acetone. Maybe mescaline and sodium salts crash at different acetone concentrations.

So this system passes a basic test. It converted mescaline fumarates to sulfates which is kind of cool (but not sure how much was lost if any).

I want to try it with cacti powder when I get the chance. This would be a real test. Process would be:

- Make a Saturated IPA NaOH solution by saturating 91% IPA with NaOH and keeping the upper layer that forms.
- Extract cacti powder
- Titrate with 10% sulfuric to pH ~ 11.5, allow to settle and decant.
- Continue to titrate down to neutral pH. Do shiny mescaline sulfate crystals form? Let's imagine that yes.
- Recover the xtals, wash with acetone (or 99% IPA if available), and dissolve in water.
- Reduce the water and add acetone slowly, try to recover the mescaline xtals and not the Na2SO4 salt or other gunky precipitates.

Note: The first time I overshot the titration and got a pH of 1.9. No crystals crashed, but when I brought the pH to ~5 the crystals showed up. This could be because we need the SO4-- ions to be present to form the insoluble mescaline salt (and not the HSO4- ions).

 

[Loveall]

Here is another system to consider: Na2CO3, IPA, Water.

Ternary diagram below, when saturating with water phases form at 80% IPA/water and saturated Na2CO3 water.

Titrating potential mescaline FB from the IPA/water layer would be interesting, but not sure if mescaline sulfate would crash well in the presence of plant stuff.

Anyway, somewhere else to potentially do tests one day.

 

[Loveall]

I've had more decent results with alkaline IPA.

Used IPA/NaOH/water mix to pull from "spent" cacti powder (re-dried after a limonene alkaline water paste process). One can do lots of limonene pulls and still get a little bit of mescaline, so I figured I'd use it for tests/experiments. Water seems to be needed and at higher NaOH concentration the water separates and stays in the cacti paste from what I can tell. After the pull more NaOH can be added to dry the IPA further too (or if no layers form you know you had enough NaOH originally).

Adding sulfuric acid to neutral crashes a bunch of stuff, I'm guessing most is Na2SO4 salt. Nice thing is that after drying the precipitate, pulling with 75.5% ethanol leaves the sodium salt behind. Upon drying the everclear it looks like mescaline sulfate crystals form (fan like needles - see below) that scrape up yellow and crystalline.

I'm going to test this kind of system (alkaline IPA/water layers to pull with water layer staying in cacti paste, then sulfucric to precipitate, then cleanup of precipitate). This includes doing Na2CO3 tests also, not only more NaOH tests. Cheers.

 

[Loveall]

The yellow crystalline scrape-up from the previous post was dissolved in minimal water. Actone was added until cloudy. That was allowed to precipitate, the yellow color stayed in the liquid which was decanted/filtered off. Sediment and filter were pulled with water and that dried to withe fan/needle xtals that gave orange in Marquis.

So to recap,

-Partially spent powder pulled with IPA/NaOH/water. Water layer seemed to stay in the cacti making a paste (because no layers are seen in the pull)
-Verified IPA was saturated with NaOH, by adding NaOH and checking for a water layer (minimize water in IPA layer).
- Neutralize with sulfuric, collect sediment
- Pull sediment with 75.5% everclear (most Na2SO4 is left behind)
- Dry everclear (perhaps adding acetone at this point is easier)
- Dissolve in minimal water, add acetone to form new precipitate (whiter)
- Decant/filter precipitate, pickup with water, evaporate in shallow pan and scrape up (image below)

Will this be practical for fresh cacti powder? Is this giving mescaline for sure or something else that is orange in Marquis? I don't know, but I'll test this alkaline IPA approach with fresh powder (maybe with NaCO3 instead of NaOH) when I get the chance.

 

[doubledog]

Very interesting, Loveall, I am really curious what is the product.

What about to evaporate IPA from step 2 and pull the residue with acetone, only after add sulphuric.
I also think that step 4 is risky as it is unclear how selective is diluted ethanol for mescaline sulphate.

 

[Loveall]

Very interesting, Loveall, I am really curious what is the product.

What about to evaporate IPA from step 2 and pull the residue with acetone, only after add sulphuric.
I also think that step 4 is risky as it is unclear how selective is diluted ethanol for mescaline sulphate.

Everytime I dry something with mescaline free base I have issues. It is reversible, but water needs to be introduced to get it to behave as expected again (e.g. when fully drying a cacti powder Ca(OH)2 water paste before a limonene pull for example). It's happened to me in several situations/experiments.

I've heard that mescaline sulfate is soluble in 75.5% ethanol from Mindlusion (Mind of you see this please correct me if I'm wrong). From what I've seen, mescaline sulfate is soluble in 75.5% everclear. On the other hand Na2SO4 is only very slighty soluble in it (I did a test and only 4mg came through in 10ml of everclear - also attaching a paper about this and an image).

This everclear separation property is important if pulling wet cacti powder with IPA made alkaline with a sodium base which is going to be treated with sulfuric.

Thanks for the feedback!

 

[doubledog]

Everytime I dry something with mescaline free base I have issues. It is reversible, but water needs to be introduced to get it to behave as expected again (e.g. when fully drying a cacti powder Ca(OH)2 water paste before a limonene pull for example). It's happened to me in several situations/experiments.

I would suspect plant solids here.
Did you have these issues also when freebase was already extracted?

mescaline sulphate is soluble in the everclear, and if sodium sulphate is not, it can be used for separation.

 

[Loveall]

I would suspect plant solids here.
Did you have these issues also when freebase was already extracted?

Good point, I haven't tried to dry the FB it after extracting from the bulk of plant matter.

 

[doubledog]

Cactus plant matter is the main culprit for difficulties with cactus extractions and most effort have to be dedicated to free the mescaline from it.

Maybe it could be helpful to write that once I tried very similar extraction of caffeine from coffee, and basic IPA did not work. Basic ethanol worked well. So some variations should be tested if things will go bad with some particular approach.

You could do a taste test of your product, and compare it to taste of sodium sulphate.

 

[Loveall]

Agreed doubledog. I think I'm going to do tests with everclear magnesium sulfate, should have less gunk and a concentrated solution should be possible.

 

[Loveall]

One more system of interest: aqueous ethanol and ammonium sulfate. It can form layers.