Double displacement with mescaline acetate?

[modern]

Is a double displacement possible with mescaline acetate and sodium sulfate or no? I'm gonna try reducing the amount of solution I have to see if it works out but is it even possible?
I'm freezing to see if something crashes out once more concentrated.

 

[downwardsfromzero]

Whichever combination has the lowest solubility product at a given temperature is the one that will crystallise first. So at 5°C, say, you'll get crystals of whichever combination is the least soluble. I'd have to look up the data for the four possible salts as it is, so why not check and get back to us with the answer.

The idea might seem plausible enough although I have a hazy recollection that something like this was tried unsuccessfully a few years back by some of the usual suspects. Have you searched the forum for anything similar?

 

[modern]

Mescaline sulfate Manske? - Preparation - Welcome to the DMT-Nexus

Mescaline sulfate Manske? is the closest I've seen but idea is different I think?

I reduced down the volume of my solution but too much since I'm pretty sure the crystals are sodium acetate. So I'll dilute it a little bit to see if anything precipitates. I thought of removing the liquid but the mescaline is likely in the acetate do to crystalizing in the fridge?

I'm only using a small amount so might be better to test with larger starting material.

 

[Loveall]

Mescaline sulfate Manske? - Preparation - Welcome to the DMT-Nexus

Mescaline sulfate Manske? is the closest I've seen but idea is different I think?

Yes that that was different as it started with cactus. Perhaps too much stuff in the plant made it not work. One of many failed experiments on the path to CIELO . If you start with mescaline acetate there is a chance it could work.

Manske (or common ion effect) just helps precipitate the less soluble salt assisting in double displacement precipitation. It is complementary the other stuff you are doing (reducing volume and temp). If you want to try to use manske to your advantage magnesium sulfate can hold more sulfate ions in a 0C solution (2.25M) than sodium sulfate (0.34M).

Edit: also need to check the other displacement salt solubilitiy (magnesium acetate). For all the salt combos just need the mescaline sulfate to be the least soluble at it should crash under the right conditions (temperature and common ion concentration) while the other salt combos remain in solution (magnesium acetate and magnesium sulfafe).

 

[modern]

So I got a different crystal and would like to confirm it is mescaline sulfate. I think the easiest way is melting point since sodium acetate melts at 56-64C and mescaline sulfate at 180C

Also does sodium acetate dissolve in isopropanol like it does in ethanol? I keep searching and can find it. Same question for mescaline sulfate? I don't understand how it dissolves in methanol but not ethanol. (I'm not strong on the chemistry side)

Mescaline solubility and other properties - Generic - Welcome to the DMT-Nexus

Hmm maybe this is still sodium acetate?
"Mescaline sulfate can be distinguished by the structure of its crystals. These are approximately 1/4" long and look like fine needles or shards of glass."

 

[Loveall]

What did you do to get this?

 

[doubledog]

It looks much more like sodium acetate, and not like mescaline sulfate. I've never seen such crystalization with mescaline sulfate, its crystals are different, there are needles and shards structures.

Never tried methanol or ethanol with mescaline sulfate, but I would definitely expect similar behaviour, as m. sulphate is soluble in water (but not very soluble), but not in IPA or acetone. It's probably about polarity of solvent, methanol is more polar than ethanol, so methanol is closer to water and ethanol is closer to IPA.

 

[Loveall]

I wonder what the OP did specifically (any cold treatment?).

Sodium Sulfate is not very soluble when cold, I think that could precipitate first. I don't think this salt is a good choice here.

In this situation I will repeat that I think magnesium sulfate has more chances of success.

 

[modern]

Yea this was sodium acetate but I think the mescaline sulfate may be in it since there was a 'wet' spot on the bottom after I heated it up past 200C. The sodium acetate was trihydrate and melted and as the water evaporated it salted again. I kept heating for a while and made sure it surpassed 200C. When I looked at the bottom there was a 'small wet spot'

So now I'll add some 99 IPA so see if anything remains.

I also reduced the liquids that I decanted from the crystals. To see if anything precipitates/crystalizes.

This crystal I got from redissolving the SA shards from the first picture in a small excess of water and put it in the fridge.

I don't have magnesium sulfate and NOT widely available to me here as Epson salt.

 

[downwardsfromzero]

On the plus side, if it's sodium acetate that crystallises out first you'll be left with mescaline sulfate in solution - but only assuming that the initial crystallisation wasn't reliant on there being a large excess of sodium sulfate to drive it. It looks as though it's worth attempting a further crystallisation from the remaining liquid; you'd need to weigh your sodium acetate trihydrate to estimate how much of it may be left in solution. The 'holy grail' may yet be in reach through further evaporation, chilling and/or the addition of cosolvent. Pray the ancestors are on our side and we may yet crack this puzzle!

 

[modern]

So the reduced liquid decanted off the sodium acetate has formed some very thin strands but is suspended so I'll let it sit for longer. I started with a small amount of mescaline so amount should be small and I'll need to revisit this in the future. I'll try to start with a known starting weight of material and work backwards just as a POC then I'll try using a crude tea extract. Maybe too many impurities from the tea acetate tar? I'm also planning on revisiting the vegetable oil pull. But will take a while.

If someone has the time to do rough calculations on amounts needed of sodium or magnesium sulfate to the acetate. I used a saturated aqueous solution of sodium sulfate but wasn't heated so not super saturated. I dissolved the mescaline acetate in vinegar so maybe I started off wrong. Any suggestions?


I added 99+ IPA to the sodium acetate that I heated and it didn't completely dissolve only slightly. I'll try heating it to see if it helps. I highly doubt the undissolved powder is mescaline sulfate and maybe un-reacted sodium sulfate?

 

[modern]

Looks like cobweb this is in the liquid decanted off the sodium acetate

 

[downwardsfromzero]

maybe un-reacted sodium sulfate?

To clear up a technical point here, when carrying out a "double displacement" with ionic salts, it's not really that they react as such, since the ionic species remain unchanged - the sulfate is still sulfate, acetate still acetate, and so on. When everything is in solution you just have a mixture of all the component ions.

One reason for there being "unreacted" sodium sulfate may be that there is an excess of it. For it to get completely "used up" you would need an equal amount of mescalinium ions as there are sodium ions: two parts of mescaline acetate to one part of sodium sulfate - and I guess estimating the former is a bit tricky.

It looks like you drove the formation of sodium acetate by using an excess of sodium sulfate plus the extra acetic acid from the mesc acetate solution, which in itself is a bit interesting. Is the solubility of sodium acetate decreased by the presence of acetic acid?

The "hot ice" phenomenon is a reasonable tentative identification for your big crystal but it would require more work to demonstrate its identity conclusively.


The cobwebby stuff gets tantalising - have you been chilling it? Is anything more forming in there?

 

[modern]

upon further heating the cobweb strings didn't dissolve. Maybe fibers from coffee filter I'm not sure and its hard to tell really.

I reduced the volume once more by half and will leave in the fridge again. I'm working with a very small amount of material around 100mg MAX of mescaline but it should be visible if it works.