Post-CIELO clean up

[Jan e Kharabat]

So I finally decided to try Cielo and that too without messing around too much and it all worked pretty well but I used smaller amounts of EA, did around 5 pulls. I was also careful about the amount of fumaric acid and only added around 1g per pull. I used magnetic stirrer for fast crystallization and it seemed to work well. The problem is... I now have 3g of fine powder extracted from 100g of cactus powder, which means, there's definitely a good amount of fumaric acid in there.
I did multiple IPA washes but for whatever reason, that does not seem to be doing much. I was thinking of doing an A/B cycle but... Which method should I use? Mix with sodium carbonate, moisten a bit and extract with IPA/acetone, or dissolve in water, basify, and extract with xylene? The last one sounds annoying... and I'm unable to find out the solubility of freebase in xylene and would hate to work with large amounts of solvent.
Has anyone had any experience with this?
Also, has anyone tried to recrystallize fumarate using dry ethanol? Or perhaps ethanol+water?

 

[DetritusTheEgo]

I only have the one CIELO extract under my belt and can't speak to the nuance of cause and affect of the deviations you've made from the tek. Figured to ask a few clarifying questions for when the more knowledgeable come through.

You state around five pulls, can I assume that is indeed five pulls? Do you know how much fumaric acid in total was added? I'm guessing around five grams just reading it as stated with five pulls. Do you know how much in grams or ml of ethyl acetate you used per pull? Do you know how much in total you collected since some is lost during the extract process? You kept each pulls ethyl acetate in it's own jar and put 1g of fumaric acid in each?

Rereading the CIELO tek it calls out solubility of citric acid monohydrate in ethyl acetate is ~50 mg per gram of ethyl acetate and ~10mg/g for fumaric acid. For each 100g of ethyl acetate your looking at 1g of fumaric to saturate it. The calculator / tek calls for the 1xEA method 250g + 150gx4 at a total of 850g of ethyl acetate and 3g of fumaric. That amount is not close to a saturation point but at those levels I'm not sure how much acid contamination to expect in the final product. If you are close to 500g of ethyl acetate and 5g fumaric then you are much closer to that point.

 

[Jan e Kharabat]

I added around 1g of fumaric acid in the first pull which was 250g and then added some more until the solution turned acidic. The subsequent 4 pulls were around 100g each and I added fumaric acid in small amounts until the solution turned acidic. But fumaric acid takes a good amount of time to dissolve in EA and I used magnetic stirrer and didn't wait longer than an hour for it to dissolve.
But anyways, I did a few boiling IPA washes and then dissolved the powder in hot distilled water. Flowery crystals formed upon cooling which show a homogenous structure and don't look anything like fumaric acid, which makes me believe that I truly do have mescaline fumarate here, but the yield is well over 2% and that seems pretty crazy...

 

[DetritusTheEgo]

My questions were alluding to you may not have excess fumaric if you are no where close to the ethyl acetate saturation point. Based on the additional context that also seems promising. Would wait for some more knowledgeable folks to chime in.

Two percent is not unheard of. I've seen people pulling 3-5% on r/mescaline. Though you can mostly just take people at their word and assume they don't have contamination of some kind. There's a post from yesterday with a 4.25%.

 

[Jan e Kharabat]

So the re-x with water produced different batches of crystals, I redissolved them in 80% ethanol and was left with shimmering white crystals which would not dissolve in ethanol at all. They were almost tasteless and had a sandy texture when chewed upon. I think that was calcium fumarate, and it was around 200mg at least (although I didn't weigh). I tried again with 90% ethanol and filtered out some more. Mescaline fumarate seems to dissolve pretty well in boiling ethanol and the re-x works pretty well, although further experiments with different ratios of water could be useful.
In any case, I redissolved everything in water, based with lots and lots of NaCO3 and extracted again with EA, and salted again, this time with FASEA to avoid fumaric acid excess. Hopefully I won't have any sodium fumarate contamination now, but I'll re-x with ethanol to make sure.

 

[BigPCYield]

I think you are doing too much. You got 3% and that is quite reasonable.

 

[Jan e Kharabat]

Yes but I wanted to figure a few things out, for example, a saturated solution of NaCO3 does not prevent ethyl acetate from picking up some water and the dissolved NaCO3. I dissolved the mescaline fumarate from the A/B cycle in 90% ethanol and was left with some undissolved sodium fumarate (since the ethanol was 90%, some sodium fumarate likely dissolved as well). I distilled the EA (around 700ml) after the A/B cycle, I messed up the distillation so some water likely ended up in the distilled EA, but the small amount of EA left in the distillation flask showed a separate layer of water settled at the bottom, this must have been around 1-2ml.

Another interesting aspect was the solubility of mescaline fumarate in ethanol. I have yet to try 100% ethanol, but in boiling 90%, it is very soluble. I needed around 50-60ml for over 2g of fumarate.

Aside from that, I've noticed a significant difference between aged and non aged cactus, non aged yielded 1.5g fumarate whereas aged was around 3g (perhaps 2.7g excluding the salt impurities).

 

[Jan e Kharabat]

Another interesting thing I noticed is the the yield nearly halves per pull. One can (and perhaps should) perform several EA pulls. My final pull yielded 30mg, the one before was around 55mg and the one before that was 100mg. So, the amount of mescaline left in the solution after my final pull was something like 15+8+4+2+1=30mg. This can be useful for figuring out when to stop.