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TEK Ethyl acetate approach [CIELO]

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My fumarate test has been crystal clear for a few hours now, revealing GORGEOUS crystals, looks like a few inch long needles and a lot of finer ones, maybe some undissolved fumaric acid in there as well, but not sure. Wow, that was fast!

No crystallization to report in the citric acid salted jar so far. I thought I saw what I thought was the beginning of oiling out, but over the last few hours, it hasn't progressed to anything oily I recognize from previous runs, so I think I might just be hypervigilant, and it's just defects in the glass I'm seeing. There are two layers, a cloudy top layer and cloudier bottom layer. Hoping that it will spontaneously nucleate crystals at some point overnight. I'm guessing this is the delayed crystallization that Loveall mentioned when using drying agents.

That said, I am EXTREMELY happy with the results from fumaric acid. Will decant, take photos and weigh them tomorrow.
 

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orchidist, Congratulations on the fumarate Xtals. You can swirl at the end to make sure all the Fumaric acid was dissolved in EA. If you still get oil with citric acid it would be a very interesting result, maybe pointing to your cactus having other alkaloids besides mescaline. Keep us posted. Thanks!
 
Thanks! I am so incredibly happy to have a positive result finally. Not that it hasn't been fun the whole time.

No cigar for me, but I did make myself a really nice snack! Toasted some nice bread, lemon marmalade I made from homegrown lemons sent by a friend, olive oil, salt, pepper, chili, fresh thyme.

Now, need to figure out some time when my partner and I can take a trip out to our favorite cabin and try what I made today. That's gonna be the hard part. I don't like tripping anywhere near the suburbs, but scheduling vacations isn't easy these days.

Getting oil again definitely would be interesting, but I sure hope we have an actual pattern established to contribute something of value to the wiki. At this point in other runs, I would have already seen lots of small iridescent droplets on the bottom 1/4" of the jar, so I'm hopeful crystals will eventually nucleate. Would be nice if I had a seed crystal of M-citrate to drop in...maybe soon

I did another extraction this evening (went for the full 100g scale this time) and set aside a few 50 mL portions to try to tick off at least some of the following questions. I'll figure out which I can do with the portions I made and salt accordingly, then salt the main batch.

Does the absence of water in the solvent inhibit crystallization of the citrate? (This seems pretty well established, but replication is always good)
Does fumaric acid crystallize reliably in cold EA?
Does fumaric acid crystallize as quickly/as well with or without a drying step in the process?
 
Cheelin said:
Running out of popcorn here, what’s the word on the citrate jar?


Btw, in case you haven’t seen this suggestion, post #10: CIELO Pull Step Question / Suggestion - Welcome discussion - Welcome to the DMT-Nexus
Click to expand...

Better get yourself some more, this movie is gonna drag on :lol:

No oil, no crystals. Just a bilayer. If there's no change by the end of the day I may try scratching the bottom of the jar with a stir rod a-la kick-starting recrystallization.

I fumarate salted two portions of my last extraction, one dried and one not, and left in the cold room, which was 64F at the time of salting, 59F when I checked this morning.

Both jars crystallized very well, but the crystals in the dried solvent developed much more quickly, and are, by my estimates, more than double the size of the ones in the un-dried solvent. Will take pics later.

In regards to that post, the thought of citric acid addition rate being a factor in oiling out has definitely crossed my mind. I have some thoughts but I'm going to try to organize those in a post later on today

Edit: fixed typo.
 

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Loveall said:
Both jars crystallized very well, but the crystals in the dried solvent developed much more quickly, and are, by my estimates, more than double the size of the ones in the dried solvent. Will take pics later.
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Did you mean undried solvent?
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Yes, sorry about that. I edited it to correct
 
orchidist said:
Cheelin said:
Running out of popcorn here, what’s the word on the citrate jar?


Btw, in case you haven’t seen this suggestion, post #10: CIELO Pull Step Question / Suggestion - Welcome discussion - Welcome to the DMT-Nexus
Click to expand...

Better get yourself some more, this movie is gonna drag on :lol:

No oil, no crystals. Just a bilayer. If there's no change by the end of the day I may try scratching the bottom of the jar with a stir rod a-la kick-starting recrystallization.

I fumarate salted two portions of my last extraction, one dried and one not, and left in the cold room, which was 64F at the time of salting, 59F when I checked this morning.

Both jars crystallized very well, but the crystals in the dried solvent developed much more quickly, and are, by my estimates, more than double the size of the ones in the un-dried solvent. Will take pics later.

In regards to that post, the thought of citric acid addition rate being a factor in oiling out has definitely crossed my mind. I have some thoughts but I'm going to try to organize those in a post later on today

Edit: fixed typo.
Click to expand...

How about dropping an M fumerate seed crystal?
 
Tilted the jar and a bunch of oil collected at the bottom. Weird! It progressed differently at the higher temperature, at least visually. Guess that's probably due to the oil's lower viscosity at this temperature, allowing it to collect at the bottom instead of remaining in small droplets on the sides of the jar.

I've gotten oil with two (ostensibly) independent sources of material. Both are very different in color, so I'm fairly confident they're different sources. May still be an issue of interfering minor alkaloids. Fumaric acid worked wonderfully with both, so maybe it is more selective.

I haven't tried extracting the third sample of powder [EDIT] yet, so there's still that to try.

It does appear, at least, that the oil, when collected into a puddle like this, appears colorless. When it formed cold, it always had some amount of brown tint to it.
 

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Interesting.

Are you sure nothing is wrong with your Millard's citric acid? You can dissolve a whole bunch in water, make sure it contains no oils. Or you could get a fresh source of citric and try again on a small pull sample.

Fumaric may be ignoring any extra alkaloids, or it may be crashing them as xtals along with any mescaline present. You can:

1) Try mini a CIELO process with citric acid on your fumarate product (if you get xtals we can say fumaric kept something in solution)
2) Send out your fumarate product out for analysis. If you get mescaline only we could say something is likely wrong with your citric acid. If you have other alkaloids besides mescaline in your fumarate product, it would be a new discovery.
 
Loveall said:
Are you sure nothing is wrong with your Millard's citric acid? You can dissolve a whole bunch in water, make sure it contains no oils. Or you could get a fresh source of citric and try again on a small pull sample.
Click to expand...

I will try that test. I did purchase a new packet about a week ago under suspicion that my old packet of milliard's might be at fault.

Loveall said:
Fumaric may be ignoring any extra alkaloids, or it may be crashing them as xtals along with any mescaline present. You can:

1) Try mini a CIELO process with citric acid on your fumarate product (if you get xtals we can say fumaric kept something in solution)
Click to expand...

I was previously unable to crystallize the results of a second A/B on my citrate oil. I do think that lends credence to the secondary alkaloid hypothesis, so I'm on board with attempting to convert some fumarate to citrate.

I think if I repeated my A/B process using the fumarate as the starting material instead of the oil, it would have less risk of re-introducing secondary alkaloids than if I brought more raw material into the mix via CIELO. I've got the equipment to do that pretty easily in an evening.

Loveall said:
2) Send out your fumarate product out for analysis. If you get mescaline only we could say something is likely wrong with your citric acid. If you have other alkaloids besides mescaline in your fumarate product, it would be a new discovery.
Click to expand...

Depending on cost, and results of (1), I might send both products, oil and fumarate crystals for analysis.
 
Another possible test would be to take the used solvent from crystallizing the fumarate, then add citric acid to it, to see if anything else crashes out. If it does, I could compare them with TLC and reagents, and send that for analysis.

Will probably split the solvent in two portions and wash one portion of the solvent with sat. Na2CO3 to remove any lingering fumaric acid in solution before introducing citric.
 
Maybe this is better for Loveall, but why wouldn’t you, as I mentioned earlier, drop an M-fumerate crystal into the citric jar and see if that drives crystallization?
 
Cheelin said:
Maybe this is better for Loveall, but why wouldn’t you, as I mentioned earlier, drop an M-fumerate crystal into the citric jar and see if that drives crystallization?
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Sorry, I meant to reply to that but I got scattered. I do think it's a good idea, and I tried it, but unfortunately it had no effect on the already oiled jar. I have one more portion of unsalted extract set aside. I wonder if I adding a couple seed crystals at the very start might help.

I'm going to hold off on that while I work on explore whether I can crystallize by converting the fumarate to the citrate. I was hoping to hold off on more citrate experiments until I could get results from Solaris, but it looks like they're not accepting new samples until at least July. I requested to be put on their mailing list, if they maintain one.

Do we know of any alternatives to Solaris?
 
Some interesting developments.

I collected the decanted solvent from my fumarate crystals, split it in two portions as described above.

The one which I did not wash remained clear on addition of the citric acid, however, it looks like maybe some additional non-citric acid crystals have formed. Will wait overnight to give it time to be sure all CA should be dissolved.

The one I washed with sodium carbonate actually clouded up a tiny bit when I added citric acid. That'll be very interesting to observe come morning.
 
orchidist said:
Cheelin said:
Maybe this is better for Loveall, but why wouldn’t you, as I mentioned earlier, drop an M-fumerate crystal into the citric jar and see if that drives crystallization?
Click to expand...

Sorry, I meant to reply to that but I got scattered. I do think it's a good idea, and I tried it, but unfortunately it had no effect on the already oiled jar. I have one more portion of unsalted extract set aside. I wonder if I adding a couple seed crystals at the very start might help.

I'm going to hold off on that while I work on explore whether I can crystallize by converting the fumarate to the citrate. I was hoping to hold off on more citrate experiments until I could get results from Solaris, but it looks like they're not accepting new samples until at least July. I requested to be put on their mailing list, if they maintain one.

Do we know of any alternatives to Solaris?
Click to expand...

Another analysis place is Energy control (contact Endlessness), based in Europe.

Let's see what you get with current tests. We can ask benzyme about the Solaris queue if needed.
 
Sorry for the delay, I will get in touch with endlessness.

Turned out the tiny quantity of solids at the bottom of the jars where I added citric acid to the previously fumaric salted solvent was not enough to show anything on my TLC plate. Probably should've just dropped some Marquis reagent on it instead. Hindsight...

I only used 100ml of solvent for this, but I have a couple liters of FA salted solvent to examine this weekend, so it's possible I may end up with enough material to run a TLC.

With regards to converting some of my fumarate back to citrate, I am hesitant to risk any more yield loss if I can help it. Fumaric acid works great for me. Still very curious to know what else is in this stuff that may be interfering, so hopefully we can get some mass specs!
 
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