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Some follow up Chem questions


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#41 pharmer

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Posted 15 June 2021 - 12:09 PM

Seems we're all related. That's Grandma Krokkers' recipe for cucumbers too :)     Absolutely positively a certainty that it's Hungarian in origin - or that's what she told me anyway


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#42 YoshiTrainer

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Posted 18 June 2021 - 10:32 AM

With the acetone clean up wash, if the acetone is freezer cold and your dirty mezcaline is freezer cold, could you combine the two, swirl and stick them together, back in the freezer? Pull out and swirl every so often until clean crystals appear as sediment? Then run them through your turkey baster/filter column, evap the acetone and wash w/warm water, collect and evap? Or does longterm exposure of mezcaline to acetone break it down? Would multiple wash/evap to get a cleaner product cause any other issues? I'd imagine if you didn't filter well enough early on that you'd notice it at this stage of the operation in the form of sediment causing slowed/clogged filtering?

#43 Phineas_Carmichael

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Posted 18 June 2021 - 08:32 PM

We do a quick swirl in the cold acetone because mescaline HCl is slightly soluble, but the impurities are more soluble. You want to get the impure product in and out of the acetone quickly so that just the impurities are dissolved. If you combine the two & let them sit, even in the freezer, you're going to lose more good product than if you did multiple quick washes.
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#44 YoshiTrainer

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Posted 21 June 2021 - 12:22 PM

Does some of the NaCl come along in to the evap dish. In a picture online, someone had cube shaped crystals left along with pin shaped crystals. The cube shaped looked exactly like NaCl. I'd guess if someone went w/the "shit ton" approach when adding NaCl, it'd carry over?

#45 Norman

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Posted 21 June 2021 - 02:43 PM

If it made it into the xylene somehow then it would move into the water in the salting solution. Also if one were salting with HCl, and lNaOh had gotten into the xylene, they would form NaCl. That would be the fault of bad technique rather than chemistry though, since neither should be in the xylene.
I think that happened to me once - I seemed to be getting fantastic yields from a relatively small extraction that I was salting with H2SO4. The yield didn’t taste bitter at all, just vaguely salty so I think I made a sulfite something.
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#46 YoshiTrainer

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Posted 21 June 2021 - 04:06 PM

I wonder how many "common" salts of mezcaline there are? Just from reading, acetic, carbonic, HCl, sulfuric, ascorbic?

#47 Norman

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Posted 21 June 2021 - 08:50 PM

I guess it would depend on what you mean by common.
In theory most acids would form a salt when combined with the alkaloid.
Based on nothing, I’ll assume that it’s stored in the plant as a citric or ascorbic acid salt so those (or whatever) would be the commonly naturally occurring ones.
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#48 YoshiTrainer

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Posted 22 June 2021 - 02:08 AM

Thank you Norman! I guess by common I was referring to acids that are readily available. In a lab setting you would have access to a much wider variety of concentrated acids. I think I was also bit curious what could be, malic acid, gibberelic, lactic?

#49 Phineas_Carmichael

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Posted 24 June 2021 - 07:55 AM

There's nothing available in the Lab that isn't available to a clandestine chemist with knowledge & willpower...

All those acids are freely available and not controlled. The mescaline salts they make might be more or less active, more or less gooey, or more or less worth experimenting with.

Mescaline Gibberelate sounds like it would be a hilarious thing to bring to the research group for a taste test!

Edited by Phineas_Carmichael, 24 June 2021 - 07:56 AM.

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#50 YoshiTrainer

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Posted 24 June 2021 - 04:19 PM

"The mescaline salts they make might be more or less active, more or less gooey, or more or less worth experimenting with."

I suppose this begs the question, which salt is "the best"? It is probably a little subjective but if Freddie walked into W-mart to get some cat food and decided to peruse their selection of salts, which would he choose?

"In the event an emulsion absolutely cannot be broken it should stay with the layer that is not moving on in the process. A defat emulsion should stay with the solvent. A freebase emulsion should stay with the aqueous."

In the case of a freebase emulsion, it is drained off with the aqueous. After salting, when the aqeous is added back to the solvent for the next pull, are you able to release the target molecule from the emulsion? When you swirl the 3 phases together in your funnel, are you pulling from the emulsion in addition to the aqueous? If you did 5 pulls carrying an emulsion, would you still get as much of the target molecule from the aqueous?
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#51 skunk

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Posted 24 June 2021 - 06:08 PM

What a great thread! Definitely enjoying all the great info getting put forth here! Will definitely be following along.

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#52 Norman

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Posted 24 June 2021 - 08:00 PM

There is no best. Best for what?
Fumarate for DMT if you want a dry salt end product but plain old DWV is tried and true for boiling bark.
Sulfate for mescaline if you know your expected yield and want to do the math to get pretty needles, HCl if not since it evaporates clean.
About anything will work for simply getting an alkaloid into an aqueous phase. If you’re going to ingest it like that, look to food grade citric or acetic. Are you going to reduce it? Then look to acetic since citric will concentrate.
There is no “one”, though I guess HCl will do just about anything, is nice and simple, strong, and doesn’t stick around.
Saying “acid” or “salt” is only about 50% more specific than saying “chemical”.
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#53 Phineas_Carmichael

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Posted 25 June 2021 - 04:20 AM

I agree with everything Norman just said.

For salting freebase mescaline from a cactus extraction, nothing beats good old aqueous HCl. It's straightforward, easily obtainable, and for the most part evaporates cleanly to form a shelf-stable crystalline product that can be easily cleaned up to acceptably decent levels of purity with very little Lab technique required.

As far as which mescaline salt is best for dosing, I don't think it matters that much. Biochem was never my forte, but it's always been my understanding that the HCl in the stomach converts whatever you take into the hydrochloride anyway. Also, in the bloodstream (avg pH 7.4) mescaline is going to exist as the freebase, which (again, in my admittedly rudimentary understanding) is what binds to the Neurotransmitter receptors & causes a psychedelic effect.

...
In the case of a freebase emulsion, it is drained off with the aqueous. After salting, when the aqeous is added back to the solvent for the next pull, are you able to release the target molecule from the emulsion?

When you swirl the 3 phases together in your funnel, are you pulling from the emulsion in addition to the aqueous?

If you did 5 pulls carrying an emulsion, would you still get as much of the target molecule from the aqueous?

Ideally, that freebase emulsion should break fairly quickly once it's out of the Sep funnel. Being sandwiched between 2 layers with its "fingers" in both makes it harder to break, plus adding NaCl & carefully applying heat are both a lot easier in a jar or beaker.

The emulsion locks up the target molecule pretty tightly, so you want to try and break it at every step of the way. You can also break a freebase emulsion by draining the aqueous out, leaving just the emulsion & non-polar in the funnel, and adding warm ph 14 NaOH solution 0.5-1.0mL at a time to the top of the funnel with gentle swirling between additions.

If an emulsion absolutely refuses to break & you must carry it through 5 pulls, then yes, yield would be reduced. But probably only in a way that would matter if a TA was grading your extraction based on a rubric provided by the Professor. You're not going to lose "dosage levels" of product to a stubborn emulsion unless the extraction (or the emulsion) is absolutely gigantic.

[EDIT] Technique-wise, you should be separating all components to their designated jars or beakers and thoroughly cleaning and drying the Sep funnel between all pulls. Put the freebase aqueous in, add the non-polar, and gently mix. Drain the freebase aqueous, add the salting solution, gently mix and drain it, then dump the non-polar out the top of the funnel before cleaning and repeating.

Dumping the freebase aqueous on top of the non-polar in a Sep funnel is ROUGH... A recipe for emulsion...[/EDIT]

Edited by Phineas_Carmichael, 25 June 2021 - 07:47 AM.

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#54 YoshiTrainer

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Posted 25 June 2021 - 09:03 AM

Thank you again gentlemen for the great information!

#55 YoshiTrainer

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Posted 10 July 2021 - 03:45 PM

In an A/B using Limonene, do you still defat using Limonene?

In an STB, is it possible to use fresh (wet) green skins and just reduce the water used?

#56 Phineas_Carmichael

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Posted 10 July 2021 - 04:34 PM

Limonene is structurally similar to and behaves like xylene/toluene so it should be just fine to use as a defat solvent.

While I've never seen an STB using fresh cactus I don't see any reason why it wouldn't work. Depending on the water content of the skins one might not need any additional water at all in a Drytek using calcium hydroxide. In a more traditional sodium hydroxide STB I'm not sure the amount of pH 14 solution would be all that reduced.
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#57 FLASHINGROOSTER

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Posted 11 July 2021 - 03:11 PM

This is also why my favorite poem from the Chem Lab exists:
"Always do what you oughtta,
Add the acid to the watah."

 

Anyone else singing this to the safety dance melody right now?

 

 

[Direct Link]


Edited by FLASHINGROOSTER, 11 July 2021 - 03:12 PM.

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#58 Phineas_Carmichael

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Posted 12 July 2021 - 12:35 AM

It only needed a little rewriting for the Lab :laugh:

[4 Bar Instrumental Intro]

Always do what you ought to,
In your Life and in the Lab.
If Teacher gives the order
And you then ignore her,
That reaction's gonna turn out bad!

We can make what we want to,
All the drugs that we can find.
But you better wear your goggles
Avoid a boondoggle
That tragi-cally leaves you blind!

[4 Bar Instrumental Break]

We'll extract what we want to,
In a well-ventilated room.
And if we dress real dope,
In gloves
and lab-coat
We'll avoid an unexpected BOOM!

We can work when we want to,
But this shit is not a game.
Get advice and heed it
Wear an apron if you need it
And look out for unattended flame!

We can dance, we can dance,
Everything's under control.
We can dance, we can dance,
If it isn't: Stop, Drop, and Roll!
We can dance, we can dance,
Everybody wear your long pants.
We can dance, we can dance,
Nobody's taking the cha-ah-ha-hance!
Safety dance
We do the safety dance!
We love the safety dance!

[4 Bar Instrumental Break]
[Synth Build bridges Break with Verse]

It doesn't matter if we want to,
At stake is your life and mine.
Always gotta use it
If we don't abuse it
Everything will turn out fine.

We dance because we want to,
We must leave your friends behind.
Because your friends don't dance
And cuz they don't dance
Well they're, no friends of mine.

We can dance, we can dance,
Everything's under control.
We can dance, we can dance,
If it isn't: Stop, Drop, and Roll!
We can dance, we can dance,
Everybody wear your long pants.
We can dance, we can dance,
Nobody's taking the cha-ah-ha-hance.

Safety dance misc to fade out...

Please forgive me a few rhythmic liberties; that first stanza is ROUGH, but I wanted to start with a reference to the original poem. It's a little easier to sing over a karaoke backing track...

[Direct Link]


Edited by Phineas_Carmichael, 12 July 2021 - 03:39 AM.

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#59 FLASHINGROOSTER

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Posted 12 July 2021 - 03:03 PM

hahaha that is awesome



#60 YoshiTrainer

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Posted 12 July 2021 - 09:04 PM

With A/B cacti extractions, once the juice is based are there extended reactions times during any of the remaining steps? During the pull, the procedure says wait 6-12 hours to separate, is this necessary? After swirling the based juice and solvent together, if it separates cleanly, do you need to wait for the target molecule to migrate? Same with the salting, after swirling if they separate cleanly, should you wait before running off the salted water?




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