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Some follow up Chem questions


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#1 YoshiTrainer

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Posted 04 June 2021 - 12:27 PM

First off, a huge thanks to the Brain Trust that participates on the various Chem related threads! I love science and enjoy reading your informative writings!

A couple follow up questions:

Is wetting the filter material (kitchen towel/men's shirt) before filtering to avoid losing solution still a good practice?

In photos from the internet, during the defat of cacti there is the dark cacti juice, a thin layer of cacti debris? then the naphtha on top. When draining off the dark cacti liquid, the middle layer becomes more apparent. (see pic) This layer stays w/the naphtha and is disposed?

I's it OK for the based liquid (w/NaCl) to remain in the HDPE jug for 6-12 hours before adding naphtha?
(edit) -answer, yes, that is where it is held while the naphtha is being salted and added back.

If there was no choice, would it be better to have your separatory funnel w/based juice and naphtha at 90F or 36F?
(edit) -answer, 90F, I'm guessing since warmed solvent and saltwater are used to break an emulsion?

Thanks again for the great threads!

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Edited by YoshiTrainer, 04 June 2021 - 03:44 PM.

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#2 YoshiTrainer

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Posted 04 June 2021 - 01:17 PM

I forgot, besides in your body, how are you storing your finished product? Im specifically asking about Mescaline but I suppose other extracts too? I'd guess, preweigh some low doses into gel caps and put in jar w/a couple desiccant packs? Then into a cool dark drawer?

#3 greenskeeper

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Posted 04 June 2021 - 04:21 PM

Mescaline freebase is not so soluble in naphtha - the preferred non-polar solvents are xylene, toluene, or limonene.

 

When defatting, after the mixture has separated and any emulsion has been resolved, keep only the dark aqueous liquid at the bottom.

 

Mescaline salts are very stable so they don't have any special storage needs. Doses in gel caps with a desiccant is good - dark and cool are fine but not necessary.

I don't know about other extracts.


Edited by greenskeeper, 04 June 2021 - 04:23 PM.

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#4 YoshiTrainer

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Posted 04 June 2021 - 05:33 PM

Thank you Greenskeeper! I've been reading so many threads, I think I got them mixed up, naphtha for DMT? May toluene or limonene be directly substituted for xylene in your process or do they require a separate process?

#5 greenskeeper

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Posted 04 June 2021 - 05:51 PM

Yeah, naphtha for DMT.

I believe xylene, toluene, and limonene are all used in exactly the same way so can be directly substituted.


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#6 YoshiTrainer

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Posted 04 June 2021 - 05:56 PM

Thank you!

#7 Phineas_Carmichael

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Posted 04 June 2021 - 08:36 PM

In the Actual Lab we almost always wet our filter media before filtering. Probably good practice in the Clandestine Lab too.

It's far easier to avoid emulsions than to break them. Mixing in one jar then Pouring a 2-phase mixture into a Sep funnel is a really rough process, mixing in the funnel is much gentler.

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. Reason being, in the defat you're probably only losing a few mg (provided its not a HUGE emulsion) and in the freebase you don't want any gunk in the solvent getting salted out with your product.

Sorry if I seem terse; I'm on break & gotta get back in. I'll have more time to write when my shift is over...

Edited by Phineas_Carmichael, 04 June 2021 - 09:25 PM.

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#8 YoshiTrainer

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Posted 04 June 2021 - 09:09 PM

No apologies necessary, I truly appreciate your time!

#9 tregar

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Posted 05 June 2021 - 02:43 AM

Yoshitrainer, I just make cactus tea, have done over 200 times, I save chem work for dmt now a days. I get no nausea with cactus tea, highly recommend, just filter the tea thru a cotton ball in a funnel and drink once boiled down to 6 to 8oz. But good luck with your defat. 


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#10 pharmer

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Posted 05 June 2021 - 05:57 AM

Warmer is better. Chemical reactions happen quicker in warmer environments


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#11 YoshiTrainer

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Posted 05 June 2021 - 11:56 AM

Thank you for your replies!

Mezcaline has always intrigued me, eating "buttons" has been on my bucket list for a long time. I really enjoy science but mostly use biology in my day to day so a few chemical reactions is exciting for me. Plus stretching some old brain cells is really enjoyable. I may try some well filtered tea to compare the 2 (someday). I'm not really a "speedy" kind of guy so I might wait for my Peruvian Torch to get a bit bigger? :)

Thank you Pharmer, that makes sense! So the ice bath during NaOH is to help cool and slow the reaction?

I'd still be curious how NaCl helps prevent/break emulsions? Reading a bit about cacti mucilage it is interesting trying to figure out the chemical reaction. Does it act as an inhibitor to prevent the mucilage from consolidating? From a cooks perspective, when you make nopales, you boil them in saltwater to alleviate the slime. When you add NaCl to the cacti juice as a preventative, does it dissolve in the solution or sediment? Does it change the electrical charge of the slime?

When adding the NaOH directly to the juice and not to water first the idea is to keep the volume roughly the same. I was wondering why not add the HCl directly to the solvent during salting to keep the volume the same also. Then I realised the water the HCL is dissolved in becomes the solution that the target molecule migrates into. Is this thinking correct?

Thank you again guys!
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#12 Norman

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Posted 05 June 2021 - 01:43 PM

NaCl causes the polar (aqueous) layer to become more polar and thus more readily separate from the non polar.
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#13 YoshiTrainer

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Posted 05 June 2021 - 02:03 PM

Thank you Norman!
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#14 Phineas_Carmichael

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Posted 05 June 2021 - 06:50 PM

Thank you Pharmer, that makes sense! So the ice bath during NaOH is to help cool and slow the reaction?

When you add any salt (and NaOH is the Hydroxide Salt of Sodium) to water some heat is released as the salt breaks apart into ions. You'll find this in a general chemistry textbook under the "heat of dissolution" section. NaOH just so happens to have a huge heat of dissolution value, so huge that it can actually raise the temperature of the water to 100*C! Obviously there are very few situations where a beaker of boiling pH 14+ solution would be desired, so the ice bath and gradual addition helps to keep the temp down.

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

We add things to the water, not the other way around. If you want to try a fun & terrifying experiment (Please Don't!) put on your labcoat, gloves, goggles, and rubber apron and add a drop of water to a small pile of crystalline NaOH. The drop will boil instantly (it's like a tiny explosion) & fling NaOH crystals all over the lab!

When adding the NaOH directly to the juice and not to water first the idea is to keep the volume roughly the same. I was wondering why not add the HCl directly to the solvent during salting to keep the volume the same also. Then I realised the water the HCL is dissolved in becomes the solution that the target molecule migrates into. Is this thinking correct?

That is correct. If you added 8 drops of HCl into the solvent you would end up with solvent with a bunch of freebase Mescaline in it & 8 drops of water with a tiny bit of Mescaline HCl.

What some people do when salting mescaline is to put 1-3 hundred mL of water in with the solvent, add a drop of HCl, mix it around & allow the phases to settle, then check the pH of the water. Repeat drop by drop until the pH is around 5.5 then separate the layers and evaporate the water to recover mescaline HCl.

This is pretty fun, Yoshi! Keep the questions coming; it might be neat to have a thread full of just general chemistry Q&A...
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#15 YoshiTrainer

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Posted 05 June 2021 - 07:09 PM

Thank you Phineas, I appreciate your responses! I'm sure I'll have more questions for you and the rest of the Brain Trust. By all means, if anyone else would like answers, feel free to post here too.

Cheers!

Ps, I'll take your word on not adding water to NaOH!

Edited by YoshiTrainer, 05 June 2021 - 07:12 PM.

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#16 omentheduck

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Posted 05 June 2021 - 08:18 PM

Great advice in this tread!


Edited by omentheduck, 05 June 2021 - 08:18 PM.

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#17 YoshiTrainer

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Posted 06 June 2021 - 01:53 PM

When under vacuum the BP of water, etc. Is lowered.

Is there such a mechanism for pH? What I mean, is there a mechanical or chemical way to only basify your cacti juice a little but make it perform as though it was 13+?

I've had different mild acid burns over the years but always feared a base burn as worse.


@Phineas, did Freddy ever test which acid is best for initial extraction, acetic, asorbic, citric or HCl?

Lastly, an A/B is actually an A/B/A extraction? (not ABBA) Since the starting and ending pH are similar? Just a massive catapult to the top of the pH chart in between.

#18 Phineas_Carmichael

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Posted 06 June 2021 - 04:21 PM

As far as I know, there's no pH equivalent for the way reduced pressure reduces BP. There's a chance that a high pressure system might make the basic phase more effective, but then you'd be working with a pressurized bomb full of NaOH solution. And you'd have to basify to 13 to extract anyway, or build some kind of crazy apparatus that could do it at pressure...

From my experience, acid burns are worse. Even pH 14 NaOH solution just makes your skin feel slimy, like bleach. In both cased that sliminess is actually the proteins in your skin breaking down. The real danger from NaOH (apart from the risk of blindness, protect your eyes!) is getting the crystals on your skin and getting physically burned by the heat of dissolution when they start to break apart on a molecular level from the moisture.

Freddy did a little work with MHRB acid extraction choices & the only thing he found was the need to choose an acid that is available, cost effective, and doesn't concentrate when the solution is reduced. Acetic, HCl, and citric all performed equally well, he never tried ascorbic, but sulfuric doesn't boil off with the water. Had to scrap that extraction and deal with a bunch of pH<1 solution...

An STB cactus extraction is technically an Acid/Base extraction, just done backwards. You could technically call it a B/A extraction, but that would just confuse people. Basify the plant matter to liberate the freebase, extract with solvent, then extract the solvent with acid to recover the salt. So yes, what we've been calling an A/B cactus extraction is really an A/B/A but again, people get confused easily.

Was all that clear? Did I get to everything? I sometimes get to rambling & forget where I was going...

Edited by Phineas_Carmichael, 06 June 2021 - 04:23 PM.

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#19 YoshiTrainer

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Posted 06 June 2021 - 05:28 PM

Thank you again Phineas!

A high pressure NaOH bomb sounds like a spectacularly bad idea!!!

I guess it is just my paranoia about strong bases. Years ago, I was dumb enough to grab a flask bare handed where nitric acid had dribbled down the side. It was interesting to watch a small divot of dead skin form over the next day or so. Thankfully live, hopefully learn. :)

I hope Freddie is well! Good to know there is not a major difference in acid choices. I remember reading of people using sulfuric acid to acidify water for their blueberry plants because it kept it's pH over time.

Thank you for clarifying A/B, STB. Freddie's work on the sloop in international waters comparing the two is a great read!
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#20 Norman

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Posted 06 June 2021 - 07:04 PM

Acid choice for salting is going to make more of a difference than for extracting before basifying since it determines what type of salt you get. I did discover early on that if you go way over with HCl in a MHRB extraction something happens to make the final product gooey as hell. Likely the excess acid making something in the bark soluble in the NP that wouldn’t be otherwise.
I burned the shoes off of my feet a couple of time when I was a dumb kid working in a chemical factory. I’ll give it to the bases just because they’re so hard to wash off and it’s so horrifying seeing your skin wash off with them. Potassium hydroxide eating it’s way under your fingernails is no fun either.
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