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Trying Again


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#1 HrVanker

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Posted 12 July 2022 - 10:52 PM

Last time I tried to extract cactus, I didn't plan too well. I didn't realize that evaporating xylene wasn't really a thing, and the only acid I had was sulfuric of unknown concentration. This time I'm trying to plan a little better. Just read through @YoshiTrainer and @el_ronhub_bird 's threads, and think a regular A/B[/A] extraction is probably best.

As far as material, I have 1096g fresh whole cactus. I just de-spined it and blended it w/ distilled vinegar. Boiled/simmered for an hour or two, strained through several layers of cheesecloth, put back in the saucepan, added more vinegar and a dash of DI water and simmered again. Currently on the second simmer.

For solvents, I have xylene but for safety reasons I think limonene is probably better. I can also get muriatic acid for salting. The idea of sulfate is attractive, but I should probably keep it simple.

I did do a little experiment w/ the H2SO4 to try and get a ballpark concentration. My scale shut off part way through, so I'll have to run it again to get more accurate results. But it seems that somewhere between 12g and 14g of NaHCO3 neutralized 20.2g of the sulfuric acid. If I did my math correctly, that means that the acid is somewhere around 40%?
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#2 Phineas_Carmichael

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Posted 13 July 2022 - 05:16 PM

Definitely get the muriatic for salting as it is much more forgiving. Mescaline sulfate crystals are beautiful, but getting them requires precise calculations.

Sulfuric is a diprotic acid; I'm not sure about your concentration estimate above. Unfortunately, I'm at work & can't double-check it just now. I'll take a closer look when I get home & can pull out a textbook to reference.
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#3 YoshiTrainer

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Posted 13 July 2022 - 05:39 PM

HrVanker, if you haven't already, please check out Greenskeeper's thread on A/B extractions. He uses Xylene too.

https://mycotopia.ne...-1#entry1481541

Between this and Phineas's help, you should be golden!

Good luck and let us know how it goes!
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#4 HrVanker

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Posted 13 July 2022 - 08:09 PM

HrVanker, if you haven't already, please check out Greenskeeper's thread on A/B extractions. He uses Xylene too.

Between this and Phineas's help, you should be golden!

I haven't checked GreensKeeper's thread yet, but saw a lot of his posts in [I think] El Ron's thread. I'll definitely get to his soon!

My desire to avoid the xylene is mostly due to safety/ventilation reasons. I tried the xylene last time and the fumes definitely got to me, plus my neighbors.

Definitely get the muriatic for salting as it is much more forgiving. Mescaline sulfate crystals are beautiful, but getting them requires precise calculations.

Sulfuric is a diprotic acid; I'm not sure about your concentration estimate above. Unfortunately, I'm at work & can't double-check it just now. I'll take a closer look when I get home & can pull out a textbook to reference.

I'll be getting the muriatic.

When I did the baking soda test, I looked up the equation for H2SO4 + NaHCO3 which comes out to 2NaHCO3/1H2SO4 to balance out.
Estimated NaHCO3 used: (0.1666535526 mol)
0.1666535526 ÷ 2 = moles of H2SO4 neutralized
After converting back to G, then dividing by mass of starting sample to yield %.
I wouldn't be shocked if that isn't correct. Lol


So far I've done 4 boils on the material and am reducing the 4qt of resulting liquid. Is it worth boiling more? I'm sure some color would still come out, but I can't imagine there's much salt left in it.

Edited by HrVanker, 13 July 2022 - 08:18 PM.

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#5 Phineas_Carmichael

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Posted 14 July 2022 - 05:56 AM

I'll be getting the muriatic.

When I did the baking soda test, I looked up the equation for H2SO4 + NaHCO3 which comes out to 2NaHCO3/1H2SO4 to balance out.
Estimated NaHCO3 used: (0.1666535526 mol)
0.1666535526 ÷ 2 = moles of H2SO4 neutralized
After converting back to G, then dividing by mass of starting sample to yield %.
I wouldn't be shocked if that isn't correct. Lol

That's some bang-up stoichiometry for percent by weight! I had forgotten that we don't have to worry about acids with more than 1 hydrogen when we're reacting them with bases, just when calculating pH in aqueous solution. Great job!!

I was concerned with the 40% because it's almost exactly double the concentration of battery electrolyte, the most readily available source of sulfuric acid in hardware & auto parts stores in my neck of the woods. Can you access the SDS for your acid to confirm? If you're not using it for salting then it shouldn't matter, but I like to keep an SDS binder for everything in my house & I encourage others to do the same.

So far I've done 4 boils on the material and am reducing the 4qt of resulting liquid. Is it worth boiling more? I'm sure some color would still come out, but I can't imagine there's much salt left in it.

5 is a nice number & I like nice numbers, but you're probably good after 4 boils. Keep the cactus mush until the end (freeze it if you're going to take more than a week) just in case. If you end up with a low yield we can try & wazzle some more magic out of it.

You're definitely on the right track. Dropping your stoichiometry numbers on me like that eliminated any doubt. You, my friend, are a Clandestine Chemist & you'll have some nice clean product soon.

*EDIT* I'm excited to talk about an extraction again!!

Edited by Phineas_Carmichael, 14 July 2022 - 06:11 AM.

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#6 HrVanker

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Posted 15 July 2022 - 06:02 PM

Thanks for validating my math, and glad I have some idea of what I'm doing! The baking soda estimate I used could be way off. I tested the neutralized solution a little later and it was in the range of 8, plus the scale shut-off thing. I just figured I'd carry through as a proof of concept.

When I received the sulfuric I did look for the SDS. I couldn't find much at the time, but I vaguely recall 32%, which is closer to 40 but still way more than 20. I know the brand is WPS (Western Power Sports), and when I search the info on the label (UN2796) all I see is "not more than 51%".

Since I did my math well, I'll do another titration and use the timer on my scale so it won't shut off.

And now, the bad news: I put the 4qt of liquid on low to reduce (2 on my med electric burner). It was reducing nice and slowly, no boiling or violent bubbling, had it going for about 6hrs before I was just below 3qt. I wanted to take it closer to 2 so I let it go. Then I woke up at 2am to the worst vinegar and burnt organic matter smell I've ever known.

Still kicking myself, because I've done similar things during grain prep. But I think I just need to set a 30min timer/alarm for these longer things so I don't fuck it up again, or find a fancy induction cook top that has vape-like temp control to prevent burning. Lol

Sorry to get the excitement up... I was excited too. Perhaps I'll source some good cuttings to try again before next year. The cuttings I have left need to root.

Thanks for the help. Will update here when relevant.

Edited by HrVanker, 15 July 2022 - 06:59 PM.

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#7 Phineas_Carmichael

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Posted 17 July 2022 - 07:07 AM

Oh, no!!!!

Burnt cactus smell is a ding-dang tragedy!!!

It's a "teachable moment" though, for anyone who reads this thread, and that's a good thing!

Any time we have an extraction in process we need to be present at all times. If we are getting sleepy we can always hit pause, throw the pot in the fridge, & resume boiling at a later date. There is no hard-and-fast rule that says the volume reduction has to happen ASAP.

I'm so very sorry this extraction didn't work out. :cry:

======

You've got mad clandestine chemist skills for sure, though! I want to see a write-up of your experiment if you can find the time to make a "titration for acid concentration identification" thread! A stand-alone write-up of that process would be worthy of the archives in my opinion.

I hate to give you homework, but I'd love to try and replicate your method. Titration is fun!

Edited by Phineas_Carmichael, 17 July 2022 - 07:27 AM.

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#8 YoshiTrainer

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Posted 17 July 2022 - 03:24 PM

I wonder, even though it overcooked, would it still be ruined? Isn't M destroyed in the 300F range? Could it have been possible to allow the pan to cool a bit, add some water and scrape up the residue like deglazing? Even if the end product had discoloration or acridness to it, it'd still be a win.

Maybe the act of desiccation would destroy the M freebase?
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#9 Phineas_Carmichael

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Posted 18 July 2022 - 12:59 AM

I like your wishful thinking Yoshi, but if one wakes up at 2am to the smell of burning that's probably the end for any extraction.

If there was any water left in the pot then the temperature couldn't get above 212*F & the target molecule would be safe. Once the water boils out, though, all bets are off. If what was left in the pot was a residue that needed deglazing I'd wager a toe that the temperature got above the degradation temp for mescaline acetate. (Remember, in the acidic phase of an extraction we're working with the salt, not the freebase)

I frequently use an IR thermometer when cooking to make sure my pan is the proper temperature for searing or deep frying. Even the lowest setting on my stove's smallest burner will heat a dry pan to 450*F if I get distracted while waiting for it to preheat. I'm sure if I left it for several hours it would get even hotter...

Edited by Phineas_Carmichael, 18 July 2022 - 01:05 AM.

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#10 YoshiTrainer

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Posted 18 July 2022 - 11:12 AM

Wishful thinking Phineas, thank you!
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