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Bridgesii/lagengormis Extraction


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#21 HrVanker

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Posted 11 November 2020 - 05:12 PM

After I started this thread, I realized that it wasn't going to happen. I mixed the powdered cactus w/ the tea and then added NaCl in an attempt to keep mold from growing, and it seemed to work. And now, after a ridiculous amount of time, this extraction is finally happening. Some minor mistakes were made, but nothing that could not be worked around.

 

Today, the tea/powdered cactus mix was acidified using sulfuric acid. Initially it was at a PH of 3-4 and allowed to stir for a while. 200ml of xylene was added to de-fat the 600ml mixture, allowed to mix in, then allowed to separate. A very stubborn emulsion formed, but with the addition of more acid, and some heat it eventually separated. I don't have any NaCl at the moment (I know, I know...), so that wasn't an option.

 

After allowing the emulsion to resolve, the xylene was a dark brown/green color. The solvent was siphoned off and discarded. There was a thin layer of fatty xylene left on the surface. Most of it was siphoned off by using the stir plate to pool it in the center of the beaker, but there was still a tiny bit left.

 

The acidic mixture was then basified using NaOH. I was aiming for a PH 10, but it ended up being 14. 200ml of xylene were then added, allowed to mix a little bit but not all the way. It is currently on the lowest stir setting, there is little to no emulsion forming, and the solvent is turning a nice yellow color.

 

More updates coming soon.


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#22 Norman

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Posted 11 November 2020 - 09:16 PM

I’m glad you picked this back up! I hate when good threads die off.
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#23 HrVanker

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Posted 17 November 2020 - 01:25 AM

Sorry for the delayed update. I'm a little embarrassed, but I ended up scrapping the whole thing...

 

When it was time to salt the goodies, Trout's workaround was attempted. This entails slowly adding dilute acid, separating the aqueous layer and PH'ing it until it stops being neutralized. Perhaps due to a mix of xylene fume exposure and several hours of work, the procedure was rushed.The fullest strength H2SO4 available (UN2796, ~40% maybe) was added in very small amounts as an attempt to hurry things along. With the first very small drops, no reaction was observed. Just a water based mixture falling through a non-polar fluid. The contents were swished around a bit, but still no visible changes. Instead of adding some distilled water, a few more drops of acid were added...

 

At one point, a drop of the aqueous/acid layer was PH'd and found to be 0, so apparently nothing was neutralized. This could be due to 3 causes:

1. The acid was too concentrated. One could imagine that too high of a concentration would salt the goodies, but still be extremely acidic. However, if this was the case one would expect the aqueous layer to change color. This did not occur, even after prolonged exposure.

2. The sulfate is soluble in both water and Xylene. Somewhere, possibly Erowid, there is mention of the acetate being soluble in both Xylene and water. Thus vinegar is useless for this specific procedure. The acid being concentrated would likely still test at 0.

3. The salts in the tea decomposed in the 14mo since this thread was started.

 

At least some lessons were learned and experience gained. The acid should definitely have been diluted. Additionally, more care will be taken, specifically: ventilation, following instructions, and using muriatic acid since it seems to be tried and true for this sort of thing.

 

I'm very interested to hear the feedback on this. It is perplexing as to why the solvent changed color, but the acid showed no change. No color change, no PH change, and no opaque precipitate was seen while shaken with the solvent. That last one may not occur with this reaction, but it seems like it should.



#24 Phineas_Carmichael

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Posted 17 November 2020 - 01:48 AM

I don’t know why he uses HCl vs sulphuric either though I don’t think it really makes much difference in the initial boil since the alks are likely in salt form in the cactus in the first place. Adding acid is just a precaution to make sure everything stays acidic.
Thinking about it, I’m not sure either if the small amount of sulfuric used would give you that cellulose breakdown either or if it would be a good thing since broken down cellulose could just end up gumming up your extraction.
I think he mentioned somewhere that the xylene/ toluene mix was because he ran out of one and switched to the other at some point. They’re very similar, xylene being just toluene with an extra methyl group.

Looking back at Freddie's notebooks, HCl was used in the initial boil because it was considerably cheaper for him to acquire at that time than sulfuric.  Muriatic acid was about $3USD per gallon and sulphuric was $8USD per quart,

 

Indeed, the xylene/toluene mix was chosen simply because of what he had on hand.

 

 

Sorry for the delayed update. I'm a little embarrassed, but I ended up scrapping the whole thing...

 

When it was time to salt the goodies, Trout's workaround was attempted. This entails slowly adding dilute acid, separating the aqueous layer and PH'ing it until it stops being neutralized. Perhaps due to a mix of xylene fume exposure and several hours of work, the procedure was rushed.The fullest strength H2SO4 available (UN2796, ~40% maybe) was added in very small amounts as an attempt to hurry things along. With the first very small drops, no reaction was observed. Just a water based mixture falling through a non-polar fluid. The contents were swished around a bit, but still no visible changes. Instead of adding some distilled water, a few more drops of acid were added...

 

At one point, a drop of the aqueous/acid layer was PH'd and found to be 0, so apparently nothing was neutralized. This could be due to 3 causes:

1. The acid was too concentrated. One could imagine that too high of a concentration would salt the goodies, but still be extremely acidic. However, if this was the case one would expect the aqueous layer to change color. This did not occur, even after prolonged exposure.

2. The sulfate is soluble in both water and Xylene. Somewhere, possibly Erowid, there is mention of the acetate being soluble in both Xylene and water. Thus vinegar is useless for this specific procedure. The acid being concentrated would likely still test at 0.

3. The salts in the tea decomposed in the 14mo since this thread was started.

 

At least some lessons were learned and experience gained. The acid should definitely have been diluted. Additionally, more care will be taken, specifically: ventilation, following instructions, and using muriatic acid since it seems to be tried and true for this sort of thing.

 

I'm very interested to hear the feedback on this. It is perplexing as to why the solvent changed color, but the acid showed no change. No color change, no PH change, and no opaque precipitate was seen while shaken with the solvent. That last one may not occur with this reaction, but it seems like it should.

 

Oh no! Did you throw everything out? We can possibly still save it if you didn't! I've been meaning to chime in for a few days but have been stupid-busy at work lately & just passed out when I got home...

 

#1: 40% is definitely too strong to be salting with. I'm not familiar with Trout's workaround though...

#2: The sulfate salts should be relatively insoluble in non polar, just like the HCl.  Sulphuric acid deprotonates its first proton just as readily. Acetic is weak...

#3: This is possible, but unlikely if the solution's pH was below 7.56...

 

If you still have everything I'd recommend evaporating the aqueous solution & seeing what you get. Sorry I didn't get into this one until it was too late :(


Edited by Phineas_Carmichael, 17 November 2020 - 01:52 AM.

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#25 HrVanker

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Posted 17 November 2020 - 02:41 AM

Oh no! Did you throw everything out? We can possibly still save it if you didn't! I've been meaning to chime in for a few days but have been stupid-busy at work lately & just passed out when I got home...

 

#1: 40% is definitely too strong to be salting with. I'm not familiar with Trout's workaround though...

#2: The sulfate salts should be relatively insoluble in non polar, just like the HCl.  Sulphuric acid deprotonates its first proton just as readily. Acetic is weak...

#3: This is possible, but unlikely if the solution's pH was below 7.56...

 

If you still have everything I'd recommend evaporating the aqueous solution & seeing what you get. Sorry I didn't get into this one until it was too late :(

 

 

Throwing it away was a huge mistake. Salting was Plan B, with evaporation of the xylene as Plan A. The realization that evaporation would smell too much and take a long time was a real bummer, then the salting was even more frustrating (admittedly due to some hastiness). All that frustration, plus some paranoia regarding (and possibly due to) the xylene smell was just a little too much that day.

 

The thought at the time was that evaporating the aqueous solution would leave a product that was too much work to separate. I am still very interested to hear what your recommendation would have been after evaporating the water. Would the H2SO4 oxidize into something more inert and easy to handle? The assumption was that it would be a strongly acidic mess that could not be dealt with due to equipment and reagent limitations.

 

Any thoughts on the lack of color change in the water layer? Presumably most of the non-polar products from the cactus tea should salt out, contributing at least some color to the aqueous layer. Even after putting it all in a beaker with a stir bar and some heat, there was no visible change to the solution, and no observable change in PH (which is far less surprising than the lack of color change).

 

As I understand it, Trout's Workaround is based on the idea that a weak acid will neutralize when reacting with a basic substance. So you salt with a dilute acid, separate and PH the water solution. If it's neutral, salt again with some more dilute acid, check the PH again, and so on. Once the aqueous layer starts to test acidic, you've salted all the goodies with [hopefully] minimal loss. 

 

Thank you for the input Phineas. This definitely won't be the last opportunity for this procedure, and it's always good to learn more.



#26 HrVanker

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Posted 08 January 2021 - 02:27 AM

Oh no! Did you throw everything out? We can possibly still save it if you didn't! I've been meaning to chime in for a few days but have been stupid-busy at work lately & just passed out when I got home...

 

#1: 40% is definitely too strong to be salting with. I'm not familiar with Trout's workaround though...

#2: The sulfate salts should be relatively insoluble in non polar, just like the HCl.  Sulphuric acid deprotonates its first proton just as readily. Acetic is weak...

#3: This is possible, but unlikely if the solution's pH was below 7.56...

 

If you still have everything I'd recommend evaporating the aqueous solution & seeing what you get. Sorry I didn't get into this one until it was too late :(

 

So the solution to an overly acidified salting/aqueous layer has been bugging me ever since that extraction got messed up. In that scenario would it be possible to neutralize and basify the acid layer until the mesc turns back into its freebase?



#27 Norman

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Posted 08 January 2021 - 04:39 PM

Always worth a try.
Whenever something goes horribly sideways like that, I throw everything back together, base it to 13.5, and start over from there.
Sometimes it works sometimes not.
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#28 Phineas_Carmichael

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Posted 09 January 2021 - 03:00 AM

So the solution to an overly acidified salting/aqueous layer has been bugging me ever since that extraction got messed up. In that scenario would it be possible to neutralize and basify the acid layer until the mesc turns back into its freebase?

 

 

Norman beat me to it again! He is one of the giants whose shoulders I stand on...  :wub:

 

The "Target Molecule" is almost always available somewhere in your extraction. You can manipulate the pH to extremes without destroying your target most of the time and it never hurts to try. This is why we say never throw anything out until the very end.


Edited by Phineas_Carmichael, 09 January 2021 - 03:09 AM.

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#29 August West

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Posted 10 January 2021 - 07:58 PM

Holy shit Phineas...how often are you around here!? I haven't noticed you in a long time...hope you and yours are well...


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#30 Phineas_Carmichael

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Posted 11 January 2021 - 02:51 AM

Holy shit Phineas...how often are you around here!? I haven't noticed you in a long time...hope you and yours are well...

 

I'm here every day, but I generally only check botanicals to see if I can help someone with an extraction. I very rarely actually sign in...

 

Here's hoping you and yours are well too! Keep your stick on the ice my man  :thumbs_up:


Edited by Phineas_Carmichael, 11 January 2021 - 02:54 AM.

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#31 Norman

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Posted 11 January 2021 - 05:58 PM

Same here. Things are slow these days - this is one of two active threads in Botanicals this year.
Anyway - maybe you could weigh in here:
https://mycotopia.ne...n/#entry1466629
I could use your perspective.
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#32 Alpoehi

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Posted 13 February 2021 - 03:28 PM

Stay tuned I‘m about to make my first Kesh‘s A/B extraction.
Just posting here so that I'll find the thread again ...

Edited by Alpoehi, 13 February 2021 - 03:29 PM.


#33 Norman

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Posted 14 February 2021 - 04:16 AM

Link to the tek?

#34 Alpoehi

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Posted 14 February 2021 - 05:18 AM

sry forgot the link:
https://wiki.dmt-nex...line_Extraction

c7b268527273f6078f22dc7aa926098b.jpg
now the journey begins ... I got 1 l juice already it just leaked out of the frozen chops. Don't know yet if I add the juice to A/B tek or if I use the juice for another tek.

#35 Alpoehi

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Posted 15 February 2021 - 12:57 PM

Holy Shit!
It works!

d02b563718c19078a485c7740d8e625c.jpg

Will post a follow-up later.
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#36 pharmer

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Posted 15 February 2021 - 03:30 PM

holy shizz, you got there in a hurry :)


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#37 Norman

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Posted 15 February 2021 - 05:07 PM

Looking good!
You should start this in a new thread. I’m curious to see how that tek went - he made it sound way easier than my experience has been.

#38 Alpoehi

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Posted 15 February 2021 - 05:29 PM

Looking good!
You should start this in a new thread. I’m curious to see how that tek went - he made it sound way easier than my experience has been.


Still have to figure out the MEK wash.
Crystals are thin like needles dont't know how to decant from MEK solvent. But yeah a new thread to summon up things maybe.
I followed instructions to the letter and can share my observations. I had no problems with emulgating or not being able to seperate layers.

#39 pharmer

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Posted 15 February 2021 - 06:04 PM

MEK has a super low boiling point. You should be able to set up a double boiler and drive off the MEK to leave behind dry crystals



#40 Norman

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Posted 15 February 2021 - 07:59 PM

I don’t think one would want to evaporate the MEK because the nasties would just end up back on the product.
I’d use something tall and narrow that would allow pouring solvent off the top without disturbing the crystals at the bottom - like a test tube.
Save everything and if you mess up just evaporate it all and start over.
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