75 replies to this topic

[Phineas_Carmichael]

No.

Once the polar/non-polar liquids (whether the polar[aqueous] liquid is acidic or basic) separate, gently mix them up again and let them settle once more. Do it about 3 times, then separate the layers.

The reaction happens when the liquids are mixed together, not at the interface of 2 separated layers.

[YoshiTrainer]

Thank you again Phineas!

[YoshiTrainer]

May a food grade silicone spatula be used for scraping down heavily based, heated, cacti mush from the walls of a Pyrex bowl? What about with low pH?

[Phineas_Carmichael]

I use food grade silicone gear for soap-making (sodium hydroxide) all the time, and the proto-soap mixture is definitely as high or higher pH than extraction chemistry. You're good to go with silicone and all the hydroxide bases we use in the Clandestine Lab.

I think your acid choice might matter more than pH value with low pH... The food-grade acids -- citric, acetic, ascorbic, etc are definitely going to play nice with silicone. Hydrochloric and sulfuric might cause problems but I don't think they will; I'd wager a toe (but not a testicle) that you'd be fine using silicone with them. Nitric and nitrous I would definitely test first...

Whatever acid you're planning on using just pour a little bit of the concentrated form into a beaker and stick a cheap spatula into it. Let them sit overnight and check out the silicone in the morning. If there's any discoloration or melting you maybe shouldn't use that utensil.

Keep in mind too that some spatulas have silicone heads and handles made of a different material. If that's what you plan to use, you should definitely test the handle the same way.

*EDIT* Sorry it took me so long to respond. I was indisposed at a delightfully mid-century modern cabin for a much-needed break from the rat-race.

Edited by Phineas_Carmichael, 08 August 2021 - 04:53 AM.

[YoshiTrainer]

Thank you Phineas, glad you had a nice getaway!

[YoshiTrainer]

This may be different for you gents but I have a Chem question relating to magic mushrooms.

" Published reports demonstrate that a 3:1
blend of ethyl acetate and ethanol is a suitable
replacement for dichloromethane without
compromising chromatographic separation1"

Does this mean EA and ethanol combination may be directly substituted for dichloromethane in extractions?

May ethanol be substituted for methanol?

These are the extractions that I'm reading about:

"Stable-isotope labeling. P. mexicana FSU13617 was grown in 50 mL
liquid MEP medium amended with 1 mM 13C11-L-tryptophan (or 1 mM
unlabeled L-tryptophan for control), for 14 d. The biomass was harvested
by filtration, lyophilized, homogenized and extracted with 20% (v/v) acetic
acid in water. After filtration, the liquid was evaporated under reduced
pressure, and the residue was solved in MeOH, filtered, and used for
LC/MS (below).
Natural product extraction. Initially, mycelia and carpophores were
lyophilized, ground, and extracted with anhydrous MeOH, as described to
extract 1 gently and to minimize its artificial dephosphorylation to 2.
[4c]

For improved carboline yields, the fungal biomasses (mycelia,
carpophores, or sclerotia) were lyophilized, pulverized, and the powder
solved in 0.1 M HCl and subsequently extracted with methylene chloride
(1:1, v/v). The aqueous phases were collected, the pH value adjusted to
12 using NaOH, which was followed by extractions with methylene
chloride. The organic phases were dried under reduced pressure in a
rotary evaporator. The resulting crude extracts were dissolved in
methanol, centrifuged and filtered, and subsequently used for
chromatographic analysis or purification. To quantify 4 titers in fungal
biomass, the areas under the curve (AUCs) in the extracted ion
chromatograms were determined and referenced to a standard curve
recorded with authentic 4.
Chromatographic purification."


I think my final question is:

I have a jar of concentrated mushroom liquor that was extracted using citric acid and water, then concentrated through boiling. The resulting product had an aspic like consistency. I added an equal volume of moonshine to the jar and placed it in the freezer. After reading the above article again, I'm wondering if I should have neutralized or based the extract before adding the ethanol? Could/should I add pickling lime or sodium carbonate to the mix? I'm eventually hoping to filter it and would like to extract all the goodness first.

Here is a link to the complete paper.

https://mycotopia.ne...s/#entry1430832

[YoshiTrainer]

A couple more questions if you guys have the time.

With cleaning glassware, warm soap and water then air dry? I remember acetone washes of the glass, was that cleaning any residue, removing water, both?

In the CIELO tek for M extraction, they use a sodium carbonate solution to neutralize the citric acid in the ethyl acetate. To make sodium carbonate you bake sodium bicarbonate (baking soda) in a 200F degree oven for an hour to drive off CO2 and H2O. It is recommended to store dry or it'll convert back to bicarbonate. My question, when mixing the sodium carbonate with water, wouldn't that convert it back to bicarbonate or is the reaction slower or is it the lack of CO2?

[Phineas_Carmichael]

Any residue should be dissolved with an appropriate solvent before the soap & water wash and air drying. Acetone wash and hit with compressed air if you want to use the glass immediately & don't want to wait for it to air dry.

For sodium carbonate you can also buy a product called "washing soda" if you don't want to heat up the house with the oven.

As for conversion back to bicarbonate, let's look at the chemistry...

Bicarbonate is NaHCO3, heating it drives off the hydrogen to form Na2CO3. Over time it will react with moisture in the air and convert back to the bicarbonate but not in significant amounts unless stored in open air in a humid environment for a long time.

Remember that when dissolved in water, salts separate into their constituent ions. So, sodium carbonate becomes 2[Na+] + [CO3-] and bicarbonate becomes [Na+] + [H+] + [CO3-]

That extra [H+] in the bicarbonate is why it's a weaker base than the carbonate. Dig it?

Edited by Phineas_Carmichael, 27 January 2022 - 06:06 PM.

[YoshiTrainer]

Thank you sir!

[YoshiTrainer]

In thinking about an A/B, during the A part, the cacti is boiled in an acidic solution 3 times then once with water. Is the heating process just to speed up the transfer of M from the cacti to solution? What if you had a 1/4 pint of dry cacti powder, put it in a pint jar, cover it with regular white vinegar and let it sit for a week. Stir it twice a day, strain and refill each week. At the end of a month, boil down to a workable amount and proceed with the extraction.

Is one acid preferred over others for the A part? The smell of vinegar was overwhelming last time so I'm thinking of trying something else. I have citric acid and a blend for brewing that is tartaric/malic/citric.

[Phineas_Carmichael]

Yeah, the heat is just to speed the extraction. A long cold soak should in theory work just as well (potentially better if fewer undesirable fats, tannins, & waxes come over) as a short hot one. Just like how you can make a cup of coffee in 5 minutes with hot water or 12 hours in the fridge if you're doing cold-brew.

As far as acid choice goes it really only matters for salting. As long as the pH is below pKa minus 2 you should be good. Vinegar is usually the go-to because it's cheap, readily available, doesn't concentrate when reduced, and doesn't damage most cookware. If smell is an issue food grade citric would tick most if not all of those same boxes with very little odor.

[YoshiTrainer]

If one was a dumb-A and forgot to defat, what would be the consequences, just more emulsion?

[CatsAndBats]

Man, I have a lot of reading to do lol, thanks for this thread tho, Yoshi-san!

[YoshiTrainer]

Cats. If you have time, here are a couple really good reads.

https://mycotopia.ne...s/#entry1481541

https://wiki.dmt-nexus.me/CIELO

Regarding the defat, would a defat after salting be worthwhile or is itt moot at this stage?

Edited by YoshiTrainer, 20 December 2022 - 11:55 PM.

[YoshiTrainer]

What do you do if you get D-limonene in your salted water?

[CatsAndBats]

What do you do if you get D-limonene in your salted water?

Drink it!

 

 

 

Just kidding, don't drink it