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Some follow up Chem questions


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#61 Phineas_Carmichael

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Posted 13 July 2021 - 08:01 AM

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.
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#62 YoshiTrainer

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Posted 13 July 2021 - 09:54 AM

Thank you again Phineas!

#63 YoshiTrainer

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Posted 02 August 2021 - 09:27 PM

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?

#64 Phineas_Carmichael

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Posted 08 August 2021 - 04:28 AM

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.

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#65 YoshiTrainer

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Posted 08 August 2021 - 11:34 AM

Thank you Phineas, glad you had a nice getaway!

#66 YoshiTrainer

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Posted 25 August 2021 - 01:56 PM

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
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#67 YoshiTrainer

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Posted 26 January 2022 - 06:50 PM

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?

#68 Phineas_Carmichael

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Posted 27 January 2022 - 06:05 PM

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.

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#69 YoshiTrainer

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Posted 27 January 2022 - 07:58 PM

Thank you sir!




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