Some Q's about ethyl acetate approach.

[Loveall]

Chilling the spent extract.

I tried to check the solubility of citric acid in room temp EA. Saturated soln allowed to sit with excess citric acid in EA for ten days.

20 ml evaporated from a glass dish and resulted in 280 mg recovery.

14 mg per gram?

How can I be so far off?

IDK, but that's a good way to measure it. I can try to measure it too.

I think you meant 14mg/ml

Can you shake it every once in a while and measure again in a few days?

 

[Gibson]

Chilling the spent extract.

I tried to check the solubility of citric acid in room temp EA. Saturated soln allowed to sit with excess citric acid in EA for ten days.

20 ml evaporated from a glass dish and resulted in 280 mg recovery.

14 mg per gram?

How can I be so far off?

IDK, but that's a good way to measure it. I can try to measure it too.

I think you meant 14mg/ml

Can you shake it every once in a while and measure again in a few days?

Right, I meant per ml. I'll check it again.

 

[vixintrex]

NaCl was abandoned because it did not add anything to the extraction. ...

Thanks!


If you are not getting xtals right away, one possibility is that your cactus has low mescaline %, do you have any idea of how potent it is?

No, it was the lower 22" of a Pach, maybe Ikaro x Malo4. No crystals on my first run, or on my second run of 35 grams either. I really tried to follow the Tek even closer this time and still no crystals.

This is the tip section from the cactus I made the powder.

On my first run I used almost twice as much EA as I should have, effed up the measurements.
(I was planning to pour the correct amount of EA into the first pull, but I was adding it from the bottle to my powder container which was sitting on my gram scale, and it reacted slower than I was pouring so I got like an extra 12 grams, then about that same extra for all the pulls.)

On my second run, all the measurements were spot on to the gram anyway.

Except for this: I deviated from the Tek by trying to dissolve my Citric Acid beforehand. Using 2.5 gm of citric acid, which I had ground fine with a mortar, and let sit in 40 ml EA to see if it would dissolve for about three days before it was added to the extract. It never did fully dissolve till after I added it to the rest of the EA. So I did have about 40 ml excess EA in my second run from that.

And I used 2.5 gm for 35 grams powder, which is more than the low amount the Tek calls for but less than high amount for fast crystallization.

I checked the pH after 72 hours of attempted crystallization at room temperature and my indicator strips showed mildly acidic.

I checked the pH of the leftover soln from the first run that I saved, and it was also mildly acidic, I also used a little excess citric acid on the first run.

"On my first run I used almost twice as much EA as I should have, effed up the measurements."

ok there it is

 

[vixintrex]

"On my first run I used almost twice as much EA as I should have, effed up the measurements."

solubility is a thing. I think this tek relies on solubility

so your only course of action now is to take that first extract and evaporate it down to like a quarter of what it was

you can do this naturally by like idk opening it up and letting it go or violently by boiling it off outdoors or something but if you want your stuff you need to reduce the volume of your solute by a lot. if you've combined solvents then you're in more trouble. but your next course of action should be to reduce your solvent by a lot

 

[Gibson]

"On my first run I used almost twice as much EA as I should have, effed up the measurements."

solubility is a thing. I think this tek relies on solubility

Yeah, had to tighten up a lot of things. I had three runs with nothing to speak of in return, but I just recovered 80mg of product from 26.4 gm powder, from the bottle wash evaporate on run four, but recovered zero crystals in the filter paper... ?

After pouring the crystallized, salted extract into the filter collection funnel I washed the crystallization jar with 10ml water twice and evaporated it on a plate. A couple hours in the oven at 110 f left it hard, shiny and dry. Scraped up easily. A small pinhead tasted quite bitter.

The collection filter was a double coffee filter. Once dry it was examined and rubbed, no crystals were found.

So 0.3% on the fourth run! : )

 

[Loveall]

Do you know if 0.3% is normal/expected for your material.

Slightly above ~1% has been more common for cactus aged in the dark. But there is a range, Merkin got 3% on whole plants and I have seen as low as 0.8% depending on the source.

 

[Gibson]

Do you know if 0.3% is normal/expected for your material.

Slightly above ~1% has been more common for cactus aged in the dark. But there is a range, Merkin got 3% on whole plants and I have seen as low as 0.8% depending on the source.

No, I don't know, I think I should get more, because I didn't get any crystals.

I have one more run that I decanted from the fridge yesterday. I decanted from a flask and it was real easy to see a globule of water, looked like several ml. I left the water behand, filtered into a collection jar and salted with the 5 gram equivalent. It'll be ready to recover crystals in a couple days.

I recovered the jar washing from my third run which was 26.4 gm powder and was salted with 2.54 gm ea. (9.6gm/100gm equivalent) and recovered 1.07gm of this brown residue. It is somewhat bitter but also sour.

It's photographed last compared with the crystals from the fourth run which are more bitter and not sour.

(I believe the brown gunk recovered is mostly Citric Acid crystals. The citric acid seems to make more cubic crystals. I threw it away.)




I think my current run, crystallizing now, should have the best recovery, with the best filtration, best paste prep, and best water separation. It's also the darkest green one so far with the most volume. (It wasn't the most volume. My first attempt was really dilute. This was the most concentrated)

I went with the lower end of the citric acid on this run, which is currently crystallizing, so I hope to avoid more citric acid in the residue like in this run, (#3) pictured below.

 

[Loveall]

Thanks for the updates. Looking forward to the results fron the 4th run.

 

[Gibson]

Thanks for the updates. Looking forward to the results fron the 4th run.

Welcome!

I reran the citric acid solubility. This time a saturated soln in room temp EA was prepared and allowed to sit for two weeks with occasional shaking. (Same soln as last time, just aged more)

30 ml was placed on a plate and evaporated in the sun till dry, then in the oven at 110f for five hours.

Recovery was 420 mg.

The upper limit of citric acid in room temp EA is around 14-15mg/ml?

 

[Loveall]

Thanks for the updates. Looking forward to the results fron the 4th run.

Welcome!

I reran the citric acid solubility. This time a saturated soln in room temp EA was prepared and allowed to sit for two weeks with occasional shaking. (Same soln as last time, just aged more)

30 ml was placed on a plate and evaporated in the sun till dry, then in the oven at 110f for five hours.

Recovery was 420 mg.

The upper limit of citric acid in room temp EA is around 14-15mg/ml?

That is very interesting. I wonder why it is different than what we expect. I can't find the refernce for 50mg/ml at the moment.

Do you know if your citric acid is monohydrate or anhydrous?

 

[Gibson]

It's Milliard Citric acid, supposed to be anhydrous.

 

[Loveall]

It's Milliard Citric acid, supposed to be anhydrous.

Ok, I'll try to repeat your result. I'll also wet some fresh EA (~3%), put that in fridge, decant of dropplets and check the solubility in that mildly wet EA. This last test would closer simulate the citric acid solubility in the EA we get from our pulls.

 

[shroombee]

That is very interesting. I wonder why it is different than what we expect. I can't find the refernce for 50mg/ml at the moment.

Here is a reference for solubility of citric acid in ethyl acetate: Pub Chem - Citric Acid

"Solubility in g/100 g saturated solution: ether 2.17; chloroform 0.007; amyl alcohol 15.43; amyl acetate 5.98; ethyl acetate 5.28. Solubility at 19 °C in g/100 g solvent: methanol 197; propanol 62.8. /Citric acid monohydrate/"

5.28 grams / 100 grams of ethyl acetate = 52.8 mg / gram of EA.

The note at the end says "citric acid monohydrate". Perhaps anhydrous citric acid is less soluble? And maybe it converts to monohydrate due to the water in the extract?

 

[Loveall]

That is very interesting. I wonder why it is different than what we expect. I can't find the refernce for 50mg/ml at the moment.

Here is a reference for solubility of citric acid in ethyl acetate: Pub Chem - Citric Acid

"Solubility in g/100 g saturated solution: ether 2.17; chloroform 0.007; amyl alcohol 15.43; amyl acetate 5.98; ethyl acetate 5.28. Solubility at 19 °C in g/100 g solvent: methanol 197; propanol 62.8. /Citric acid monohydrate/"

5.28 grams / 100 grams of ethyl acetate = 52.8 mg / gram of EA.

The note at the end says "citric acid monohydrate". Perhaps anhydrous citric acid is less soluble? And maybe it converts to monohydrate due to the water in the extract?

Thank you so much for finding that shroombee, I'll add it as a reference to the TEK.

Yes, a tiny bit of water could definetly matter a lot. I think you found early on how different the solubility of citric acid was depending on water in EA. That was during our original early work on the TEK.

 

[Loveall]

That is very interesting. I wonder why it is different than what we expect. I can't find the refernce for 50mg/ml at the moment.

Here is a reference for solubility of citric acid in ethyl acetate: Pub Chem - Citric Acid

"Solubility in g/100 g saturated solution: ether 2.17; chloroform 0.007; amyl alcohol 15.43; amyl acetate 5.98; ethyl acetate 5.28. Solubility at 19 °C in g/100 g solvent: methanol 197; propanol 62.8. /Citric acid monohydrate/"

5.28 grams / 100 grams of ethyl acetate = 52.8 mg / gram of EA.

The note at the end says "citric acid monohydrate". Perhaps anhydrous citric acid is less soluble? And maybe it converts to monohydrate due to the water in the extract?

Thank you so much for finding that shroombee, I'll add it as a reference to the TEK.

Yes, a tiny bit of water could definetly matter a lot. I think you found early on how different the solubility of citric acid was depending on water in EA. That was during our original early work on the TEK.

Updated TEK info:

Q: What is the upper limit of citric acid that can be added to the extract?

A: The solubility of citric acid monohydrate in ethyl acetate is over 50 mg per gram of ethyl acetate[23]. Note that plant matter or other unwanted extraction products (such as water) may affect the solubility. Stay well under 50 mg/gram limit and do not chemichally dry the extract to ensure no undissolved citric acid is mixed in with the mescaline citrate. Under mostly anhydrous conditions the solubility of anhydrous citric acid in ethyl acetate has been measured as low as 10mg/g [24].

Thanks Gibson/shroombee for helping the TEK info be more precise. I think this resolves the solubility of citric question (at least for me).

Gibson, how is your 4th attempt looking? Any xtals? Thanks.

 

[Gibson]

Kind of hard to tell, it's pretty dark. (fifth, I got jar washing crystals from the fourth)

 

[Gibson]

Got some crystals and a lot of crust. I think they're sucking through the filter where the funnel holes are.

I only used a single coffee filter this time. I used a double last time. Maybe I didn't look close enough last time, because the filters looked the same after filtering. Before washing.

Last time I washed the coffee filter with 5ml EA x2. After the wash I didn't see any crystals so I threw the filter away.

Both times there were a few sparkles on the surface of the filter before the wash, and the second one didn't get washed.

Looks like crystals.

But I wasn't able to collect any crystals from the filter, even after drying well, nothing could be removed from the filter. It was bitter, so I washed it with 5ml x2 and added it to the collection jar wash to evaporate.



Thanks for the numbers Shroombee. I'm searching for the solubility of Mesc citrate in water and EA.

Why are my crystals so fine? Or non-existent? I used the low citric acid amount for slow crystallization.

I stirred for 5-10 seconds after adding the citric acid to the extract, and moved the jar a few times over three days. Is that enough to prevent large crystals?

 

[Loveall]

It seems like your yields are low Gibson. Any yield measurement yet?

What do you know about the expected alkaloid content of your plant material?

 

[Gibson]

It seems like your yields are low Gibson. Any yield measurement yet?

What do you know about the expected alkaloid content of your plant material?

.14 gm from 38.8 gm powder, all recovered as crystal jar residue wash. No crystals recovered from the filter, maybe I'm just seeing fluffy white filter paper and not actual fine crystals in the photos?


This comes to 0.36%, maybe it's weak powder. It was supposed to be active tea, but not the best or anything, some people thought it was great, but no actual measurements available.

 

[Gibson]

It seems like your yields are low Gibson. Any yield measurement yet?

What do you know about the expected alkaloid content of your plant material?

I did another run and got free crystals this time. There wasn't much bottle wash apparent this time, so I didn't process that yet. I may just keep my crystallization flask with what little it has on the walls for my next run and collect the precipitate on the walls after that.

I got 269 mg mescaline citrate from 47 grams powder. (0.57%) This powder may be weak, I have some TBMs that may be ready to test in a few months. They're doubling about every three months.

I started with 35 grams powder / 8.75gm lime and used the TEK amount of water for that (95ml), but the paste was too runny, so I added another 4gm powder/1gm lime to the mix over about 10 minutes Three times. (total extra 12gm powder/ 3gm lime.)

This is the same final ratio of paste water to powder as using 202ml water for 100gm powder, instead of the 270ml the TEK calls for.

I had previously experienced emulsification on the 5th or 6th EA pull, this time the paste remained workable and drained well, with the consistency of apple sauce at the end of the 6th pull.

I have about 50gm of this powder left, and since it seems to have a high moisture content, based on the required amount of paste water, I'll dry it for an hour in the oven before processing and see if the weight changes. It doesn't appear moist or anything, it's a fine dry powder.

This was my sixth run, and it's encouraging to get some crystals in the coffee filter.

Why do we use two filter during crystal recovery? All the crystals seemed to be caught by the first filter.

The last pic is my TBMs, not what I used for this powder.