Some Q's about ethyl acetate approach.

[Loveall]

I just recently saw this and feel it's relevant here...

https://www.reddit.com/r/sanpedrocactus/comments/w24r7r/sasha_shulgin_discussing_a_cacti_that_contains_no

Hopefully the link works, I'm still trying to figure out upload stuff for this site.

Yeah, that is super interesting research on a different species.I believe the full talk is somewhere (psychedelic salon) but cant find it at the moment.

 

[downwardsfromzero]

I just recently saw this and feel it's relevant here...

https://teddit.net/r/sanpedrocactus..._shulgin_discussing_a_cacti_that_contains_no/

Hopefully the link works, I'm still trying to figure out upload stuff for this site.

Yeah, that is super interesting research on a different species.I believe the full talk is somewhere (psychedelic salon) but cant find it at the moment.

Here's a link from the comments:
[youtube]

Hope it's the right one!

 

[Loveall]

Thaks DWFZ, I enjoyed it. I guess reddit comments can be useful

 

[Gibson]

Thanks for the Shulgin link!

I got some powder and am trying to crystallize. Been 24 hours don't see any.

I followed Cheelin's closely. Used my milligram scale this time.

I did a 20gm powder run. These amounts:

20 gm powder
5 gm lime
60 mL water
189.2 mL EA

#1 47.3 mL
#2-6 28.38 mL (2 Tablespoons)

1g Citric Acid

During the first five pulls the paste was sort of a porous pudding that solvent leaked out of like a sponge, during the start of mixing the last pull the paste congealed. That last pull is pictured in the last photo, it didn't always look like that.

pH before citric acid was basic 8-9

I ground my citric acid pretty fine with a mortar and measured out 1.005 gm and added after about an a couple hours in the fridge last night. There were no visible particles or water drops.

pH after citric acid last night and now is 5-6.

 

[merkin]

I ground my citric acid pretty fine with a mortar and measured out 1.005 gm and added after about an a couple hours in the fridge last night. There were no visible particles or water drops.

Did you decant thru filter again after settling in fridge? I would leave it longer in the fridge like at least around 12 hours. I can never see anything in the beaker at that stage (green EA is too dark/dense), but on decanting the water is visible on the bottom and sides of the glass and the liquid seems clearer but its not transparent. I think the 'clarity' of the EA is very important for crystals.

Did it cloud when you added the citric? I usually see crystal within 20-30 minutes of adding citric (and getting immediate clouding).

 

[Gibson]

I ground my citric acid pretty fine with a mortar and measured out 1.005 gm and added after about an a couple hours in the fridge last night. There were no visible particles or water drops.

Did you decant thru filter again after settling in fridge? I would leave it longer in the fridge like at least around 12 hours. I can never see anything in the beaker at that stage (green EA is too dark/dense), but on decanting the water is visible on the bottom and sides of the glass and the liquid seems clearer but its not transparent. I think the 'clarity' of the EA is very important for crystals.

Did it cloud when you added the citric? I usually see crystal within 20-30 minutes of adding citric (and getting immediate clouding).

No I didn't decant. Didn't see anything to decant.

No, I didn't see any clouding.

Feel like I screwed up, probably too much water dissolved in there. Any way to dry it at this point and recover crystals?

I got a separatory funnel on my shopping list.

Now I'm past 72 hours, no crystals. Not sure what to do with this green liquid.

I'll try again with the sep funnel next week. I ordered some beakers, graduates, and droppers to make it easier. and some anhydrous potassium carbonate and mag sulfate that might help.

 

[Gibson]

I did another run, tried to do my best. Measured really exactly, everything to the ml or gram.

Did the pulls last night, and let it cool and settle in the fridge overnight.

First picture, kinda reddish is with flash, second without.

I don't see any water layer or particles. Maybe there's a little swirl of water right in the tip?

Wish me luck. I'll let it settle more today.

 

[Gibson]

 

[Loveall]

Looks good. Remove the possible water and transfer the rest to room temp. It should become nice and clear.

Do you have pH paper? You can test for potential mescaline, paper should turn alkaline. If it doesn't your material may not be active (?).

Then salt with excess citric. You can try ~10g per liter of EA, abouy double what the TEK says. Swirl for a few minutes to dissolve the citric acid. You should see clouds. Rest and after anfew hours you should see the first xtals.

 

[Gibson]

Looks good. Remove the possible water and transfer the rest to room temp. It should become nice and clear.

Do you have pH paper? You can test for potential mescaline, paper should turn alkaline. If it doesn't your material may not be active (?).

Then salt with excess citric. You can try ~10g per liter of EA, abouy double what the TEK says. Swirl for a few minutes to dissolve the citric acid. You should see clouds. Rest and after anfew hours you should see the first xtals.

Hi Loveall, I'm doing my second attempt with the sep funnel. I found water droplets adhering to the wall, and I'm learning how to use it.

Did you find a benefit to drying the extract before salting with Sodium Carbonate?

What does it mean when the paste coagulates on the fifth or sixth pull? Is that too much water in the paste?

The best I've gotten is a little brown stuff on my filter paper, but there was a sort of a goo on the walls of my crystallization jar. I'm drying that filter paper, but I don't expect much.

I have my best attempt cooling in the funnel now. I realize I have to decant it to leave the droplets behind on the wall.

And I wonder if I should dry it with some Sodium Carbonate, then filter that out before salting. What ratio amount of Sodum Carbonate should I use?

Sorry for the questions, I'm still reading a lot of the ethyl acetate approach thread and there's a lot of details.

 

[Loveall]

Looks good. Remove the possible water and transfer the rest to room temp. It should become nice and clear.

Do you have pH paper? You can test for potential mescaline, paper should turn alkaline. If it doesn't your material may not be active (?).

Then salt with excess citric. You can try ~10g per liter of EA, abouy double what the TEK says. Swirl for a few minutes to dissolve the citric acid. You should see clouds. Rest and after anfew hours you should see the first xtals.

Hi Loveall, I'm doing my second attempt with the sep funnel. I found water droplets adhering to the wall, and I'm learning how to use it.

Did you find a benefit to drying the extract before salting with Sodium Carbonate?

What does it mean when the paste coagulates on the fifth or sixth pull? Is that too much water in the paste?

The best I've gotten is a little brown stuff on my filter paper, but there was a sort of a goo on the walls of my crystallization jar. I'm drying that filter paper, but I don't expect much.

I have my best attempt cooling in the funnel now. I realize I have to decant it to leave the droplets behind on the wall.

And I wonder if I should dry it with some Sodium Carbonate, then filter that out before salting. What ratio amount of Sodum Carbonate should I use?

Sorry for the questions, I'm still reading a lot of the ethyl acetate approach thread and there's a lot of details.

No benfit to a chem dry, but I wasn't getting goo either. If you have goo it may help. When dried thoroughly citric acid took a long time to dissolve in the salting step, so a little water is OK and may help move things along.

You defienetly want to decant. Separatory funnel is not a standard part of the TEK until you wash the used solvent.

Are you extracting in a warm environment (e.g. summer garage)? You want to extract at room temperature.

The paste goes from loose and sandy to a big blog over time when extracting. The singñe blob is described as coagulated paste. Yes, the blob could happens faster with more water as I have observed, but also if the pulls are warmer pulls.

 

[Gibson]

Yeah, I got confused by the sep funnel. Been awhile since I did any chemistry.

I think it worked this time. I decanted and filtered, and added citric acid and got clouds and crystals right away. This is about an hour later. I did use 2.5 gm citric acid for 26 gm cactus powder which is almost the 10 gram per ratio. Hope I'm not just seeing undissolved citric acid?

Now I need to figure out how to collect the crystals.

Did you find benefit from the microwave paste technique?

How toxic is ethyl acetate? It seemed like it zonked me out doing the pulls.

Does a coffee filter catch even the fine crystals? And do they come out of the filter easy when they're dry?

I want to kick myself for starting with the live cactus first. At least I saved the tip and it's growing real well. And I definitely should have used some smaller batches at the beginning also.

 

[Loveall]

Yes that looks like what the product can look like. You have smaller xtals, almost a powder maybe because you used more citric acid than is needed. Not an issue at all, it is just faster xtalization and less fluffy xtals.

That is not undisolved citric. Notice it is not in granular form. All the citric dissolves up to 50mg/ml.

Ehtyl acetate is not considered that toxic. Children, women, and men with extra style, use it to remove fingernail paint. The body breaks down any small absorbed amounts into acetic acid and ethanol. It is still a solvent, so don't inhale the fumes direcly and work in a ventilated area.

It is very easy to recover the product and rinse in a filter. Follow the TEK instructions and enjoy. Cheers.

Want to ask again, did you extract in a warm place? I think warm EA absorbs a lot more water, making the fridge step important to avoid goo.

 

[Gibson]

Want to ask again, did you extract in a warm place? I think warm EA absorbs a lot more water, making the fridge step important to avoid goo.

Thanks, Extracts done with room temp EA and paste. About 71 F.

 

[Loveall]

OK. Also, rest the salted extract for 3 days before filtering. A few more xtals may form during the longer resting period.

 

[Gibson]

Thanks Loveall, yes I'm waiting before trying to recover crystals.

I have about 40 gm powder left. I might try it all in one batch of paste if I get a decent batch of crystals from this one.

Should I read up more on the microwave tek people were trying? Seems like they microwaved off about half the water from the paste before doing the pulls. (Read in the tek where it decreased yields, I'll skip it)

What should I evaporate on? Cheelin says K. A glass baking dish for evaporating jar wash

I have a glass dinner plate that might be big enough.

I'm going to try to recover some solvent I saved from the first runs where I didn't get any crystals. There may be some alkaloid still in it. I don't know.

Say there's some mescaline in there, and I suspect there was way too much water also. If I add Sodium Carbonate wash water to it, any mescaline should dissolve in the water, and the citrate should fall off the mescaline, but will the mescaline freebase react with the sodium carbonate any other way?

Could I just add Sodium Carbonate granules to the saved salted EA pull to neutralize it and put the mescaline free base into solution in the EA, then filter off the Sodium Carbonate? I read if you leave it too long it turns gooey from the water. Then could I use that EA for my next fresh paste pulls?

How to make the Sodium Carbonate wash?

Wash spent extract with ~10% sodium carbonate water solution. About 1/3 of the solvent volume is enough for neutralization.

Is that one part in 10 by weight? Like 90gm water + 10gm sodium carbonate?



Thanks for making the Tek, I appreciate you have the time to help this blockhead.

 

[Gibson]

I got this form, if the idea even works.

I made my last batch of paste with 38.8gm powder, and used the low end of the water the tek calls for. 105ml scaled for 100gm powder that's 270ml.

The paste looked great, and seemed to extract really well, I got a lot of dark Extract, but it still congealed while I was stirring for the final pull. Later than before, last time it congealed the beginning of the fifth stir.

When it congealed the solvent even got trapped behind it, it stopped draining like it was supposed to. I had to lift up the glob to let the last of the solvent drain.

 

[shroombee]

How toxic is ethyl acetate? It seemed like it zonked me out doing the pulls.

Among other things, ethyl acetate is used to decaffeinate coffee beans. It's generally safe. It zonks me out too if I breathe too much. But I seem to get used to it over time and can then work through it.

The fine crystals you're seeing at the bottom of your beaker are similar to what I get when doing fast crystallization (excess citric acid with a magnetic stirrer). Nice work!

 

[Loveall]

What should I evaporate on? Cheelin says K. A glass baking dish for evaporating jar wash

I have a glass dinner plate that might be big enough.

Any glass flat surface should be OK. Be careful when you scrape up the xtals so they don't fly away if using a plate.

I'm going to try to recover some solvent I saved from the first runs where I didn't get any crystals. There may be some alkaloid still in it. I don't know.

Did you see clouding that cleared? That would mean most of the mescaline precipitated as goo. I have never recovered any from spent solvent.

Say there's some mescaline in there, and I suspect there was way too much water also. If I add Sodium Carbonate wash water to it, any mescaline should dissolve in the water, and the citrate should fall off the mescaline, but will the mescaline freebase react with the sodium carbonate any other way?

You would have free base mescaline. Some in the water, some in the solvent (partitioned between the two layers). There would be virtually no sodium carbonate or sodium citrate in the solvent, that would all be in the water.

Could I just add Sodium Carbonate granules to the saved salted EA pull to neutralize it and put the mescaline free base into solution in the EA, then filter off the Sodium Carbonate? I read if you leave it too long it turns gooey from the water. Then could I use that EA for my next fresh paste pulls?

This is a tricky question. Yes the sodium carb would absorb water, but to fully react with the dissolved citric acid it is better to do an alkaline water wash like you mention below. If it did fully react without the extra water and if you did have mescaline somehow, then yes, you would end up with most of the mescaline in FB form in the EA. But that's a lot of ifs.

How to make the Sodium Carbonate wash?

Wash spent extract with ~10% sodium carbonate water solution. About 1/3 of the solvent volume is enough for neutralization.

Is that one part in 10 by weight? Like 90gm water + 10gm sodium carbonate?

Yes

One test you can do with the spent extract is put it in the fridge. See how much excess water is in it. If you get a watwr layer, any mescaline citrate will surely be in that water layer. Seeing how much water you get in the fridge from an extract that did not xtalize will also be an interesting observation in itself (please share). You can add thar water to the next extraction. Again, I don't think you have any left in the EA based on my tests, but I may have had less water than you.

Also, you are not a blockhead. We all had questions when we started. Its about learning, sharing, and expanding together

 

[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?