TEK Ethyl acetate approach [CIELO]

[Cheelin]

BTW, did Shroombee’s dry-mix-then-water paste this afternoon, already clearing and showing snowflakes.

Separate 15g powder runs of materials A, B, C (same material as previous 12 runs, those runs used 25g of each material)

Each run using:
3.75g pickling lime
45mL distilled water
6 pulls with EA vol: 30mL, then 5x22mL
0.7g citric acid

Same prep as described earlier for Standard Method, except mix powder & lime before adding water. Both methods use passive salting.

Results:
A = 1.2% (Filtrate 0.166g, Water Wash 0.009g)
B = 0.9% (Filtrate 0.131g, Water Wash 0.009g)
C = 1.4% (Filtrate 0.187g, Water Wash 0.017g)

Difference between dry mix vs wet mix is primarily due to Jar Water Wash residue yields.

My conclusion:
If you are getting brown, sticky crap from your water wash, try this approach to see if it eliminates the crap.

 

[Loveall]

BTW, did Shroombee’s dry-mix-then-water paste this afternoon, already clearing and showing snowflakes.

Separate 15g powder runs of materials A, B, C

Each run using:
3.75g pickling lime
45mL distilled water
6 pulls with EA vol: 30mL, then 5x22mL
0.7g citric acid

Same prep as described earlier for Standard Method, w passive salting.

Results here, later.

Cool, what is the "dry-mix-then-water paste"? It's heavenly to see Crystals In EA.

 

[Cheelin]

Lol, instead of mixing the water and lime, and then adding the cactus powder; you mix the cactus powder and lime, then add the water.

I love seeing those little snowflakes floating in there.

 

[Loveall]

Lol, instead of mixing the water and lime, and then adding the cactus powder; you mix the cactus powder and lime, then add the water.

I love seeing those little snowflakes floating in there.

Gotcha. Are you noticing any difference with the change in order when making the paste?

 

[Cheelin]

So far, after 12+ hrs, compared to doing other way, I can’t tell much difference. Solvent is moderately green & transparent, needles on the walls, layer of snowflakes on bottom.

The idea behind this approach, is perhaps better mixing/particle contact between lime and cactus powder. Since I now, apparently, have nailed the tek, I wouldn’t expect to see much difference in my results (except perhaps in yield), but for someone getting low proportion of crystals in their filter and/or brown, sticky product in evaporated water wash, this may help.

We’ll see how filter and water wash/evap products compare to the std process in my earlier 12-run experiment. I’ll filter Saturday night, have wash water residue a few days later.



Getting excited to do my version of Shroombee’s quick crystallization method, still noodling on my approach, and need to find a chunk of time.

The standard process is taking me about 50 minutes per run, start to citric acid dump, then passive crystallization time, which i’m running 56 hours just to get max crystallization, but at some point around 24hrs is probably point of diminishing returns (but not always).

It would be nice to get a complete run done in less than 60 minutes, but before i nailed the tek, i was not getting many crystals in my filter this way. And for me, the goal is to maximize yield & purity in the filter, minimize recrystallization residue.

 

[Loveall]

60 minutes with the excess citric and shaking for quick xtalization is definitely possible. I did it live a couple months ago in the nexus chat, uploading pictures during the process. Since EA evaps fast (folded the filter with the xtals and shook it in the air for super fast evap), had dry white xtals ready to go consume in less time that it takes to make a simple tea

I wonder if less water initially would make the TEK more robust. Idea would be to start with cactus/lime add water with stirring until you get a fluffy paste. Forcing a fixed amount of water may not be ideal for every starting plant powder. Seems like it could be too wet for HLP, for example.

HLP, if you see better results with less water in the paste you may have found a robustness knob I was not aware of.

 

[Cheelin]

Good idea, Loveall.

 

[highlightprotein]

then passive crystallization time, which i’m running 56 hours just to get max crystallization, but at some point around 24hrs is probably point of diminishing returns (but not always).

I just noticed a strange result with slow crystalization: I'm seeing crystals form AFTER the 24 hours.

My last two extractions have used slow crystalization with 5mg citric acid per gram of EA. Exactly 24 hours after dropping the acid I filtered the EA into another jar and stored the used EA. However this morning I took a look at both jars and noticed that they both still have crystals. Beautiful white needle crystals. It looks like quite a lot. The microwaved/slow crystalization appears to have less crystals than the non-microwaved/slow crystalization but I am not sure.

The first extraction I did with fast crystalization did not do this.

Has anyone else noticed this? Not sure if I am doing something wrong or if this is normal. But I'm glad I didn't neutralize the used EA immediately after or I would have missed this. If it is normal perhaps the tek should be updated to wait longer than 24 hours?

HLP, if you see better results with less water in the paste you may have found a robustness knob I was not aware of.

I'll try it. For now I'll stick with the "standard" process a few more times, just because I worry that due to my inexperience I may simply be making some mistakes somewhere.

 

[Cheelin]

HLP, you’re cool, dude.

As i’ve mentioned, there is variability in how quickly crystallization completes. I don’t know the reason, for it. My recco, let the crystallization continue for 48-72 hours; if you’re in a rush, filter after 24hrs, re-cap jar and let it crystallize some more (then filter & re-cap), until no more crystals form; then de-acidify solvent for future use.

 

[highlightprotein]

Sounds good. Loveall, would you consider updating the tek with that suggestion?

For my non-microwaved extraction, I recovered 115mg now after waiting ~36 hours (I am expecting only 150mg based on past yields with this material, so this is quite a lot to materialize after the 24 hour mark). It contained beautiful needle white crystals.

For my microwaved extraction, at the 24 hour mark I recovered needle white crystals. But now, after ~56 hours I recovered some more I have not weighed yet; it is white, but it doesn't look like needle crystals. Rather it looks kind of chalky. I assume this is mescaline. Would anyone be able to guess why it looks like chalk instead of needle? The

 

[Cheelin]

Chemists, re: brown, sticky residue

Crystals captured in the filter, and well-washed with fresh EA, are unlikely to have much, if any, contamination (hence my obsession with collecting them in the filter rather than the residue). For me, the water washed evaporate is another matter.

One component of the brown, sticky residue that earlier ended up in my evaporate has an acidic “taste”, presumably Citric that was undissolved or “loosely bound” to other molecules. If citric acid is part of the residue, could lime also be in there? Could these be contributing to the brown, sticky?

I’ve done some fresh EA washes, dried the filtrate, and then warm water washed the filter & filtrate, finding in some cases small chalklike white chunks that don’t stain orange/red in marquis.

 

[Loveall]

Sounds good. Loveall, would you consider updating the tek with that suggestion?

For my non-microwaved extraction, I recovered 115mg now after waiting ~36 hours (I am expecting only 150mg based on past yields with this material, so this is quite a lot to materialize after the 24 hour mark). It contained beautiful needle white crystals.

For my microwaved extraction, at the 24 hour mark I recovered needle white crystals. But now, after ~56 hours I recovered some more I have not weighed yet; it is white, but it doesn't look like needle crystals. Rather it looks kind of chalky. I assume this is mescaline. Would anyone be able to guess why it looks like chalk instead of needle? The

TEK updated for 72 hours of crystalization :thumb_up:

There are lots of things that affect xtalization which we don't control, so differences are expected.

Congrats on the needles.

 

[Loveall]

Chemists, re: brown, sticky residue

Crystals captured in the filter, and well-washed with fresh EA, are unlikely to have much, if any, contamination (hence my obsession with collecting them in the filter rather than the residue). For me, the water washed evaporate is another matter.

One component of the brown, sticky residue that earlier ended up in my evaporate has an acidic “taste”, presumably Citric that was undissolved or “loosely bound” to other molecules. If citric acid is part of the residue, could lime also be in there? Could these be contributing to the brown, sticky?

I’ve done some fresh EA washes, dried the filtrate, and then warm water washed the filter & filtrate, finding in some cases small chalklike white chunks that don’t stain orange/red in marquis.

Lime and lime salts should not be present in EA, they should be insoluble - even for water saturated EA. I did a test pulling plain lime with used EA and salting with citric, nothing precipitated. There is a lot of plant stuff (other alkaloids, small proteins, etc) that can make it into EA, especially if it has a lot of water or if water is squeezed into the extract. However, the lime should take care of the proteins and give them a + charge so they don't go into EA (assuming the paste is mixed well to get to all the protein). If the unwanted plant stuff that makes it into the EA is sensitive to pH it can precipate, more so for the lower pH. The potential for getting this unwanted stuff in EA may go up a lot with water content. I'm just guessing though on this part.

 

[highlightprotein]

I've just concluded a little experiment, three extractions on the same San Pedro powder, and I seem to have a similar result to Cheelin: non-microwaved 69ron paste had significantly higher yield. In addition, the non-micorwaved contained 0 yellow coloring in my evporated material.

However I am a noob, these are my first extractions, so it is likely I am not controlling all my variables particularly well. So please take this with a grain of salt. I'm getting some more cactus soon and will retry the experiment.

Extraction #1: Microwaved, Chilled EA with 1 minute pulls, fast crystallization 15mg/g: 0.180g mesc citr / 39g cactus powder == 0.46% yield

Extraction #2: Microwaved, Chilled EA with 3 minute pulls, slow crystallization 5mg/g: 0.244g mesc citr / 40.5g cactus powder == 0.60% yield

Extraction #3: NOT microwaved, Chilled EA with 3 minute pulls, slow crystallization 5mg/g: 0.361g mesc citr / 40.5g cactus powder == 0.89% yield

So I got a pretty significant boost in yield with not microwaving, about double in my case.

In addition, the non-microwaved experiment CONTAINED 0 YELLOW COLORING. I was very happy about this. For #1 and #2, I only get the white crystals in my filter; the evaporated stuff always contains some kind of yellow coloring and was kind of stickyish. But for #3, both the filter and the evaporated stuff had no yellow coloring. This was really cool.

 

[highlightprotein]

HLP,

We all have our own level of risk tolerance. I definitely would not regularly use a plastic that dissolves in a solvent I’m using to produce a consumable product. Plastics are made from hydrocarbons, typically petroleum-based ones. Not the best for a human body.

The hydrocarbons in the plastic are (in this instance) practically inert. The problem here is the plasticizers that are used to keep the plastic film flexible. Those are what are dissolving in the EA, and many of them have hormone-disrupting properties. A further undesirable complication is that once the surface of the plastic has been leached of plasticiser it becomes brittle and starts shedding microplastic fragments, so the rinsing method will just lead to a different type of problem.

Too bad lol, I had about a half quart of EA I cleaned using this method. I think I'll toss it now and buy a sep funnel.

 

[Cheelin]

Ok Loveall, just concerned that there may be non-cactus residues left in the crystallization jar after the EA that remains in the jar volatilizes.

 

[Cheelin]

Cool HLP! White crystals in the filter are a great thing.

Your low yields seem to indicate a low alk material. Your uncolored evaporate seems to indicate improved processing technique.

Keep up the good work.

As for differences in the process variations, time will tell if the results are real, given that Loveall and Shroombee, maybe others, haven’t noticed these yield diffs. My bottomline, though, is that extra work should be justified by extra end value; which i haven’t yet seen from the variations beyond the std process - in anyone’s results.

 

[Loveall]

About the 60 minute process, I also squeezed the folded filter with paper towels to remove EA before air shaking it.

 

[Cheelin]

Loveall, not sure if your post 560 is in response to my 558.

558 is in reference to the following:

After the crystals have formed, the contents of the crystallization jar are emptied into a filter to drain the EA and wash the filtrate with fresh EA. However, crystals adhered to the walls and bottom of jar, as well as loose crystals that are difficult to drain into the filter, remain in the jar, along with some amount of EA.

After the jar dries (EA volatilizes), whatever was in solution (cactus and non-cactus solids) remains in the jar, only to be water washed into evap dish with crystals. The non-cactus residues are what i’m talking about. I would put money on there being citric in this, I’m thinking there may be lime, too.

For me, not a big deal since i’m only getting about 15% of total yield from residue. Since I’m only doing extraction for my infrequent personal use; worst case, I can just dump the residue (though I’ll play around with trying to purify this for grins). May be diff situation for others, especially if much of their yield is brown and sticky.

Just trying to provide complete info, may not really matter to some/most people.

 

[Loveall]

Loveall, not sure if your post 560 is in response to my 558.

558 is in reference to the following:

After the crystals have formed, the contents of the crystallization jar are emptied into a filter to drain the EA and wash the filtrate with fresh EA. However, crystals adhered to the walls and bottom of jar, as well as loose crystals that are difficult to drain into the filter, remain in the jar, along with some amount of EA.

After the jar dries (EA volatilizes), whatever was in solution (cactus and non-cactus solids) remains in the jar, only to be water washed into evap dish with crystals. The non-cactus residues are what i’m talking about. I would put money on there being citric in this, I’m thinking there may be lime, too.

For me, not a big deal since i’m only getting about 15% of total yield from residue. Since I’m only doing extraction for my infrequent personal use; worst case, I can just dump the residue (though I’ll play around with trying to purify this for grins). May be diff situation for others, especially if much of their yield is brown and sticky.

Just trying to provide complete info, may not really matter to some/most people.

No, post 560 was about how to dry the bulk crystals in the filter by squeezing them (and the filter) in a paper towel.

I don't understand the concern when finally evaporating the EA in the jar. After 3-4 rinses of the jar with fresh EA, no noticable plant matter or citric acid should be left: almost all of it should have been rinsed out. Or am I miss understanding? FYI, I send these rinses through the filter to push away any off-colors of the bulk product there.