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Ethyl acetate approach [CIELO] Options
 
Cheelin
#661 Posted : 12/20/2021 6:02:14 PM

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Thanks Loveall.

I’ll do a side-by-side of std vs boiling water in near future.

Also will tinker with the Plan B approach.

HLP, when you have results and time, please post your method and comments.

Expecting to post results table tomorrow for 24-run experiment, in original post #568.
 

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shroombee
#662 Posted : 12/20/2021 8:05:25 PM

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Loveall wrote:
Also, we have people reporting crystals for paste with densities anywhere from 48 to 60g per 1/4 cup, so my theory on paste consistency being a factor seems bunk.

We would need the density of paste that results in goo to know for sure whether density is a non-factor.

BTW, I wish I could play along, but I don't have my materials so not able to do any extractions right now. I'm actively following this thread though.
 
Cheelin
#663 Posted : 12/20/2021 8:26:56 PM

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Is anyone actually getting crappy product for reasons other than learning curve? I’m all for fixing obvious problems, and making the tek as robust as possible, but, other than learning curve, what exactly is the problem?

No disrespect intended, but, so far, based on my numerous, consecutive results, the standard tek has held up, in terms of yield and apparent quality, as good or better than all the variations and deadend “fixes”.

I do believe that issues may arise from how the powder is produced (particle size, uniformity, moisture content, plant tissue composition, etc.). But, I would try to fix the root cause of these, rather than futz with the actual extraction tek.

For now, I’ll be focused on cleaning the stuff generated by poor technique/learning curve, and on solvent re-use.

When I have enough of my own material, I’ll develop a powder prep tek for it that matches my current starting material.

Imo, we have a great standard tek! If we have a good cleanup method for problem runs, and can rehab and extend solvent life, seems to me we’ll have a simple, complete, effective, and high-purity mescaline citrate extraction method.


But, if someone thinks these other efforts are really worthwhile, why not try to re-create the problem that is of concern. This would be my initial approach to solving it.
 
Loveall
#664 Posted : 12/21/2021 9:55:06 AM

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shroombee wrote:
Loveall wrote:
Also, we have people reporting crystals for paste with densities anywhere from 48 to 60g per 1/4 cup, so my theory on paste consistency being a factor seems bunk.

We would need the density of paste that results in goo to know for sure whether density is a non-factor.

BTW, I wish I could play along, but I don't have my materials so not able to do any extractions right now. I'm actively following this thread though.


I agree that we wound need to know the density of paste that resulted in goo to know for sure, it just seems unlikely since the large range 48 to 60g per 1/4 cup was OK.

Shroombee, what is your opinion on what causes goo for some? As an early pioneer you saw different results, interested in your current perspective. Is it paste MC%? Adherence to proper technique? Starting material?

Reading back through the thread, not fully dried and not fully ground cactus could cause goo. Maybe the cactus powder needs to be very dry and very fine for the TEK to work, otherwise there could be too much "free" water. Maybe a finer powder can grab onto water more efficiently than one with larger particles. Maybe the amount of surface-water contact matters along with MC%. Also, as has been mentioned before, fully drying cactus material changes the solubility of some components (e.g. by denaturing proteins).

Or it could just be not adhering to the TEK steps. Or both could contribute. Or could be other reasons of course.
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Cheelin
#665 Posted : 12/21/2021 1:56:09 PM

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HLP, aside from your currently poor yields which sound like they are due to low alk material, how would you evaluate your recent results, how they have changed over time, and why do you think they have changed?

Anyone else who has had yield or quality issues with product produced using this tek, please chime in, too.




Results posted for 24-run experiment, see post #568
 
shroombee
#666 Posted : 12/22/2021 6:54:52 AM

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Loveall wrote:
Shroombee, what is your opinion on what causes goo for some? As an early pioneer you saw different results, interested in your current perspective. Is it paste MC%? Adherence to proper technique? Starting material?

I don't have a guess. But your question inspired a thought... now that a group of us can consistently create xtals, how about we intentionally try to create goo by deviating one variable at a time from a known good process that yields xtals?
 
Cheelin
#667 Posted : 12/22/2021 12:04:23 PM

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Xactly
 
Loveall
#668 Posted : 12/22/2021 12:35:08 PM

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Cheelin wrote:
Results posted for 24-run experiment, see post #568


Wow, what a tremendous amount of quality work 🙏
Essentially, the chilled approach and microwave approach lowered yields (repeating your previous result). Salting method had no major impact (new result). What about xtal size, any comments/observations there?

The microwave option has been removed from the TEK, perhaps we should also remove the chilled paste option too?

9% MC on your cactus powder is interesting, definitely want to measure mine now. Perhaps we should control this variable, what if some has 20% MC? After controlling MC, yields would be more accurate/standard, at best it could even make the process more robust or even break down chlorophyll and make EA easier to reuse (see table below from attached paper). A simple oven step at low heat (~200F) for a few hours should do the trick. Like shroombee said, this MC% could swing the actual paste ratio as ~ 1/(1-MC).

shroombee wrote:
how about we intentionally try to create goo by deviating one variable at a time from a known good process that yields xtals?


I suggest we don't do this. There are a lot of things to change and even if we find goo, how do we know that was the same problem that an actual user had? Point is, there are lots of ways to break the process, I think it is better to focus on making it more robust. I believe it is pretty robust already, but I would like to add simple controls if they are easy (e.g cactus powder MC) and remove some color from EA so it is easier to reuse. Would also be nice to get product to not stick to the walls (e.g. boiling water paste).
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Cheelin
#669 Posted : 12/22/2021 2:30:00 PM

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Thanks Loveall.

I thought the first pic in the 24-run post would say it all about particle size, but my pics just don’t display here like they do on my phone. The passive method is like having a snowglobe with small snowflakes in it; when filtered, the delicate snowflakes break into beautiful needles that sparkle in the light, The active stirring method is beautiful in it’s own way, with immediate precipitation of very tiny particles that don’t trigger the thought of “crystals” imo, looking more like powdered sugar.

I know there are hcl bigots out there who claim that this tek precipitates citric acid, and I must admit that the active stir product’s appearance always triggers that thought in my mind. BUT, a simple taste comparison between the the passive and active product simply shows that they are identical from a taste perspective, with absolutely zero perception of acid (wine research has determined humans can detect flavor & perception differences down to the parts per trillion range). I challenge anyone who doubts my claim about zero perceptible acidity, to produce this tek’s product and then taste it, followed by a taste of the most minuscule amount citric acid, and then honestly tell me that this tek, when properly done, produces citric acid precipitate of sufficient quantity to be detected by the human tongue.

Regarding product sticking to the walls, my work shows this to be a trivial issue. It will be impossible to completely eliminate crystals sticking to the walls/bottom of the salting jar. Even the active stirring leaves “crystals” adhered to the wall, albeit smaller and fewer of them than the passive option. A way to minimize the adhered crystals left in the jar and ending up in the evap dish is as follows:
1. Use a Wide-Mouth jar/beaker for salting/crystallization, so that there is no shoulder in the jar to entrap loose crystals
2, The jar/beaker should have a volume 2X the volume of salting solution, so that adequate swirling can occur before pouring the solution through filter
3. Begin the filtering process with vigorous swirling of the solution, then pour approx 3/4 of solution into filter, re-swirl remaining solution vigorously, and in one quick motion dump the contents in the filter
4. Using a pipette or syringe, take 10-20mL (for 1/2 pint of solution, more if a bigger load) of Fresh EA, from the top of the j/b drain onto & circling the side walls, swirl vigorously and dump, repeat once and let j/b dry.
5. After j/b is dry, boil a little distilled water, follow step 4 but substituting the boiling water for the EA. After swirling, but before dumping (this time into glass evaporating dish), tilt j/b and turn so that the warm water briefly covers all the walls of the jar,

The above process will minimize the amount of evaporation needed and residue produced . Take a look at the splits between product that ends up in the filter and evap residue, in my results tables. The residue amounts are tiny.


As regards the wiki: if it were my tek, i would drop the description of all variations from the wiki, so that the wiki shows the “standard tek”, along with 5g citric/100g material passive and active salting/crystallization options, a problem product cleaning method, and a solvent reclaim method. I would add a comment discussing the importance of proper technique, which for most people new to extraction involves a learning curve. I would also add a comment directing all those who can not produce the proper end product, to this thread for possible variations of the standard tek, and help.

As far as work on making the tek more robust, i’d limit future work on the wiki to 3 topics: specifying powder characteristics to some reasonable extent; developing a brown, sticky product cleaning method; and determining the maximum number or effective solvent reuses (and the method).

All other work to improve the tek would be addressed, on this thread, and only when the problem can be recreated by someone other than the poster who has it. An appendix on the wiki would list verified problems and their solution.


One additional issue to consider: while I understand, appreciate, and agree with this sites’s reluctance to allow easy membership, most of the issues producing the proper product from this tek will happen to newbies who can’t post.
 
Loveall
#670 Posted : 12/22/2021 9:31:29 PM

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New results:

- Oven dried 100g of power at 175C for a few hours. After two hours the weight stopped changing at 92g. Therefore my MC% has been 8%.
- Proceeded with the standard TEK (added 308g of water to compensate).
- The extract is dark green. At this oven temp, the color of EA is not improved as far as I can see
- EA is currently xtalizing, will report on yields, I expect no change/no issues.
- Conclusion: I was able to measure my MC% and it was very close to Cheelin's. We still get different paste consistencies (mine looks looser than his). No issues with either of us getting xtals consistently.

I think the TEK is robust. Will be interested in anyone else getting goo consistently instead of xtals and their plant/prices details. As far as I know, everyone is getting xtals at this point.

Cheeling, I get the same results you do when it comes to xtalization. Dropping 5g acid gives big xtals, stirring 15g of acid gives a fine powder that tis much denser. Both are mescaline citrate with same yields. If dropped as little as 0.8g of acid and the extract fully xtalized and was slightly acidic with pH paper. Will keep the TEK as is, but the process window is very large - which is good.

I've also squeezed the french press hard and had no issues xtalizing. After squeezing, I broke up the compacted paste and some solvent came loose which can be squeezed out. The extra drops don't really matter, same yield after 6 pulls as the standard method.


If a lot of xtals stick to the wall hitting them with a butter knife or spoon knocks them off the wall.


We've kicked the tires of the new TEK pretty hard and it seems robust, giving similar answers. Cheelin noticed a slight drop in yield with the microwave and cold extract method so those are now gone from the TEK. To get EA that is not extremely dark green and may be easier to reuse I added the boiling water option, that really reduces the color in the extract and does not seem to reduce yields (would be interested in someone's check on this, maybe careful measurents do shoe a drop, IDK).

Newbies can post in the welcome area and ask about the CIELO Tek there. That seems to work (e.g. HLP).

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_Trip_
#671 Posted : 12/22/2021 11:06:46 PM

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Awesome work Cheelin.

So looking at those results the chilled EA killed yields more than anything else. Where as the microwave method without chilled EA was almost on par (within 10% yield from your best run). And same average yield as a few other runs.

So Loveall I would ask for the purpose of solvent reuse, is it necessary to completely get rid of the microwave step from the TEK? Or does a brine wash/ hot water paste correct this?

I would argue getting rid of chilled EA is more important.

Regardless I would like to add one more variable and that is hot EA pulls, I've seen better yields doing hot pulls but crystal color suffers, however this was with 15-20mg salting. Color may be corrected with 5mg. Thoughts?

Disclaimer: All my posts are of total fiction.

 
Loveall
#672 Posted : 12/22/2021 11:14:56 PM

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I think microwave yields are lower looking at Cheelin's data. The combined (microwave + chilled) was the lowest, making the signal seem real. Maybe we need to calculate a p value 😅

Using boiling water yielded fine for me (but also I did not notice a significant difference with the microwave, However my data was not as thorough as Cheelin's). Boiling water is a lot simpler than the microwave. Also, not everyone has a microwave. So I replaced the microwave option with boiling water to keep the EA a light yellow/green and easier to reuse.

Your heat comment is interesting. Maybe next time I will not wait for the boiled water paste to cool and pull after 15 minutes, while heat is present. Not sure how long the chlorophyll needs to break down, but if it is within this time frame maybe we can get the best of both worlds all at one for a quick, light colored, and high yielding extract.
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_Trip_
#673 Posted : 12/22/2021 11:22:51 PM

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I would be keen to try the boiling water instead of a microwave next run, would simplify it. I've used a hot water bath for the EA and french press in the past, this seemed to work well.
Disclaimer: All my posts are of total fiction.

 
Cheelin
#674 Posted : 12/23/2021 4:30:27 AM

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Thanks _Trip_.
 
Cheelin
#675 Posted : 12/23/2021 4:52:27 AM

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Loveall, I plan to do a boiling water version of the bulk wet mix std process, with a set of 3 runs similar to those in the 24-run expmt and same material, hopefully tomorrow/Friday.

If heat during the pulls leads to higher yields than the std process in someone else’s runs, i’ll consider using the materials, and doing the extra work for a 3-run set of this variation, later.

I’m very leery of doing any more runs of treatments that don’t meet or exceed std process yields, especially just to get lighter colored solvent. I have yet to see anyone demonstrate that clear neutral yellow solvent adds any value over clear neutral green solvent.

I intend to test yellow vs green solvent reuse in multiple consecutive runs soon.
 
Loveall
#676 Posted : 12/23/2021 10:24:51 AM

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I'm pretty sure we understand the mescaline citrate salt form: (MesH)H2Cit thanks to data presented by several people.

I'm going to do a titration experiment to add to this data. Also, to make sure the salt form doesn't change under different pH conditions.

For each 1g of mescaline freebase (Mes), assumimg that to first order that is the major component being titrated,

For (MesH)H2Cit: 910mg of citric are needed to produce 1.910g of xtals
For 2(MesH)HCit: 455mg of citric are needed to produce 1.455g of xtals
For 3(MesH)Cit : 303mg of citric are needed to produce 1.303g of xtals

So by keeping track of the pH as citric acid is being added, and stopping when pH paper becomes neutral, and knowing the final yield, the salt form can be known. I typically get 1.2% yield with my current powder, so I would need ~571mg of citric acid to neutralize the extract if the salt form is indeed (MesH)H2Cit. I can check at/above 190mg and 286mg to verify the extract is still alkaline on pH paper.

I also wonder if adding 190mg of citric and then giving time for xtals for form would produce the 3(MesH)Cit form and neutralize the solution over time.
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Cheelin
#677 Posted : 12/23/2021 1:53:58 PM

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👍🏻 Loveall!
 
Cheelin
#678 Posted : 12/23/2021 6:09:00 PM

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Tested a 45g quantity of material, bulk prep’d & wet mixed, using std process, subdivided into 3 portions. using same material used in 24-run experiment. The only difference between this treatment and (B,0,0,0,1) is that the water used to make the paste was boiled before mixing with the pickling lime.

During the 8-minute mix, the paste was noticeably more liquidy than my normal paste, looking more like pudding than playdough. After the 10 minute rest, the paste was much more rubbery than usual, looking more like silly putty that the usual rubbery version of playdough.

When pulling, the paste remained rubbery and clumpy throughout all 6 pulls, rather than becoming applesauce appearance by the end of the final pull. Unlike pulling the paste made from ambient temp water, the 1st pull hardly absorbed any solvent, and although not measured, the volume of solution from each pull looked roughly equal. The color of the 1st pull was slightly darker than fresh solvent, with each subsequent pull taking on a slightly darker shade of yellowish-green, combined pulls look the ligjtest color of any treatment yet.

The 3 runs were salted/crystalized the same way as each 3-some in the 24-run exprmt, results are in the attached table.


Additionally, three other sets of treatments were run: a 3-run test without the 1-hour settling period after the final pull; a 4-run, 2-way test of the active stirring option, using 5-minute or 10-minute magnetic stir with 24-hr rest, at the equivalent of 5 or 15g citric acid per 100g powdered material; and an 8-run, 2-way test of 20-minute magnetic stir with 4 different rest periods before filtering (1hr, 3hr, 6hr, 12hr), at the equivalent of 5 or 15g citric acid per 100g powdered material.

All of these runs were done with the same material used in the 24-run experiment, using wet mix standard paste. The 3-run test used 45g of powder, bulk prepared, split into three portions; the 4-run test used 60g of powder, bulk prepared, split into 4 portions; the 8-run test used two batches x 60g of powder, bulk prepared, split into 4 portions each.

Results of these runs are in the attached table.

Main Points:
1. All passively crystallized runs produced white needles and minimal, white, jar wash residue; all magnetic stir runs, regardless of citric acid option, produced white powder and minimal, white, jar wash residue; all runs tasted identical, moderately bitter, no acidity.

2. Using boiled water, produces a paste that is more difficult to extract and reduces yield (roughly equivalent to the microwave treatment (B,0,1,0,1) yield). The mixing and/or pulling processes can likely be adjusted to improve yield, but will require more effort than just using ambient temp water.

3. Eliminating the 1-hour settling period after the final pull, slightly reduces yield.

4. Magnetic stir period slightly affects yields: high to low yield ranking is 10-min, 5-min, 20-min.

5. Both citric acid levels produce similar yield for a given stir method, indicating that there is no need to use more than 5g citric acid per 100g of powdered material.

6. When using magnetic stirring, yield roughly peaks 3 hours after stirring.
Cheelin attached the following image(s):
Untitled.png (166kb) downloaded 84 time(s).
 
Loveall
#679 Posted : 12/23/2021 6:52:05 PM

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I noticed the boiling water paste congeal also so I added some boiling water before pulling to loosen it up (25ml for a paste with 100g of cactus). I wanted EA to penetrate well that's why I broke it up with fresh boiling water right before pulling. I don't think it was enough to raise the temp significantly, just enough to make a loser paste so it would be easier for EA to get in there.

I've started to go by paste feel. Looser paste with a little bit more water seems easier to pull. More compact paste is harder to pull, and yields can be lower (that is what I got with the failed "min water" paste). No issues with goo or xtalization when I add a little more water to get the paste I want.


I worry your boiling water run may yield less because the paste was so compact. We will see. I think that the xtals that form may be larger than the standard TEK. They may form faster too. curious to see what you get.

I've also started squeezing with the french press. After squeezing, I break up the compressed mass with a knife and a little more EA comes out, so I squeeze that out again, and repeat of needed. Only takes a few seconds each time at the end of a pull. Sakkadelic would be proud. I think I'm getting a tiny bit more yield this way (1.3% instead of 1.2%). No crystalization issues and I've squeezed pretty hard. We were being cautious about this when people where getting goo to avoid water and recommending only lightly squeezing or no squeezing at all, but it doesn't seem that was the cause of some people seeing goo.

After not seeing water/particles for a few consecutive runs, I've stopped waiting for an hour. I would still recommend it for newcomers. Xtalization happens the same as when waiting (yields, etc).

Overall, the TEK is being extremely robust for me, even when I push the parameters around. Over time a feel for it develops, especially for what a good water paste consistency is.

Looking forward to your results Cheelin 🙂
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Cheelin
#680 Posted : 12/24/2021 4:35:57 AM

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Like I have said, Loveall, you nailed it, this tek would make Shulgin proud!

I think the paste making and pulling/filtering parts of the tek, as well as passive salting/crystallization are good enuff for my purposes, with my efforts hitting the point of diminishing returns. Looking now to minimize time on the active salting/crystallization method for those who want the fastest process without yield loss. I got a little carried away and did a few more runs today than planned, lol. I’ll show results in the earlier post, when done.
 
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