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Ethyl acetate approach [CIELO] Options
 
shroombee
#481 Posted : 12/1/2021 6:47:56 AM

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Cheelin wrote:
Thanks Shroombee, the good ole cannabis winterization tek, any particular order of EA and cold everclear/ipa/acetone?

I don't think it's necessary to do all three. We know resin TEK using 99% IPA pulls a lot of gunk and basically zero mescaline, so the idea is to pull that gunk before basing and pulling with EA, with the theory that the gunk contributes to goo formation. Now that I think about it, an EA pre-wash should work better than IPA (?) since EA is our solvent for pulling the mescaline.

BTW, the natural mescaline salt (mescaline malate) in the cactus is more soluble in ethyl alcohol, so we wouldn't want to use everclear for the pre-wash. Plus it's more expensive than the other solvents.
 

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Cheelin
#482 Posted : 12/1/2021 7:13:05 AM

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Thanks Shroombee, I’ll experiment with this when i have issues with a particularly gooey source of material.

Btw, I really appreciate that one detailed process description you posted somewhere in the middle of this thread. Lots of my issues have been related to the lack of fine details in the wiki.
 
shroombee
#483 Posted : 12/1/2021 8:03:13 AM

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Cheelin wrote:
Thanks Shroombee, I’ll experiment with this when i have issues with a particularly gooey source of material.

Btw, I really appreciate that one detailed process description you posted somewhere in the middle of this thread. Lots of my issues have been related to the lack of fine details in the wiki.

Good to know the excruciating detail is appreciated! Laughing Feel free to add clarifications to the wiki, or if you're not comfortable editing it, let us know what wasn't clear and how we can make improvements.
 
Cheelin
#484 Posted : 12/1/2021 12:34:23 PM

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I’ll post my own version here, soon. What a great tek!

Now, if someone could develop a small-sample simple and fast diy cactus alkaloid test, that can be used in the garden…
 
Loveall
#485 Posted : 12/1/2021 1:53:02 PM

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shroombee wrote:
Cheelin wrote:
Thanks Shroombee, I’ll experiment with this when i have issues with a particularly gooey source of material.

Btw, I really appreciate that one detailed process description you posted somewhere in the middle of this thread. Lots of my issues have been related to the lack of fine details in the wiki.

Good to know the excruciating detail is appreciated! Laughing Feel free to add clarifications to the wiki, or if you're not comfortable editing it, let us know what wasn't clear and how we can make improvements.


I second this and encourage to update the wiki with any details you think could help others. Don't worry about breaking the Wiki, edits can be rolled back if needed 🙂
💚🌵💚 Mescaline CIELO TEK 💚🌵💚
💚🌳💚DMT salt e-juice HIELO TEK💚🌳💚
💚🍃💚 Salvinorin Chilled Acetone with IPA and Naphtha re-X TEK💚🍃💚
 
Cheelin
#486 Posted : 12/1/2021 2:15:49 PM

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Lol, you think your post had excruciating detail.

I’ll post it here, and Loveall, you, and others above my paygrade can decide if any of it belongs in the wiki. My goal is to provide a recipe that is spoonfed repeatable, step-by-step, by those who know enough to do some damage, but aren’t chemists.

So far, looks like a white Christmas.
 
shroombee
#487 Posted : 12/1/2021 6:43:58 PM

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Cheelin wrote:
Lol, you think your post had excruciating detail.

You're right - the posts themselves are fine. I feel it's excruciating measuring everything during the extractions, taking detailed notes, writing the posts, editing, trying to ensure I'm clear in my communication, etc. Worth it though when folks find the sharing helpful. Smile

Quote:
So far, looks like a white Christmas.

Thumbs up
 
Cheelin
#488 Posted : 12/1/2021 9:26:17 PM

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I hear ya, Shroombee, and appreciate the precision and effort that you & Loveall, in particular, put into this tek. When developing a new process you don’t know which small changes will affect the outcome, or its repeatability; so you have to be careful and precise. I can’t tolerate that part well, it is part of the reason I couldn’t be a researcher; and is one of the reasons why I respect those who can.

I’ve now done enough extractions with this tek, that i think the working process is not that demanding of research-level precision. But you don’t know that until after the process is adequately developed.

The single most important step that has helped me, is focusing on the first 8 minutes of the tek. The better I have been able to thoroughly mix the playdough, the higher quality my results have been. The second major improvement came from breaking up the doughball into pieces (1/2” max) before beginning the first pull. Next would be filtering to crystal clear before salting.

I’m sure there are significant potential time and effort reductions possible (for a tek that already takes less than an hour of actual work). So, having a reasonable level of precision is also useful for that imprpvement effort as well.

I expect the CIELO Tek will become quite popular for producing the end product simply, quickly, and purely, with readily available and relatively safe materials. Particularly due to the quick process, i also expect it will be quite useful for gardeners testing for alkaloid content, in their decisions about which plants to cull or keep, absent the type of test I mentioned earlier.

Congrats and thanks to all who made these improvements possible!
 
_Trip_
#489 Posted : 12/1/2021 9:43:23 PM

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Cheelin wrote:


The single most important step that has helped me, is focusing on the first 8 minutes of the tek. The better I have been able to thoroughly mix the playdough, the higher quality my results have been.



That's interesting I recently found no difference rushing the 8 minutes. I still got the same end result percentage wise with the same cacti.
I'll have to do a proper side by side comparison to be sure. I still think 8 minutes as per the Tek is a safe bet though.

Edit: Just to clarify when i say rushed I don't mean like 30 secs maybe 4-5mins (but stirred well). Usually I do go 8-10 minutes. I don't recommend less I just recently did a run where i rushed the mix to see what would happen and it didn't yield any less, however this was with 20g of cacti material so it was easier to stir than 100g.

I do like to give it a thorough stir between microwave bursts too.
Disclaimer: All my posts are of total fiction.

 
Cheelin
#490 Posted : 12/1/2021 10:05:56 PM

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Did you get significant amounts of pure white crystals?

I suspect that crystal quality, is much more sensitive to thorough paste mixing than yield.

The 6 runs I completed yesterday are almost completely clear, and seem to only have needles and snowflake crystals as precipitate. We’ll see if that is the case after final drying. In earlier runs, where i just quickly and casually mixed the playdough, I’ve had 2-4% yields, but hardly a crystal in my filter.
 
Loveall
#491 Posted : 12/1/2021 10:16:42 PM

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It is very important to mix the paste well. Mix long enough for the texture to change to a smooth fluffy paste. The texture changes as the cacti is broken down, do not stop mixing too early. The TEK speaks to this and has a picture. 8-10 minutes is enough, but stirring needs to be purposeful.

If not mixed well enough to get the right texture the paste is not ready.
💚🌵💚 Mescaline CIELO TEK 💚🌵💚
💚🌳💚DMT salt e-juice HIELO TEK💚🌳💚
💚🍃💚 Salvinorin Chilled Acetone with IPA and Naphtha re-X TEK💚🍃💚
 
Cheelin
#492 Posted : 12/1/2021 10:32:12 PM

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I certainly agree with “purposeful”.

But when I proportionately reduce the ingredients for a 25g run, my “paste” become almost playdough-like and requires a fold-&-squish technique. Microwaving does make it fluffy and more like individual particles, chilling makes it a harder doughball (prob due to 24 hrs delay, perhaps somewhat due to chilling).

 
shroombee
#493 Posted : 12/2/2021 2:40:55 AM

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Cheelin wrote:
The single most important step that has helped me, is focusing on the first 8 minutes of the tek. The better I have been able to thoroughly mix the playdough, the higher quality my results have been. The second major improvement came from breaking up the doughball into pieces (1/2” max) before beginning the first pull. Next would be filtering to crystal clear before salting.

It's interesting you get playdough when the volumes are proportionally reduced down. So when the ratio of surface area to volume increases, the mixture gets clumpy. Conversely, when the ratio of surface area to volume decreases (as the amounts are scaled up), the mixture gets fluffy and easier to stir. I know some of the more experienced folks would be able to explain the science behind this.

One thing you can try is to thoroughly mix the powdered cactus with the lime, then add water. Perhaps more water than necessary then microwave it down. I used to do this "dry cactus plus lime mix" with the limonene tek.

Quote:
Congrats and thanks to all who made these improvements possible!

Thanks for jumping in with your experiences!
 
Cheelin
#494 Posted : 12/2/2021 3:03:54 AM

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Thanks, i thought about the overwatering one with additional microwave evap, hadn’t thought about dry mixing then water. They’ll be on my list for testing in the future.

I’m also wondering if this is a signal that there is an opportunity to reduce stir time by some amount, maybe/maybe not proportionally. Will put this on my test list, too.
 
shroombee
#495 Posted : 12/2/2021 3:42:09 AM

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One other idea is to mix a 100 gram batch and then split it up into the smaller experiments. We've tested basing times from 10 minutes up to 72 hours with no difference in yield. So you could also set mixtures aside for use a day or three later.
 
Cheelin
#496 Posted : 12/2/2021 3:49:45 AM

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That definitely would be an option. But, i’d just go ahead and save 3 production runs, and do it all at once. Lol
 
Cheelin
#497 Posted : 12/2/2021 3:29:56 PM

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Loveall has created a simple, quick, efficient, and relatively safe process, using easily obtainable materials and equipment, to produce high-purity mescaline citrate from mescaline producing cacti. He, Shroombee, and nearly everyone participating in this thread, have contributed to the development of the tek. I encourage anyone using this tek to throughly familiarize themselves with the contents of the wiki and this thread.

Hopefully, the following detailed set of steps, materials, and equipment, will help you to produce consistent and repeatable results, to identify the source of issues you may encounter, and to get you up the learning curve quickly. Your results may vary based on your source material, and your ability to do the tek as it is described.


After the process is described, a yield summary is presented for 25g quantities of 3 different powders of unknown parentage with composition described by vendor as “flesh only”, “San Pedro, Ecuador, T. pachanoi” (material A), “San Pedro, Peru, T. pachanoi” (material B), and “Peruvian Torch, T. peruvianus” (material C). Each source material was run using the following variations of the tek:
Variation (0,0)- std tek with no microwaved paste and no chilling of paste and solvent;
Variation (1,0) - std tek with microwaved paste but no chilling of paste or solvent;
Variation (0,1) - std tek with no microwaved paste, but with freezer chilled solvent and refrigerated paste (both for 24 hours);
Variation (1,1) - std tek with microwaved paste, and freezer chilled solvent and refrigerated paste (both for 24 hours).

Shroombee’s quicker and effective, Stir & Dump salting process is described in this thread. Due to the limited quantity of powder that was available, a yield comparison was not run for that excellent salting option.


General Process:
Basing -> Microwave “Paste” or Not -> Chill Solvent & “Paste” or Not -> Solvent Pulling -> Passive Salting -> Filtering & Solvent Washing -> Warm Water Washing & Evaporation -> Packaging

Materials per 25g powder run:
Mrs.Wages Pickling Lime - 6.25g
Distilled Water - 75mL
Kleen Strip M.E.K. Substitute (ethyl acetate solvent) - 235mL for extraction, plus additional 20 to 50mL for washing crystals
Milliard Citric Acid - 1.1g
MColorpHast pH 0-14 Universal Indicator - 1 strip

Equipment:
Scale
Microwaveable Bowl
Stainless Steel (SS) Funnel
White Paper Coffee Filters
Quart Wide-Mouth Canning Jars, Bands, Lids (2 to 4)
Pint Wide-Mouth Canning Jar, Band, Lid
60mL syringe with industrial (blunt) needle
SS French Press
SS Tablespoon
Tinfoil Weigh Boats
Timer
Graduated cylinder or measuring cup
Glass Bakeware
Single-Edge Razorblade
Storage Jar or Parchment Paper

Basing:
In a microwaveable bowl, mix lime and water till milklike;
During an 8 minute period, mix in powder in 3 individual additions, create maximum contact between powder and lime solution by using spoon to continuously fold and press “paste”;
Let rest 10 minutes;

If microwaving paste:
Weigh the bowl with “paste” in it;
Calculate target weight (total weight minus 50g evap water);
Microwave on high for 2 minutes, stir until color is uniform, weigh;
If not at target weight, microwave on high for 1 minute, stir, weigh, repeat until target weight is reached (a few grams lower than target is not a big deal).

If not microwaving “paste”, move on to next step.

If chilling:
Put “paste” in canning jar, cover with lid, put in refrigerator for 24 hours;
Partially fill a separate canning jar with 250-260mL MEK Substitute, cover with lid, put in freezer for 24 hours;

If not chilling:
Partially fill a canning jar with 250-260mL MEK Substitute;
Move on to next step.

Solvent Pulling:
Put “paste” from previous step into French Press;
If necessary, break up “paste” into chunks no larger than 1/2”;
Set timer for 1 minute if using chilled solvent, or 3 minutes if using ambient temp solvent;
Take jar of MEK Substitute from previous step, and suck 50mL into syringe;
Empty Syringe into French Press;
Stir “paste”-solvent mixture for 80 revolutions during 1 minute;
Let mixture rest 2 minutes if using ambient temp solvent, no rest if using chilled solvent and “paste”;
Then, pour pull through single filter paper-funnel into clean canning jar, until drip rate is less than 1 drip per second;
Repeat for 5 more pulls, but fill syringe with only 37mL solvent each time (first pull will have minimal liquid drainage, quantity of pulled liquid will increase with each successive pull);
After final pull, put maximum squeeze on the “paste” to fully drain unbound solvent into filter;
Let combined pulls rest for at least 1 hour.

[To check solvent recovery, put an empty canning jar next to the one containing the pulls; add sufficient tap water to match the height of the liquid in the pull jar; pour out water into graduated cylinder or measuring cup; determine amount of water in mL, calculate (mL water/mL total solvent added in 6 pulls); calc should be close to 90%.]

Passive Salting:
Put filter-funnel on clean canning jar;
Pour combined pulls through filter;
If solution is not crystal clear, let settle, decant liquid off of residue, through filter (if having difficulty filtering, pour liquid through a stack of 2 or 3 new filters). When crystal clear, filter into a 1 pint canning jar, add citric acid, gently swish contents 2 to 3 horizontal revolutions (liquid should become cloudy), put lid on, and place jar in a location where it won’t be disturbed;
1 hour later, swish jar contents 2-3 horizontal revolutions, then dip pH paper into liquid (should be in the pH = 5 range), re-cover jar, and place jar back in storage area until liquid is crystal clear (these runs were stored 56 hours to provide extended crystallization time, most runs cleared within 24 hours)..

Filtering & Solvent Washing:
Pour 3/4 of liquid in crystallization jar through filter-funnel, swish remaining liquid several times, pour thru filter;
Suck up 10ml fresh solvent into syringe, wash walls of jar, swish to collect unbound crystals, pour thru filter, repeat as necessary to collect unbound crystals (try to minimize use of solvent, a separate approach will be used to collect crystals adhered to jar walls and bottom);
If material in filter is not white, wash with minimal clean solvent to remove color, when no change in color is observed stop washing;
Let filter drip dry, then carefully remove filter from funnel, place on a paper towel to dry; cover recovered solvent, and set aside to later treat for reuse as described in wiki and this thread;
Carefully fold filter containing crystals, and store undisturbed overnight, to allow for complete evaporation of solvent, then carefully transfer crystals to parchment paper envelope or sealed jar for longer-term storage.
Let solvent evaporate from crystallization jar.

Warm Water Washing & Evaporating;
Heat up some distilled water;
Fill syringe with 40mL water, squirt 20mlL on walls of crystallizing jar, swirl to dissolve adhered crystals off of walls and bottom of jar, pour contents into a shallow glass pan (large enough for you to later scrape up residue with a single-edge razor blade), then repeat with remaining 20mL.
Let water evaporate, scrape up dried residue with razor blade;
If residue is discolored, you can try to remove color by washing in a filter using fresh solvent, then drying and storing as described above.


Results:
See attached table

Conclusions:
1. Consistent small-sample extraction of high-purity product is possible, across different species/varieties and process variations, using careful & purposeful preparation.
2. Although elapsed time (due to filtering/settling, passive crystallization, and jar wash evaporation) can take several days, actual processing time can be minimized to under 1 hour per run.
3. Variations from the standard process provide no apparent yield or quality benefit.


The poorly rendered pics below show what has been retrieved from the filters of all 12 runs. Also attached is a representative pic of the residue from the crystals that adhered to the walls/bottom of the crystallization jars; which were warm water washed, evaporated, and scraped.

00A, 00B, 00C: Standard Process, materials A, B, C
11A, 11B, 11C: Standard Process + Microwaved Paste + Chilled Paste & Solvent, materials A, B, C
01A, 01B, 01C: Standard Process + Chilled Paste & Solvent, materials A, B, C
10A, 10B, 10C: Standard Process + Microwaved Paste, materials A, B, C
Cheelin attached the following image(s):
image.JPG (824kb) downloaded 338 time(s).
image.jpg (743kb) downloaded 340 time(s).
image.JPG (2,357kb) downloaded 296 time(s).
image.jpg (1,551kb) downloaded 267 time(s).
image 2.jpg (307kb) downloaded 225 time(s).
image.jpg (1,954kb) downloaded 222 time(s).
 
Cheelin
#498 Posted : 12/4/2021 8:01:54 PM

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Has anyone used a freeze dryer to evaporate the water in the warm water wash and evaporation process?

If so, please describe results.

Thanks
 
Cheelin
#499 Posted : 12/5/2021 6:29:47 PM

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Bioassay of sample from earlier run, sample not from the runs above:
150mg appears to be a +/- dose on the Shulgin scale, will confirm w 200mg in future.

Seems 60ish % of HCl may be the case.

Effects first noticed 1 hr after dissolving in small glass of Tang, drinking on an empty stomach.
 
Loveall
#500 Posted : 12/5/2021 9:48:56 PM

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Cheeking, looking good. Interesting that the chilled pulls are giving less yield (so far). If that holds it would be different than what I got. Do you know what temp your freezer is at? Let's see what you get after adding the xtals that stick to the wall.

If you look at the filters that caught the xtals, I imagine the standard process has heavy green ring(s). The color of the xtals indicates that the green color seen in the solvent was wicked away effectively. That matches what I saw.

It seems you are working with two species and both gave xtals. That matches _Trip_'s observations.

Consensus is that the salt form is 60% equivalent to HCl (thanks for adding to this). Not verified analytically yet though.

Thanks for the detailed work 👍
💚🌵💚 Mescaline CIELO TEK 💚🌵💚
💚🌳💚DMT salt e-juice HIELO TEK💚🌳💚
💚🍃💚 Salvinorin Chilled Acetone with IPA and Naphtha re-X TEK💚🍃💚
 
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