TEK Ethyl acetate approach [CIELO]

[_Trip_]

Right, I found in some earlier experiments that removing water ice seemed to facilitate xtal formation. However, those experiments gave me less yield than the current tek where I get xtals immediately upon adding citric with the magnetic stirrer.

Yeah, even with my limited runs so far that's consistent with what I have found as well. Water seems to decrease yields quite a bit which is why I rate the microwave method to reduce that water content.

I need to try with the microwave option but without cold pulls on the same cactus powder I've been using; to see if there's any difference in yield.

 

[Loveall]

If water content is causing noise, maybe we should just to do a "standard" chemichal dry with CaCl2 (over the counter deicer pellets).

I did this chemichal dry and didn't notice a difference in yield. However, it could make the TEK more robust for everyone in general under a wider range of conditions.

The professionals usually have a solvent chemical dry before salting, and maybe we should just copy that approach to have a wider process margin.

Added step would be simple, simply add CaCl2 pellets to the clean extract at about 5% by weight (5g for every 100g of ethyl acetate). They will visibly absorb water moisture. Decant and rinse them once with fresh ethyl acetate to get the last bit of product.

On the salt form experiments, I haven't tried the slow evap yet, I got busy with life stuff all of a sudden.

About the CIELO TEK name, it is a nod to the natives who named their cactus "San Pedro" after the catholic priests explained that Saint Peter has the keys to heaven (CIELO means heaven in Spanish). Also, seeing crystals crashing in ethyl acetate is heavenly.

 

[Nachooo]

Don't know why you named it CIELO TEK should be the Ultimate Fucken Mescaline TEK.

I like the name CIELO...means sky or heaven in spanish (same word for two concepts clearly related some way)...so a great name..even if it is by chance...

EDIT: I just have read the previous post..so it was named for that reason LOL!

 

[_Trip_]

If water content is causing noise, maybe we should just to do a "standard" chemichal dry with CaCl2 (over the counter deicer pellets).

Look my kitchen chemistry is poor quality at the best of times, but the water observation I've noticed, if other people are noticing something similar I think CAC12 sounds like a great idea to look into. However, on my recent runs (doing the microwave method and reducing water content by 2/3rds) I've noticed no floating ice crystals when freezing the extracted EA. So CAC12 may not be necessary but still worth looking into.

About the CIELO TEK name, it is a nod to the natives who named their cactus "San Pedro" after the catholic priests explained that Saint Peter has the keys to heaven (CIELO means heaven in Spanish). Also, seeing crystals crashing in ethyl acetate is heavenly.

Cielo is a good name.

Talking about my poor chemist skills I did try to convert 400mg of mescaline citrate to HCL obviously using distilled water, caustic soda, xylene and HCL acid 'pulls'.
I pulled 2 times on the HCL acid pulls and evaporated the water.

I have done the whole process of xylene and acid (x2) pulls 3 times now (obviously using the same original base and same xylene). So 3 evaps in total.
I'm still in the process of evaporating one last acid pull (which should turn up next to nothing) which i will continue to do until I evaporate nothing.

But my results so far are indicating it's probably Dihydrogen as I'm closer to the 62% mark than anything (i've factored in the I've probably lost a little bit through the process and there's some tiny HCL crystals stuck in the corner of the glass dish (hard to get to with a razor).

If it is dihydrogen, 400mg should convert to 248mg HCL. I've converted and collect 215mg so far. There's still a 4th evap happening now which I don't think will turn up much. And I'm factoring in 5-10% loss due to some crystals stuck in corners of dishes etc and my average kitchen chemistry skills. However I have tried to be very careful with this process.

If this next evap turns up 25mg or less I'd be leaning towards dihydrogen.

However I wouldn't be trusting my chemistry too much, 'take it with a grain of salt' or so to speak.

 

[Loveall]

Thanks so much for the conversion experiment _Trip_

~62% like you are getting is good info, especially if someone else can confirm. We go by whatever the experiments say and each data point is very valuable (thanks again). The salt could also be a hydrate. For reference compared to (MesH)Cl by weight:

- (MesH)H2Cit: ~62% the dose by weight
- (MesH)H2Cit.H2O : ~59% the dose by weight
- (MesH)H2Cit.2H2O: ~56% the dose by weight

Since you are at ~54% and still have some left to scrape up we can rule out trihydrate. Let's see what you get in the end, you may be able to rule out the dihydrate if you get past the 56% mark.

 

[_Trip_]

I'm going to do one more evap,I've scraped up every mg I can and there's still a tiny amounts in corners of dishes. I would reckon a small percentage was lost during conversion as well (potentially).

I'm leaning towards (MesH)H2Cit, I've got 236mg now. So that's 59%, one more evap could turn up 5 maybe 10 more mg plus a few mg in the corner of the dishes?

It's a very narrow margin for kitchen chemistry.

This would explain my 3.4% with the same Bridgesii powder. When I did an A/B (HCL) on the same powder I pulled about 1.3-1.4%. Converting that mescaline citrate pull of 3.4% by weight to HCL that would put me at 1.48% in comparison. (Again i acknowledge comparing Teks isn't an accurate measurement).

But I don't believe we're looking at (MesH)3Cit or (MesH)2HCit.

I guess there's other potential issues:
How pure was the distilled water?
Could any debris have got in the dish? (I shouldn't have as i had a fan on it).
This wasn't done in a lab.
Etc.

 

[Loveall]

Thanks _Trip_, TEK has been updated with your result.

The process you followed sounds good and your data landed right on one of the possibilities, so it all looks consistent. Will be great if someone else can confirm one day.

We've had some feedback that by mass the citrate from this TEK it was weaker than the sulfate, wich some folks are acustomed to. While a lot more anecdotal, that observation is consistent with yours.

Thanks again for your work

Edit: I believe your 3.4% mescaline citrate yield would be equivalent to ~2% Mescaline HCl based in the numbers you are getting.

 

[_Trip_]

No worries, glad to have given it a go.

I hope it helps narrow it down. It'll be interesting to see someone with a proper set up or lab access to confirm exactly what form is being created.


I pulled 2.4g citrate from 70g (3.4%)approx.
2.4g x 62% =1.48% HCL by weight.

Or is that wrong?

 

[Loveall]

No worries, glad to have given it a go.

I hope it helps narrow it down. It'll be interesting to see someone with a proper set up or lab access to confirm exactly what form is being created.


I pulled 2.4g citrate from 70g (3.4%)approx.
2.4g x 62% =1.48% HCL by weight.

Or is that wrong?

I would say it like this,

2.4g of citrate from 70g is a 3.4% yield.

If converted to HCl, since the smaller conversion gave 240mg out of 400mg, would expect 2.4g*240/400 = 1.44g of mescaline HCl from the same 70g, which is a ~2% yield.

When you did the extraction with this powder using xylene and going strait to HCl with an equivalent of 70g of powder, did you get a yield of 1.4% (which would be about 1g of mescaline HCl), or was it 1.4g from 70g (which would be a yield of 2%)?

 

[_Trip_]

Sorry no, from the A/B (HCL)it was from 100g. Which was about 1.3-1.4% after been cleaned with MEK/IPA/Acetone.

Using Cielo Tek the citrate was from 70g. Sorry yeah ofcourse i get where the 2% is. Meaning the Cielo Tek has definitely come out ontop, bigger (or similar) yield from less material, for HCL equivalent. Thanks for the correction.

 

[shroombee]

Congrats _Trip_ on your results, and thanks for posting your data and experimenting with the HCL conversion.

Will be great if someone else can confirm one day.

I can't get xylene in my location. Can I base with lime, pull with limonene, and salt multiple times with HCl water? Will that get us an accurate enough result to confirm? I can also try the direct-to-HCl conversion, evaporating at 95 degrees in the dehydrator.

We've had some feedback that by mass the citrate from this TEK it was weaker than the sulfate, wich some folks are acustomed to. While a lot more anecdotal, that observation is consistent with yours.

I've noticed the two times I dosed the mescaline citrate, I felt it should be stronger for the amount I took. I thought perhaps there was a mix of mescaline citrate and additional alkaloids contributing to the weight of the dose. Now it appears the reason for the gentler trip is the form of the mescaline salt.

My yields have been about 1.6% with CIELO, which I also felt was high for this material. An approximate yield of 1.0% is what I had figured based on the strength of tea and the lime/limonene/HCl tek. And not coincidentally, ~1.0% is what would be expected by converting 1.6% x 240/400 = 0.96%

 

[_Trip_]

Last evap I have official come in at 244mg of HCL from 400mg citrate, scrapping up every little speck i could.

 

[Loveall]

Last evap I have official come in at 244mg of HCL, scrapping up every little spec i could.

Yep, that is consistent with the dihydrogen salt.

We also measured the pH of the product in water at 3.55. This is acidic, and consistent with the dihydrogen salt I believe. One way of looking at the pKa situation, is that since citric acid's pKa's are 3.1, 4.7, and 6.4, a solution with pH < 2.55 is 90% H3Cit3, when pH~3.9 it is mostly H2Cit-, when pH~5.5 mostly HCit3--, and when pH > 7.4 it is 90% Cit3---. So the pH measurement of 3.55 is also consistent with the dihydrogen salt to first order (the MescalineH+ cation makes things more complicated so numbers are not exact as DWFZ mentioned).

As shroombee mentioned, his bioassays were consistent with the dihydrogen salt.

So all the evidence we have sold far is consistent with dihydrogen salt. One caveat is that the TEK dynamics may change things (e.g. not using excess citric or slowly salting with drops of CASA). I believe _Trip_ used the "drop acid" salting method while shroombee uses his quicker swirl method. In general, it is always a good idea when first trying out the product to start with lower doses before normalizing the dose up by 1/60%, just in case the dihydrogen salt doesn't form under all TEK conditions.

I believe you can salt limonene with HCl, but it must be diluted in water and salting should shoot for ~pH7, avoiding very low pH which could break down the limonene. I would wash the limonene with plain water which should pull some free base and result in a basic pH, carefully adjust the pH with HCl to ~pH6 (lower is fine I imagine, I would just avoid extremely low pH), salt with the same water (pH should go up), and repeat the process with the same water until pH stops changing when salting. Then evaporate. I have never done this, so it is theoretical, maybe someone with more limonene/HCl experience can advise.

 

[_Trip_]

Loveall just to confirm would calcium chloride be a good way to eliminate water for solvent reuse after cleaning with sodium carbonate then?
Just to ensure your ethyl acetate is ready for reuse with zero water in it.

 

[Loveall]

Yeah calcium chloride pellets should dry it up nicely if you want, better than the freezing/filter step I think.

Or after the wash, you can use sodium carbonate powder itself (here potassium carbonate is mentioned, but sodium carbonate should work fine). In the US, super washing soda is the monohydrate form, which will absorb water in ethyl acetate I believe (forming decahydrate). I tried this once and it seemed to work.

Since we already have washing soda for the water wash to remove citric acid and reuse the solvent, we should be able to add washing soda powder to dry the solvent after separating the layers.

Side note:

Washing soda powder (monohydrate) could also remove water before the citric salting step. This could make the TEK a lot more robust for folks in general. We wouldn't be adding any more ingredients to the process. Also, the monohydrate is stable at room temp and normal humidity, so no need for special storage.

I'm liking the idea a lot. I'm gonna test this next time. Simply add ~5% washing soda powder to the extract, swirl a few times, let it rest for an hour, and decant. If there is no loss or issues, I think we should recommend it in the TEK even if some of us don't see an improvement since it could help someone that ends up with too much water (e.g. they squeeze to much, let cold EA absorb moisture without a lid on, etc). I would be an insurance of sorts, so the TEK simply works on a wider range of conditions.

 

[_Trip_]

I would imagine calcium chloride would do the same job, before salting?

I also gather sodium carbonate and calcium chloride won't affect the free base mescaline in the EA?


Where I'm from pellets aren't available but pool shops do stock pure calcium chloride in powder form. For those who can't get de-icer.


If calcium chloride doesn't react with FB mescaline I would be happy to try 5% before salting with citric acid on my next run.

 

[Loveall]

I would imagine calcium chloride would do the same job, before salting?

I also gather sodium carbonate and calcium chloride won't affect the free base mescaline in the EA?


Where I'm from pellets aren't available but pool shops do stock pure calcium chloride in powder form. For those who can't get de-icer.


If calcium chloride doesn't react with FB mescaline I would be happy to try 5% before salting with citric acid on my next run.

Yes, as long as it is anhydrous CaCl2. I'm not very familiar with pool products.

The CaCl2 pellets are easy to decant. Loose powder may be problematic and messy if it becomes wispy, I don't know. I would do a small test on plain ethyl acetate to make sure the drying agent you plan to use is easy to decant and/or filter and won't make a mess..

Free base mescaline is not affected in my experience. I've done a CaCl2 solvent drying test and it and had no negative yield issues (no improvement either, but I didn't have xtalization issues to begin with). CaCl2 can contain the alkaline impurities CaClOH and Ca(OH)2, but that is not an issue (we are pulling from Ca(OH)2 anyway). Acidic impurities would be a problem since they could salt the free base prematurely, and we are in the clear there

 

[_Trip_]

Too easy Loveall cheers for the information.

I'll do a test on the product I have.

If it separates easily I'll look to incorporate it with another run.

 

[CuriousSeeker]

Hello, this great tek has inspired the reopening of my garage lab! I've run it twice and want to ask a question about the odd result from the second extraction.

The first extraction used 100 g of ground 'Icaros DNA' purchased in 2011 (probably the same batch mentioned earlier in this thread) and followed the tek to the letter. I used the microwave option, did 5 ethyl acetate pulls, and 15 g citrate was used with magnetic stirring. This resulted in 725 mg of tan crystals captured in a coffee filter and 631 mg of pretty white crystals that were stuck to the jar wall. I used a microwave platter to evaporate the warm water used to reclaim the crystals stuck to the glass jar wall, and the microwave itself was used to remove about half the water, the rest being evaporated with a fan. The solvent was washed following the tek. The overall extraction resulted in 1.4%, which seemed about right.

The second extraction also followed the tek to the letter except that 108 grams of the same cactus material was used along with the washed solvent from the prior run. When the 15 grams of citrate with magnetic stirring didn't appear to do anything I added another 10 grams for a total of 25 g citrate. At this point clouds of crystals quickly formed and a total of 4.2 grams of light tan crystals were captured in the coffee filter with almost nothing stuck to the jar wall. A 3.9% recovery seems higher than expected, particularly when compared to the first run, and the crystals are harder than those from the first batch. I suspect the washed solvent introduced the differences, are there any suggestions as to what these crystals might be and how to separate out the mescaline citrate?

 

[shroombee]

The first extraction used 100 g of ground 'Icaros DNA' purchased in 2011 (probably the same batch mentioned earlier in this thread) and followed the tek to the letter. I used the microwave option, did 5 ethyl acetate pulls, and 15 g citrate was used with magnetic stirring. This resulted in 725 mg of tan crystals captured in a coffee filter and 631 mg of pretty white crystals that were stuck to the jar wall. I used a microwave platter to evaporate the warm water used to reclaim the crystals stuck to the glass jar wall, and the microwave itself was used to remove about half the water, the rest being evaporated with a fan. The solvent was washed following the tek. The overall extraction resulted in 1.4%, which seemed about right.

I've used Icaros DNA (Peruvian Torch) for all my runs so far. Good to know the 2011 vintage works and produces about the same yield (I'm getting 1.6% from more recent vintage).

3.9% yield on your second extraction definitely sounds like too much. Have you tried washing with fresh ethyl acetate? That should leave the mescaline citrate. After evaporating the ethyl acetate you can evaporate it to yield the unknown alkloids. Curious whether they would be active.