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Ethyl acetate approach [CIELO] Options
 
Loveall
#801 Posted : 1/13/2022 5:55:23 PM

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Cheelin wrote:
So, I just finished doing the 48hr filtering on the 9-treatment set of runs, using 5g of cactus powder, with powder that has ~1.1% yield with this tek, and fresh EA. These runs appear to be demonstrating, especially at this small run size, the amazingly consistent robustness of the paste recipe and pastemaking process.

Congrats to Loveall, Shroombee, and all the others who contributed to the pastemaking development effort.

Since the quantities of product are small (1.1% of 5g = 0.055g), the final filtering and jar wash/evap yields could swing the apparent results, i’ll hold off on any further comments until those results are in.


I'm looking forward to the final data on this πŸ‘
πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
πŸ’šπŸŒ³πŸ’šDMT salt e-juice HIELO TEKπŸ’šπŸŒ³πŸ’š
πŸ’šπŸƒπŸ’š Salvinorin Chilled Acetone with IPA and Naphtha re-X TEKπŸ’šπŸƒπŸ’š
 

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Cheelin
#802 Posted : 1/13/2022 6:28:25 PM

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Loveall, please also do the calcs re % of M HCl for the likely salts that crystallize

 
Cheelin
#803 Posted : 1/13/2022 6:38:19 PM

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Re: solvent reuse saga, just for grins, dropped some citric into an UnWashed used solvent run (solvent was from a 15g equivalent citric salting) that was totally cloudy 48+ hrs after pulling, will filter it tomorrow.

One way to make green crystals.

We’ll see if the green washes off.

Green does wash off completely, revealing needles and a white plate-like material and dust. The dust and plates have a very faint acid flavor, but is mostly tasteless. Yield: 0.440g at 48hrs, 2.9%.

This solvent had cleared at time of filtering; likely due to the salting to trigger crystallization. The other unwashed re-used (5g eeuiv citric) solvent run that I did not salt is still completely cloudy.
Cheelin attached the following image(s):
Green Snow.jpg (192kb) downloaded 198 time(s).
After EA Wash.jpg (322kb) downloaded 142 time(s).
After Drying.jpg (359kb) downloaded 142 time(s).
 
Cheelin
#804 Posted : 1/13/2022 7:20:15 PM

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Loveall wrote:
Cheelin wrote:
Looking like the toughest part of developing this tek is going to be the work on reusing solvent. Take a look at the 36 hr yields for part I. of the reused solvent trial above.


So yield was higher with reused solvent? That is surprising.

The yield stayed the same for me when reusing, but I didn't freeze to remove water. I'll repeat your experiment and see what I get.


So, an obvious question regarding this strange yield result is: could the higher yields of the washed used solvent runs be due to precipitation of something that remained in solution after the washes? Sodium Carbonate, perhaps?

HLP never answered my question about his suspect run. I asked if he was using reused solvent?

Not sure how to approach this question. As I mentioned, all the solvents used in this run started out crystal clear, no haze!

As a first stab, I just put 0.4g citrate in 50mL of clear unwashed solvent and clear washed solvent, to see if anything precipitates. I’ll also, as mentioned, do another set of runs, to see if the results are different.


I won’t be consuming any product run in reused solvent until, I get comfortable that what precipitates/crystallizes is the intended product.
 
Loveall
#805 Posted : 1/13/2022 8:30:42 PM

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Cheelin wrote:
Loveall wrote:
Cheelin wrote:
Looking like the toughest part of developing this tek is going to be the work on reusing solvent. Take a look at the 36 hr yields for part I. of the reused solvent trial above.


So yield was higher with reused solvent? That is surprising.

The yield stayed the same for me when reusing, but I didn't freeze to remove water. I'll repeat your experiment and see what I get.


So, an obvious question regarding this strange yield result is: could the higher yields of the washed used solvent runs be due to precipitation of something that remained in solution after the washes? Sodium Carbonate, perhaps?

HLP never answered my question about his suspect run. I asked if he was using reused solvent?

Not sure how to approach this question. As I mentioned, all the solvents used in this run started out crystal clear, no haze!

As a first stab, I just put 0.4g citrate in 50mL of clear unwashed solvent and clear washed solvent, to see if anything precipitates. I’ll also, as mentioned, do another set of runs, to see if the results are different.


I won’t be consuming any product run in reused solvent until, I get comfortable that what precipitates/crystallizes is the intended product.



Been thinking about the higher yield you got with reused solvent. Have you tried adding citric after washing (before any new pulls)? There should be no significant amount* of sodium carbonate in the washed solvent and sodium citrate should not appreciably cloud or precipitate. If needles do form, maybe removing the water while freezing allowed traves of leftover mescaline to crash as a citrate. If so, before salting one could freeze and remove water in the metal strainer, the salt and see if yield go up (?). I would keep the filtered ice in case mescaline is trapped in there.

I can't see how we are precipitating anything that could be bad. Worst case, you have citrical πŸ˜…

As a complement to this, I can do a test where I split am extract in two and chemichally dry one side of the split with sodium carb, then decant and salt to see if there is a difference in yields. I did this a while ago and I did not see an improvement (that was with CaCl2 and Epson salt drying tests though). I think it is worth repeating again based on what you are seeing.


*This post with NaCl data has ~3 ppm for the salt in the organic phase. Assuming a similar number for sodium carb, that is 700g*3e^-6 ~ 2mg
πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
πŸ’šπŸŒ³πŸ’šDMT salt e-juice HIELO TEKπŸ’šπŸŒ³πŸ’š
πŸ’šπŸƒπŸ’š Salvinorin Chilled Acetone with IPA and Naphtha re-X TEKπŸ’šπŸƒπŸ’š
 
Loveall
#806 Posted : 1/13/2022 8:42:51 PM

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Loveall wrote:
I've started a separate test salitng with different organic acids just for the fun of it after doubledog posted some pretty mescaline tartrate xtals this morning.

I extracted 50g of powder into EA (703g) after about 45 minutes of work πŸ™‚. I split this into 6 small jars with 65g of extract each and reserve the rest (703-65*6= 313g).

Expecting ~ 65mg of mescaline citrate equivalent in each of the small jars.

I'm passively salting each jar with 120mg of different organic acids:

- Citric (control): Usual cloudiness
- Malic: Cloudy
- Tartaric: Cloudy
- Vitamin C: Cloudy
- Fumaric: Cloudy
- Benzoic: No clouds (bottom left in second picture), instead, I saw bubbles in EA after adding this acid. So it seemed like it didn't work originally, but now I'm seeing a tiny amount of xtals forming (?). This acid is interesting because it should be soluble in Xylene, so one could use it to salt that solvent directly, lazy stile (CIXLO?).

Will report back on what precipitates in each jar and weight of each salt. The weight ratios could illuminate the salt stoichiometry too. Hopefully we get a bunch of different CIELOs.


Update after a few hours:

- Citric (control): Cloudy, typical opaque needles are forming on the wall
- Malic: Cloudy, no sign of needles, will wait longer
- Tartaric: Cloudy, seeing needeles similar to citric πŸ™‚
- Vitamin C: Cloudy, no sign of needles will wait longer
- Fumaric: Two layers, one cloudy (top) one clear (bottom). The clear layer is growing and in it there are shards, not needles. They look like flat glass pieces. They sparkle strongly at an angle and look very transparent head on. They are so pretty! πŸ˜πŸ€©πŸ™‚
- Benzoic: No clouds, tiny amount of crystals. Will give it more time...
πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
πŸ’šπŸŒ³πŸ’šDMT salt e-juice HIELO TEKπŸ’šπŸŒ³πŸ’š
πŸ’šπŸƒπŸ’š Salvinorin Chilled Acetone with IPA and Naphtha re-X TEKπŸ’šπŸƒπŸ’š
 
Cheelin
#807 Posted : 1/13/2022 8:56:44 PM

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Loveall wrote:
Been thinking about the higher yield you got with reused solvent. Have you tried adding citric after washing (before any new pulls?)

Quote:


In process


Cheelin wrote:
As a first stab, I just put 0.4g citrate in 50mL of clear unwashed solvent and clear washed solvent, to see if anything precipitates.


Follow-up report: no precipitate in either sample.

Will do this test again after completing test of 2nd washing approach.
 
Loveall
#808 Posted : 1/14/2022 1:31:17 PM

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Loveall wrote:
Loveall wrote:
I've started a separate test salitng with different organic acids just for the fun of it after doubledog posted some pretty mescaline tartrate xtals this morning.

I extracted 50g of powder into EA (703g) after about 45 minutes of work πŸ™‚. I split this into 6 small jars with 65g of extract each and reserve the rest (703-65*6= 313g).

Expecting ~ 65mg of mescaline citrate equivalent in each of the small jars.

I'm passively salting each jar with 120mg of different organic acids:

- Citric (control): Usual cloudiness
- Malic: Cloudy
- Tartaric: Cloudy
- Vitamin C: Cloudy
- Fumaric: Cloudy
- Benzoic: No clouds (bottom left in second picture), instead, I saw bubbles in EA after adding this acid. So it seemed like it didn't work originally, but now I'm seeing a tiny amount of xtals forming (?). This acid is interesting because it should be soluble in Xylene, so one could use it to salt that solvent directly, lazy stile (CIXLO?).

Will report back on what precipitates in each jar and weight of each salt. The weight ratios could illuminate the salt stoichiometry too. Hopefully we get a bunch of different CIELOs.


Update after a few hours:

- Citric (control): Cloudy, typical opaque needles are forming on the wall
- Malic: Cloudy, no sign of needles, will wait longer
- Tartaric: Cloudy, seeing needeles similar to citric πŸ™‚
- Vitamin C: Cloudy, no sign of needles will wait longer
- Fumaric: Two layers, one cloudy (top) one clear (bottom). The clear layer is growing and in it there are shards, not needles. They look like flat glass pieces. They sparkle strongly at an angle and look very transparent head on. They are so pretty! πŸ˜πŸ€©πŸ™‚
- Benzoic: No clouds, tiny amount of crystals. Will give it more time...


After ~24 hours:

- Citric (control): Clear, beautiful needles as usual. Will recover and measure weight soon.
- Malic: Cloudy, still no sign of needles πŸ‘Ž
- Tartaric: Cloudy with xtals forming very slowly. Not sure I would repeat 😐
- Fumaric: Clear, beautiful slender shards. Could also be described as wide needles, some are pretty large (~as tall as a fingernail). Could be a viable alternative to citric, pending yield measurement πŸ™‚. I believe fumaric solubility is 35mg/g in EA, which is lower than citric at 50mg/g. Should be enough to substitute in the TEK, but the process window and forgiveness for screw up is not as large.
- Benzoic: Clear as before, still a tiny amount of crystals (no change). I wonder what the miniscule amount of xtals are. Could be an equilibrium with the mescaline salt, or it could be a trace alkaloid salt that is not soluble while the mescaline salt remains soluble (?). I've added 1/4 tsp more of benzoic acid to see if I can force the mescaline salt out. So far πŸ‘Ž

A pattern seems to be emerging: Linear organic acids that have symmetry (citric, tartaric, fumaric) produce xtals, while others (malic, vitamin C, benzoic) do not. The central -OH group in malic makes it less symmetric I think. If this pattern continues, succinic and maleic should produce decent CIELO xtals too, perhaps I will test those one day for fun.
Loveall attached the following image(s):
Screenshot_20220114-082844-091.png (163kb) downloaded 165 time(s).
πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
πŸ’šπŸŒ³πŸ’šDMT salt e-juice HIELO TEKπŸ’šπŸŒ³πŸ’š
πŸ’šπŸƒπŸ’š Salvinorin Chilled Acetone with IPA and Naphtha re-X TEKπŸ’šπŸƒπŸ’š
 
Cheelin
#809 Posted : 1/14/2022 1:58:53 PM

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Nice work.

Of course, another pattern is once again reinforced: you did it right the first time!
 
Cheelin
#810 Posted : 1/14/2022 4:59:50 PM

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Updated post above with pics of the filtered product from the cloudy run of unwashed reused solvent that i salted (β€œgreen crystal” run).

Loveall, if you can spare 15g of powder, you might replicate this with unwashed reused solvent (mine was from a previous run using 15g equiv of citric). Maybe you tell what the white platelike and powdery material is.
 
Loveall
#811 Posted : 1/14/2022 10:34:05 PM

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Looks like calcium citrate. That's what slowly settled out of my unwashed solvent reuse after like a week. If so, it won't dissolve in water well (not absorbed by paste). I believe it is soluble in dilute acids, vinegar should dissolve it after water doesn't if that is what it is.
πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
πŸ’šπŸŒ³πŸ’šDMT salt e-juice HIELO TEKπŸ’šπŸŒ³πŸ’š
πŸ’šπŸƒπŸ’š Salvinorin Chilled Acetone with IPA and Naphtha re-X TEKπŸ’šπŸƒπŸ’š
 
Cheelin
#812 Posted : 1/14/2022 10:43:13 PM

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So since the solvent was unwashed, the calcium came from lime that was in-solution?

If it is calcium citrate, and is not soluble in water, can I just add water to dissolve M, filter out calcium citrate, and recrystallize via evaporation?

Or do you suggest some other separation method?


Wrt to removing this from used solvent prior to reuse, shouldn’t we add an additional step to the washing procedure, to increase the purity of product in the next use of the reused solvent? Or, would it just be better to add a step like above for purifying product after using reused solvent?

If i reuse solvent, want pure needles using best lazy process
 
Loveall
#813 Posted : 1/14/2022 11:36:38 PM

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I think this happened, could be wrong:

Unwashed solvent had citric acid. The citric acid reacted with calcium hydroxide forming calcium citrate at the surface of the paste. Unfortunately, calcium citrate is not very soluble in water, so instead of being absorbed by the watery paste, a bunch of calcium citrate ended up in the solvent as fine particles. This continued until the citric acid was all used up, then without acid present, and assuming enough Calcium Hydroxide was in the paste (there should be plenty to neutralize all the citric acid unless it was scaled down to a small batch?), mescaline was able to freebase and be absorbed by the solvent.

So with reused unwashed paste, there is both calcium citrate fine parties (insoluble in either water or EA) and freebase mescaline in the EA.

The more citric acid in the unwashed solvent the more calcium citrate.

A small amount of hot water should do a good job at separating calcium citrate from mescaline citrate I believe. As long as the citric acid did not overwhelm the calcium hydroxide in the paste, product should be present.
πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
πŸ’šπŸŒ³πŸ’šDMT salt e-juice HIELO TEKπŸ’šπŸŒ³πŸ’š
πŸ’šπŸƒπŸ’š Salvinorin Chilled Acetone with IPA and Naphtha re-X TEKπŸ’šπŸƒπŸ’š
 
Cheelin
#814 Posted : 1/14/2022 11:46:28 PM

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Ok, i’ll test. The run yielded 2.9%, at least 1/3 of that should be in the filter after the hot water wash.


Well that didn’t work. All of it went through the filter. After evap, yielded ~95% of input quantity.

I’m about to say fuck it, with trying to clean up this product pulled with unwashed solvent; let’s just say, if you want to reuse unwashed solvent that was salted with the equivalent of 15g citrate, you’ll get substantial amounts of citracal in your product. Won’t hurt you, but will make dosage more difficult to measure/determine. I’ll try to rehab it later with the 5g cactus powder approach.

Moving on to salting the still cloudy run pulled with unwashed reused 5g citrate equivalent solvent. Expecting similar results but with lower amounts of citracal.


[So tempted to distill this, but will likely require fractional distilling, due to the likelihood of forming ethanol in the process, which then starts going beyond the laziness zone (plus fire hazard), since EA and Ethanol have such close boiling points.]
 
Loveall
#815 Posted : 1/15/2022 5:46:28 PM

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Cheelin wrote:
Ok, i’ll test. The run yielded 2.9%, at least 1/3 of that should be in the filter after the hot water wash.


Well that didn’t work. All of it went through the filter. After evap, yielded ~95% of input quantity.

I’m about to say fuck it, with trying to clean up this product pulled with unwashed solvent; let’s just say, if you want to reuse unwashed solvent that was salted with the equivalent of 15g citrate, you’ll get substantial amounts of citracal in your product. Won’t hurt you, but will make dosage more difficult to measure/determine. I’ll try to rehab it later with the 5g cactus powder approach.

Moving on to salting the still cloudy run pulled with unwashed reused 5g citrate equivalent solvent. Expecting similar results but with lower amounts of citracal.


[So tempted to distill this, but will likely require fractional distilling, due to the likelihood of forming ethanol in the process, which then starts going beyond the laziness zone (plus fire hazard), since EA and Ethanol have such close boiling points.]



Maybe citrical dissolved because monomescaline citrate is slightly acidic. In neutral water it is slightly acidic.

In my case, after a week all the citrical had settled. I decanted and salted.

Washing the solvent with sodium carb water is necessary.
πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
πŸ’šπŸŒ³πŸ’šDMT salt e-juice HIELO TEKπŸ’šπŸŒ³πŸ’š
πŸ’šπŸƒπŸ’š Salvinorin Chilled Acetone with IPA and Naphtha re-X TEKπŸ’šπŸƒπŸ’š
 
Cheelin
#816 Posted : 1/15/2022 6:22:00 PM

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Loveall wrote:
Washing the solvent with sodium carb water is necessary.


Looks like I’ll throughly demonstrate that!

Follow-up report: the suggested β€˜let citrical form, settle, then decant solvent before salting” is an effective mitigation approach. I did not try to measure changes, but substantially less non-needles in the filter…obviously yrmv based on the quality of decant.


Hoping I don’t end up with a similar problem in my next washed solvent run. This time, I’ll wash, settle, then freeze.
 
Loveall
#817 Posted : 1/15/2022 8:34:28 PM

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Cheelin wrote:
Loveall wrote:
Washing the solvent with sodium carb water is necessary.


Looks like I’ll throughly demonstrate that!


Hoping I don’t end up with a similar problem in my next washed solvent run. This time, I’ll wash, settle, then freeze.


I've washed multiple times and reused without issue. As long as all the citric is netutralized in the wash there are no citrical issues.

Instead of freezing after washing with sodium carbonate saturated water, I like to add some sodium carb powder to the EA after pippeting off the bottom water layer. The fresh sodium carb soaks up any remaining water and clarifies the solvent. After the solids settle, I decant and I'm good to go. I no longer freeze, but understand the convinience of it over separating liquid water at room temp. Both approaches seem good to me, and I've done both.
πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
πŸ’šπŸŒ³πŸ’šDMT salt e-juice HIELO TEKπŸ’šπŸŒ³πŸ’š
πŸ’šπŸƒπŸ’š Salvinorin Chilled Acetone with IPA and Naphtha re-X TEKπŸ’šπŸƒπŸ’š
 
Cheelin
#818 Posted : 1/15/2022 10:03:15 PM

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Washing with sodium carbonate right now; i’ll do it both ways, then run against fresh EA.

Also washing the β€˜yellow’ runs, will choose how to finish their treatment (freeze or not), based on next run.

Pic of these in the Jan 9 washing treatment post.
 
Cheelin
#819 Posted : 1/16/2022 5:44:06 AM

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Jan 12 post on small batch pastemaking variables and yield has been updated for final results.
 
Loveall
#820 Posted : 1/16/2022 10:43:57 AM

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Cheelin wrote:
Jan 12 post on small batch pastemaking variables and yield has been updated for final results.


Awesome.


Cheelin wrote:
The only paste that was unusual during solvent pulling was L1: its 1st pull was gummy, all if its subsequent pulls were snotlike.


This is 50% less lime, right?. Was L+ (50% more lime) less snotty during the later pulls? Of yes and I repeat higher yield, this could be a TEK improvement (go from 25g of lime to 40g of lime).

Also, I decreased the paste mixing time to 5 minutes in the TEK. I have also observed that this can be enough time to get to the right consistency. I have also observed that the 10 minutes of rest is not needed, Cheelin's data supports a reduction in paste resting time

We have removed 15 minutes from the TEK. Speed run from raw cactus powder to white xtals could be done in 45 min.

I've tried to cut down on the resting time between during the pulls, but that makes it more likely for water dropplets to end up in the extract. This water is a likely source of goo for beginners, so I would like to keep this rest period. However, the dropplets come out of solution quickly on the extract too. It could be possible to not wait two minutes during each pull (save 12 minutes). Then, let combined extract rest for the two minutes and decant the water drops (they stick to the jar wall mostly). That could save 10 minutes. Save 5 more minutes elsewhere and it may be possible to go from raw powder to white xtals in 30 minutes, just for the fun of it. I think I'll try this soon.

Sonic 30 minute run proposal:
- Make paste: 7 minutes (includes measuring ingredients and 5 minutes of stirring)
- Pulls: 9 minutes (6x1 + time to squeeze out with french press)
- Xtalize: 6 minutes (3 minutes to rest water drops out/decant, 3 minutes shaking hard with citric). While waiting for water dropplets for form, the next jar with citric in it can be prepared along with the filter assembly for the next step - so no time is wasted.
- Recover: 8 minutes to get xtals into filter, wash, dry outside of filter squeezing with paper towels and using a hair drier.

I really want to try this out and set a personal record πŸ˜…. It may take longer to cap the product into 5 or 6 250mg capsules πŸ˜‚
πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
πŸ’šπŸŒ³πŸ’šDMT salt e-juice HIELO TEKπŸ’šπŸŒ³πŸ’š
πŸ’šπŸƒπŸ’š Salvinorin Chilled Acetone with IPA and Naphtha re-X TEKπŸ’šπŸƒπŸ’š
 
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