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Ethyl acetate approach [CIELO] Options
 
Loveall
#941 Posted : 1/31/2022 12:06:04 AM

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Good luck orchidist. Hope those clouds become Xtals for you.
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
 

STS is a community for people interested in growing, preserving and researching botanical species, particularly those with remarkable therapeutic and/or psychoactive properties.
 
orchidist
#942 Posted : 1/31/2022 12:12:15 AM

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Cheelin wrote:
6 - 12 hrs after salting, crystals should start forming on your container walls, should be viewable by shining a flashlight through the solution.


Unfortunately only clouds still, I'm pretty sure due to the fact that I pretty generously overpoured the solvent for my first couple pulls. Perhaps it's too dilute? My french press is metal and pretty large, so it was tough to see what was going on, and the plunger doesn't go far enough to compress the quantity of paste I had. Solvent was crystal clear at the time I added the citric acid.

I'm thinking for this run I'm going to get out the magnetic stirrer and add the amount for quick crystallization, see if I can recover from the mistake. Going to find a more suitable press for the next attempt.
 
Loveall
#943 Posted : 1/31/2022 12:42:04 AM

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orchidist wrote:
Cheelin wrote:
6 - 12 hrs after salting, crystals should start forming on your container walls, should be viewable by shining a flashlight through the solution.


Unfortunately only clouds still, I'm pretty sure due to the fact that I pretty generously overpoured the solvent for my first couple pulls. Perhaps it's too dilute? My french press is metal and pretty large, so it was tough to see what was going on, and the plunger doesn't go far enough to compress the quantity of paste I had. Solvent was crystal clear at the time I added the citric acid.

I'm thinking for this run I'm going to get out the magnetic stirrer and add the amount for quick crystallization, see if I can recover from the mistake. Going to find a more suitable press for the next attempt.


How long have you been waiting? Give it time and patience, the clouds will settle.
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
#944 Posted : 1/31/2022 1:09:37 AM

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Loveall wrote:
Cheelin wrote:
So, if I used the correct numbers and multiplied them correctly, the HCL yield equivalents were: 37mg for citrate, tartrate, & fumerate; and 28mg for malate. May have to slightly downgrade my ethyl acetate + citrate β€œsuperiority” comment. Very nice consistency of M extraction, for Ethyl Acetate solvent, though!


Malate also comes in at ~ 37mg of HCl (41*.89 ~ 36.5mg).

It's cool how the mass yields can confirm the salt forms.

Citric and fumaric xtalized faster. Citric is fluffier and easier to handle. It has more of a process window since it is more soluble in Fumerate ( more robust to oversalting). Citric is still my favorite.



I mistakenly multiplied by 0.68, thanks for the correction. I’m stickin with citrate!
 
Cheelin
#945 Posted : 1/31/2022 1:23:55 AM

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orchidist wrote:
Cheelin wrote:
6 - 12 hrs after salting, crystals should start forming on your container walls, should be viewable by shining a flashlight through the solution.


Unfortunately only clouds still, I'm pretty sure due to the fact that I pretty generously overpoured the solvent for my first couple pulls. Perhaps it's too dilute? My french press is metal and pretty large, so it was tough to see what was going on, and the plunger doesn't go far enough to compress the quantity of paste I had. Solvent was crystal clear at the time I added the citric acid.

I'm thinking for this run I'm going to get out the magnetic stirrer and add the amount for quick crystallization, see if I can recover from the mistake. Going to find a more suitable press for the next attempt.



If it wasn’t cloudy before you added citric acid, the subsequent cloudiness generally means you’re on the right path. The larger volume will reduce crystal size, so at this point you may not see more than what looks like specks of dust on the glass. My advice is to hold your horses until, at least, the 24 hr mark.

Most presses, the plunger can be unscrewed from the strainer, then the strainer can be pressed against the paste to get some additional liquid out. I don't advise doing this until the last pull, so that you don’t get fine sediment going through your filter, but last one can get a lot out.

I have several different size presses, but a 4-cupper can do the job on 15g, it’s what i just used for the five 15g runs I did earlier today. It isn’t critical to squeeze the paste, especially when your learning goal is not yield, but should be getting the proper end product. A 2-cupper, though, works very well with 15g runs, once you nail the tek.

Hang in there, you’ll nail it.


[Not to make you feel bad, but to give a future reference point, my 5 jars were salted 3 hours ago, all jars covered with 3/8” snowflakes]
 
orchidist
#946 Posted : 1/31/2022 2:30:30 AM

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It was getting close to 24 hours at the time I threw in more acid. Unfortunately, I did it before seeing the replies, it cleared up, but yielded the mysterious brown goo. Perhaps I was over eager to call my pulls crystal clear before proceeding. If so, whoops.

I will let this one continue to sit, but I'm thinking this is likely to be one for the learning curve. I have enough cactus flour to do a bunch of runs, so I'll take my press apart and try again some time this week.

cheelin wrote:
Hang in there, you’ll nail it.


[Not to make you feel bad, but to give a future reference point, my 5 jars were salted 3 hours ago, all jars covered with 3/8” snowflakes]


I have no intention of giving up! And, no insult taken. It's very much like my other hobby, I failed over and over with certain species while others in the community had thriving examples of them. Learned quickly to use it as motivation. Kept trying and eventually had my own. Luckily with this tek, the iterations are much, much faster!
 
Cheelin
#947 Posted : 1/31/2022 2:37:40 AM

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That’s the attitude, get back on the bike.

Dry that goo out and save it for doing a 5g recovery run after you nail the tek (method a few pages back).

Looking forward to your success.
 
Loveall
#948 Posted : 1/31/2022 8:26:15 AM

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orchidist, on your next attempt, can you split your pulls in two and only salt one side? If you get goo again I'd like you to put the other side in the fridge for 24 hours and see if any dropplets or junk crashes.

Also, on the result you have: can you decant and swirl the goo you already have in fresh EA? Want to see if that desiccates the goo. Keep an eye on the decanted solvent for any new precipitation there.
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
#949 Posted : 1/31/2022 1:40:12 PM

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Loveall wrote:
orchidist, on your next attempt, can you split your pulls in two and only salt one side? If you get goo again I'd like you to put the other side in the fridge for 24 hours and see if any dropplets or junk crashes.

Also, on the result you have: can you decant and swirl the goo you already have in fresh EA? Want to see if that desiccates the goo. Keep an eye on the decanted solvent for any new precipitation there.



You’re tempting me.

Time to get serious about recreating this somewhat common rookie mistake?

Perhaps a small run, taking 1/4 to salting, 1/4 adding some powder (for cloudiness) then salting, adding a few mLs of water to the remaining combined pulls, splitting into 2 jars: one to be salted; the other to be frozen, strained/filtered, then salted. Work backwards from there.

Where else could there be fuckups that lead to goo?

May force me to do the too much/too little lime and citrate runs, too.

I still attribute this to poor technique, likely due to overconfidence when doing this deceptively simple tek, especially by people who think past chem tinkering inoculates them somehow (like me). But, in my case, it happened after salting.
 
orchidist
#950 Posted : 1/31/2022 11:25:43 PM

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loveall wrote:
orchidist, on your next attempt, can you split your pulls in two and only salt one side? If you get goo again I'd like you to put the other side in the fridge for 24 hours and see if any dropplets or junk crashes.

Also, on the result you have: can you decant and swirl the goo you already have in fresh EA? Want to see if that desiccates the goo. Keep an eye on the decanted solvent for any new precipitation there.


Will do! I'll decant and set it aside later tonight, I am thinking I might take half the solvent and super fine powder from this first attempt, wash with sodium carbonate, separate it, allow some solvent to evaporate, and then retry the crystallization. Thoughts?

cheelin wrote:
I still attribute this to poor technique, likely due to overconfidence when doing this deceptively simple tek, especially by people who think past chem tinkering inoculates them somehow (like me). But, in my case, it happened after salting.


That is EXACTLY how I felt going into this Laughing
 
Cheelin
#951 Posted : 1/31/2022 11:33:53 PM

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Lol πŸ‘πŸ»
 
Cheelin
#952 Posted : 2/1/2022 3:48:30 AM

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Let’s see if I can make goo!

Perhaps someone can give me their method. In the meantime:

Cactus powder - 20g
Pickling Lime - 5g
Distilled Water - 60ml
8 minute stir
10 minute rest

6 x 3 min pulls
1st pull 47mL fresh ethyl acetate
Pulls 2-6 28mL/pull fresh ethyl acetate

Combined pulls split 4 ways evenly, approx 43ml per jar

Treatments:
T1 - salted with 0.25g citric acid, passively crystallize (pc) 48 hrs
T2 - added 0.4g cactus powder, shook vigorously, salted with 0.25g citric acid, pc 48 hrs
T3 - added 1mL distilled water, shook vigorously, salted with 0.25g citric acid, pc 48 hrs
T4 - added 1mL distilled water, shook vigorously, placed in freezer for 24 hrs then strained/filtered, salted with 0.25g citric acid, pc 48 hrs

1/31, After 6 hours:
T1 - clear solvent, crystals floating and on walls & bottom, as usual
T2 - lower 1/4 sediment, middle 1/2 cloudy solvent, top 1/4 clear
T3 - clear solvent, a few tiny crystals on bottom
T4 - (not yet salted) lower 1/4 white ?crystal/ice? layer, middle 1/2 clear solvent, top 1/4 solvent and ice needles
No signs of goo in any jar

2/1:
T4 was strained and filtered after 24 hrs in freezer; 3.6g of ice in strainer, approx 1 - 1.5g ice in filter; no sediment/particles large enough to be trapped in filter; all contents returned to jar, solvent clear; salted with 0.25g citric acid, started 48 hr pc.

Seems that substantial water, beyond the added 1mL, was present in solution, this 3.5 to 4g of water represents about 8-9% of total solution volume, which must have originated in the paste and solvent. To approximate the amount of water in the solvent, 75ml of solvent was placed in freezer to be filtered and weighed after 24 hrs.

Per Loveall’s request, added 1/2mL distilled water to T3, will continue to add same amount every 24 hrs, for next few days.

2/2:
Added another 1/2mL distilled water to T3, bringing total added water to 2.0 ml. Jar now has more than 1/8” water layer below solvent.
Koi
No apparent goo in any of the jars. Will let them go another 24 hours, then filter.

75mL of fresh solvent that was in freezer for 24 hrs did not have any ice layers or floating shards.

2/3:
Filtered all 4 jars, yields: T1 0.076g 1.5%, T2 0.193g, T3 0.033, T4 0.060. I wouldn’t pay too much attention to the specific weights, from a yield standpoint, this trial is about quality not yield. However, since these all represent roughly 25% of a 20g cactus powder run, and the magnitude differences are large, an explanation is useful:

T1 is the control, which other treatments should be compared with;

T2 is the run that 0.4g β€œsediment” was added to, the resulting filtrate was a combination of mostly sediment and some needles, the filtrate was dried and water washed to separate the M, then evap’d residue was scraped, residue contains very fine sediment plus a large proportion of sparkly crystals, I estimate that at least 60% of the yield is very fine cactus powder sediment;

T3 had multiple water additions, M citrate is highly water soluble, and this treatment appears that a substantial portion of its frebase M had not crystallized by the time it was filtered, thus losing over half of its potential yield in the spent solvent pour;

T4 was also water washed (half of T3), but it looks like most of its crystallization occurred normally, so that when filtered, almost all of the M citrate was solid and thus was collected in the filter.

None of the jars contained anything describable as goo. T1 and T4 had the normal needles; T2 had mixed sediment and crystals that were expected for the given treatment; T3, treated initially like T4 with 1 mL distilled water, then two additional 1/2 mL doses of distilled water did have unusual crystal development - basically 20-30 white clumps of tiny crystals.

My conclusions:
1. Sediment or water, in the combined pulls, do not on their own cause goo formation;
2. Combined pulls should still be completely free of sediment and water droplets/layers, in order to minimize contamination & yield losses.


Cheelin attached the following image(s):
Sediment & Water.jpg (97kb) downloaded 68 time(s).
 
orchidist
#953 Posted : 2/1/2022 4:02:01 AM

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I transferred the goo to fresh ethyl acetate. It does appear to have dessicated, it's brittle. I was able to crush it with a stir rod.

I noticed the color of the solution changed from emerald to olive when the goo formed. I can't find much info, but it could be chlorophyll losing the manganese ion, converting to phaeophytin. Wonder if that has anything to do with goo formation. A source or two say that reaction occurs in acidic conditions. Come to think of it, when it formed, I'm pretty sure it coalesced around undissolved citric acid at the edge of the beaker where the flow was not sufficient to keep the crystals moving.
 
orchidist
#954 Posted : 2/1/2022 4:10:33 AM

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cheelin wrote:

T1 - salted with 0.25g citric acid, passively crystallize (pc) 48 hrs
T2 - added 0.4g cactus powder, shook vigorously, salted with 0.25g citric acid, pc 48 hrs
T3 - added 1mL distilled water, shook vigorously, salted with 0.25g citric acid, pc 48 hrs
T4 - added 1mL distilled water, shook vigorously, placed in freezer for 24 hrs then strained/filtered, salted with 0.25g citric acid, pc 48 hrs


I think using the citric acid rate for quick-crystallization might be worth investigating with excess water.
 
Cheelin
#955 Posted : 2/1/2022 4:12:34 AM

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orchidist wrote:
I transferred the goo to fresh ethyl acetate. It does appear to have dessicated, it's brittle. I was able to crush it with a stir rod.

I noticed the color of the solution changed from emerald to olive when the goo formed. I can't find much info, but it could be chlorophyll losing the manganese ion, converting to phaeophytin. Wonder if that has anything to do with goo formation. A source or two say that reaction occurs in acidic conditions. Come to think of it, when it formed, I'm pretty sure it coalesced around undissolved citric acid at the edge of the beaker where the flow was not sufficient to keep the crystals moving.


Regardless of goo formation, ime, solvent always changes hue by time salting cloudiness clears. I can’t out the possibility that the reaction behind the hue change could, under certain conditions, have some effect on goo formation, though.
 
Cheelin
#956 Posted : 2/1/2022 4:22:43 AM

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orchidist wrote:
cheelin wrote:

T1 - salted with 0.25g citric acid, passively crystallize (pc) 48 hrs
T2 - added 0.4g cactus powder, shook vigorously, salted with 0.25g citric acid, pc 48 hrs
T3 - added 1mL distilled water, shook vigorously, salted with 0.25g citric acid, pc 48 hrs
T4 - added 1mL distilled water, shook vigorously, placed in freezer for 24 hrs then strained/filtered, salted with 0.25g citric acid, pc 48 hrs


I think using the citric acid rate for quick-crystallization might be worth investigating with excess water.


If I don’t get goo from this first set of treatments, I will move on to absence/excess lime and citric…where I personally believe the issue arises.

I find T4 bottom white layer to be an unanticipated interesting situation. Can’t wait to see what that is. I only added 1mL of water, and solvent has not yet been salted. Seems it can only be ice (from solvent?), lime, or freebase M.
 
Loveall
#957 Posted : 2/1/2022 3:03:12 PM

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T4 - Could be plant proteins that precipitate when cold. I think I've come across this before. They can show up in the fridge too. Decanting them (or not) does not seem to affect the standard process: Free base mescaline does not seem to crash with cold, it is a lot more sensitive to salting.

For T3, What do you think of adding water ~0.5ml at a time see if you can get goo to show up eventually?
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
#958 Posted : 2/1/2022 3:08:20 PM

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orchidist wrote:
I transferred the goo to fresh ethyl acetate. It does appear to have dessicated, it's brittle. I was able to crush it with a stir rod.


This is interesting and points to water being a possible issue originally I think. Does it feel xtaline after decanting/drying? I wonder what would happened if you dissolves this dessicated product in minimal hot water (~2ml) and then combined that with EA (~100ml or so).

orchidist wrote:
Will do! I'll decant and set it aside later tonight, I am thinking I might take half the solvent and super fine powder from this first attempt, wash with sodium carbonate, separate it, allow some solvent to evaporate, and then retry the crystallization. Thoughts?


Sorry which super fine powder?

I think it makes sense to split your next pull. If straight forward salting doesn't work, drying with sodium carbonate before salting the next split makes sense. This is a very standard lab practice, we just skip it because we found it not necessary - except that we have this goo issue some folks encounter.

I recently did just this, spit a pull and dried one side with sodium carb. No issues on either side, Xatals in both. The sodium carb side would be more robust to excess water issues though, if that is a thing.
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
#959 Posted : 2/1/2022 7:45:23 PM

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Loveall wrote:
T4 - Could be plant proteins that precipitate when cold. I think I've come across this before. They can show up in the fridge too. Decanting them (or not) does not seem to affect the standard process: Free base mescaline does not seem to crash with cold, it is a lot more sensitive to salting.

2/1:
For T3, What do you think of adding water ~0.5ml at a time see if you can get goo to show up eventually?


T4 turned out to be ice, see original post: https://www.dmt-nexus.me...p;m=1136784#post1136784

Will adjust T3 as you requested.

Updated the washing post for 48 hr filtering, will filter once more: https://www.dmt-nexus.me...p;m=1136657#post1136657


2/2: Both posts above updated today.
 
Cheelin
#960 Posted : 2/2/2022 5:45:39 PM

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Moving on to next goo re-creation experiment. This one will test too litlle/much of pickling lime and citric acid, also 250ppm tap water will be used instead of distilled water.

Two 30g paste batches, one with 10% of scaled pickling lime, the other with double the scaled amount; each batch pulled as normal with scaled amounts of fresh EA; combined pulls from each batch split 6 ways: 3 to be actively crystallized, 3 to be passively crystallized; three levels of citric acid: 10% of scaled 5g dosage, scaled 5g dosage, 400% of scaled 5g dosage.

Specifically:
Cactus powder - 30g/ batch
Pickling lime - Batch A 0.75g, Batch B 15g
250ppm tap 🚿 : 90mL per batch

8 minute stir, fold, mash
10 minute rest

6 x 3 minute standard pulls; fresh EA: 1st pull 71mL, pulls 2-6 43mL; each pull coffee filtered, combined pulls rested 1hr, then split into 6 equal portions per batch

For each batch, 3 portions will be actively magnetic stirred (sub-batch 1) for 10 minutes, then rested for 24hrs before filtering; 3 portions will be passively crystallized (sub-batch 0) for 48 hrs before filtering. Each 3-portion sub-batch will be individually dosed with either 0.03g (X), 0.25g (Y), or 1.00g (Z).

2/2:
Processing Observations:
Batch A - paste became sticky pudding-/guacamole-like during mixing, stayed that way until becoming sticky snot-like first to last pulls; first 2 pulls very light, almost yellow hue, darkening on pull 3, combined pulls somewhat lighter than normal; solvent recovery about 70%; combined pulls pH 9-10.

Batch B - paste became somewhat drier and more crumbly than my usual cookie dough/playdough during mixing, stayed that way until pulling, when it eventually became somewhat more runny and finer grained than my normal applesauce consistency by last pull; hue substantially darker than normal for first 4 pulls, then lightening in 5th & 6th pulls, combined pulls substantially darker than normal; solvent recovery about 80%; combined pulls pH 9-10.

Salting proceeded as normal: all active jars clouded during magnetic stirring and precipitated shortly afterwards; all passive jars clouded, and later were crystallizing as normal.

2/3: The six active crystallization treatments, for both levels of lime and three levels of citrate, have been filtered. The jars will be washed and evap’d, with yields (fwiw) posted later. All jars produced white powder product as is normal for this crystallization method. Nothing that could be called β€œgoo” was produced.

2/5: Got delayed. The passive crystallization jars were filtered today, none had goo.

Also, weighed all filtrate samples, as follows:
Low Lime. Active Crystallization: low citrate 0.038g, standard citrate 0.040g, high citrate 0.046g
Low Lime, Passive Crystallization: low citrate 0.071, standard citrate 0.068g, high citrate ?0.029g?

High Lime, Active Crystallization: low citrate 0.048g, standard citrate 0.042g, high citrate 0.038
High Lime, Passive Crystallization: low citrate 0.070g, standard citrate 0.069g, high citrate 0.071g

2/6: Jar washes evaporated, final yields:

Low Lime. Active Crystallization: low citrate 0.045g, standard citrate 0.047g, high citrate 0.047g
Low Lime, Passive Crystallization: low citrate 0.077g, standard citrate 0.0.076g, high citrate ?0.043g?

High Lime, Active Crystallization: low citrate 0.052g, standard citrate 0.051g, high citrate 0.047g
High Lime, Passive Crystallization: low citrate 0.076g, standard citrate 0.070g, high citrate 0.087g


Conclusions:
Goo production is not simply due to too little/much of lime or citric acid.
Low Lime adversely impacts yield, high lime may have marginal positive impact on yield, if any.
Citrate level above 0.6% of cactus powder weight has little to no effect on yield.
 
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