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Ethyl acetate approach [CIELO] Options
 
Loveall
#881 Posted : 1/23/2022 2:55:59 PM

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igorcarajo wrote:
Loveall wrote:
To verify, you got clouds and no xtals? Cheelin gave you good advice. Keep us posted.

I don’t think there were any clouds.


There should be clouds, it is not a good sign to not have them: I think no clouds indicate no product was pulled. Are you sure you used Ca(OH)2 (and enough of it) and ethyl acetate? How sure are you the cactus is active?
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Cheelin
#882 Posted : 1/23/2022 3:07:02 PM

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Loveall wrote:
Cheelin wrote:
How much sodium carbonate do you use in the 2nd drying?


About 20g per quart of EA (~900g).

Logic is that used EA can be ~3.4% water (or maybe a little more because of plant stuff changing the EA). Coming off saturated wash, it should be ~2% water (a guess based on the NaCl published data). My sodium carb is the monohydrate (arm and hammer super washing soda). The monohydrate (124 g/mol) is stable in room conditions, and can absorb 9 molecules of water (162g/mol).

So in 900g of EA,
~20g could be water
-20g of my washing soda wash can absorb 20*(162/124) ~ 26g of water

Therefore, the 26g washing soda should absorb most/all the water (~20g) in the washed EA.

You can also see clumps of washing soda forming. The clumps should be the decahydrate. People say in lab notes that you want clumps and a little bit of excess powdery drying agent to know the solvent is dry.



Thanks, will use A&H SWS.
 
igorcarajo
#883 Posted : 1/23/2022 4:24:17 PM
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Loveall wrote:
There should be clouds, it is not a good sign to not have them: I think no clouds indicate no product was pulled. Are you sure you used Ca(OH)2 (and enough of it) and ethyl acetate? How sure are you the cactus is active?

It is possible that the cactus has no alkaloids, although I made two extractions (with NaOH, xylene, and HCl) from cacti that I got from the same place and I got a small yield. My calcium hydroxide is a few years old. Could that have something to do with it? My ethyl acetate is indeed ethyl acetate and it was brand new. My citric acid is several years old. Also, the plant material that I dehydrated was just the outer dark green flesh. I didn’t use the waxy skin, spines, or inner white flesh. But I don’t think that would be a problem, right? I’ve read that the dark green outer flesh is where most of the alkaloids are.
 
Loveall
#884 Posted : 1/23/2022 4:53:31 PM

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igorcarajo wrote:
Loveall wrote:
There should be clouds, it is not a good sign to not have them: I think no clouds indicate no product was pulled. Are you sure you used Ca(OH)2 (and enough of it) and ethyl acetate? How sure are you the cactus is active?

It is possible that the cactus has no alkaloids, although I made two extractions (with NaOH, xylene, and HCl) from cacti that I got from the same place and I got a small yield. My calcium hydroxide is a few years old. Could that have something to do with it? My ethyl acetate is indeed ethyl acetate and it was brand new. My citric acid is several years old. Also, the plant material that I dehydrated was just the outer dark green flesh. I didn’t use the waxy skin, spines, or inner white flesh. But I don’t think that would be a problem, right? I’ve read that the dark green outer flesh is where most of the alkaloids are.


Yes, that part of the plant is great to use. Ca(OH)2 is OK to use when old. How much was the small yield from older runs? Anything showing up in the jar after the last couple days?
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
 
igorcarajo
#885 Posted : 1/23/2022 5:07:46 PM
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Loveall wrote:
Yes, that part of the plant is great to use. Ca(OH)2 is OK to use when old. How much was the small yield from older runs?

From a 1 kg piece of cactus I got 550 mg of tan mescaline HCl.

Loveall wrote:
Anything showing up in the jar after the last couple days?

It hasn’t even been 24 hours since I salted the ethyl acetate. There seems to be a small amount of something syrupy at the bottom that wasn’t there before. I’m not sure what that would be. I’m pretty sure it’s not water because water would flow freely, not β€œcrawl”.
 
Loveall
#886 Posted : 1/23/2022 5:26:41 PM

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igorcarajo wrote:
Loveall wrote:
Yes, that part of the plant is great to use. Ca(OH)2 is OK to use when old. How much was the small yield from older runs?

From a 1 kg piece of cactus I got 550 mg of tan mescaline HCl.

Loveall wrote:
Anything showing up in the jar after the last couple days?

It hasn’t even been 24 hours since I salted the ethyl acetate. There seems to be a small amount of something syrupy at the bottom that wasn’t there before. I’m not sure what that would be. I’m pretty sure it’s not water because water would flow freely, not β€œcrawl”.


Sounds like a normal yield from the previous run, assuming g 1Kg fresh is ~50g dry, and 1% yield for dry powder.

The syrup sounds like what we call goo. Some people get that, especially on their first run. Not sure why, could be from too much water in your EA initially (or from something else). You can try to add more EA to the xtalization jar (effectively lowering the water content %) and swirl the goo back into solution see if crashes back as xtals. If you wait long enough to make sure the goo is done crashing you can also decant most of the EA, then add some fresh EA and swirl (this will reduce the water % content more). This assumes your fresh EA is dry (usually the case).
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
#887 Posted : 1/23/2022 6:20:29 PM

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Update re small sample runs:

Just passing 36hrs since salting, half-way there. Things are going well, was hoping to show series of same-shots during crystallization, but floating and wall crystals have fallen to bottom, making comparison shots difficult, with a camera that already does poorly with macro-photog pics. Attached is a pic of the 5g cactus powder pull, i’ll try to post 72hr shots of each tube in the original post, just before I filter.

This run is done with what I call β€œreverse dilution” where each tube has roughly the same volume of solvent, but different amounts of β€œextract”, so the pulls from the 1g cactus powder has a higher dilution, lower extract concentration than the 5g tube. Crystallization theory says that lower concentration solutions generally produce smaller crystals, and that is what is happening: where the crystals get progressively larger going from the pinhead-sized 1g crystals up to the 3/8” crystals in the 5g tube.

Hoping to get 1.1% yields in all these tubes, but will be satisfied if I can get a linear yield trend for this ingredient recipe.
Cheelin attached the following image(s):
Salting +36 hrs.jpg (51kb) downloaded 111 time(s).
 
Cheelin
#888 Posted : 1/23/2022 6:39:41 PM

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Loveall wrote:
igorcarajo wrote:
Loveall wrote:
Yes, that part of the plant is great to use. Ca(OH)2 is OK to use when old. How much was the small yield from older runs?

From a 1 kg piece of cactus I got 550 mg of tan mescaline HCl.

Loveall wrote:
Anything showing up in the jar after the last couple days?

It hasn’t even been 24 hours since I salted the ethyl acetate. There seems to be a small amount of something syrupy at the bottom that wasn’t there before. I’m not sure what that would be. I’m pretty sure it’s not water because water would flow freely, not β€œcrawl”.


Sounds like a normal yield from the previous run, assuming g 1Kg fresh is ~50g dry, and 1% yield for dry powder.

The syrup sounds like what we call goo. Some people get that, especially on their first run. Not sure why, could be from too much water in your EA initially (or from something else). You can try to add more EA to the xtalization jar (effectively lowering the water content %) and swirl the goo back into solution see if crashes back as xtals. If you wait long enough to make sure the goo is done crashing you can also decant most of the EA, then add some fresh EA and swirl (this will reduce the water % content more). This assumes your fresh EA is dry (usually the case).



So, Loveall, after the goo dissolving work you mention, what do you think about then re-salting?

This story sounds familiar, reminiscent of your near-neutral-pH run that produced what you thought might be a higher potency form of M citrate.

Maybe the paste was somehow overlimed, and just needed more acid to get it to the critical point.
 
Cheelin
#889 Posted : 1/23/2022 6:54:08 PM

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Igor, do you have pH strips? If so, can you test the pH of the solution before diluting as Loveall suggested?
 
Loveall
#890 Posted : 1/23/2022 7:21:53 PM

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Quote:
So, Loveall, after the goo dissolving work you mention, what do you think about then re-salting?

This story sounds familiar, reminiscent of your near-neutral-pH run that produced what you thought might be a higher potency form of M citrate.

Maybe the paste was somehow overlimed, and just needed more acid to get it to the critical point.


Well, I don't know what the issue is but here is my guess.

I think the goo igorcarajo is seeing may be mescaline citrate + water. If so, the mescaline is already in salt form and more citric is not needed. I don't think it is reminiscent of the near neutral goo since excess citric was used. By adding EA and swirling the goo, the hope is that water is absorbed by the dryer EA. The "desiccated" goo may become xtals/powder.

I don't think overliming the paste changes the need for citric amount. The lime is bound in the paste and doesn't make it into the EA. Only neutral (free base) cactus stuff makes it to the EA*.

*The exception to this was when citracal formed because of using unwhased solvent. I think it can be avoided by washing the solvent well.
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
#891 Posted : 1/23/2022 7:40:55 PM

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Loveall wrote:
Quote:
So, Loveall, after the goo dissolving work you mention, what do you think about then re-salting?

This story sounds familiar, reminiscent of your near-neutral-pH run that produced what you thought might be a higher potency form of M citrate.

Maybe the paste was somehow overlimed, and just needed more acid to get it to the critical point.


Well, I don't know what the issue is but here is my guess.

I think the goo igorcarajo is seeing may be mescaline citrate + water. If so, the mescaline is already in salt form and more citric is not needed. I don't think it is reminiscent of the near neutral goo since excess citric was used. By adding EA and swirling the goo, the hope is that water is absorbed by the dryer EA. The "dessecated" goo may become xtals/powder.

I don't think overliming the paste changes the need for citric amount. The lime is bound in the paste and doesn't make it into the EA. Only neutral (free base) cactus stuff makes it to the EA*.

*The exception to this was when citracal formed because of using unwhased solvent. I think it can be avoided by washing the solvent well.


I’ll apologize for getting the citrate addition backwards on that run. And, i’ll defer to your moisture explanation, partly cuz my time is more valuable atm than digging into why goo forms. However, i believe that pH maybe playing a role here.
 
igorcarajo
#892 Posted : 1/23/2022 8:02:22 PM
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Cheelin wrote:
Igor, do you have pH strips? If so, can you test the pH of the solution before diluting as Loveall suggested?

According to my crappy pH strip, it’s 2.
 
Cheelin
#893 Posted : 1/23/2022 8:19:51 PM

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igorcarajo wrote:
Cheelin wrote:
Igor, do you have pH strips? If so, can you test the pH of the solution before diluting as Loveall suggested?

According to my crappy pH strip, it’s 2.



Ime, that is extreme. Do you have any ides what pre-salting pH was.

Here is my pH experience: fresh EA 5ish, pulled solvent 6ish, salted solvent 4ish.
 
Loveall
#894 Posted : 1/23/2022 9:03:13 PM

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Cheelin wrote:
igorcarajo wrote:
Cheelin wrote:
Igor, do you have pH strips? If so, can you test the pH of the solution before diluting as Loveall suggested?

According to my crappy pH strip, it’s 2.



Ime, that is extreme. Do you have any ides what pre-salting pH was.

Here is my pH experience: fresh EA 5ish, pulled solvent 6ish, salted solvent 4ish.


I wonder if the extreme pH could be a sign of excess water. If fresh EA is added to absorb water activity and pH goes up and xtals form it would be very interesting.
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
 
igorcarajo
#895 Posted : 1/23/2022 9:35:11 PM
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Would the ethyl acetate from the hardware store have water in it? If so, would it be desirable to somehow dry it?
 
Loveall
#896 Posted : 1/23/2022 10:23:38 PM

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igorcarajo wrote:
Would the ethyl acetate from the hardware store have water in it? If so, would it be desirable to somehow dry it?


I think it doesn't, but not 100% sure. If you have arm and hammer washing soda that will dry it. CaCl2 also dries it. MgSO4, but that is a pain to filter (for me at least).

I would just use it straight from the can.

I'm running a small test: Dissolving citric in EA fr the can and measuring pH. Them will add water to see if it drops.
πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
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πŸ’šπŸƒπŸ’š Salvinorin Chilled Acetone with IPA and Naphtha re-X TEKπŸ’šπŸƒπŸ’š
 
Cheelin
#897 Posted : 1/23/2022 10:47:51 PM

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Been doing multiple runs of 1g cactus powder, focused on a few recipe & process changes, as well as alternative paste and pulling equip/techniques. Will be salting soon, will have results mid-week.

Overall, there is an association/correlation between the darkness of pulls and crystal yield. All of these runs today are darker & just as clear as the 1g run that is currently crystallizing in the recent 5-run trial, so hopefully some progress being made.
 
Cheelin
#898 Posted : 1/24/2022 7:34:01 AM

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Loveall wrote:
I'm running a small test: Dissolving citric in EA fr the can and measuring pH. Them will add water to see if it drops.


Citric didn’t dissolve well in fresh EA, but I got:
5 pH EA -> 4 pH EA + citrate -> 2 pH EA + citrate + water

But, the pathway is missing: EA + (-OH)
 
Loveall
#899 Posted : 1/24/2022 9:21:12 AM

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Cheelin wrote:
Loveall wrote:
I'm running a small test: Dissolving citric in EA fr the can and measuring pH. Them will add water to see if it drops.


Citric didn’t dissolve well in fresh EA, but I got:
5 pH EA -> 4 pH EA + citrate -> 2 pH EA + citrate + water

But, the pathway is missing: EA + (-OH)


Yeah, citric in dry EA takes a while to dissolve, but it should eventually. Mine is still dissolving for the test.

How much water did you add?

Doesn't this mean that more water in EA will give lower pH on the strip? I don't understand what do you mean by "the pathway is missing: EA + (-OH)"?

What I think happens (could be wrong) is that in EA, citric acid dissolves without much depronation. As more water is present it can depronate more.
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
#900 Posted : 1/24/2022 9:25:50 AM

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Cheelin wrote:
Been doing multiple runs of 1g cactus powder, focused on a few recipe & process changes, as well as alternative paste and pulling equip/techniques. Will be salting soon, will have results mid-week.

Overall, there is an association/correlation between the darkness of pulls and crystal yield. All of these runs today are darker & just as clear as the 1g run that is currently crystallizing in the recent 5-run trial, so hopefully some progress being made.


This is great, awesome way to optimize. Looking forward to the results.
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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