TEK Ethyl acetate approach [CIELO]

[Cheelin]

Thanks Loveall, my pleasure.

The data is incomplete, but i do not expect the warm water wash to significantly impact the overall trends, but we’ll see.

FWIW, I took a measurement of surface temp of jar lid in freezer w ir gun, 0 F. Glass and clear liquid are not best for ir gun measurements, tool lazy to use liquid thermometer at the time.

Your process and mine, for chilling, vary somewhat, so maybe that explains at least part of difference. I do not add any pressure until last pull; and i make no attempt to maintain out-of-fridge/freezer temp, except to work quickly. Additionally, as indicated earlier, my refrigerated paste comes out like hard playdough, requiring chopping up before starting pulls.

I suspect that chilled yields are lower primarily because the material spends insufficient time in solution before pulling. Partly intentionally for goal that you guys intended, and partly, because my “paste” gets so hard.

I encourage others to replicate my methodology, so that we can identify process differences vs operator error. Not saying my process or ability is the best.

Bottom line, for me, i get acceptable yields , but more importantly, for me, pure crystals in my filter, hopefully little/no gunk in dish (still to be determined).

Cheers!

 

[_Trip_]

Great write up Cheelin.

I've done both chilled and room temp pulls. I haven't noticed a massive difference in yields (I'll have to take more note of it next runs). But what I have noticed is the EA is 'dirtier' when using room temp and crystals come out slightly more tan-yellow when doing room temp pulls.

I might do a side by side comparison next run.

 

[Loveall]

Thanks Loveall, my pleasure.

The data is incomplete, but i do not expect the warm water wash to significantly impact the overall trends, but we’ll see.

FWIW, I took a measurement of surface temp of jar lid in freezer w ir gun, 0 F. Glass and clear liquid are not best for ir gun measurements, tool lazy to use liquid thermometer at the time.

Your process and mine, for chilling, vary somewhat, so maybe that explains at least part of difference. I do not add any pressure until last pull; and i make no attempt to maintain out-of-fridge/freezer temp, except to work quickly. Additionally, as indicated earlier, my refrigerated paste comes out like hard playdough, requiring chopping up before starting pulls.

I suspect that chilled yields are lower primarily because the material spends insufficient time in solution before pulling. Partly intentionally for goal that you guys intended, and partly, because my “paste” gets so hard.

I encourage others to replicate my methodology, so that we can identify process differences vs operator error. Not saying my process or ability is the best.

Bottom line, for me, i get acceptable yields , but more importantly, for me, pure crystals in my filter, hopefully little/no gunk in dish (still to be determined).

Cheers!

Ah, good point, a colder fridge (cold enough to change the paste consistency) could very well explain the difference.

 

[Cheelin]

Thanks _Trip_.

My pics aren’t the greatest, but the std process (@ ambient temp) definitely makes solvent the darkest, The solvents in the other three variations are all lighter, with subtle diffs between them.

At some point, i’ll do a comparison of the process using treated dark vs treated light reused solvent, to see if having a lighter colored solvent makes a difference in yield, crystal appearance, or number of solvent uses. If not, seems to me that there’s really no need to do the other variations, since filtrate quality of original runs appear similar, and I don’t see much yield improvement occurring with the additional treatment, with my results or those of others here.

My work so far has strengthened my opinion that not getting clean crystals out of the process has more to do with poor powder grind, poor mixing, poor pulls, or poor filtering. In other words, poor technique rather than the need for variations from standard process is more likely to be the cause of quality issues.

 

[Cheelin]

Loveall, I will definitely test longer chilled pulls at some point, probably a side-by-side using 1min stir + 2 min rest: ambient vs chilled temp.

 

[_Trip_]

My pics aren’t the greatest, but the std process (@ ambient temp) definitely makes solvent the darkest, The solvents in the other three variations are all lighter, with subtle diffs between them.

Yeah i believe part of the reason Loveall came up and experimented with cold pulls was due to EA reuse and cleaner crystals.

Microwaving also helps EA reuse.

 

[Loveall]

My work so far has strengthened my opinion that not getting clean crystals out of the process has more to do with poor powder grind, poor mixing, poor pulls, or poor filtering. In other words, poor technique rather than the need for variations from standard process is more likely to be the cause of quality issues.

I got the same results (xtals with all combos). However, the added options (microwave, chilled pulls) gave larger xtals (slow acid diffusion). Since source cacti can vary a lot, maybe there are situations when the adding the "cleaner" options is needed (even with perfect technique).

Time will tell. Maybe with good technique, E. pachanoi, E. lageniformis, E. scopulicola, E. peruviana all give xtals with no added options. Your work is a data point in that direction (along with _Trip_, shroombee, and others). If folks like highlightprotein end up with xtals and not goo that will also be telling.

 

[Cheelin]

_Trip_, yep, solvent reuse is important, but i will focus on that in the future.

So, far what i am seeing is that microwaving and chilling do not improve crystal appearance (naked eye) or yield. but improved technique does.

I’m willing to change my opinion, though, if i see sufficient evidence to the contrary.

 

[_Trip_]

That's interesting because I didn't quite find that.


It might be worth taking a poll to see who's doing things differently might help narrow down these variations and figure out exactly what the issues are with people getting goo etc.
For example I've always used a lab filtered others maybe using cloth or coffee filters. Might be worth collecting some individual data.

In either case, its a great Tek. It's still early days and I'm sure it'll be refined in time.

 

[Cheelin]

Loveall, I don’t really care about crystal size as long as they predominantly end up in my filter. I do care about speed, though; so i plan on replicating this with Shroombee’s stir & dump salting method to check crystal appearance and yield. Looking forward to that when I get a chunk of time.

I see no biological or chemical reason why careful use of the std tek would not work for Trichocereus of any species, but like you say, time will tell.

I’d like to also see how small a sample I can get measurable and repeatable results from, Besides producing small amounts of product for personal use, I have a number of garden/propagation/selection related projects that I think this tek would be great to use for, especially if the standard process with stir & dump (fastest method) can produce consistent results using, say, 5g samples.

 

[Loveall]

Loveall, I don’t really care about crystal size as long as they predominantly end up in my filter. I do care about speed, though; so i plan on replicating this with Shroombee’s stir & dump salting method to check crystal appearance and yield. Looking forward to that when I get a chunk of time.

I see no biological or chemical reason why careful use of the std tek would not work for Trichocereus of any species, but like you say, time will tell.

I’d like to also see how small a sample I can get measurable and repeatable results from, Besides producing small amounts of product for personal use, I have a number of garden/propagation/selection related projects that I think this tek would be great to use for, especially if the standard process with stir & dump (fastest method) can produce consistent results using, say, 5g samples.

For small garden samples, titration may be best. You could keep a saturated EA citric solution, and count how many drops are needed for pH paper to not be basic and/or for new clouds to stop forming.

 

[Cheelin]

Thanks for the leads Loveall, added to the todo list.

Gonna have to break out the burets, and analytical chem books, figure out how to convert to ppm or % dry wt. Used to do this for a certain commodity a long time ago, but machines took over that task and all I know how to do anymore is read the results and determine next steps.

 

[highlightprotein]

Cheelin that was epic, thanks for the big experiment. For now I think I'm going to stick with chilled EA just because I like the idea of reusing it.

If folks like highlightprotein end up with xtals and not goo that will also be telling.

I got light yellow crystals when using San Pedro (instead of Bridgsii which yielded goo) with microwave, chilled EA, fast crystalization with 15mg citric acid per gram.

As far as I know, I used exactly the same technique with Bridgsii and with San Pedro. But I am a beginner so it is possible I did something differently on my second extraction with San Pedro. My tenative belief is that the San Pedro[edit]I mean Bridgsii[/edit] caused the goo.

I'm not sure why I got light yellow instead of white crystals.

 

[Cheelin]

That's interesting because I didn't quite find that.


It might be worth taking a poll to see who's doing things differently might help narrow down these variations and figure out exactly what the issues are with people getting goo etc.
For example I've always used a lab filtered others maybe using cloth or coffee filters. Might be worth collecting some individual data.

In either case, its a great Tek. It's still early days and I'm sure it'll be refined in time.

Sorry, I missed your reply earlier.

To my eyes, the crystals from each material I ran look pretty consistent across all 4 variations, and pretty similar compared to each other. So, for the process I described, the benefit of doing the extra variations isn’t adding much value, especially if the yields turn out to be the same or lower. I tried to be very explicit about my methodology, in case someone else wanted to mimic it (btw, no need to do 12 runs, just run a side-by-side using my method with 25g of material in the std process and 25g in your favorite variation). Hopefully someone will, before I run some more, and let me know if i just got lucky, so I can run out and buy a lotto ticket.

 

[Cheelin]

Cheelin that was epic, thanks for the big experiment. For now I think I'm going to stick with chilled EA just because I like the idea of reusing it.

If folks like highlightprotein end up with xtals and not goo that will also be telling.

I got light yellow crystals when using San Pedro (instead of Bridgsii which yielded goo) with microwave, chilled EA, fast crystalization with 15mg citric acid per gram.

As far as I know, I used exactly the same technique with Bridgsii and with San Pedro. But I am a beginner so it is possible I did something differently on my second extraction with San Pedro. My tenative belief is that the San Pedro caused the goo.

I'm not sure why I got light yellow instead of white crystals.

Thanks & keep at it, highlightprotein! If you look back a few pages, you’ll see that I was not happy with my early results. I think the learning curve for nailing the required techniques outweighs any of the differences attributable to the variations. But, follow your intuition. The more you experiment, the quicker you’ll get up the learning curve, especially on technique. I bet it’s already contributing to your improved results.

ps: I’m running the equivalent of 4.4g citriic acid for a 100g run (i’m actually doing 25g runs and use 1.1g citrate and passive salting), I specifically decided to use a lower amount of citric because i thought the 15g level was contributing to the significant acid “flavor” and also the stickyness/goeyness of my final product. If you continue to have issues with gooeyness or taste acid, you might drop the level of citric acid to the point where your pH changes from basic (ie above pH=7) to around pH=5, seems to me that perhaps other molecules are also dropping out when pH is lower than 5 (this may be a particular issue that occurs when people are still improving their mixing, pulling, and solvent clearing techniques).

One other thing i’ve noticed: if you have a significant amount of crystals/precipitate that you don’t wash through the filter with fresh EA, especially with the stuff that you water wash out of the decanted crystallization jar, any excess/undissolved citric will remain in the residual product after you evaporate your warm water wash. If you taste any acid (sourness, as opposed to bitterness) n your final product, your salting or washing technique needs improvement.

 

[highlightprotein]

Does anyone know if ethyl acetate will soften/eat through a zip lock bag (polyethylene)?

Today I neutralized some used EA and then attempted to separate the EA from the H2O via a gravy separator. It was pretty tedious and time consuming to do. I should get a separatory funnel. But until then it would be nice if I could use a zip lock bag and cut off the corner to let the water drain out.

Also is there any ideas to further clean the used EA? For example would a brine wash be useful at all?

 

[_Trip_]

Next time I clean my EA I'll be doing a brine wash, sodium carbonate wash and then add CaCl2 to dry the solvent. EA holds some water. The water wont form a distinct layer until its loaded up with excess water. So a chemical dry can't hurt.

I've reused EA with just a sodium and CaCl2 wash with great success but if you wanted to go all out and be realy thorough, I'd take Loveall's advice and do a brine wash as well.

 

[Cheelin]

Does anyone know if ethyl acetate will soften/eat through a zip lock bag (polyethylene)?

Today I neutralized some used EA and then attempted to separate the EA from the H2O via a gravy separator. It was pretty tedious and time consuming to do. I should get a separatory funnel. But until then it would be nice if I could use a zip lock bag and cut off the corner to let the water drain out.

Also is there any ideas to further clean the used EA? For example would a brine wash be useful at all?

Test a baggie, put it in a bowl/jar, put a teaspoon of the solvent in baggie.

To remove the water, put cover on a jar with liquid in it (leave a little airspace for expansion), put jar in freezer over night, pour off solvent in the morning, the frozen puck of water can then be tossed.

Except for repeating the info in tek/this thread re: “Reclaim Solvent”, I can’t add anything on your third question.

You could distill the EA, but that’s a whole other can of worms. Never use an open flame/spark source around EA!

 

[shroombee]

ps: I’m running the equivalent of 4.4g citriic acid for a 100g run (i’m actually doing 25g runs and use 1.1g citrate and passive salting), I specifically decided to use a lower amount of citric because i thought the 15g level was contributing to the significant acid “flavor” and also the stickyness/goeyness of my final product..

Cheelin: This is interesting. Have you tested 5 mg/gram of EA versus 15 mg/gram of EA on the same extract and seen any difference? I've done tests where I split my extract into different jars and then xtalized using either 5 mg/grams or 15 mg/gram and found no difference in yield nor the quality of the end product - other than the 5 mg/gram jar having fluffier xtals that were more likely to stick to the sides of the jar (thus requiring a warm water wash to recover).

If you continue to have issues with gooeyness or taste acid, you might drop the level of citric acid to the point where your pH changes from basic (ie above pH=7) to around pH=5, seems to me that perhaps other molecules are also dropping out when pH is lower than 5 (this may be a particular issue that occurs when people are still improving their mixing, pulling, and solvent clearing techniques)

How are you testing the pH?

One other thing i’ve noticed: if you have a significant amount of crystals/precipitate that you don’t wash through the filter with fresh EA, especially with the stuff that you water wash out of the decanted crystallization jar, any excess/undissolved citric will remain in the residual product after you evaporate your warm water wash. If you taste any acid (sourness, as opposed to bitterness) n your final product, your salting or washing technique needs improvement.

Are you thinking there could be undissolved citric in the salted extract? The solubility of citric in EA is over 50 mg/gram, so excess citric ending up in the final product wasn't something we felt would be an issue (assuming we're not just evaporating EA to yield the mescaline).

 

[Cheelin]

ps: I’m running the equivalent of 4.4g citriic acid for a 100g run (i’m actually doing 25g runs and use 1.1g citrate and passive salting), I specifically decided to use a lower amount of citric because i thought the 15g level was contributing to the significant acid “flavor” and also the stickyness/goeyness of my final product..

Cheelin: This is interesting. Have you tested 5 mg/gram of EA versus 15 mg/gram of EA on the same extract and seen any difference? I've done tests where I split my extract into different jars and then xtalized using either 5 mg/grams or 15 mg/gram and found no difference in yield nor the quality of the end product - other than the 5 mg/gram jar having fluffier xtals that were more likely to stick to the sides of the jar (thus requiring a warm water wash to recover).

Nope, no side-by-side. In my earlier, disappointing 6 separate runs, I ran 5g, 15g, passive, magnetic mix. Something was causing no crystals in filter, brown sticky crap in evaporating dish, more acid than bitter. So I decided that, in addition to the 3 main technique improvements that I’ve previously discussed, there was likely an issue with the citric salting. I decided to take an approach that minimized the citric addition, by looking at pH. In the early runs, I measured some of the pH levels after salting, and at least one was in the 2 to 3 range, so i decided to shoot for 5, and - at least for the passive salting method - it seems to have worked, I get almost all yield as nearly white crystals/needles in my filter, and absolutely no acid “taste” in the filtrate and almost similar white, gooeyless, pure bitter wash water residue. My gut feel is that, depending on operator skill level (which may be why you and Lovell are not seeing some of the problems others are seeing), perhaps other molecules are getting extracted that drop out at lower pH levels.

If you continue to have issues with gooeyness or taste acid, you might drop the level of citric acid to the point where your pH changes from basic (ie above pH=7) to around pH=5, seems to me that perhaps other molecules are also dropping out when pH is lower than 5 (this may be a particular issue that occurs when people are still improving their mixing, pulling, and solvent clearing techniques)

How are you testing the pH?

I hour after passive salting, I dip a pH strip. I did this for all 12 runs of my experiment, spot checked some runs just before filtering crystals, got same result.

One other thing i’ve noticed: if you have a significant amount of crystals/precipitate that you don’t wash through the filter with fresh EA, especially with the stuff that you water wash out of the decanted crystallization jar, any excess/undissolved citric will remain in the residual product after you evaporate your warm water wash. If you taste any acid (sourness, as opposed to bitterness) n your final product, your salting or washing technique needs improvement.

Are you thinking there could be undissolved citric in the salted extract? The solubility of citric in EA is over 50 mg/gram, so excess citric ending up in the final product wasn't something we felt would be an issue (assuming we're not just evaporating EA to yield the mescaline).

Mentioned substantial acid “flavor” above. I don’t think it is a solubility issue, per se, i think it may be tagging along somehow with something else that is dropping out. Or, could just be poor stirring, but I got worst acid “taste” after heavy/long stirring. I truly believe that technique is playing a major confounding role in the problems some of us are/were having, and better operators are not seeing these issues.

I’ll be replicating my methodology in the future (which i believe has significantly upped my technique), i’m hoping to demonstrate repeatability, which would provide some credence to my intuitive approach in this case, even if my explanation for it is wrong.