TEK Ethyl acetate approach [CIELO]

[Loveall]

The freezer ICE/xtal is interesting. I did a feezer test too and the mescaline xtals stay at the bottom, the water ICE floats. If you are seeing stuff at the bottom separate from the stuff at the top, the bottom stuff could be the product we want - see if you can separate it out (I ended up dumping the ICE, leaving the bottom part in the jar.

So one thing you haven't tried yet is the simple tek with excess citric acid during salting, right? I highly recommend testing that, it keeps on working for me. Not sure how "anhydrous" my citric acid is because I was sloppy keeping it closed for the past year or so. I will dry it in the oven to be sure. When it works, you will quickly see xtals sticking to the jar. More stuff crasshes over the next few hours, one day seems like enough time to get back the clear solution.

I'm updating the TEK with one observation. Giving the lime paste a little longer to react before adding ethyl acetate gave better yields from the same cactus material, so I'm increasing that time.

 

[shroombee]

So one thing you haven't tried yet is the simple tek with excess citric acid during salting, right?

I did do a salting with a lot of excess citric acid, but this is the one where we manipulated the water content by drying with CaCl2 and then adding 1% water. Experiment #1, pull #3. I added 847 mg citric acid to this pull of 180 grams solvent. This pull did not xtalize and there is no ICE either.

BTW, I'm going to rename the runs with a "Batch #" rather than "Experiment #" in my log notes and edit my previous posts for clarity to future readers.

Edit: Decided to name them by a "Run #" rather than "Batch #" to avoid confusion with different batches of cactus chips.

The freezer ICE/xtal is interesting. I did a feezer test too and the mescaline xtals stay at the bottom, the water ICE floats. If you are seeing stuff at the bottom separate from the stuff at the top, the bottom stuff could be the product we want - see if you can separate it out (I ended up dumping the ICE, leaving the bottom part in the jar.

My jars have floating ICE and also what appears to be ICE stuck to the bottom of the jars. I'll leave the jars alone for another 24 hours, then will pour stuff off and see what we have.

Not sure how "anhydrous" my citric acid is because I was sloppy keeping it closed for the past year or so. I will dry it in the oven to be sure

I ran a couple solubility experiments with my home made citric acid monohydrate:

Test #1) Dropped a rice-grain sized chunk of citric acid monohydrate into anhydrous ethyl acetate. The grain did not dissolve after 10 minutes. It had no change. After 10 minutes I broke it up but it was basically hard like the anhydrous citric acid.

Test #2) Rice-grain chunk into 3% water plus ethyl acetate. Did not dissolve after 3 minutes. Broke it up manually. It did seem to break up a little easier than Test #1.

I'm updating the TEK with one observation. Giving the lime paste a little longer to react before adding ethyl acetate gave better yields from the same cactus material, so I'm increasing that time.

Good to know. I can probably do a run later today. I'll pull four times, combine pulls, then split the combined pulls into four jars. Assuming about 200 grams solvent per jar, these are some suggested experiments:

1) Salt with 400 mg citric acid monohydrate (2 mg acid to 1 gram solvent);
2) Salt with 600 mg citric acid monohydrate (3 mg acid to 1 gram solvent);
3) Add 1% water, salt with 400 mg citric acid monohydrate (2 mg acid to 1 gram solvent);
4) Dry to anhydrous, salt with 600 mg citric acid monohydrate (3 mg acid to 1 gram solvent);

Acid should be relative to mescaline content, these are probably good enough approximations. Stir thoroughly using magnetic stirrer. Place all the jars in the freezer. Thoughts?

 

[Loveall]

I'm measuring my citric acid to see what I have. Drying it in the oven to see if looses any weight (10% loss would indicate I had the monohydrate).

I think trying #1 makes sense to see what happens, especially if I find that I was using the monohydrate this whole time...

I should now what I have in a few hours

 

[downwardsfromzero]

Best thread on the internet!

Some thoughts:
anhydrous EtOAc might easily dehydrate a single crystal of citric acid monohydrate, at least enough to adversely affect its solubility.
CaCl2 might form a complex with freebase mesc. It certainly does with ammonia, and cannot be used for drying ammonia for this reason. If yields seem reduced after dehydrating the EtOAc pulls with CaCl2 this possibility ought to be considered. So, don't ditch your spent CaCl2 prematurely! A few clever calculations should be able to indicate how likely this complex formation actually is (but why do I always get ideas like this when I need to sleep?)

Keep up the great work :thumb_up:

 

[Loveall]

Thanks DWFZ, good points.

Shroombee, I did not see a 10% weight drop from my citric acid after a few hours in the oven at 200F. Got 0.5% loss though, probably from absorbed moisture (a tiny part of the citric acid stuck to itself at the top layer). I think this means my citric acid is still mostly anhydrous. I think it makes sense for you to over acidify the simple extract, see if xtals crash. pH paper being green on the first pulls is a great sign. So are the clouds and turbidity. Just need to get all that to crash.

Malic acid is working for me too IF I add excess and have some red on the pH paper. When neutral/orange, the malate (?) clouds kind of settle but don't really coalesce into xtals. It is similar to citric, maybe a little better even. Tartaric seems more temperamental and doesn't want to crash even with excess.

 

[shroombee]

Best thread on the internet!

Thanks - we're trying! :lol:

I did not see a 10% weight drop from my citric acid after a few hours in the oven at 200F. Got 0.5% loss though, probably from absorbed moisture (a tiny part of the citric acid stuck to itself at the top layer). I think this means my citric acid is still mostly anhydrous.

I ran an experiment comparing anhydrous citric acid to my monohydrate. 30 minutes at 200 degrees did not change the weight of either sample. I'm curious about that. The monohydrate started to discolor slightly.

Next I turned the oven up to 300 degrees for an hour. The anhydrous melted, turned yellow, and lost 23% of its mass. The monohydrate melted into a burnt orange/red and lost 76% of its mass. Melting point of anhydrous is 307 degrees and monohydrate is 212 degrees. Photo attached. This is probably the easiest test to confirm anhydrous versus monohydrate.

I'll run another experiment where I leave citric acid samples in the oven at 200 degrees for a few hours.

Malic acid is working for me too IF I add excess and have some red on the pH paper. When neutral/orange, the malate (?) clouds kind of settle but don't really coalesce into xtals. It is similar to citric, maybe a little better even.

Okay my malic acid is arriving tomorrow... :lol:

Regarding all this excess citric or malic acid, is the excess going to stay in the ethyl acetate or will it end up in the final product?

 

[Loveall]

Excess (after reaction with FB is done) stays dissolved in the final product from what I see (to a point). Because the organic acids are soluble in ethyl acetate (with my cuttent materials), and also we have some water from the pull. There is published data for malic acid + ethyl acetate solubility (see attached paper), It's about 3.7mg per gram of solvent at room temp (no water I presume), and 2.3mg/g at 10C. Fridge temp is not mentioned, I image it would be at least 1mg/g at 4C (they give parameters for theoretical calculations if anyone is interested).

Thanks for testing the citric acid monohydrate vs anhydrous at 200F. If neither is loosing weight then I don't know what I have. I thought it would dry up in the oven based on some info out there.

 

[shroombee]

Excess (after reaction with FB is done) stays dissolved in the final product from what I see (to a point). Because the organic acids are soluble in ethyl acetate (with my cuttent materials), and also we have some water from the pull. There is published data for malic acid + ethyl acetate solubility (see attached paper), It's about 3.7mg per gram of solvent at room temp (no water I presume), and 2.3 at 10C. Fridge temp is not mentioned, I image it would be at least 1mg/g at 4C (they give parameters for theoretical calculations if anyone is interested).

Can you find solubility data for anhydrous citric acid in ethyl acetate? Monohydrate is 5.28g/100g (52.8 mg per gram of solvent). Maybe that's a good reason to use citric acid instead of malic.

Thanks for testing the monohydrate vs anhydrous at 200F. If neither is loosing weight then I don't know what I have. I thought it would dry up in the oven based on some info out there.

Try heating a sample to +250F. Monohydrate should melt whereas anhydrous should stay solid.

 

[shroombee]

Results of latest citric acid experiment, anhydrous versus monohydrate:

Anhydrous sample weighs 1,665 mg. Monohydrate weighs 706 mg. My toaster oven set temperature is probably not accurate, so these results should be taken as a general outline. Unlike the previous experiment, I placed a piece of aluminum foil over the samples to act as a shield to prevent the samples from being burned by the top heating element.

200F, 3 hours: no change in weight, color, or texture of either sample;
220F, 1 hour: no change in either sample;
250F, 1 hour: no change in weight of either sample, monohydrate is getting a beige color but it has not melted;

280F, 1 hour: Anhydrous has not changed weight, getting a beige color and the grains are starting to stick together, not yet melted. Monohydrate turned a caramel color and the grains melted together into blobs. Monohydrate lost 57 mg, approximately 8% of its starting weight.

Attached photo shows anhydrous at the top. It isn't clear in the photo, but the grains in the anhydrous sample are still distinct although sticking together.

Loveall, I would guess you won't measure a change in the weight of your citric acid unless you reach a temperature where the sample has discolored and has melted. Depending on that temperature, you'll have a good idea of whether your citric acid is anhydrous or monohydrate.

I based some cactus a few hours ago and planned to do the ethyl acetate pulls after an hour of basing, but I promised myself I would make some progress on another hobby first (the one that makes money). :lol: And so I didn't get to the pulls. So by the time I do so I'll probably have 12 hours basing this run of cactus.

 

[downwardsfromzero]

An observation from a different thread

Some people have suggested that citric acid may contribute to emulsions but, to be fair, malate (from malic acid, said to be the principle acid in cacti and hence the salt form of mescaline extracted with this method) isn't necessarily all that different:
citric - HOC(COOH)(CH2COOH)2
malic - HOCH(COOH)CH2COOH

Re: thermal dehydration of citric acid - citric acid decomposes when heated to form aconitic, citraconic, mesaconic and itaconic acids. The colour change is potentially problematic. Use of a lower temperature and lower pressure may be desirable.

[edit: there's also the question of citric acid reacting with aluminium...]

 

[shroombee]

DFW, the purpose of heating the citric acid is to determine whether Loveall is working with anhydrous or monohydrate. We wouldn't use this heated acid for salting.

Observation for today... I based 50 grams of powdered cactus last night and didn't get around to pulling with ethyl acetate. So the cactus and lime sat covered for 22 hours before I added 100 grams of ethyl acetate this evening. I thought the cactus would be goopy sitting so long, but it was a little stiff. I worked it gently with a fork to break it up. The cactus absorbed a lot of the first addition of ethyl acetate so I added another 100 grams, then let it sit a total of 10 minutes. I recovered 139 grams of solvent from this 1st pull (lost 61 grams to the cactus Spirits). It is normal for me to lose that much solvent to the cactus in the first pull.

Each additional pull I added 100 grams solvent, pushed the cactus around gently in the bowl, waited 10 minutes, and recovered a full 100 grams solvent.

The cactus was noticeably crumbly for pulls #1, 2, 3. It then starts sticking together and by pulls #5 and #6 it stays together as a big blob of cactus. So it's the pulling process with ethyl acetate that encourages the cactus to become sticky, not the basing (at least up to 22 hours).


Here is the interesting thing about the pulls. These are the pH paper colors, not the solvent color from the previous two runs (#1 and #2), plus this current run #3:

Run #1 (Solvent added soon after basing, 12 hours per pull),
Run #2 (Solvent added soon after basing, 10 minutes per pull):
Pull #1: Dark green;
Pull #2: Dark green, but slightly lighter than pull #1;
Pull #3: Moderate green;
Pull #4: Very light green;
Pull #5: No color change;

For this Run #3 (22 hours basing before adding solvent, 10 minutes per pull):
Pull #1: Dark green;
Pull #2: Dark green;
Pull #3: Dark green, but slightly lighter than previous two pulls;
Pull #4: Green, slightly lighter than previous pull;
Pull #5: Very light green;
Pull #6: Just a bare hint of green, but can be considered no change;

So I needed at least one extra pull to get to a "no change" pH state, which we believe to indicate there is no freebase present in the solvent and thus we have exhausted the cactus.

Followup experiments:
1) Do the additional pulls with apparent freebase presence imply higher yields? It may be the earlier pulls were actually less effective, thus requiring more pulls to retrieve the freebase.

2) Would long basing (24 hours+) followed by fast pulls (less than 5 minutes each ) increase yields versus slower pulls (1+ hours for example). This theory based on the cactus having about 30 minutes staying crumbly before starting to get sticky. And does sticky cactus make pulls less effective so the mescaline does not migrate as readily to the fresh solvent?


First photo is Run #3 with the pH paper from the 6 pulls, roughly an hour after retrieving the first pull. Note that the color fades over time, so pull #5 is initially very light green but after waiting 10-20 minutes before this photo was taken, the color change is no longer apparent.

Second photo is after salting the combined pulls with 2 mg citric acid anhydrous per gram of solvent. The strip labelled "P6+" is the pH paper dipped into a little pool of solvent that I didn't retrieve from the cactus when decanting pull #6, maybe 10 minutes after decanting. Notice it is fairly green like pull #3-4. I didn't do a pull #7 to investigate this.

 

[Loveall]

I have found that longer basing gave higher yields when going from a few minutes to one hour. Will try a full day. The increase in yields was maybe 20% or so.

Is the salted #3 experiment crashing? The bottom of the paper strip is not very red (looks orange), you may need more citric acid for crashing to happen. See below for one of my examples that crashed to beautiful active xtals, posted earlier. Notice there is no orange color on the right edge of the pH paper that was dipped in ethyl acetate. The green side is lighter than yours, but that was for the combined pulls, the first pull was as dark as your first pulls.

The blob holding on to the mescaline is a good question. Yields seem good so I'm not too worried about it to first order. I threw water and ethyl acetate to one of the blobs and it did not seem to release anything.

If you can get the cloudiness to crash, we will have process that was reproduced. Also, any results with malic?

Thanks for the good work shroombee.

 

[ijahdan]

Great thread, reminds me of the VDS protocol thread on harmaline to THH reduction a few years ago. Got that pioneer spirit feel to it. Ive got some cactus powder lying around, which I occasionally eat, brew tea with or do a 69ron extraction on. This ethyl acetate approach looks fairly straightforward. Im a bit paranoid about ordering these kind of chemicals on the internet though, but assume it's not on any watched lists (uk)?

 

[shroombee]

I have found that longer basing gave higher yields when going from a few minutes to one hour. Will try a full day. The increase in yields was maybe 20% or so.

I wonder where is the upper limit of basing time for increasing yields? 1 hour, 24 hours, 1 week?

Is the salted #3 experiment crashing? The bottom of the paper strip is not very red (looks orange), you may need more citric acid for crashing to happen.

Run #3(A):
- 25% of the combined pulls;
- Salted with 2 mg citric per gram of solvent;
- Placed in the freezer;

It formed slushy ICE on top, no ICE on the bottom, no xtals, but it's still cloudy. This morning I poured it all into a strainer to separate out the slushy ICE. Then salted with an additional 1 mg citric per gram of solvent. See photo of pH paper: far right is with additional 1 mg/gram, 2nd from right is immediately before adding the additional 1 mg/gram, 3rd from right is from last night so the color has faded.

Edit: Comparing to last night's photo, the green fades but maybe the red/orange does not fade. Also, 2nd from right may be more red than last night's 3rd from right because water ICE was removed before dipping the pH strip.

Now the solvent should have 3 mg citric per gram of solvent assuming proportional distribution of the original 2 mg citric in the liquid solvent versus the ICE which was separated out. Magnetic stir for 3 minutes, noticed powder falling to the bottom of the jar. Magnetic stir for another 5 minutes to see if the powder would dissolve. No, it all settled to the bottom of the jar (see photo looking up at the bottom of the jar of the yellowish solvent, with the powder in the corner). Maybe it's mescaline citrate? Solvent is no longer cloudy. What's the best way to separate this powder from the solvent?

I separated the slushy top ICE into ethyl acetate (18.9 grams) and what appears to be water (2.7 grams). The water is evaporating into a small collection of xtals. The ethyl acetate looks to have nothing except greenish oils.

Loveall, have you tried pulling your xtalized ethyl acetate with water and then evaporating the water to see if you get additional yield?

Some changes happening with Run #2(A):
Jar was in the freezer and formed slushy ICE floating on top and ICE stuck to the bottom. I left it in the freezer and nothing else really happened. So last night I took the jar out (after 60 hours in the freezer) and I separated the top ICE, bottom ICE, and the liquid solvent (into a new, clean jar).

This morning I noticed the solvent jar had a small number of xtals at the bottom of the jar (see photo of the jar with the dark emerald green solvent where there are a handful of xtals forming). I put that jar into the frig and a few more xtals formed along with a little glitter. Not much else after 4+ hours.

I evaporated the (now melted) bottom ICE and got xtals (see photo of glass baking dish with water in the corner and lots of xtals forming) which I scraped into a powder (photo shows slightly wet powder next to razor blade). The powder is off-white and tastes a little salty/bitter. Not sour. The top ICE evaporated to nothing. Just a small amount of greenish oil.

I'm debating what to do with this jar in the frig. It is still not quite clear. Wait longer, move to freezer? Add more citric? It currently has 1.375 mg citric per gram of solvent. I am currently salting new pulls at a minimum of 2 mg citric per gram of solvent and maybe 3 mg is better.

If you can get the cloudiness to crash, we will have process that was reproduced. Also, any results with malic?

It seems like we're starting to make progress with the citric. I haven't tested malic yet. The solubility of malic in ethyl acetate is supposedly much less than the solubility of citric. So I'm concerned we'll end up with excess malic in the end product.

I have about 480 grams of Run #3 combined pulls waiting to be salted. I figured I would split into 3 more samples of 160 grams each and try a few things:

(B): Salt with 3 mg citric per gram of solvent (maybe more?). Place in frig for a while to see if I get xtals before trying the freezer;
(C): Freeze without adding citric. See if I get ICE. Then either let it melt back into the solvent or pull the ICE out before salting. The theory being excess water is interfering with xtal formation;
(D): Use citric acid monohydrate? This assumes Loveall might be using monohydrate rather than anhydrous. Still waiting for a definitive answer on that one. Loveall, can you order some anhydrous and test with that?

Thanks for the good work shroombee.

:thumb_up:

 

[shroombee]

Great thread, reminds me of the VDS protocol thread on harmaline to THH reduction a few years ago. Got that pioneer spirit feel to it. Ive got some cactus powder lying around, which I occasionally eat, brew tea with or do a 69ron extraction on. This ethyl acetate approach looks fairly straightforward. Im a bit paranoid about ordering these kind of chemicals on the internet though, but assume it's not on any watched lists (uk)?

Thanks! The different results are helping us to better understand the edge cases. Hopefully we'll have complete understanding soon. Great job Loveall for being the pioneer and making so much progress!

Ethyl acetate is commonly used to decaffeinate coffee and tea. It's approved in Canada as a carrier and extraction solvent, which somehow makes me feel better about using it.

Edit: Ethyl acetate is available OTC as "M.E.K. Substitute". Before ordering, you may want to wait until we figure out whether the different purities of our ethyl acetate contribute to the different results.

 

[shroombee]

Loveall, are you using fresh solvent for your runs? I've been using fresh solvent for each of the 3 runs I've done.

Also, have you salted pulls separately to test pulls with more or less freebase content? I'm wondering if saturation is a factor, like with DMT freeze precipitation. So if I evaporate some solvent volume will xtals be more likely?

 

[Loveall]

Those crystals forming in the green solvent look like what I get sometimes. The stuff in the jar with the yellow color looks exactly like what I always get now with the simple tek (if I add enough citric acid).

I've always used fresh solvent so far. Want to re-use at some point just not gotten around to it.

Since yields were good, I was thinking most everything is crashing. What I did is wash the xtals with fresh ethyl acetate. The washes evaporate to essentially nothing, so I'm thinking the salt won't go into solution, but the extraction does have some water (unlike fresh ethyl acetate) so this is an open question.

I have salted the 4th pull separately. As long as there is excess citric acid xtals formed. Very few because it was the 4th pull, but they were there. I don't think saturation is needed.

I haven't done water pulls. I imagine citric acid would be pulled too, along with any mescaline citrate if it did not crash.

Definetly add more citric to see if it helps xtalization. It should dissolve and cannot hurt anything, unless overdone by a lot. Extra citric could push the citrate out of solution by forcing the reaction in the wiki entry to the right.

If you have malic, I recommend trying it in a small sample. At room temp it is soluble at 3.7mg per gram of solvent. It seems to xtalize better/faster vs citric acid. If you are having more issues than me getting xtals to form with citric acid (even after you add extra citric), I suggest trying malic. Add extra malic too, we want those pH strips to have some red all the way at the bottom (not just away from the tip) - that is how I'm getting the best results.

 

[Loveall]

Separate post to answer this important result:

Now the solvent should have 3 mg citric per gram of solvent assuming p:grin: roportional distribution of the original 2 mg citric in the liquid solvent versus the ICE which was separated out. Magnetic stir for 3 minutes, noticed powder falling to the bottom of the jar. Magnetic stir for another 5 minutes to see if the powder would dissolve. No, it all settled to the bottom of the jar (see photo). Maybe it's mescaline citrate? Solvent is no longer cloudy. What's the best way to separate this powder from the solvent?

Yes, I believe this is it . The picture with the yellow extract, right? I think you got it. I even see some smaller xtals sticking to the wall which is typical.

So you removed some water (freezer ice) and added more citric and the clouds crashed, right? I think the key step was adding the extra citric acid. I say that because I only need to add excess citric, as long as I do that I don't need to remove water.

To recover you can swirl the powder into solution and pour everything through a coffee filter. It will catch the crystals. Rinse the jar and the xtals with some fresh ethyl acetate and let them dry. They scrape/fall off the filter very easily onto a sheet of paper for example. They will be fluffy and easily fly away towards heaven, so be a little careful. If you couldn't dislodge a small amount to xtals on the sidewall, dissolve them in water, pour in a shallow baking dish and evaporate them - they will make beautiful long needles this way, especially when evaporated slowly without heat.

Unfortunately, I don't think there is a fixed value of citric acid we can give. Any citric acid that reacts with mescaline is in salt form and won't count towards an excess. If your cactus is higher yield than mine, then you need even more citric acid than me to have excess citric, because more was neutralized by mescaline FB. We want those pH strips red throughout, it seems to always crash in that case.

One thing I don't understand is that you mention the pH paper from yesterday faded, but I still see the same orange towards the bottom of the strip in yesterday's picture (post #71). It looks like removing the ice increased the pH, and then you added more citric and it crashed within minutes.

I think that we are finding that adding citric pushes the following reaction to the right.

3Mes(↑) + H3Cit(↑) ⇒ 3(MesH)Cit(↓)​

Next time, I suggest to directly add more citric acid. That seems to force xtalization.

 

[Loveall]

Shroombee, I got some results today also:

- Simple tek
- Salt slowly to ~neutral, clouds don't crash -> this is where I/we went into a loop of removing water, microwaving, etc. I think those things do help, and I got stuck on them for a bit, and drying the solvent may not work if citric acid is anhydrous, but there is simpler way (see next step).
- Add more citric acid. Eventually pH paper becomes red and crashing occurs. Overtime solution becomes clear.
- Filter and add more citric, no new clouds and no new crashing. I think this is the lazy man way of verifying that precipitation was completed in the previous step. The proper way would be to do an A/B on this and be extra sure.

 

[shroombee]

I made a few clarity edits in my previous post with the xtal photos to call out which photo I'm referring to.

One thing I don't understand is that you mention the pH paper from yesterday faded, but I still see the same orange towards the bottom of the strip in yesterday's picture (post #71). It looks like removing the ice increased the pH, and then you added more citric and it crashed within minutes.

I think you're right. I know the green fades but the red/orange may not. And when I dipped the pH strip before adding more citric it was more red than last night's pH strip, leading me to believe last night's acid pH strip faded like the green ones do.

Those crystals forming in the green solvent look like what I get sometimes. The stuff in the jar with the yellow color looks exactly like what I always get now with the simple tek (if I add enough citric acid).

I thought "xtals" referred to the sharp spiky formations (in the dark green jar). I didn't know the yellow jar could also be referred to as xtals.

The washes evaporate to essentially nothing, so I'm thinking the salt won't go into solution, but the extraction does have some water (unlike fresh ethyl acetate) so this is an open question.

Can you clarify the "salt" and "solution"? What do you mean by the open question?

So you removed some water (freezer ice) and added more citric and the clouds crashed, right? I think the key step was adding the extra citric acid. I say that because I only need to add excess citric, as long as I do that I don't need to remove water.

Right, clouds crashed while magnetic stirring. Only took maybe a minute.

Unfortunately, I don't think there is a fixed value of citric acid we can give. Any citric acid that reacts with mescaline is in salt form and won't count towards an excess. If your cactus is higher yield than mine, then you need even more citric acid than me to have excess citric, because more was neutralized by mescaline FB. We want those pH strips red throughout, it seems to always crash in that case.

What has been throwing me is that the original microwave tek called for 250 mg citric added to about 800 grams of combined pulls. Meaning 0.3 mg citric per gram of solvent. The tek then was updated to 500 mg citric and is now at 1,200 mg citric (1.5 mg per gram of solvent).

I'm up to as much as 3.0 mg of citric per gram of solvent which is 10x the amount in the original tek, and still twice the current version of the tek. I hope this amount of excess acid I'm adding isn't covering up another issue such as ethyl acetate or citric acid differences.

If you have malic, I recommend trying it in a small sample. At room temp it is soluble at 3.7mg per gram of solvent. It seems to xtalize better/faster vs citric acid. If you are having more issues than me getting xtals to form with citric acid (even after you add extra citric), I suggest trying malic.

I just got the malic acid and will try it.

Edit: Keeping in mind that citric acid monohydrate solubility in ethyl acetate is 52.8 mg per gram of solvent (14x versus malic). So citric potentially has a larger safety margin if the concern is excess acid ending up in the final product.

Add extra malic too, we want those pH strips to have some red all the way at the bottom (not just away from the tip) - that is how I'm getting the best results.

What color "red" on the pH legend? Like the equivalent of pH 2? Or maybe next time you're at Home Depot you can pick up a paint color swatch that matches the red in your pH strips and let me know. I know it's not Behr "Jamaica Bay". :lol:

- Add more citric acid to get pretty acidic. Crashing occurs and over time solution becomes clear.
- Filter and add more citric, no new clouds and no new crashing. I think this is the last man way of verifying that precipitation was completed in the previous step. The proper way would be to do an A/B on this and be extra sure.

Sounds like a good verification. We might want to try the A/B as the final process once the salting is reliable and we test other variations such as basing time.

Edit: Once we have reliable parameters on salting, we should probably A/B as the final step to verify the basic process before we run experiments designed to optimize yield or labor.

As you continue to add acid, do you get immediate crashing? That's what happened with my yellow solvent photo. I added the acid and as I was magnetic stirring, I noticed the fine powder swirling around in the jar.