CIELO goo - current best recovery method?

[starbob]

So, if I understand your steps, in both cases you needed to triturate the goo/glue with fresh solvent AND some mescaline citrate.

Right, both jars with trituration and M citrate. I regret not waiting longer with trituration only to keep that isolated test-wise...

I think a big difference between your goo run and previous good xtalization runs is going to be mescaline concentration in your EA. Let us know your yields and amount of solvent you were Xtalizing from please.

Let's just say my 'good xtalization' runs are not going to help much there haha. My track record has not been great so far honestly, learning experience and powder potency. I also haven't been accurately measuring my final extract total volume just eyeing between the lines on the mason jars. I may have had one other high water botched run I didn't note below.

100g PC powder 0mg yield (botched it, tons of water in paste)
20g PC powder ~10mg yield 0.05% (didn't measure it before failed re-X attempt) 
     (~200mL final EA in salting jar)
22g PC22 powder 0mg yield (botched it, CA accidently waaay over 50g/ml limit -_- )
20g PC8 powder ~15mg yield 0.075% 
     (140~150mL final EA in salting jar)
14g bridgeLEE powder goo 623mg yield 4.45% 
     (~140mL final EA in salting jar when goo formed, 60mL fresher added to arrive
 at 200mL mark before crystallization occured. To reiterate, the separated goo in 
small jar had fresh 60mL, then decanted for another fresh 60mL current)

[Edit: EA estimates]
[Edit2: bridgesii LEE yield]

 

[starbob]

I didn't combine them before filtering like I was thinking earlier (dunno why I thought that was a good idea in the first place).
Original extract jar result was 138mg
Small goo/glue jar result was 485mg
(this larger portion is probably not super pure though, larger chunks were kinda yellow like you can see in my video previously)
total 623mg

I tried my best to scrape off the crystals suck on the jar walls of each, running some fresh EA splashes over em and what not.
I didn't do a warm water jar recovery for either jar. The small jar didn't have much stuck on it from what I could tell, it's not like the crystals were super clear or fine where it would be hard to see. The larger jar I can't water wash to combine that with final yield here because...
I mixed some older batch EA in with it and it started crystallizing some more this jar is the gift that keeps on giving. I think it was one of my older botched jobs, maybe the one where I added too much citric acid, no clue..

 

[orchidist]

Right, both jars with trituration and M citrate. I regret not waiting longer with trituration only to keep that isolated test-wise...

Did you try trituration on its own? Or is it just that the seed crystals were added, and when that didn't work, you added fresh EA and then observed crystals? I didn't need to seed mine, it crystallized spontaneously as excess CA was removed from the goo.

Definitely recommend getting a notebook and start recording everything, a package of labels to put on your jars is really helpful too. I wouldn't be able to keep track of anything I've got going on without it. If you're up to it, get a cheap indoor thermometer and record the temperature while you're doing the extraction and salting steps too.

It also might be much easier to control the amount of water/solvent you're using by weighing it instead of using the gradations on your jars, which are probably not very accurate. 1 gram of water is 1mL at room temperature. 1 gram of EA is approximately 0.9mL. I've been using mass for everything throughout just to keep things as repeatable as possible.

Between the cactus paste that produced goo and the ones that yielded crystals, were there any noticeable differences in the consistency of the paste? The one I had success with without first treating the solvent with a strong drying agent had a much firmer consistency than the one that gives me goo. I cannot replicate that consistency with the cactus that yields goo regardless of whether I'm on the dry or wet side of the recommended range, though reducing the amount of water used did solve my oiling out issue.

I suspect that mucilage might play an important role, since it is well known for its ability to hold onto water, and the quantity of it would make a big difference in the appearance of the paste. I'm wondering if the low yields are actually due to low potency, or something like this confounding the results.

 

[Loveall]

Product looks pure starbob.

I think we have 3 kinds of users:

1) TEK simply works with citric and no solvent drying. I've gotten more feedback from friends that don't post and this is the norm for them.
2) TEK was not done properly giving goo and it begins to work when done correctly
3) TEK was done properly but use of K2CO3 as a drying agent OR fumaric as salting acid is needed to avoid goo. People that encounter this situation have ~0.5% or lower yields. A possible concern is that low mescaline concentration, free water, and excess citric acid could be conducive to forming salt/acid/water goo when using citric.

Thoughts? Anyone disagree with these rough observations so far? Seems like this is the story that is emerging.

If this is the case, we can simply reccomend Fumaric instead of citric in the standard TEK and make xtalization more robust.

 

[starbob]

Right, both jars with trituration and M citrate. I regret not waiting longer with trituration only to keep that isolated test-wise...

Did you try trituration on its own? Or is it just that the seed crystals were added, and when that didn't work, you added fresh EA and then observed crystals?

Right, when M crystals alone didn't seem to work in the original jar with (what I thought was not much goo left in it), I moved the 1st round fresher EA from small jar to original jar. And in the other jar I kind of did the inverse; removing the majority of the goo to the smaller jar, decanted original extract EA off that as much as I could with syringe, added fresh EA to that and waited some days days scratching it about before *impatiently* adding M crystals. I feel like it could be either seed crystals or fresh EA just needed more time to work, dunno.

Really appreciate the advice, my notes have been a mess on evernote and I certainly will start labeling my jars. I swear I normally try to make a habit of double or triple labeling samples of things. I switched from weight to volume on liquids so I could to try to follow Cheelin's method to the letter, but I never attempted to measure each pull and thought I'd only need to loosely account for the volume right before salting (just to have visibility I was going nowhere near the citric:EA solubility max).
I attached my rough calculator spreadsheet and print out I'm using now, but I think I'm going to try fumaric acid next go.

"Between the cactus paste that produced goo and the ones that yielded crystals, were there any noticeable differences in the consistency of the paste?"

Do you mean the consistency before doing EA pulls? No, I wouldn't say so. Since my first 1-2 tries I've been trying to keep it at a kind of stiffer play-doh thanks to all the great feedback here.

 

[starbob]

"Product looks pure starbob."

I can't tell ya how happy I am to hear that
Now dry, the yellower chunks before filtering are indistinguishable from the rest.

I don't feel confident I can comment on the emerging patterns with goo formation, but to your 3rd point: my yield was not ~0.5% or lower when I got goo this first time. Unless I'm doing my math wrong or you meant my case just falls into your 2nd point.

My takeaways for next time:
- got better lids and glass syringes
- try fumaric (since I have no other use for the fumaric I bought )
- use some minimum amt of fresh EA to make a separate acid solution
-- and mix that in a bit slower

 

[orchidist]

Product looks pure starbob.

I think we have 3 kinds of users:

1) TEK simply works with citric and no solvent drying. I've gotten more feedback from friends that don't post and this is the norm for them.
2) TEK was not done properly giving goo and it begins to work when done correctly
3) TEK was done properly but use of K2CO3 as a drying agent OR fumaric as salting acid is needed to avoid goo. People that encounter this situation have ~0.5% or lower yields. A possible concern is that low mescaline concentration, free water, and excess citric acid could be conducive to forming salt/acid/water goo when using citric.

Thoughts? Anyone disagree with these rough observations so far? Seems like this is the story that is emerging.

If this is the case, we can simply reccomend Fumaric instead of citric in the standard TEK and make xtalization more robust.

I think 2 and 3 may be the same. After my first total failure to extract from a paste that was too dry, I ended up rigidly sticking to a 3:1 ratio in my early attempts and only got goo. Now, I can crystallize citrate by reducing water content in the paste, but it's looking like the margin of error/optimal yield range is narrow for this particular cactus. I'm still climbing back up toward 3:1 to try to find the optimum, and oil tipping point, so I can't dismiss the possibility that some of the optimal extraction range might overlap the too wet to crystallize without drying range.

It also looks like some form of drying is going to be worth it to improve yield for the alternative acids too. So changing acids adds an extra step and two special ordered chemicals, instead of just the K2CO3. Changing up the acid could become a matter of preference though. I really love the way the succinate looks, but others may not care as much about that and would rather the most OTC option.

The other thing I'd recommend for the wiki is to suggest weighing the water instead of using volume. Issues with precision/accuracy may occur with common volumetric kitchen tools, especially with smaller scale extractions.

 

[shroombee]

A possible concern is that low mescaline concentration, free water, and excess citric acid could be conducive to forming salt/acid/water goo when using citric.

Thoughts? Anyone disagree with these rough observations so far? Seems like this is the story that is emerging.

I'm not sure about the low mescaline concentration because we've crystalized from later pulls that have low concentration. Or perhaps those later pulls gave xtals only because the majority of the water was already extracted from the paste in the earlier pulls?

 

[orchidist]

"Between the cactus paste that produced goo and the ones that yielded crystals, were there any noticeable differences in the consistency of the paste?"

Do you mean the consistency before doing EA pulls? No, I wouldn't say so. Since my first 1-2 tries I've been trying to keep it at a kind of stiffer play-doh thanks to all the great feedback here.

Yeah that's what I meant, and that makes sense. It would be a more informative comparison to look at the consistency of two different cacti, one that yields crystals and one that yields oil, given the same amount of water. The stiffer one would probably hold onto its water better during extraction

I'm not sure about the low mescaline concentration because we've crystalized from later pulls that have low concentration. Or perhaps those later pulls gave xtals only because the majority of the water was already extracted from the paste in the earlier pulls?

I'm thinking if the mucilage/water holding capacity thing is correct, water could be pulled out in the first few runs and the cactus paste could end up too dry to extract any more product, which would result in low yield and wet solvent. Attached a plot of how I think that behavior would look. Trouble is figuring out a way to test that...the why probably doesn't matter as much as how to deal with it anyway.

 

[skelly0311]

I'm having a similar issue with goo. The goo seems to precipitate at the bottom of the EA, and sort of sticks to itself as I move my beaker with EA around. I am using bridgesii monstrous short form, and I know from experience this is high in mescaline content, so I must be doing something wrong. The outline of my process is below:

1. Mixed approximately 70 ml of water with 7.2 grams of CaOH in a fresh press
2. poured 28.63 grams of dried bridge into CaOH/water solution
3. added approximately 10 ml of water to create a thick mashed potato consistency
4. first pull with EA was with 58.75 grams of EA
5. I then did 7 more pulls with EA at an average of approximately 36 grams of EA
6. The EA pulls took 25 minutes total
7. Added 1.43 grams of citric acid powder to decanted EA/cactus alkaloids
8. used a mag stir on low/medium for 12 minutes

I noticed the goo I described above after around 24 hours. It has now been 72 hours, I decided to filter the EA/goo though a double coffee filter, and the finished product is in the pic shown.

Should I put this goo back into fresh ethyl acetate? or should I put it back in the ethyl acetate it was in previously and simply add more fresh EA to that jar. Just trying to figure out any way salvage what should be a good amount of mescaline

 

[Loveall]

I'm having a similar issue with goo. The goo seems to precipitate at the bottom of the EA, and sort of sticks to itself as I move my beaker with EA around. I am using bridgesii monstrous short form, and I know from experience this is high in mescaline content, so I must be doing something wrong. The outline of my process is below:

1. Mixed approximately 70 ml of water with 7.2 grams of NaOH in a fresh press
2. poured 28.63 grams of dried bridge into NaOH/water solution
3. added approximately 10 ml of water to create a thick mashed potato consistency
4. first pull with EA was with 58.75 grams of EA
5. I then did 7 more pulls with EA at an average of approximately 36 grams of EA
6. The EA pulls took 25 minutes total
7. Added 1.43 grams of citric acid powder to decanted EA/cactus alkaloids
8. used a mag stir on low/medium for 12 minutes

I noticed the goo I described above after around 24 hours. It has now been 72 hours, I decided to filter the EA/goo though a double coffee filter, and the finished product is in the pic shown.

Should I put this goo back into fresh ethyl acetate? or should I put it back in the ethyl acetate it was in previously and simply add more fresh EA to that jar. Just trying to figure out any way salvage what should be a good amount of mescaline

The TEK uses Ca(OH)2, not NaOH.

You can dry to drop goo in fresh AE and break up the goo and see if xtals come out

 

[skelly0311]

Sorry, I was rushing when I wrote this. I just edited that after I wrote it. I did use CaOH.

 

[skelly0311]

Would you recommend I use a magstir when I put the decanted goo into fresh EA?

 

[Loveall]

I don't know, a magnetic stirrer could work, yes.

 

[skelly0311]

Thanks for the response, really appreciate your help. I think right now, I'm gonna wait for it to dry(assuming it will), grind it up into finer powder, then put in fresh ethyl acetate and magstir it for 10 minutes or so.

I have no idea why I got goo, It seems like I did everything right, and everything should have been scaled appropriately with the 28.63 grams of dry cactus powder I used.

 

[Loveall]

Thanks for the response, really appreciate your help. I think right now, I'm gonna wait for it to dry(assuming it will), grind it up into finer powder, then put in fresh ethyl acetate and magstir it for 10 minutes or so.

I have no idea why I got goo, It seems like I did everything right, and everything should have been scaled appropriately with the 28.63 grams of dry cactus powder I used.

Did you filter the extract with a coffee filter when pulling? Did you rest the extract with citric before salting yo verify no water dropplets formed?

 

[skelly0311]

Yes, I did use a coffee filter when doing the pulls. I then let the solution rest for an hour and I do not recall seeing any water droplets. What would the water droplets look like in the ethyl acetate anyways? Would the water just coagulate to the bottom or something?

 

[Loveall]

Yes, I did use a coffee filter when doing the pulls. I then let the solution rest for an hour and I do not recall seeing any water droplets. What would the water droplets look like in the ethyl acetate anyways? Would the water just coagulate to the bottom or something?

They look like drops at the bottom/walls. While an hour should work in most cases, begginers are encouraged to rest the extract longer in the fridge (24h) to really make sure no water forms over time.

 

[skelly0311]

Ok, my first run I used PC Pedro, and got a white solid at the bottom as opposed to crystals. I figured it was because I used a mag stir and that broke up the crystals into a powder. (end product in pic below)

I remember before adding the citric acid, there was a small coagulant at the bottom. This morning I put EA in water just to see what these water droplets look like, and the coagulant didn't look like that. It kinda stuck together more. Either way, I'm assuming that coagulant shouldn't have been there, as the alkaloids should dissolve in the EA, is that correct?

Next time I do the Tek I'm going to follow Orchids advice and try a 2.85:1 paste ratio. I'll also ease up on pushing the fresh press when decanting.

Thanks again!

 

[Loveall]

Ok, my first run I used PC Pedro, and got a white solid at the bottom as opposed to crystals. I figured it was because I used a mag stir and that broke up the crystals into a powder. (end product in pic below)

I remember before adding the citric acid, there was a small coagulant at the bottom. This morning I put EA in water just to see what these water droplets look like, and the coagulant didn't look like that. It kinda stuck together more. Either way, I'm assuming that coagulant shouldn't have been there, as the alkaloids should dissolve in the EA, is that correct?

Next time I do the Tek I'm going to follow Orchids advice and try a 2.85:1 paste ratio. I'll also ease up on pushing the fresh press when decanting.

Thanks again!

Right, the coagulant should not have been there. Only clear EA extract should be present when salting to get xtals right away.