69 ron tek not working well, any help? (pics)

[mud1]

I followed the wiki instructions for 69 ron's limonene tek pretty closely, I have several very accurate scales and measures as well as ph strips.

I started with dry cactus skins, powdered them in a vitamix. I added the lime to cactus and mixed, then added distilled water. After mixing it all, tested the ph was above 12.

After an hour or so (longer than the 5 min in the instructions), I added limonene and stirred and let sit for 4+ hours.

After that, I pressed down the french press and poured 200 ish ml of the original limo into a beaker and put vinegar and stirred with a glass rod. extracted the vinegar and repeated this 3 times and evaporated:

I ended up with practically nothing (though the resin smells like overripe apples, not sure if that is correct). I also tested the vinegar after the limonene wash and its ph was still very low (3-4).

I realized maybe I didn't stir enough or let the vinegar-oil mix sit long enough so for the second pull, I added like 50 ml more limo and let sit overnight and then did more vinegar pulls today. When mixing, I actually used a pipette to basically form an emulsion with the vinegar and oil and waited for that to break. Each wash took about 2 hours and this is what you see in the glass pyrex container and though it is still drying, it does not look like it will produce much.

I tested the cactus mix in the french press after this and the ph has dropped to a 10-11, so I was considering adding more lime.

I'm pretty sure I did everything right, can someone help me diagnose what could be wrong?

Thanks!

 

[_Trip_]

I've never had much success with that tek personally but it could be that the cacti isn't potent to begin with. Was it a pedro? How much did you start with dry? And what was the final yield?

 

[mud1]

I've never had much success with that tek personally but it could be that the cacti isn't potent to begin with. Was it a pedro? How much did you start with dry? And what was the final yield?

That's possible, it started as 100 grams dry, T pachanoi (which I am aware has a wide variance), there is only ~25 mg on the razor blade. That's 0.025% yield, and not all of it is even mescaline...

 

[ijahdan]

Ive had success with this tek in the past. Takes a lot of limonene though, I used almost 1 litre for 100g cactus powder. You need about 3 limonene pulls of 300ml each (some will be absorbed by the paste, so you wont recover the full amount), then salt out each of these 3 times with vinegar. I was still only getting about 0.5% yields from decent cactus though. Check out the new CIELO tek next time. Similar, but better.

 

[shroombee]

If you can obtain ethyl acetate in your area, the CIELO tek will probably work much better for you than the 69ron lime/limonene tek.

With lime/limonene, I've had better results salting with HCL to around pH 6.0 rather than using vinegar. If desired, you can then purify further by washing the resulting powder with cold, dry acetone and then cold, dry IPA.

 

[mud1]

Thanks for the relies and suggestions, for an update, I just left the limo cactus mix together longer and did one vinegar pull every other day. I also used carbonated water and citric acid for some of the pulls too. I currently have around 1 gram of black goo.

Does any one know if this is normal? Did I not dry it enough? I'm guessing most of this gram is not going to be mescaline, right?

I will eventually try CIELO tek, but I've heard that can result in more crystals than expected due to an excess of citric acid, is that true?
Also I have heard that the mesc citrate is far less potent than mesc acetate/hcl (which I don't really have access to hcl)

 

[Loveall]

During CIELO the citric acid is in solution in ethyl acetate. It is not in xtal form in the solvent.. After catching the mescaline citrate xtals in a filter, fresh ethyl acetate is used as a wash to remove any citric acid traces from the snall ammount of original ethyl acetate wetting the product.

Yes, monomescaline citrate is less potent by weight vs mescaline HCl. However, you get more citrate product by weight so nothing is lost. In terms of free base weight the yield is the same.

I think CIELO takes a lot less work to get to a very clean xtaline product. The materials used are very specialized for cactus. If you try it, practice with a small sample (scale the TEK) and dont rush or lool for short cuts at first. Good luck.

 

[mud1]

During CIELO the citric acid is in solution in ethyl acetate. It is not in xtal form in the solvent.. After catching the mescaline citrate xtals in a filter, fresh ethyl acetate is used as a wash to remove any citric acid traces from the snall ammount of original ethyl acetate wetting the product.

Yes, monomescaline citrate is less potent by weight vs mescaline HCl. However, you get more citrate product by weight so nothing is lost. In terms of free base weight the yield is the same.

I think CIELO takes a lot less work to get to a very clean xtaline product. The materials used are very specialized for cactus. If you try it, practice with a small sample (scale the TEK) and dont rush or lool for short cuts at first. Good luck.

Thanks, that makes a lot of sense. Is the dissolved citric acid the reason you need to wash the solvent out with soda after? I think other teks that use d limo don't need to wash, right?

 

[shroombee]

(which I don't really have access to hcl)

Here is the HCL I used with 69ron tek. Now I'm all-in on CIELO:

Dr. Clark Hydrochloric Acid Drops

 

[Loveall]

Thanks, that makes a lot of sense. Is the dissolved citric acid the reason you need to wash the solvent out with soda after? I think other teks that use d limo don't need to wash, right?

Yes, that is right. An alkaline wash is needed to return EA to neutral. Limonene does not require this.

However, if you don't do this wash and reuse the EA it sill works because the excess lime in the wet cactus paste neutralizes the old excess citric acid, but a cloud with calcium citrate appears when extracting. Still works but waiting for that cloud to settle before salting the freebase mescaline takes a loooong time. The wash before reuse is fast/convenient. However, if one doesn't mind waiting a few days for calcium citrate to settle or has a good way to filter it, the soda wash can be skipped. Just FYI.

 

[mud1]

(which I don't really have access to hcl)

Here is the HCL I used with 69ron tek. Now I'm all-in on CIELO:

Dr. Clark Hydrochloric Acid Drops

Thanks for the link, though that looks a bit too pricey for such a small amount. I might just stick to citrate since the mesc content is the same. Though for reference, since this HCl is liquid unlike the citric acid crystals, do you do a normal wash of acid in the EA instead of waiting for crystallization to happen?

Thanks, that makes a lot of sense. Is the dissolved citric acid the reason you need to wash the solvent out with soda after? I think other teks that use d limo don't need to wash, right?

Yes, that is right. An alkaline wash is needed to return EA to neutral. Limonene does not require this.

However, if you don't do this wash and reuse the EA it sill works because the excess lime in the wet cactus paste neutralizes the old excess citric acid, but a cloud with calcium citrate appears when extracting. Still works but waiting for that cloud to settle before salting the freebase mescaline takes a loooong time. The wash before reuse is fast/convenient. However, if one doesn't mind waiting a few days for calcium citrate to settle or has a good way to filter it, the soda wash can be skipped. Just FYI.

Gotcha, is it fine to wash the EA with normal baking soda (bicarb) or NaOH? I'm fine with getting washing soda if needed, but I'd prefer to just use what I have on hand.

 

[mud1]

Also a quick question about safety, I saw the original CIELO tek uses the Klean Strip brand of MEK substitute, which the MSDS looks good, it says 100% ethyl acetate.

But still, I want to be extra safe and understand the risks. Are there any chemicals that might be present in the EA to be wary of? Is there something like an evap test I can perform on the EA to make sure?

I also see this, which is listed as technical grade and its MSDS is also 100% EA, but I wasn't sure if "technical grade" even means anything.

Any other recommendations? Price shouldn't be a factor when it comes to safety

 

[Loveall]

I never tried using HCl with EA since it may break down into ethyl alcohol and acetic acid in harsh pH conditions, so I avoid that. Dilute HCl or short pull times may be fine though, I don't know. This would also take NaOH out as a wash for me. Sodium bicarbonate should work I think, but I never tried it.

Do an evap test on your source of EA. I have done the evap test with that brand and it was very clean. Small aditives may not always published in MSDS. A notorious example is coleman camping gas (naphtha) and it's anti corrosion additives :thumb_dow

 

[mud1]

This would also take NaOH out as a wash for me.

Oh so you think NaOH would be too strong of a base to work with EA? I was actually hoping to use KOH or NAOH, but saw that you said in another post not to do that at all:

CIELO attempt troubleshooting - FAQ - All your basic questions and answers - Welcome to the DMT-Nexus

 

[_Trip_]

I never tried using HCl with EA since it may break down into ethyl alcohol and acetic acid in harsh pH conditions, so I avoid that.

I asked mindlusion about that he said he uses HCl in EA often and it won't breakdown the EA.

 

[Loveall]

I never tried using HCl with EA since it may break down into ethyl alcohol and acetic acid in harsh pH conditions, so I avoid that.

I asked mindlusion about that he said he uses HCl in EA often and it won't breakdown the EA.

Good to know. I wonder if the concentration matters. He may use HCl in IPA instead of aqueos too.

 

[_Trip_]

I asked him in chat a little while ago, so for memory I'm fair sure we were talking about undiluted HCl in EA. He was saying he uses it a bit for crystalising a number of alkaloids. I specifically asked him because of your tek.

 

[mud1]

So dilute HCl would probably be fine? Are there any real benefits to using HCl over citrate besides being more dense?

Also does this mean NaOH or KOH might be okay, or would that need further testing?

 

[_Trip_]

Not sure about diluted, as Loveall eluded to there hasn't been any members testing it for the CIELO tek or atleast reporting it back. Your welcome to report back and be the first.
However, citric acid forms nice crystals and can be purchased at any grocery store. Also EA holds citric acid at 50mg/ml so if you stick to say 10-20mg/ml you definitely wont see any excess citric acid crash out. So why not use that?
As for bases I would imagine most would work but again besides maybe sodium carbonate I dont think anyone has tried other bases or at least reported back results in regards to the CIELO tek. Calcium hydroxide should be easy to find.

 

[mud1]

Not sure about diluted, as Loveall eluded to there hasn't been any members testing it for the CIELO tek or atleast reporting it back. Your welcome to report back and be the first.
However, citric acid forms nice crystals and can be purchased at any grocery store. Also EA holds citric acid at 50mg/ml so if you stick to say 10-20mg/ml you definitely wont see any excess citric acid crash out. So why not use that?
As for bases I would imagine most would work but again besides maybe sodium carbonate I dont think anyone has tried other bases or at least reported back results in regards to the CIELO tek. Calcium hydroxide should be easy to find.

Yeah I don't see any reason to use HCl over citric acid at this point.

As for NaOH vs CaOH2, I'm worried about the pH more than the availability, since mesc pKa is 9.56 it follows:
9.56 50% freebase
10.56 90% freebase
11.56 99% freebase
12.56 99.9 %freebase

And CaOH2 ph is 12.5 ish. Which seems fine, but I've noticed in my 69ron tek that the cactus ph drops over time, which means less extracted. If I use NaOH with a pH of 14, even if the pH drops a little, I wouldn't need to worry about the pKa. I guess I could always add more CaOH to the mix but that's very inconvenient since it's re-introducing a "dangerous" step into the process.