I'm giving the CIELO tek a second attempt, and put my EA in the fridge after the pulls, i.e. this step:



I put my bottle a little too close to the fan, as a result, when I checked back a few hours later, I had a layer of ice on the bottom instead of water. The EA remained liquid since its freezing temperature is -83 C.

I haven't separated the parts yet, but. if we start putting the jar in the freezer, this seems like a potential improvement - solid ice is a lot easier to separate than two liquids.

Assuming you filtered the EA as you poured your pulls into the jar, at this stage, you can pretty haphazardly (but don't actually do it haphazardly) pour the EA layer into an new jar without worrying about water getting in your final mix.

Are there any potential issues with this idea? To be fair I'm not at the stage to pour out the EA and mix with acid, so I don't have my final results yet to vouch for this.

The colder the EA gets, the more likely condensation is to form around it, which may confound the attempts at water removal. Thus it would be a matter of ensuring that the EA can be kept away from atmospheric moisture while separating it from any ice crystals.

IIRC, it is necessary for there to be a little dissolved moisture in the EA to help the citric acid react effectively. It could be that freezing excessively might lead to the EA being too dry but that sort of negates my prior thoughts to a certain extent.

Water droplets are quite stick hence I typically find it unproblematic to separate a few drops of water from some other water-immiscible solvent because of how they stick to the beaker.

Either way, once you've separated the EA from the water there's little reason to believe that you'll encounter difficulties. At the same time there's only really one way to find out what happens with your proposed adjustment.

I have tried freeze-drying solvent in similar circumstances but that was with butyl acetate and desiccant dried acetone so the results aren't really comparable. So, all that said, maybe best wait for someone who's practiced with CIELO to the letter rather than my haphazard 'CIB(A)LO' tinkerings because there could be a nuance that I've overlooked as a result.

I think it should work. We've seen the ice before. It is a standard part of the reuse process.

Looking forward to what you get. Ideally a split can be done to check yield with the freezer. Good luck.

This would be a cool thing to attempt next time, I already separated my liquids and added acid, so unfortunately can't test this out.



Interesting points, I did notice that condensation was forming very quickly as soon as I took my jar out. But if the dryness of freezing cancels out the condensation, that would be good. Otherwise I imagine you could use something like an EA safe plastic to freeze it in so there would be less condensation, as well as pour as fast as possible from the fridge.



As a general update, I acidified my EA over 24 hours ago, the liquid is still cloudy today with no visible crystals, I can't recall if this was the same last time, but I'm going to give it the full 72 hours before I worry lol

So an update:

Unfortunately I still got a ton of brown goo, poured it into a dish, let it dry a bit but there was a lot stuck in my jar, so I added a tiny bit of water and recrystalized.

This is the final result:


That is 4g, but I can't say what the true yield is because this also includes a few of my failed previous attempts.

Weird thing is that it was quite a bit of goo, so I must either have not waited long enough for the water to collect in the fridge.

I will probably try the freeze method again with more patience next time and see if I get better results.

In the meantime, I will probably do some fine EA washes of the crystals to hopefully remove the brown color.

Product looks mostly xtaline and decent.

Have you tried the standard 24h fridge and decant method yet?

By that do you mean just doing the regular CIELO tek? If so that's basically what I did besides the accidentally freezing the water in the 24 hr fridge step. (my guess with how I ended up with good is probably just not waiting long enough, or just bad pouring technique)


For a more general update, I tried washing the brown crystals with fresh EA with a coffee filter but that didn't do much, the crystals are kind of sticky and don't come apart very easily. As a result there was hardly any change after a few washes (I even used a glass stick to try to stir/break crystals up). I have decided to call this good enough and hopefully execute the the tek better next time.

Yep that's what I mean. Result looks decent and you get to where you want with time. I think the product you have will be very adequate already. A very small amount of impurity can change the color/feel of the xtals.