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The toughest part...

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muad dib

muad dib

Rising Star
Of the whole extraction process has been bringing a jar full of xtals from freezing to room temperature...

So far, the technique I have developed is as follows:

1) Turn your container upside down after pouring off the majority of the solvent to squeeze out a bit more while everything is still <32f - tilt the container slightly while doing so
2) Place containers from the freezer into the refrigerator once the remaining solvent has drained away and been released
3) Place containers atop something that can retain a cooler temperature like a pyrex dish to further ease the containers to room temperature, making sure they are tilted to allow air to circulate
4) Crack fridge door to prevent moisture buildup
5) Use a small, high rpm fan to vent off traces of solvent while in the fridge and once you think it's safe to remove the containers
6) Remove pyrex dish along with containers to further slow the cooling of the containers and continue to use a fan (the dish retains the coolness of the fridge

Am I over-thinking this? Is there a better way? I live in a fairly humid environment so condensation is likely more of a problem for me than many nexians.

Thanks!
Muad'dib
 
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Why bother so much?

Once finished freeze-precipitation I remove my beaker sealed with food wrap film from the freezer. Warm it in my hands until there is no more condensation on the beaker walls. Unwrap it. Pour off the solven and dry the product under a fan on low. The beaker stands upright or slightly tilted, so no small loose crystals are blown away.

Am I doing something wrong?
 
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I use 1/2 pint mason jars for freeze precip's. I just pull it out, remove the ring, offset the lid and pour off the naphtha. The lid helps keeps loose crystals from falling out. I set it about 5 feet in front of a fan for a bit and that's it.
 
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I wouldn't bother so much, but I always end up with a meltage problem unless I go through the aforementioned steps... I also use 1/2 pint Mason jars.

I'm absolutely sure warming up the jar and immediately letting it sit at room temperature would result in melted goo even if the condensation is removed from the outside and the jar is sealed. There would surely still be some amount of solvent contained in the xtals that would cause them to melt once they started to warm.

I honestly have no idea where I could be going wrong, but it does feel necessary to bring them to room temperature extremely gradually. My only explanation is the humid climate I live in.

Does anyone else live in an area that gets regular 90-100% humidity have any light they could shed?

Thanks for the answers, guys.
Muad'dib
 
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WSaged said:
Buchner Funnel/Filter!!!
Click to expand...

I bought a tiny one especially for this purpose. Never had to use it. Spice is usually stuck to the beaker bottom and walls. Even if there are a few loose crystals, they fall to the bottom. There is no problem to decant naphta alone.

Am I exceptionally lucky?

muad dib said:
I wouldn't bother so much, but I always end up with a meltage problem unless I go through the aforementioned steps... I also use 1/2 pint Mason jars.

I'm absolutely sure warming up the jar and immediately letting it sit at room temperature would result in melted goo even if the condensation is removed from the outside and the jar is sealed. There would surely still be some amount of solvent contained in the xtals that would cause them to melt once they started to warm.
Click to expand...

Here is what I do differently:

1. My beaker is only 120 ml. That is more than enough, because I always reduce my NP solvent as much as possible.

2. Once I open the jar I immediately pour off the remaining solvent and put it under the fan. As long as there is any solvent in the jar, forced evaporation will cause noticeable temperature drop (it's simple physics). This keeps the spice from dissolving into the solvent. When the solvent is gone, there is no more meltage or rather redissolving problem.

3. Well, and after all, what's the problem with molten spice? It is as good as the fluffy crystalline one as long as all the solvent is gone.

muad dib said:
My only explanation is the humid climate I live in.
Click to expand...

Hmmm.. Could be. Ever checked your humidity? But then again, see point 3 above:).
 
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i freeze percipitate my spice in Ziploc Plastic Containers.
This way, the crystals still mildly adhere to the walls, but they come off clean if i just slightly brush them off with the round edge of a butter knife. Then i pour the resulting slurry through a coffee filter while ice cold, and press the crystals dry between the filter and some paper towel.

I find this much better than trying to work with glass dishes, sometimes the crystals just stick and smear over the glass when you try to remove them. Using a plastic container, your crystals will not stick and can simply be poured off :)

i feel that this should be added to the FAQ, because it made the toughest part A LOT EASIER for me.
 
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I use a method very much like trickster and it works like a champ.

No muss... no fuss... no moisture... no filtering.

Filtering seems to be a pain for no that will cause more yield loss than gain in my experience. If a few crystals get loose use that naptha again for the next extraction.
 
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seriously you guys, you are going do do a big facepalm once you try the plastic containers for freeze precipitation.
ZERO crystals stuck, they all end up in the coffee filter, and the naphtha that drains is used for the next pull.
 
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