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Problem with recent freeze precip

F

froggydays

Esteemed member
Hi,

I have done a few successful extractions with a/b tek and freeze precipitation. However recently I have ended up a few times now with some kind of water/icy precipitate (see for example the big central blob in the picture) that melts after I get the boxes out of the freezer, instead of obtaining the normal dmt white or yellow crystals that dry out.

One caveat is that I have been, as I read should be possible, reused the same naphta (zippo lighter fluid) for all runs. Can this be a problem? I do notice that even after 12 hours there is always some residue in the soluble naphta when I pour it off.

One other problem i might think off I may have added too much vinegar? Can you easily add too much?

Method:
Heat jurema with vinegar 3 hours
Add NaOH
Zippo (60, 40mL consecutively)
Invert solution several times
Freeze precipitate for 12+ hours

Thanks for any suggestions!
 

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Are you covering your collection dish while It is the freezer?

Are you able to work in your freezer while you decant your napatha? Keep everything cold while you work, then get it under a fan once your solvent is removed...

Just some ideas I'm sure someone else will chime in with some ideas


Skunk
 
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froggydays said:
Okay I do cover them but I'm not sure they're airtight, that could indeed be a reason, thanks. I'll try it.

What do you mean with decant?
Click to expand...
By decanting I'm referring to removing the Napatha from the collection dish, I have a large deep freeze, and find it works best to actually work in the freezer while I remove the solvant from the collection dish. it helps keep everything cold and helps prevent the DMT crystals from melting back into the napatha.

I find when you remove it from the freezer the napatha wilk heat up quickly and make a mess.

Once I've removed all the napatha from the dish in the freezer, ill have a fan set up and put the dish on its side with a coffee filter under the dish land let everything dry and evaporate off.

froggydays said:
I will for now order some new containers and naphta.

Thanks!
Click to expand...
I just cover my dish with cling wrap / plastic kitchen saran wrap. That seals it up pretty tight.

Skunk
 
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Even if they are airtight (as they should be), naphtha will end up absorbing water. An easy way to dry it is just to add a certain amount of calcium chloride to it (in an airtight container), leave it from some hours, and pour carefully while filtering the naphtha. That should leave it completely dry.
 
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SkunK said:
By decanting I'm referring to removing the Napatha from the collection dish, I have a large deep freeze, and find it works best to actually work in the freezer while I remove the solvant from the collection dish. it helps keep everything cold and helps prevent the DMT crystals from melting back into the napatha.

I find when you remove it from the freezer the napatha wilk heat up quickly and make a mess.

Once I've removed all the napatha from the dish in the freezer, ill have a fan set up and put the dish on its side with a coffee filter under the dish land let everything dry and evaporate off.


I just cover my dish with cling wrap / plastic kitchen saran wrap. That seals it up pretty tight.

Skunk
Click to expand...
Okay thanks! I do remove or decant the naphta immediately after I get the containers out of the freezer. Unfortunately I don't have a standalone freezer in my home.

I'll look up the "wet" naphta part later.

I also tried to freeze precipitate the naphta I have left now after a few runs, but that didnt really result in much. Same issue, lot of ice on the bottom but afterwards no crystals.
 
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