- Joined
- Dec 4, 2021
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Also, something strange:
I saved the black slurry part of the reaction mixture, and combined it with the aqueous layer from the freebase separation. Poured in a bunch of acetone and left it standing overnight in a temperature just above freezing.
When I came to fetch it this morning there was the expected clear layer on top, but the bottom layer was SOLIDIFIED with clear, rock hard crystals. So hard the have to be chiseled loose. I tried solving some of them in tolune, acetone and water, but they're insoluble. The crystals themselves are clear as ice, but they.ve formed around the black nanoslurry of the CuSO4.
See attached picture taken into the beaker.
What on earth could this be?
I saved the black slurry part of the reaction mixture, and combined it with the aqueous layer from the freebase separation. Poured in a bunch of acetone and left it standing overnight in a temperature just above freezing.
When I came to fetch it this morning there was the expected clear layer on top, but the bottom layer was SOLIDIFIED with clear, rock hard crystals. So hard the have to be chiseled loose. I tried solving some of them in tolune, acetone and water, but they're insoluble. The crystals themselves are clear as ice, but they.ve formed around the black nanoslurry of the CuSO4.
See attached picture taken into the beaker.
What on earth could this be?
Attachments
- Joined
- Dec 4, 2021
- Messages
- 442
- Solutions
- 1
- Reaction score
- 431
- Points
- 63
After giving it some thought and a bit of experimentation, I'm pretty sure these are borate crystals. They dissolve just fine in warm acidified water.
- Joined
- May 21, 2022
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- By WinterDust
-
13 Jan
@MadHatter, jesus christ this has annoyed me for a long time, but I can finally put it into rest.
You are correct, the "sludge" is borate crystals from the NaoH, I just did another reaction and the outcome was exactly the same.
Best regards
You are correct, the "sludge" is borate crystals from the NaoH, I just did another reaction and the outcome was exactly the same.
Best regards