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Author: Subject: Glacial Acetic Acid synthesis wo sulfuric
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[*] posted on 18-5-2017 at 06:14

Hi J_SUM1,
I reckon that I was rough as guts with the temperature, so that may have something to do with it.

The SO2 smell suggests some chemical change.
Also, my effort reported above was without stirring: I was relying on the NaHSO4.H2O melting at 58 degrees, thereby allowing the reaction to take place. In retrospect, the Na2SO4.4H2O may have grabbed the water as soon as formed and prevented this from happening. It would be worth repeating with more controlled temperature, and mixing which I currently do not have.

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[*] posted on 18-5-2017 at 16:18

Sodium bisulfate and potassium bisulfate have a eutectic around 140 C. I'd try making that (liquid) and adding an acetate salt to the melt, probably calcium acetate (CaSO4 precipitates?).

Might be able to convert some NaHSO4 to KHSO4 by recrystallization. Possibly by taking advantage of the low solubility of potassium persulfate K2S2O8 which can then decompose/rehydrate to KHSO4.
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