- Purification of Acetic acid
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Usual impurities of (CAS NO.) are traces of and other oxidisable substances and water. (Glacial acetic acid is very hygroscopic. The presence of 0.1% water lowers its m by 0.2°C.) Pwificd by adding some acetic anhydride to react with water present, heating for 1h to just below boiling in the presence of 2g CrO3 per 100 mL and then fractionally distilling. Instead of CrO3, 2-5% (w/w) of KMnO4, with boiling under reflux for 2-6h, has been used.
Traces of water have been removed by refluxing with tetraacetyl diborate (prepared by warming 1 part of boric acid with 5 parts (w/w) of acetic anhydride at 60°C, cooling, and filtering off), followed by distn.
Refluxing with acetic anhydride in the presence of 0.2g % of 2-naphthalenesulfonic acid as catalyst has also been used. Other suitable drying agents include CuSO4 and chromium triacetate: P2O5 converts some acetic acid to the anhydride. Azeotropic removal of water by distn with thiophene-free benzene or with butyl acetate has been used. An alternative purification uses fractional freezing.
Rapid procedure: Add 5% acetic anhydride, and 2% of CrO3. Reflux and fractionally distil.
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