Determination of acetic anhydride in presence of acetic acid

Acetic anhydride, in the presence of pyridine, reacts quantitatively with anhydrous oxalic acid to form acetic acid, carbon dioxide, and carbon monoxide. Based on this reaction, two small-scale procedures have been devised for the determination of this anhydride. The first, in adaptation of Rosenbau...

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Bibliographic Details
Published in:Microchemical journal 1965-01, Vol.9 (4), p.423-428
Main Authors: Tiwari, R.D., Sharma, J.P., Shukla, I.C.
Format: Article
Language:English
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Summary:Acetic anhydride, in the presence of pyridine, reacts quantitatively with anhydrous oxalic acid to form acetic acid, carbon dioxide, and carbon monoxide. Based on this reaction, two small-scale procedures have been devised for the determination of this anhydride. The first, in adaptation of Rosenbaum's macroprocedure, involves reaction of a 10–25 mg sample with a weighed amount of oxalic acid under appropriate conditions and titration of the excess of this acid with permanganate. The second procedure involves reaction of a 10–15 mg sample with the pyridine-oxalic acid mixture in a special vessel, sweeping of evolved gases with oxygen through a sulfuric acid trap, conversion of carbon monoxide to carbon dioxide by passage through a heated tube packed with copper oxide, and a gravimetric finish based on absorption of the dioxide by sodium hydroxide-coated asbestos.
ISSN:0026-265X
1095-9149
DOI:10.1016/0026-265X(65)90065-2