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Volumetric analysis of metals in glacial acetic acid. Casey, Allan Terence


Recent work has demonstrated that certain metal salts of inorganic acids may easily be titrated with perchloric acid in glacial acetic acid. To test the accuracy of the method, a series of titrations was run on the acetates of twenty-three representative metals. The resulting curves show that accurate reproducible end points may be obtained for the acetates of the more electropositive metals, while those of aluminum, chromium and iron yield anomalous results. An explanation for this is offered. The acetates of tin, bismuth, antimony, uranium and copper are too weak to be determined by this method. Metals, oxides, or other more difficultly soluble compounds may be conveniently introduced into acetic acid solution by first dissolving in nitric acid (or in certain cases aqua regia), followed by the addition of sufficient acetic anhydride to react with all the water and decompose all the nitrate present. Quantitative analytical separations may be effected using such common reagents as oxalic, nitric, and tartaric acid, hydrogen iodide and hydrogen sulphide. They were used in analysing eleven metal mixtures, with accuracy comparable to the more lengthy gravimetric process often required in aqueous solution.

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