An Introductory Course of Quantitative Chemical Analysis - With Explanatory Notes by Henry P. Talbot
page 95 of 272 (34%)
page 95 of 272 (34%)
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oxidizing agent, and for the production of chlorine, depends upon the
percentage of MnO_{2} in the sample. This percentage is determined by an indirect method, in which the manganese dioxide is reduced and dissolved by an excess of ferrous sulphate or oxalic acid in the presence of sulphuric acid, and the unused excess determined by titration with standard permanganate solution. PROCEDURE.--Grind the mineral in an agate mortar until no grit whatever can be detected under the pestle (Note 1). Transfer it to a stoppered weighing-tube, and weigh out two portions of about 0.5 gram into beakers (400-500 cc.) Read Note 2, and then calculate in each case the weight of oxalic acid (H_{2}C_{2}O_{4}.2H_{2}O) required to react with the weights of pyrolusite taken. The reaction involved is MnO_{2} + H_{2}C_{2}O_{4}(2H_{2}O) + H_{2}SO_{4} --> MnSO_{4} + 2CO_{2} + 4H_{2}O. Weigh out about 0.2 gram in excess of this quantity of !pure! oxalic acid into the corresponding beakers, weighing the acid accurately and recording the weight in the notebook. Pour into each beaker 25 cc. of water and 50 cc. of dilute sulphuric acid (1:5), cover and warm the beaker and its contents gently until the evolution of carbon dioxide ceases (Note 3). If a residue remains which is sufficiently colored to obscure the end-reaction of the permanganate, it must be removed by filtration. Finally, dilute the solution to 200-300 cc., heat the solution to a temperature just below boiling, add 15 cc. of a manganese sulphate solution and while hot, titrate for the excess of the oxalic acid with standard permanganate solution (Notes 4 and 5). |
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