Boston Paper - A Method for the Estimation of Manganese in Steel

The determination of manganese by precipitation with potassium chlorate from a solution in concentrated nitric acid, filtration through asbestos, and solution in a reducing agent whose excess is estimated, is open to the objections that the filtration and subsequent solution of the binoxide are apt to be very slow, and that the asbestos may (according to Troilius), unless perfectly purified, affect the titration. In the following modification, filtration is avoided. I give the method as I use it for Bessemer steel. In an 8-ounce Griffen beaker dissolve 1 gramme drillings in 15 c.c. nitric acid (1.2 sp. gr.). Evaporate to 5 c.c.; add 20 c.c. concentrated nitric acid and precipitate with chlorate as usual, avoiding a large excess; then add about 60 c.c. warm water, and 10 c.c. of the oxalic solution; stir until of a clear light yellow color, and titrate with permanganate while the solution is at about 80' C. The binoxide should dissolve immediately when the oxalate isadded. The titration is rapid, and the end-reaction, though transient, easily caught after a little practice. The standard solutions used are: 15 grammes crystallized ammonium oxalate to a liter, and 1.6 grarnmes potassium permanganate to a liter. For standardizing the permanganate, to 10 c.c. of the oxalic solution is added 50 c.c. of hot water, and a solution of 1 gratnme of steel in concentrated nitric acid, from which the manganese has been removed by potassium chlorate and filtration through asbestos. I have made a large number of determinations in steel, pig-iron,