Chicago, Ill Paper - The Estimation of Phosphorus in Iron and Steel

While engaged in experimenting with the usual methods for estimating phosphorus in iron and steel, it occurred to me that potassium chlorate might be used to oxidize the carbon, and thus avoid the tedious and vexatious evaporations necessary for successfully carrying out the usual methods. After many trials, the following plan was adopted : Take, for analysis, of Bessemer or other low-carbon steels, from 3 to 5 grammes; of crucible steel, 10 grammes; of pig-iron, 1 to 5 grammes, according to the percentage of phosphorus supposed to be present. Of iron, high in phosphorus (1 per cent.), take 1 gramme. Place in a No. 4 evaporating dish the amount of iron or steel decided upon, cover with a funnel which will just fit inside the dish, and then add gradually HNO3, (1.20 specific gravity), using 12 C.C. of acid for each gramme of steel or iron taken. (A larger quantity of acid will be required for small samples.) When the full amount of acid has been added, and the violent action has ceased, place the evaporating dish on a sand-bath, add 10 C.C. HNO3, (1.40 specific gravity), and boil till the bulk of the solution is reduced about onehalf. Then add 10 C.C. HNO3, (1.40 specific gravity), continue the boiling, and add from time to time, during the next 15 minutes, small portions of pulverized KCIO3, till about 2 grammes have been added. (If the solution shows signs of going dry, more strong acid must be added.) This will precipitate the manganese, with some iron. Sometimes it happens that the manganese does not come down readily, and more KCIO3, or further concentration, or both, will be required. The process is not complete till the manganese is precipitated, which may be known by the appearance of a dark, mirror-like deposit on the dish, at the edge of the solution. Boil the solution 5 minutes after the last addition of KCIO3, and then add cautiously (to prevent sudden explosions) 5 C.C. strong HCl. This will dissolve the precipitated manganese and iron. Continue the boiling till the chlorine is all expelled, adding from