Halifax Paper - Mr. E. D. Campbell's Colorimetric Process for Estimating Phosphorus in Iron and Steel

The greatest objection to be brought against the present methods for estimating phosphorus in iron and steel, is the time consumed in the operation. The following method, originated and perfected by Mr. E. D. Campbell, assistant in the chemical laboratory of the University of Michigan, will, 1 think, if carefully followed out, give results that are sufficiently accurate for technical purposes, and will give them in less time than they can be obtained by any other process. The process consists in comparing the color obtained by the action of stannous chloride upon a solution of the phospho-molybdate precipitate obtained from the solution of iron or steel, with that obtained from a standard solution of molybdie acid which represents a given amount of phosphorus. The operation is as follows : Take of ordinary steel 1 grm. and treat as in any of the wellknown processes until the phosphorus is precipitated as ammoniumphospho-molybdate. When precipitated, the phospho-molybdate precipitate is filtered out, thoroughly washed with an acid solution of ammonium nitrate, and, finally, twice with water, to remove most of the ammonium nitrate. The precipitate is then dissolved in about 1 c. c. of 10 per cent. potassium hydrate, which is let fall drop by drop on the filter till the precipitate is dissolved ; the filter is now washed with about 25 or 30 c. c. of water, and the potassium hydrate solution, which now consists of 25-32 c. c. of solution, is boiled until the peculiar frothy appearance, which first appears on boiling, is entirely gone. The solution is then cooled until perfectly cold, and about 10 or 15 c. c. of strong hydrochloric acid added ; if the solution is kept cold this will form no precipitate, but a light yellow or colorless solution. The solution is now ready for the addition of stannous chloride, and the subsequent comparison of color produced with that obtained from the standard molybdie acid. The comparison is made in tubes that are calibrated like carbon-tubes, but which are larger, about 5/8-inch bore, and graduated to 100 c. c.; this makes them about 18 inches long. To make the comparison of color, first transfer the now acid solu