New York Paper - The Determination of Sulphur in Sulphides and in Coal and Coke

The use of bromine as an oxidizing agent, particularly for sul phur, has become very general in analysis, replacing the stronger oxidizing acids. The object of this paper is to describe briefly the experience which we have gained with this reagent in the laboratory of Lafayette College in the oxidation of metallic sulphides. Most of the simple sulphides, as blende, pyrite, etc., when exposed to the combined action of an alkaline hydrate and bromine, and finally to hydrochloric acid, are completely and promptly dissolved. The procedure is as follows: The very finely pulverized mineral is first treated, in a beaker, with a solution of sodium hydrate of a spe cific gravity of 1.25, and heated ; bromine is then cautiously added to supersaturation, and finally hydrochloric acid to acid reaction. If any of the sulphide is not taken up, the same operation may be re peated. It is necessary, however, that the mineral be very finely pulverized. Instead of using the pure bromine, a saturated solu tion of bromine in potassium bromide may be used with equally good effect. The process is advantageously simplified by making a saturated solution of bromine in the concentrated alkali. This is done by pouring bromine into a solution of sodium hydrate, of the above given specific gravity, until no more is taken up, and then adding a little of the sodium hydrate solution until the liquid does not give off free bromine. The procedure with this solution is as follows: The pulverized mineral is moistened with, say, 10 cc. of the solution, and heated, then hydrochloric acid added to just acid reaction. Two more additions of the alkaline solution, in amounts of 20 cc. each, are added at intervals of about ten minutes, each addition being followed by hydrochloric acid. The total amount of the alkaline solution (containing the bromine) used is, therefore, 50 cc., and the amount of hydrochloric acid should not exceed that necessary to make the solu tion acid after each addition of the alkali. The mixture should be kept hot. After the final addition of acid, the contents of the beaker is taken to dryness and heated in an air-bath to 110° to 115°C., to render silica insoluble. The dry mass is then taken up by hydro' chloric acid and water and, after filtration, the sulphuric acid is pre