This section is from "Scientific American Supplement Volumes 275, 286, 288, 299, 303, 312, 315, 324, 344 and 358". Also available from Amazon: Scientific American Reference Book.
By H SCHAEPPI.
Ten grms. of sulphur, pulverized as finely as possible, are covered with hot water and a few drops of nitric acid digested for some time, filtered, and washed till the washings have no longer an acid reaction. Thus calcium chloride and sulphate are removed, and calcium sulphide, if present, is destroyed. The sulphur thus prepared is covered with water at 70° to 80°, a few drops of ammonia are added, and the mixture is digested for a quarter of an hour. All the arsenic present as sulphide is dissolved, and the ammoniacal liquid is variously treated according to the degree of accuracy required. For perfectly accurate determinations the ammoniacal solution is mixed with silver nitrate, and all the sulphur present in the state of arsenic sulphide is thrown down as silver sulphide, acidified with nitric acid, filtered, and washed. The precipitate of silver sulphide is dissolved in hot nitric acid and determined as silver chloride. From the weight of the latter the arsenic sulphide is calculated. As a less accurate but more rapid method, the ammoniacal solution of arsenic sulphide is cautiously neutralized with pure dilute nitric acid and considerably diluted. It is then titrated with decinormal silver nitrate till a drop of the solution is turned brown with neutral chromate. The arsenic is easily calculated from the quantity of silver nitrate consumed. For very rough determinations it is sufficient to treat ten grms. of finely-ground sulphur with nitric acid, to extract with ammonia, and to add silver nitrate. From the intensity of the color, or the quantity of the precipitate of silver sulphide, it may be judged if the sulphur is approximately free from arsenic or strongly contaminated. The author states that, contrary to the general belief, reddish yellow sulphur is more free from arsenic than such as is of a full yellow color.