Birmingham Paper - Note on Arsenic Determination

The difficulty of exact neutralization by ammonia of the acid solution obtained in the determination of arsenic by the method of fusion with carbonate of soda and nitrate of potassium, led me to try the effect of neutralization by oxide of zinc. I obtained most satisfactory results, and found a great saving of time. The oxide of zinc being added in excess, there is no delicate testing with lit? mils paper and tedious alternate adding of dilute ammonia arid acid until the proper point is reached. The excess of oxide of zinc, too, seems to hold, from the filter, the gelatinous silica and alumina, which are usually precipitated upon neutralization, and thus to render the washing of the precipitated arseniate of silver almost invariably much more rapid. Except the substitution of the neutralization by oxide of zinc for the more tedious method by ammonia, the details of the process are practically the same as those published by Mr. Richard Pearce, of Argo, Colorado (Proceedings of the Colorado Scientific Society, vol. i.), who shows what very accurate results can be obtained by the fusion process. I have made numerous tests of comparison between the two methods of neutralization, and find that those by the oxide of zinc agree almost exactly with the old method. Increasing the quantity of nitric acid, even to considerable excess, to be neutralized by the oxide of zinc did not affect the precipitation of arseniate of silver. The process may be outlined as follows : Take 4 to 1 gramme finely pulverized ore, and mix in a porcelain crucible with eight to ten times its weight of a mixture of equal parts of carbonate of soda and nitrate of potassium (Kerl. Metallurgische Probirkunst gives 4 to 5 nitre to 14 soda). Gradually bring to fusion and keep so, three to five minutes. Cool. Disintegrate in hot water. Filter and wash with hot water. Acidify the filtrate with nitric acid, and boil to expel carbonic acid and nitrous fumes. Cool. Add an excess of an emulsion of oxide of zinc. The bottom of the beaker should have quite a layer of oxide of zinc, after stirring.