Spectrochemical Assay for Traces of Tungsten

THE research laboratory of this Company was recently faced with the problem of determining trace amounts of tungsten in a series of classifier sands. A spectrographie survey revealed the feasibility of using this instrument in the final evaluation, but a check of the common methods in use for the isolation of tungsten (3, 4) showed these methods to give incomplete separation for trace amounts. An investigation into the possibility of modifying these procedures, or developing others, was thus indicated. ASSAY PROCEDURE Weigh 10 grams of 200-mesh ore or concentrate into a 400-ml. beaker, wet the sample well with about 20 ml. of water, and add 100 ml. of hydrochloric acid. Cover, digest at 60° to 70° C. for about 1 hour, and then boil down to approximately 25 ml. Cool, add 25 ml. of hydrochloric acid and 10 ml. of nitric acid, and again boil to former volume. Add 20-ml. portions of nitric acid with successive boiling clown until chemical action is complete. Then add 20-ml. portions of hydrochloric acid until all nitric acid is removed. Take nearly to dryness on a law-temperature hot plate, but do not bake. Take up in 10 ml. of hydrochloric acid and 20 ml. of water and heat on a law-temperature hot plate until all iron goes into solution. Dilute to 200 ml. and heat to just below boiling. Stir in pulp of about half of a No. 41 Whatman filter paper (12.5-cm.) and continue digestion on plate with occasional stirring for 15 to 20 minutes.