RI 7184 Colorimetric Method For Arsenic In Coal

A chemical method of determining microgram quantities of arsenic in coal was investigated by the Bureau of Mines to supplement a semiquantitative spectrographic method of determining arsenic in coal ash. In accordance with a method recommended by the International Organization for Standardization, 1-gram samples of coal are decomposed by wet oxidation with boiling sulfuric acid (H2S04) and nitric acid (HN03) to remove the organic matter. After heating to fumes of SO3 to remove HN03, the arsenic is separated as arsine by the action of zinc in H2S04 solution. The arsine is absorbed in dilute iodine solution in which the arsenic is determined colorimetrically by the molybdenum-blue reaction. Two modifications of the method for obtaining the arsenic in solution, in addition to the wet oxidation method, give satisfactory results. The modifications are (1) furnace ashing with MgO added to the coal, followed by treatment with H2S04, and (2) extraction of arsenic from the coal by dilute HNO3 without ashing. Float-and sink-tests show that arsenic is associated mainly with mineral matter in the three coals examined. High-temperature ashing tests show that very little arsenic is volatilized from coal ash below 1,000° C, but it is virtually all removed from the ash at 1,300° C.