Note on the estimation of borate in natural waters
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Methods are described which afford a determination of each member of the alkali group and are successful in dealing with the quantities of the rare alkalies found in rocks and minerals. The procedures are relatively rapid and based chiefly on the use of chloroplatinic acid, absolute alcohol and ether, and ammonium sulfate. The percentages of all the alkalies found in a number of minerals are given.
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Fluorine in minerals may be determined with the nephelometer to about 1 per cent of the fluorine. The determination is made on an aliquot of the sodium chloride solution of the fluorine, obtained by the Berzelius method of extraction. The fluorine is precipitated as colloidal calcium fluoride in alcoholic solution, gelatin serving as a protective colloid. Arsenates, sulfates, and phosphates, which interfere with the determination, must be removed.
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The zirconium-alizarin method has been modified to facilitate the convenient and accurate determination of small amounts of fluoride in a large number of water samples. Sulfuric acid is used to acidify the samples to reduce the interference of sulfate. The pH is accurately controlled to give the most sensitive comparisons. Most natural waters can be analyzed by the modified procedure without resorting to correction curves. The fluoride content of waters containing less than 500 parts per million of sulfate, 500 parts per million of bicarbonate, and 1000 parts per million of chloride may be determined within a limit of about 0.1 part per million when a 100-ml. sample is used.
The preliminary hearth heating method (A and E) gave results within the A. S. T. M. tolerances for all duplicates obtained in the same laboratory. Checks between different laboratories within A. S. T. M. tolerances were obtained for coals containing up to about 3.6 per cent mineral carbon dioxide, but these ashes contained larger amounts of retained sulfur. The determination of ash by the cold furnace method (B and F) gave duplicate results within A. S. T. M. tolerances for all samples in the U. S. Bureau of Mines laboratory and for samples up to about 1.6 per cent mineral carbon dioxide content in the Illinois Geological Survey laboratory. Checks between average values from the two laboratories were within A. S. T. M. tolerances for all samples.
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The well-known tendency of cobalt to be retained by the iron-alumina precipitate produced by ammonia has generally been ascribed to a specific adsorption by the large surface of this gelatinous precipitate. Whatever its cause, it can be overcome by precipitating the iron as phosphate at a pH of 3.5. The precipitate is easily filterable and practically all the cobalt passes into the filtrate.