Determination of chlorine in rocks, soils and organic materials by heating powdered sample in strong phosphoric acid, and some additional investigations on the related reactions.

概要

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The decomposition of several salts in strong phosphoric acid (SPA) was examined. These halides were decomposed and hydrogen halides evolved by heating the samples with SPA at various temperatures. Based on these data an adequate reagent was chosen for the efficient separation of various elements which can form volatile halides. The recommended distillation condition was applied to determine the chlorine content in solid samples, such as rocks, soils or some organic materials. The sample was heated in an SPA medium and a distillate of hydrogen chloride was absorbed in a sodium hydroxide solution. The solution was subjected to volumetric analysis with a silver nitrate solution for chlorine in the range of 10−2 to 10−4 mol and to spectrophotometric determination with mercury thiocyanate for elements less than 10−4 mol. Furthermore, from the results of X-ray diffraction measurements of the original and the SPA-treated samples, it was confirmed that the main crystal structure of a rock sample could be decomposed by heating with SPA. The chlorine analysis was performed for Japan Geological Survey standard rocks, JG-1 and JB-1, and a synthesized complex compound.
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