Abstract

An improved, automated methods for the determination of bismuth in geological materials at the sub-microgram per gram level is described. After a closed-vessel digestion using nitric, hydrochloric, and hydrofluoric acids and evaporation twice with perchloric acid, a hydrochloric acid solution of the sample is automatically mixed with masking and reducing agents, further acidified with hydrochloric acid, and finally reacted with sodium borohydride to form bismuthine (BiH/sub 2/). The bismuthine is then separated from the analytical stream using a modified phase separator and then decomposed in a quartz tube furnace positioned in the path of an atomic absorption spectrophotometer. Bismuth quantification is done using aqueous calibration standards and peak height measurements. Interferences are minimized, therefore allowing the analysis of most geological materials without the method of standard additions. The relative standard deviation of the digestion and instrumental procedure is 2.0% at 50..mu..g Bi/L. The reagent blank is 0.2 ..mu..g Bi/L. Results for 32 standard reference materials are presented, 14 of which do not have published Bi values.

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