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通过铁收集和黄原酸盐萃取分离后,用石墨炉原子吸收光谱法测定矿石、精矿及相关材料中的碲。

Determination of tellurium in ores, concentrates and related materials by graphite-furnace atomic-absorption spectrometry after separations by iron collection and xanthate extraction.

作者信息

Donaldson E M, Leaver M E

机构信息

Mineral Sciences Laboratories, Canada Centre for Mineral and Energy Technology, Department of Energy, Mines and Resources, Ottawa, Canada.

出版信息

Talanta. 1990 Feb;37(2):173-83. doi: 10.1016/0039-9140(90)80020-g.

Abstract

A method for determining approximately 0.01 mug/g or more of tellurium in ores, concentrates, rocks, soils and sediments is described. After sample decomposition and evaporation of the solution to incipient dryness, tellurium is separated from > 300 mug of copper by co-precipitation with hydrous ferric oxide from an ammoniacal medium and the precipitate is dissolved in 10M hydrochloric acid. Alternatively, for samples containing 300 mug of copper, the salts are dissolved in 10M hydrochloric acid. Tellurium in the resultant solutions is reduced to the quadrivalent state by heating and separated from iron, lead and various other elements by a single cyclohexane extraction of its xanthate complex from approximately 9.5M hydrochloric acid in the presence of thiosemicarbazide as a complexing agent for copper. After washing with 10M hydrochloric acid followed by water to remove residual iron, chloride and soluble salts, tellurium is stripped from the extract with 16M nitric acid and finally determined, in a 2% v/v nitric acid medium, by graphite-furnace atomic-absorption spectrometry at 214.3 nm in the presence of nickel as matrix modifier. Small amounts of gold and palladium, which are partly co-extracted as xanthates if the iron-collection step is omitted, do not interfere. Co-extraction of arsenic is avoided by volatilizing it as the bromide during the decomposition step. The method is directly applicable, without the co-precipitation step, to most rocks, soils and sediments.

摘要

本文描述了一种测定矿石、精矿、岩石、土壤和沉积物中碲含量约0.01μg/g及以上的方法。样品分解并将溶液蒸发至近干后,碲通过与氢氧化铁在氨性介质中共沉淀,从大于300μg的铜中分离出来,沉淀溶解于10M盐酸中。或者,对于含300μg铜的样品,将盐类溶解于10M盐酸中。所得溶液中的碲通过加热还原为四价态,并在硫代氨基脲作为铜的络合剂存在下,从约9.5M盐酸中通过单次环己烷萃取其黄原酸盐络合物,与铁、铅及其他各种元素分离。用10M盐酸随后用水洗涤以除去残留的铁、氯离子和可溶性盐后,碲用16M硝酸从萃取物中反萃取出来,最后在2%(v/v)硝酸介质中,在镍作为基体改进剂存在下,于214.3nm处用石墨炉原子吸收光谱法测定。如果省略铁的收集步骤,部分以黄原酸盐形式共萃取的少量金和钯不产生干扰。在分解步骤中通过将砷挥发为溴化物避免其共萃取。该方法无需共沉淀步骤,直接适用于大多数岩石、土壤和沉积物。

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