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本文试验了在醋酸缓冲液介质中,以少量锡(Ⅱ)作戴体,用铜试剂-氯仿萃取分离钨中微量釩的条件,经萃取分离获得的釩于20N硫酸介质中用2,2′-二2羧基二苯胺显色,于610毫微米处,进行光度测定。釩在5—50微克/25毫升范围内服从比耳定律,测定灵敏度为0.08微克/毫升。50毫克锡(Ⅳ)、1毫克钼(Ⅵ),500微克铜(Ⅱ)、镍(Ⅱ)、钴(Ⅱ)、铁(Ⅲ)不干扰。铬、铈等干扰,可在萃取时分离之。氧化还原性物质干扰,如过氯酸、硝酸等必须事先用硫酸冒烟赶尽。本法可测定三氧化钨中0.0005—0.03％釩,相对误差为±7—±12％,手续简便、快速。
In this paper, we studied the conditions for the extraction of trace vanadium from tungsten with a small amount of tin (Ⅱ) as a dopant in acetic acid buffer medium and the extraction of vanadium from tungsten by extraction with chloroform. - dicarboxy diphenylamine color, at 610 nm, photometric determination. Vanadium follows the Beer’s Law at a concentration of 5-50 μg / 25 ml and has an assay sensitivity of 0.08 μg / ml. 50 mg tin (Ⅳ), 1 mg molybdenum (Ⅵ), 500 μg copper (Ⅱ), nickel (Ⅱ), cobalt (Ⅱ) and iron (Ⅲ) did not interfere. Chromium, cerium and other interference can be separated in the extraction. Redox substance interference, such as perchloric acid, nitric acid, etc. must be preceded by sulfuric acid smoke rush. This method can be determined tungsten trioxide 0.0005-0.03% vanadium, the relative error of ± 7- ± 12%, the procedure is simple and fast.