焦性没食子酸树脂相光度法测定痕量钒(Ⅴ)
RESIN-PHASE PHOTOMETRIC DETERMINATION OF VANADIUM(Ⅴ) WITH PYROGALLIC ACID AS COLOR REAGENT
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摘要: 于pH 6.6的乙酸盐缓冲溶液中,五价钒离子与焦性没食子酸反应生成有色络合物.此络合物可吸附于717强碱性阴离子交换树脂上,并在树脂相上于600 nm波长处,以按试样分析相同步骤制备的树脂空白作参比测得其吸光度.对显色反应、呈色络合物在树脂上的吸附、共存离子的干扰及其消除等条件作了研究和优化.在树脂相光度测定的条件下,钒(Ⅴ)浓度在0-37 μg/25 mL间遵守比耳定律,摩尔吸光系数达5.57×104L·mol-1·cm-1,约为水相测定的10倍,应用于测定钢中钒,大量铁(Ⅲ)须预先用溶剂萃取予以分离,显色时再加CyDTA作掩蔽剂,测定结果的RSD(n=5)值小于3%,回收率在98.6%-102.6%之间.Abstract: In an acetate buffer medium of pH 6.6,a colored complex was formed between pentavalent vanadium ion and pyrogallic acid.The colored complex was then adsorbed onto 717 strongly alkaline anion exchange resin,and its absorbance was measured on the resin phase at the wavelength of 600 nm againt a resin blank treated in the same way as in the sample analysis.The conditions of the color reaction,the adsorption of the colored complex onto the resin,the interference of co-existing ions and its elimination were studied and optimized.Under the condition of resin-phase photometry,Beer′s law was kept in the range of 0-37 μg per 25 mL of solution with a molar absorptivity of 5.57×104L·mol-1·cm-1,which is 10 time greater than the value measured in aqueous solution.Vanadium in steel was determined by this method after removal of the matrix iron(Ⅲ) by solvent extraction and masking by adding CyDTA.RSD of the results was found to be less than 3%,recoveries obtained were in the range of 98.6%-102.6%.