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催化极谱法测锡具有很高的灵敏度,一般可测至0.0001％。主要有锡—卤素—钒体系、锡—硫酸—氯化钠—氯化四苯胂体系等,其中以锡—卤素—钒体系的灵敏度最高。我们对锡—卤素—钒体系进行了筛选,并确定利用高氯酸和碘化钾的反应制备氢碘酸作底液来测定钢铁中微量锡的分析流程。本法可不经任何分离和富集手续,直接测定0.0001～0.1％的锡,测定0.0x％时,相对偏差小于10％,分析结果与标准值很吻合。 一、仪器与试剂 JP—1A型示波极谱仪,三电极系统,在导数电路上并联1个10000PF的电容器。 盐酸为特纯试剂,硝酸、高氯酸、碘化钾均为优级纯试剂,其余试剂为分析纯级。 所用的水为二次离子交换水。
Catalytic polarographic determination of tin has a high sensitivity, generally measurable to 0.0001%. The main tin - halogen - vanadium system, tin - sulfuric acid - sodium chloride - tetraphenylarsine chloride system, of which tin - halogen - vanadium system, the highest sensitivity. We screened the tin-halogen-vanadium system and determined the analytical procedure for the determination of trace amounts of tin in steel using the reaction of perchloric acid and potassium iodide to prepare hydriodic acid as the bottom liquid. This method can be directly measured 0.0001 ~ 0.1% tin without any separation and enrichment procedures, the relative deviation of less than 10% when the determination of 0.0x%, the analysis results are consistent with the standard values. First, instruments and reagents JP-1A-type oscilloscope polarography, three-electrode system, parallel in the derivative circuit of a 10000PF capacitor. Hydrochloric acid as a pure reagent, nitric acid, perchloric acid, potassium iodide are excellent grade pure reagent, the rest of the reagents for analytical grade. The water used is secondary ion exchange water.