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方波极谱测定铅是很灵敏的,用它测定纯硅中的微量铅(<0.001%)是比较理想的方法。由于铅在许多底液中均可产生良好的还原波,所以在选用底液时应考虑空白的影响。盐酸底液波形好,空白低,但又存在铅波与锡波的重叠干扰。本法用加溴水加热赶锡,消除了锡的干扰,纯硅中的共存元素除锡外均不影响铅的测定。在3N盐酸介质中,铅的峰电位为-0.48伏(对汞池阳极),铅含量在0～0.4微克/毫升,波高与浓度呈线性关系。试样加标准回收率为92～102%,本法与X-荧光,原子吸收法测定数据进行对照,结果一致。
Square-wave polarography is very sensitive to the determination of lead, using it to determine trace lead in pure silicon (<0.001%) is the ideal method. Because lead can produce good reduction waves in many bottom fluids, the effect of a blank should be taken into account when choosing a bottom fluid. Hydrochloric acid bottom liquid waveform is good, the space is low, but there is overlap of lead wave and tin wave interference. This method is heated with bromine water to catch tin, eliminating the interference of tin, pure silicon in addition to elements of tin do not affect the determination of lead. In 3N hydrochloric acid medium, the peak potential of lead is -0.48 V (for mercury anode) and the lead content is 0 to 0.4 μg / mL. The wave height is linear with the concentration. The standard recovery of the sample was 92 ~ 102%, the method with the X-fluorescence, atomic absorption spectrometry data for control, the results are consistent.