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采用NaOH溶液溶解样品,并以HCl酸化。通过补加一定量的HCl(1+1),使分取后的试液酸度保持在约2%,以HCl(φ=2%)为载流,KBH4-K_3[Fe(CN)_6]-NaOH溶液为还原剂,实现了氢化物发生原子荧光光谱法对高硅铝合金中低含量铅的测定。试验优化了高硅铝合金碱溶酸化的最佳条件,考察了铝基体、钠基体以及其他杂质离子对测定结果的影响,其干扰可以忽略不计。在选定的工作条件下,铅的质量浓度在1~10μg/L范围内呈线性关系,相关系数为0.9997,方法检出限为0.33μg/g。按照实验方法对铝合金样品和标准样品进行测定,标准样品的测定值与给定值相符,相对标准偏差(RSD,n=6)在2.3%~5.3%之间。
Samples were dissolved with NaOH solution and acidified with HCl. By adding a certain amount of HCl (1 + 1), the acidity of the test solution after the dispensing was kept at about 2%. With KBH4-K_3 [Fe (CN) _6] - NaOH solution as reductant to achieve the determination of low content of lead in high silicon aluminum alloy by hydride generation atomic fluorescence spectrometry. The optimum conditions for alkali-acidification of high-silicon aluminum alloy were optimized. The effects of aluminum matrix, sodium matrix and other impurity ions on the determination results were investigated. The interference was negligible. Under the selected working conditions, the concentration of lead in the range of 1 ~ 10μg / L showed a linear relationship, the correlation coefficient was 0.9997, the detection limit was 0.33μg / g. According to the experimental method, the aluminum alloy sample and the standard sample are measured, and the measured value of the standard sample is in accordance with the given value, and the relative standard deviation (RSD, n = 6) is between 2.3% and 5.3%.