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[目的]建立原子荧光光谱法测定尿锑浓度的检测方法。[方法]尿样经混合酸消化后,加入硫脲和抗坏血酸使5价锑还原为3价锑,再加入硼氢化钾还原生成锑化氢,由氩气载入石英原子化器中分解为原子态锑,在锑空心阴极灯发射光的激发下产生原子荧光,荧光强度与标准系列比较定量。[结果]尿锑浓度为0.0~10.0μg/L的线性关系较好,相关系数为0.999 4~0.999 9;最低检出限为0.06μg/L;相对标准偏差为1.9%~2.4%;平均加标回收率为99.7%。[结论]建立的湿法消解-氢化物发生-原子荧光光谱法测定尿锑实用、快速、准确、灵敏度高、基体干扰少,便于推广运用,尤其适用于大批量人群职业健康体检尿锑的检测。
[Objective] To establish a method for the determination of urinary antimony concentration by atomic fluorescence spectrometry. [Method] After the urine samples were digested by mixed acid, thiourea and ascorbic acid were added to reduce the 5-valent antimony to 3-valent antimony. Then, potassium borohydride was added to reduce the antimony hydride to form antimony hydride. State antimony, generated in the antimony hollow cathode lamp excitation light excitation atomic fluorescence, fluorescence intensity compared with the standard series of quantitative. [Result] The linear relationship between the concentration of urinary antimony and 0.0 ~ 10.0 μg / L was good, the correlation coefficient was 0.999 4 ~ 0.999 9, the minimum detectable limit was 0.06 μg / L, and the relative standard deviation was 1.9% ~ 2.4% The standard recovery was 99.7%. [Conclusion] The established wet-digestion-hydride generation-atomic fluorescence spectrometry has the advantages of practical, rapid, accurate, high sensitivity and less matrix interference, which is convenient for popularization and application. It is especially suitable for the detection of urinary antimony in occupational health examination of large-scale population .