采用原子荧光光谱法测定皮革及其制品中砷、锑和汞的含量。样品经硝酸和过氧化氢消解,试样溶液中加入硫脲和抗坏血酸混合溶液作为还原剂。在酸性介质中加入硼氢化钠-氢氧化钠溶液使与溶液中各离子反应生成氢化物。分析中砷、锑、汞的载气流量分别为300,400,400 mL·min-1。3种元素的质量浓度分别在一定的范围内与荧光强度呈线性关系,方法的检出限(3s/k)依次为0.22,0.16,0.04 μg·L-1。应用此法对皮革及其制品进行分析,测定值的相对标准偏差(n=5)均小于10%,回收率在94.0%~107%之间。

AFS was applied to the determination of As, Sb and Hg in leather and its products. The sample was digested with mixed solution of HNO3-H2O2, and reduced with mixed solution of thiourea and ascorbic acid. Hydrides of the 3 elements were generated from acidic solution using NaBH4 solution (dissolved in NaOH solution) as reducing reagent. Flow-rates of the carrier gas selected were 300 mL·min-1 for As and 400 mL·min-1 for Sb and Hg. Linear relationships between values of fluorescence intensity and mass concentration of the 3 elements were found in definite ranges, with detection limits (3s/k) of 0.22 μg·L-1 (for As), 0.16 μg·L-1 (for Sb) and 0.04 μg·L-1 (for Hg).The proposed method was applied to the analysis of leather and its products, giving values of recovery in the range of 94.0%-107% with RSD′s (n=5) less than 10%.