铝合金样品用盐酸及硝酸的混合酸溶解,于分取的部分试样溶液中加入碘化钾-硫脲混合溶液后用盐酸(5+95)定容为50 mL,供氢化物发生-原子荧光光谱法测定其中痕量锑.用40 g·L-1碘化钾溶液作为锑(Ⅴ)的预还原剂,40 g·L-1硫脲溶液作为其他可形成氢化物的元素的掩蔽剂,选用20 g·L-1硼氢化钾溶液作为产生锑化氢的还原剂,氢化物发生反应在盐酸(5+95)介质中进行,锑的质量浓度在0.05~50.0 μg·L-1范围内与相应的荧光强度呈线性关系.方法的检出限(3s/k)为0.016 μg·L-1.应用此方法分析了两件铝合金标准样品,测得锑量的结果与认定值相符,测定值的相对标准偏差(n=8)分别为2.14%和3.16%.

Sample of aluminum alloys was dissolved in mixed acid of conc. HCl and conc. HNO3. An aliquot of the sample solution was taken and diluted to 50 mL in a volumetric flask with HCl (5+95) after adding a mixed solution of thiourea and KI. The solution was used for determination of trace amount of antimony by HG-AFS. 40 g·L-1 potassium iodide solution was suitable to be used as pre-reductant for Sb(Ⅴ),and 40 g·L-1 thiourea solution was used as complexing agent for other co-existing hydride forming elements. 20 g·L-1 KBH4 solution was used as reductant for SbH3 generation which was carried out in a medium of HCl (5+95). Linear relationship between values of fluorescence intensity and mass concentration of Sb was obtained in the range of 0.05-50.0 μg·L-1,with the detection limit (3s/k) of 0.016 μg·L-1. The proposed method was used in the analysis of 2 standard samples of aluminum alloys,giving results of Sb contents in consistency with the standard values and values of RSD′s (n=8) found were 2.14% and 3.16% respectively.