试样溶于适当的混合酸中,蒸至恰干,用pH 3.0的苯二甲酸氢钾缓冲溶液溶解残渣.用硫代乙酰胺和三氯化钛共沉淀从试样溶液将锡(Ⅳ)及铅(Ⅱ)分离,所得沉淀溶于浓盐酸中制成盐酸(1+9)的试液,并分部分此溶液分别进行锡及铅的氢化物发生-原子荧光光谱法测定.对方法的精密度和回收率做了试验,测得锡的相对标准偏差(n=6)在0.74%~0.96%之间,回收率在98.1%~100.9%之间;测得铅的相对标准偏差(n=6)在0.64%~1.41%,回收率在97.6%~100.6%之间.

The sample was dissolved an appropriate acid mixture and evaporated to dryness.The residue was taken up with a phthalate buffer solution of pH 3.0 Tin(Ⅳ) and lead(Ⅱ) in the sample solution were separated by co-precipitation with thioacetamide and titanium trichloride.The precipitate obtained was dissolved with conc.HCl,and an aliquot of the sample solution in HCl(1+9) was used for AAS determinations separately.Tests for precision and recovery were made,giving values of RSD′s (n=6) in the ranges of 0.74%-0.96% (for Sn),0.64%-1.41% (for Pb),and values of recovery in the ranges of 98.1%-100.9% (for Sn),97.6%-100.6% (for Pb).