摘要
样品(0.400 0 g)置于50 mL样品管中,加入盐酸-硝酸-水(3+1+4)混合液10 mL,饱和氟化氢铵溶液1.0 mL,经石墨消解仪斜坡升温进行消解。消解液冷却10 min,用水定容至50 mL。分取10.0 mL,用水稀释至20 mL,所得溶液采用电感耦合等离子体质谱法测定其中银及铂族元素(钌、铑、钯、铱、铂、金)的含量。以标准加入法补偿基体效应制作标准曲线。在质谱分析中采用标准模式。7种元素的检出限(3s)在0.01~0.80μg·L^(-1)之间。按标准加入法进行回收试验,回收率在94.0%~105%之间,相对标准偏差(n=11)在0.70%~2.1%之间。按上述方法分析铜冶炼渣尾矿样品,结果与石墨炉原子吸收光谱法测定结果基本一致。
The sample (0. 400 0 g) was placed into a 50 mL sample tube. HCl-HNO3-H2O (3+1+4) mixed solution (10 mL) and 1.0 mL of saturated ammonium hydrogen fluoride solution were added, and the mixture was digested in a graphite digestor by ramp temperature rise. After cooling for 10 min, water was added to the digested solution to make its volume up to 50 mL. An aliquot of 10.0 mL was taken, and diluted to 20 mL with water. The solution was used for 1CP-MS determination of Ag and platinum group elements (Ru, Rh, Pd, It, Pt, Au). The standard addition method was used to correct the matrix effect in preparation of standard curves. Values of detection limits (3s) found for 7 elements were in therange of 0. 01-0. 80 μg· L^-1. Test for recovery was made by standard addition method, giving results in the range of 94. 0%-105%, with RSDs (n=11) ranged from 0. 70% to 2. 1%. The sample of copper smelting slag tailings was analyzed by the proposed method, giving results in consistency with those by graphite furnace atomic absorption spectrometry (FAAS).
出处
《理化检验(化学分册)》
CAS
CSCD
北大核心
2018年第1期69-72,共4页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)