沉淀分离电感耦合等离子体原子发射光谱法测定高纯银中21种痕量元素

Determination of twenty-one trace elements in high purity silver by inductively coupled plasma atomic emission spectrometry after precipitation of silver

应用氯化银沉淀法分离银后,超声雾化ICP-AES法测定高纯银中Al,Ca,Cr,Fe,Mg,Mo,Ni,Ti,Ba,Bi,Cd,Co,Cu,In,Li,Mn,Pb,Sn,V,Y及Zn21种痕量元素。对银沉淀时待测杂质元素的损失、光谱测定条件进行试验。结果表明,当试液中10mg/mL的银被沉淀时,待测元素几乎不与氯化银共沉淀;在所选定的波长下测定,当铁、铬、钙、镍、镁、铅的质量浓度小于10μg/mL时没有明显光谱干扰。本法测定范围为10～320μg/g,回收率在93%～105%之间,相对标准偏差在19%～11.4%范围(n=6)。

Twenty-one trace amounts of impurity elements like Al, Ba, Bi, Ca, Cd, Co, Cr, Cu, Fe, In, Li, Mg,Mn,Mo,Ni,Pb,Sn,Ti,V, Y and Zn in high purity silver are determined by ultrasonic nebulziation inductively coupled plasma atomic emission spectrometry after precipitation of silver as silver chloride. The loss of impurity elements in the precipitation of silver, and selection of spectral conditions for the determination of silver are tested. The results show that the elements analyzed can not be almost eopreeipitated when less than 10 μg/mL of silver are precipitated. No clear spectral interference is observed under the optimum wavelength of analytical lines, when iron, chromium, calcium, nickel,magnesium,lead are present in not greater than 10μg/mL. The scopes of determination are 10-320 μg/g for every element. The rates of recovery are 93 %- 105 %. The relative standard deviations lie between 1.9% and 11.4%.