研究了采用磷酸钇(YPO4)作为共沉淀载体选择性分离富集NiCl2,MnSO4溶液中的痕量Pb^2+和Fe^3+,并用火焰原子吸收光谱(FAAS)测定的方法。共沉淀受pH,YCl3和H3PO4溶液用量的影响。结果显示,在溶液pH3.0~4.0时,YPO4能够定量共沉淀氯化Ni中的Pb和Fe以及硫酸Mn中的Pb。对于20mL溶液,Pb和Fe的检出限分别为1.63×10^-2mg·L^-1和4.58×10^-2mg·L^-1。在NiCl2溶液中,Pb和Fe的标准加入回收率分别为100.91%和99.73%;在MnSO4溶液中,Pb和Fe的标准加入回收率分别为99.45%和98.98%。实验基本消除了基体干扰,取得了较满意的结果。
Using yttrium phosphate as the coprecipitation collector for the separation and preconeentration of trace lead and iron in nickel chloride and manganese sulfate, flame atomic absorption spectrometric (FAAS) determination was described in the present paper. Coprecipitation parameters including the pH of the solution, and the amounts of YCl3 and H3PO4 were discussed. It was found that lead and iron in nickel chloride could be coprecipitated quantitatively in the range of pH 3.0~4.0, and so could be lead in manganese sulfate. The detection limits (3σ) of lead and iron in 20 mL solution were 1.63 × 10^-2 mg·L^-1 and 4.58 × 10^-2 mg·L^-1 respectively. In NiCl2 solution the standard addition recoveries for lead and iron were 100. 91% and 99.73% respectively, and in MnSO4 solution the standard addition recoveries were 99.45% and 98.98% respectively. The method has eliminated the interference of matrix, and the result is satisfied.