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使用硝酸和高氯酸溶解氧化镍样品,溶液过滤后,采用恒电流电解重量法测定滤液中镍。加入10mL 500g/L柠檬酸铵,电解液酸度为pH 10,电解过程中所需的电解电流和电解时间为2A/2h。选择Ni 341.486nm、Co 238.892nm、Cu 324.752nm、Zn 206.191nm、Fe259.940nm、Mn 257.610nm作为分析谱线,采用基体匹配法绘制校准曲线消除基体效应,使用电感耦合等离子体原子发射光谱法(ICP-AES)测定沉积在铂阴极上的钴、铜、锌、铁、锰,并测定电解残余液和酸不溶残渣中的镍、锰、铁。镍、铁、锰含量分别为电解在铂阴极的镍、铁、锰,电解液中残余镍、铁、锰,残渣回收浸出液中镍、铁、锰共3个部分测定值的总和。实验方法各元素的检出限为0.002 4~0.020μg/mL,校准曲线的线性相关系数均大于0.999。按照实验方法测定氧化镍样品中镍、钴、铜、锌、铁和锰含量,测定结果的相对标准偏差(RSD,n=10)在0.11%~7.5%之间。实验方法用于氧化镍样品的测定,结果与国标方法以及原子吸收光谱法的测定结果相吻合。
Nickel and perchloric acid were used to dissolve the nickel oxide sample. After the solution was filtered, the nickel in the filtrate was measured by galvanostatic gravimetric method. Add 10mL 500g / L ammonium citrate, the electrolyte acidity of pH 10, the electrolysis process required electrolysis current and electrolysis time 2A / 2h. Ni 341.486nm, Co 238.892nm, Cu 324.752nm, Zn 206.191nm, Fe 259.940nm and Mn 257.610nm were selected as the analytical lines. The calibration curves were obtained by matrix matching method to eliminate the matrix effect. Inductively coupled plasma atomic emission spectrometry ICP-AES) for the determination of cobalt, copper, zinc, iron and manganese deposited on a platinum cathode and determination of nickel, manganese and iron in the electrolytic residue and in the acid insoluble residue. The contents of nickel, iron and manganese are the sum of the measured values of nickel, iron and manganese in the leached solution of nickel, iron, manganese and electrolyte in the nickel, iron, manganese and electrolyte recovered from platinum cathodes. The detection limit of each element in the experimental method was 0.002 4 ~ 0.020 μg / mL, and the linear correlation coefficient of the calibration curve was greater than 0.999. The nickel, cobalt, copper, zinc, iron and manganese contents in the nickel oxide samples were determined experimentally. The relative standard deviations (RSD, n = 10) of the results were between 0.11% and 7.5%. The experimental method was applied to the determination of nickel oxide samples. The results were in good agreement with the results of GB method and atomic absorption spectrometry.