电感耦合等离子体发射光谱法测定镍矿石中镍铝磷镁钙

摘要

The simultaneous determination of Ni, Al, P, Mg, and Ca in nickel ores by inductively coupled plasma atomic emission spectrometry (ICP-AES) has been developed and is described in this paper. The sample was dissolved in nitric acid with hydrofluoric acid as flux. Perchloric acid was added and heated in order to remove hydrofluoric acid. After dissolving the salts with hydrochloric, Ni, Al, P, Mg and Ca were determined by ICP-AES. The selected spectral lines forNi, Al, P, Mg and Ca were 221. 6 nm, 396.1 nm, 178. 2 nm, 285. 2 nm and 393. 3 nm, respectively. The matrix effect was corrected by adding the same amount of Fe as the measured sample into the standard curve. The recoveries were 98. 00% -100.50%. The precisions of Ni, Al, P, Mg and Ca were all less than 1 % and the detection limits were 0. 0054 μg/mL, 0. 0028 μg/mL, 0. 0060 μg/mL, 0. 0030 μg/mL and 0. 0013 μg/mL, respectively. Compared with other methods, this method increased sensitivity and decreased the detection limit. It was applied to the determination of nickel ores from Indonesia, and the measured results were consistent with the standard values and RSD was below 1 % ( n = 6 ).%样品用硝酸溶解,氢氟酸助溶,高氯酸冒烟除去氢氟酸,盐酸溶解盐类后,在选定的测量条件下用电感耦合等离子体发射光谱法( ICP - AES)测定镍矿中镍、铝、磷、镁、钙.选择Ni 221.6 nm、Al 396.1nm、P 178.2 nm、Mg 285.2 nm、Ca 393.3 nm分别作为镍、铝、磷、镁、钙的分析线；通过在标准曲线中加入与待测样品等量的铁,消除基体干扰的影响.方法回收率为98.0％ ～ 100.5％,镍、铝、磷、镁、钙的精密度均小于1％,检出限分别为0.0054、0.0028、0.0060、0.0030、0.0013 μg/mL.与同类ICP - AES方法比较,本法灵敏度提高,检出限降低.方法用于测定印度尼西亚的两批次镍矿石样品,结果与化学法的测定值基本一致,相对标准偏差小于1％(n=6).