电感耦合等离子体原子发射光谱法测定精炼镍中10种杂质元素

精炼镍是冶炼不锈钢的优质原材料,产品有通用镍、镍豆等,需要检验其中的杂质元素。采用硝酸(1+1)溶解样品,选择Si 251.612nm、Mn 257.610nm、P 178.217nm、Fe259.940nm、Cu 324.754nm、Co 238.892nm、Mg 279.553nm、Al 396.153nm、Zn 206.191nm、Cr 267.716nm为分析线,离峰扣背景校正法消除背景干扰,无镍基体匹配的方法绘制校准曲线,使用电感耦合等离子体原子发射光谱法(ICP-AES)测定了精炼镍中硅、锰、磷、铁、铜、钴、镁、铝、锌、铬等10种元素。方法中各元素校准曲线的线性相关系数均大于0.999 5;各待测元素的检出限为0.000 12%~0.001 9%。按照实验方法测定精炼镍样品和Nickel200标准样品中硅、锰、磷、铁、铜、钴、镁、铝、锌、铬,样品测定结果的相对标准偏差(RSD,n=11)在1.0%~10%之间,而标样的测定值和认定值相符。对精炼镍试样的加标回收率在90%~105%之间。

Determination of ten impurity elements in refined nickel by inductively coupled plasma atomic emission spectrometry

Refined nickel is a high-quality raw material for stainless steel smelting. The refined nickel products include general nickel and nickel bean. The impurity elements should be detected. The sample was dissolved with nitric acid (1+1). Si 251.612 nm, Mn 257.610 nm, P 178.217 nm, Fe 259.940 nm, Cu 324.754 nm, Co 238.892 nm, Mg 279.553 nm, Al 396.153 nm, Zn 206.191 nm and Cr 267.716 nm were selected as analytical lines.The background interference was eliminated by off-peak background deduction correction method. The calibration curve was prepared by nickel-free matrix matching method. The content of 10 elements in refined nickel (including silicon, manganese, phosphorus, iron, copper, cobalt, magnesium, aluminum, zinc and chromium) was determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). The linear correlation coefficients of calibration curves of elements were higher than 0.999 5. The detection limits of elements were between 0.000 12% and 0.001 9%. The content of silicon, manganese, phosphorus, iron, copper, cobalt, magnesium, aluminum, zinc and chromium in refined nickel sample and Nickel200 standard sample was determined according to the experimental method. The relative standard deviations (RSD, n=11) were between 1.0% and 10%. The found results of standard sample were consistent with the certified values. The recoveries for refined nickel samples were between 90% and 105%.