电感耦合等离子体原子发射光谱法测定硫酸氧钒中钙镁镍铜铝铁

采用盐酸溶解样品,使用基体匹配法配制校准曲线消除基体效应的影响,选择Ca 317.933 nm、Mg 285.213 nm、Ni 211.647 nm、Cu 324.754 nm、Al 396.152 nm、Fe 238.204 nm作为分析线,电感耦合等离子体原子发射光谱法(ICP-AES)测定硫酸氧钒中钙、镁、镍、铜、铝、铁。进行了1.6 mg/mL钒离子和3.0 mg/mL硫酸根共存体系中基体效应、光谱干扰和连续背景叠加对待测元素测定的影响试验。结果表明,该质量浓度的硫酸根离子对测定不产生影响,而钒对部分待测元素谱线产生光谱干扰,钒基体效应对待测元素均产生正干扰。采用钒基体匹配和同步背景校正相结合的方式消除钒基体的影响,并且优选出未受光谱干扰的各待测元素分析谱线及其背景校正和检测区域,根据试验结果确定了ICP-AES工作条件。钙、镁、镍、铜、铝、铁的质量分数在0.000 1%～0.10%范围内与发射强度成线性,各元素校准曲线的相关系数均大于0.999,背景等效浓度为-0.000 3%～0.000 4%,方法中各元素的检出限为0.000 1%～0.000 3%(质量分数)。按照实验方法测定硫酸氧钒中钙、镁、镍、铜、铝、铁,结果的相对标准偏差(RSD,n=8)为2.6%～14%。实验方法用于测定2个硫酸氧钒样品中钙、镁、镍、铜、铝、铁,结果与电感耦合等离子体质谱法(ICP-MS)的测定结果相吻合。

Determination of calcium,magnesium, nickel,copper, aluminum and iron in vanadyl sulfate by inductively coupled plasma atomic emission spectrometry

The sample was dissolved with hydrochloric acid. The influence of matrix effect was eliminated by preparation of calibration curve using matrix matching method. The Ca 317.933 nm, Mg 285.213 nm, Ni 211.647 nm, Cu 324.754 nm, Al 396.152 nm and Fe 238.204 nm were selected as the analytical lines. The contents of calcium, magnesium, nickel, copper, aluminum and iron in vanadyl sulfate were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). The influence of matrix effect, spectral interference and continuous background overlapping on determination was investigated in coexistence system of 1.6 mg/mL vanadium ion and 3.0 mg/mL sulfate ion. The results showed that the determination was not affected by the sulfate ion at this concentration. However, the vanadium ion had spectral interference with the spectral lines of some testing elements. The matrix effect of vanadium exhibited positive interference to all testing elements, and was eliminated by matrix matching and synchronous background correction. Moreover, the analytical lines without spectral interference, the background correction and detection region were optimized and selected. The operation conditions of ICP-AES were confirmed according to the experimental results. When the mass fraction of calcium, magnesium, nickel, copper, aluminum and iron was in range of 0.000 1% and 0.10%, it was linear to the emission intensity. The linear correlation coefficients of calibration curves were higher than 0.999. The background equivalent concentration was -0.000 3%-0.000 4%. The detection limits of the proposed method were between 0.000 1% and 0.000 3% (mass fraction). The contents of calcium, magnesium, nickel, copper, aluminum and iron in vanadyl sulfate were determined according to the experimental method. The relative standard deviations (RSD, n=8) were between 2.6% and 14%. The found results were consistent with those obtained by inductively coupled plasma mass spectrometry (ICP-MS).