微波消解-耐氢氟酸系统进样电感耦合等离子体发射光谱法测定锰矿中铝磷镁铁锌镍

采用混合酸作溶剂微波消解试样，样液定容后，直接用耐氢氟酸进样系统（Duo HF KIT）进样，电感耦合等离子体发射光谱法（ICP AES）测定锰矿石试液中的铝、磷、镁、铁、锌、镍，避免因为引入硼酸掩蔽氟离子而带来的基体干扰，缩短了检测时间。测定时选择波长为369.152 nm{85}、186.942 nm{481}、280.270 nm{120}、240.488 nm {140}、213.856 nm {457} 和341.476 nm {99}光谱线分别作为Al、P、Mg、Fe、Zn、Ni分析线，采用基体匹配方法来消除锰的基体效应。本法已测定国家锰矿标准物质中铝、磷、镁、铁、锌、镍，并与国标方法测定结果相比对，分析结果与认定值及国标方法的测定值相符，且重复性好。各元素的加标回收率为94%~107%，测定结果的相对标准偏差(RSD, n=12)小于1.1％。

Determination of aluminum, phosphorus, magnesium, iron, zinc and nickel in manganese ore by inductively coupled plasma atomic emission spectrometry with hydrofluoric add resistant sampling system after microwave digestion

The samples were dissolved by microwave digestion using mixed acid as solvent. After dilution, the aluminum, phosphorus, magnesium, iron, zinc and nickel in manganese ore were determined by inductively coupled plasma atomic emission spectrometry (ICP AES) using hydrofluoric acid resistant sampling system (Duo HF KIT). The matrix effect of boric acid introduced for masking fluorine ion was prevented , and the detection time was shortened. The spectral lines for Al, P, Mg, Fe, Zn and Ni were 369.152 nm{85}, 186.942 nm{481}, 280.270 nm{120}, 240.488 nm {140}, 213.856 nm {457} and 341.476 nm {99}, respectively. The matrix effect of manganese was eliminated by matrix matching method. The proposed method had been applied to the determination of aluminum, phosphorus, magnesium, iron, zinc and nickel in certified reference materials of manganese ore. The determination results were compared with those obtained by national standard method. It was found that the analytical results were consistent with the certified values and those obtained by national standard method. Moreover, the repeatability was good. The recoveries of elements were 94% 107%, and the relative standard deviations (RSD, n=12) were smaller than 1.1 %.