电感耦合等离子体原子发射光谱法测定湿法磷酸中8种元素

发布时间：2018-06-29 07:42

本文选题：电感耦合等离子体原子发射光谱法(ICP-AES) + 多向观测　；参考：《冶金分析》2017年06期

【摘要】：采用硝酸-盐酸混合酸溶解,5%(V/V)盐酸作为稀释酸,试液使用超声振荡混匀,基体匹配法绘制校准曲线消除基体效应的影响,建立了使用多向观测-电感耦合等离子体原子发射光谱法(ICP-AES)同时测定湿法磷酸中铝、镁、铁、钾、钠、锰、钙和铬的分析方法。根据分析线的选择原则,结合待测元素的检测范围,选择无干扰或干扰小、峰形对称、灵敏度高的谱线作为分析线。通过径向观测方式,减小样品稀释倍数,降低电离干扰,测定含量较高的铝、镁、铁;通过轴向观测方式,提高灵敏度,测定含量较低的锰、钙、铬;通过轴向衰减观测方式,减小谱线强度,测定含量较低的钾和钠。被测元素在一定质量浓度范围内与其发射强度呈线性,校准曲线的线性相关系数为0.998 6~0.999 9。方法的检出限为0.001 5~0.009 1μg/mL。按照实验方法测定两个湿法磷酸样品中的铝、镁、铁、钾、钠、锰、钙和铬,结果的相对标准偏差(RSD,n=12)为2.1%~8.1%。选择两个湿法磷酸样品,分别采用基体匹配法和标准加入法并使用ICP-AES测定,再采用其他化学方法进行比对(其中,铁采用邻菲哆啉比色法测定,铝采用不预分离干扰的氟盐取代-EDTA滴定法测定,钙采用高锰酸钾滴定法测定,锰采用过硫酸铵-亚铁滴定法测定,钾、钠、铬和镁均采用火焰原子吸收光谱法测定),所得铝、镁、铁、钾、钠、锰、钙和铬的测定结果基本吻合。
[Abstract]:In this paper, 5% (V / V) hydrochloric acid was dissolved in mixed acid of nitric acid and hydrochloric acid as diluent acid. Ultrasonic oscillation was used to mix the solution, and the matrix matching method was used to draw calibration curve to eliminate the influence of matrix effect. A method for simultaneous determination of aluminum, magnesium, iron, potassium, sodium, manganese, calcium and chromium in wet phosphoric acid by multidirectional observation-inductively coupled plasma atomic emission spectrometry (ICP-AES) has been established. According to the selection principle of analytical lines and the detection range of the elements to be tested, the spectral lines with no or little interference, symmetrical peak shape and high sensitivity are selected as analytical lines. By means of radial observation, the dilution multiple of the sample is reduced, the interference of ionization is reduced, the high content of aluminum, magnesium and iron is determined, the sensitivity is improved by axial observation, and the manganese, calcium and chromium with lower content are determined, and the observation mode of axial attenuation is adopted. The intensity of the spectral line was reduced, and potassium and sodium with low content were determined. The emission intensity of the tested elements is linear in a certain range of mass concentration, and the linear correlation coefficient of the calibration curve is 0.998 ~ 0.999 9. The detection limit of the method was 0.001 渭 g / mL. Aluminum, magnesium, iron, potassium, sodium, manganese, calcium and chromium in two wet phosphoric acid samples were determined according to the experimental method. The relative standard deviation (RSDN ~ (12) of the results was 2.1% and 8.1%. Two samples of wet phosphoric acid were selected and determined by ICP-AES, matrix matching method and standard addition method, and then compared by other chemical methods. (among them, iron was determined by o-phenanthroline colorimetry. Aluminum was determined by fluorine-substituted EDTA titration without preseparation interference, calcium by potassium permanganate titration, manganese by ammonium persulfate titration, and potassium, sodium, chromium and magnesium by flame atomic absorption spectrometry. The results of determination of magnesium, iron, potassium, sodium, manganese, calcium and chromium are in good agreement.
【作者单位】：昆明理工大学化学工程学院;云南省有色金属真空冶金重点实验室;
【基金】：云南省重点新产品开发计划(No.2015BA008)
【分类号】：O657.31;TQ126.35

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