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中国无机分析化学:2020,10(3):48-54
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基于电感耦合等离子体-发射光谱(ICP-OES)的红外干扰烟幕材料中镁、铝、铜元素的定量分析
梁玉兰1, 张普敦1, 陶然婷1, 聂凤泉2, 师宏心2, 吴昱2, 金青君2, 赵建峰2, 毕鹏禹2
(1.分析测试中心,北京化工大学;2.防化研究院 北京)
Quantitative Analysis of Magnesium, Aluminum and Copper in IR Interfering Smoke Material by Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES)
Yulan Liang1, Pudun Zhang1, Ranting Tao1, Fengquan Nie2, Hongxin Shi2, Yu Wu2, Qingjun Jin2, Jianfeng Zhao2, Pengyu Bi2
(1.Analysis Test Center,Beijing University of Chemical Technology;2.Research Institute of Chemical Defense,Beijing)
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投稿时间:2019-10-24    修订日期:2019-10-30
中文摘要: 某红外干扰烟幕材料中镁、铝、铜元素的含量直接影响其干扰性能。化学滴定法是测定金属元素含量的传统方法,但这种方法过程繁琐、冗长,只能依次测定,且在铝和铜同时存在下无法对镁元素定量分析。本工作建立了一种电感耦合等离子发射光谱(ICP-OES)常量定量分析方法,即采用浓硝酸消解样品,对消解液过滤、稀释后直接进行ICP-OES分析。当Mg、Al、Cu的分析线选择279.5 nm、167.0 nm和324.7 nm时,其检测限分别达到0.013 μg/mL、0.040 μg/mL和0.025 μg/mL,且样品测定的加标回收率均在102% ~ 105%之间,相对标准偏差在1.0% ~ 3.0%之间(n = 8),表明方法的准确度和精密度均良好。本工作还对该方法的总标准偏差进行了溯源,并与络合滴定法结果进行了比较。显著性检验表明两种方法的结果无显著性差异,但ICP-OES法更简便、快速,并能对三种元素同时测定,因此可完全替代传统的化学滴定法。
Abstract:The contents of magnesium (Mg), aluminum (Al) and copper (Cu) in an IR interfering smoke material directly affect the anti-interference performance. Chemical titration is a traditional method for determining the content of metal element, it is complicated and time consuming, and each element can only be determined sequentially. Besides, the quantification of Mg cannot be performed in the presence of both Al and Cu. An inductively coupledplasma optical emission spectroscopy (ICP-OES) coupled with a sample pretreatment method was developed in this work to quantitatively determine Mg, Al and Cu. Specifically, the sample was digested with concentrated nitric acid, and the ICP-OES analysis was directly performed on the digested solution after filtration and dilution. When the resonance lines 279.5 nm, 167.0 nm and 324.7 nm were selected for determination of Mg, Al and Cu, the limits of detection (LODs) of them were 0.013 μg/mL, 0.040 μg/mL and 0.025 μg/mL, respectively. The spiked recoveries for the three elements were in the range 102-105%, and the relative standard deviations (RSDs) were in the range 1.0% ~ 3.0% (n = 8), indicating that both the accuracy and the precision of the method are good. This work traced the total standard deviation of the developed method and compared it with the results of complexometric titration. It showed that there was no significance difference between the results of the two methods. However, the developed ICP-OES method was simpler and faster, and able to determine the three elements simultaneously. It can be completely substituted for traditional chemical titration method.
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梁玉兰,张普敦,陶然婷,聂凤泉,师宏心,吴昱,金青君,赵建峰,毕鹏禹.基于电感耦合等离子体-发射光谱(ICP-OES)的红外干扰烟幕材料中镁、铝、铜元素的定量分析[J].中国无机分析化学,2020,10(3):48-54.
Yulan Liang,Pudun Zhang,Ranting Tao,Fengquan Nie,Hongxin Shi,Yu Wu,Qingjun Jin,Jianfeng Zhao,Pengyu Bi.Quantitative Analysis of Magnesium, Aluminum and Copper in IR Interfering Smoke Material by Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES)[J].Chinese Journal of Inorganic Analytical Chemistry,2020,10(3):48-54.

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