电感耦合等离子体发射光谱(ICP-OES)法测定红外干扰烟幕材料中的镁、铝、铜

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。建立了一种采用浓硝酸消解样品,对消解液过滤、稀释后直接用电感耦合等离子发射光谱(ICP-OES)法测定某红外干扰烟幕材料中镁、铝、铜元素含量的方法。当Mg、Al、Cu的分析线选择279.5、167.0和324.7 nm时,其检测限分别达到0.013、0.040和0.025μg/mL,且样品测定的加标回收率均在102%~105%,相对标准偏差在1.0%~3.0%(n=8),表明方法的准确度和精密度均良好。还对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。

Quantitative Analysis of Magnesium, Aluminum and Copper in IR Interfering Smoke Material by Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES)

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 coupled plasma 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 279.5,167.0 and 324.7 nm were selected for determination of Mg,Al and Cu,the limits of detection(LODs)of them were 0.013,0.040 and 0.025μg/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.The total standard deviation of the developed method was traced and compared 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 completely substitute traditional chemical titration method.