微波消解-ICP-AES法测定镍铁中镍、硅、铬、钻、磷、铜  

Determination of nickel,silicon,chromium,cobalt,phosphorus,copper in nickel iron by microwave digestion ICP-AES

作　　者：张明 Zhang Ming(Test and Inspection Institute,Jiangyin Xingcheng Special Steel Works Co.,Ltd.,Jiangyin 214429,Jiangsu,China)

机构地区：[1]江阴兴澄特种钢铁有限公司试验检测所,江苏江阴214429

出　　处：《特钢技术》2025年第1期54-58,共5页Special Steel Technology

摘　　要：本试验采用正交试验分别确认微波消解的功率、温度、保持时间、混合消解酸比例,同时考察基体效应、镍铁中镍硅铬钻磷铜的分析谱线选择和共存元素干扰,测定各元素的线性方程和检出限,并进行了精密度试验和加标回收试验,建立了一套完整的微波消解-ICP-AES法测定镍铁中镍硅铬钻磷铜的检测方法。结果表明,镍铁的最佳消解方案是为:消解功率600W,消解酸HNO_(3)+H_(2)SO_(4)+H_(2)O_(2)比例(mL)为8+4+1,反应温度220℃,保持时间25min。采用ICP-AES光谱仪测定时,当铁基量为0.05g时对镍铁中各待测元素无明显干扰,共存元素镍对磷的干扰可用IEC校正消除。方法检出限为0.0003%~0.011%,镍铁中镍、硅、铬、钻、磷、铜的线性关系均良好,相对标准偏差(RSD)均<5%,回收率在95.5%~104.5%。该试验方法的精密度和准确度良好,适用于镍铁中镍硅铬钻磷铜含量的检测。This experiment used orthogonal design to confirm the power,temperature,holding time,and mixed digestion acid ratio of microwave digestion.At the same time,the matrix effect,selection of analytical spectral lines for nickel silicon chromium cobalt phosphorus copper in nickel iron,and interference from coexisting elements were investigated,The linear equations and detection limits of each element were determined,and precision tests and spiked recovery tests were conducted.A complete microwave digestion ICP-AES method was established for the detection of nickel silicon chromium cobalt phosphorus copper in nickel iron.The results showed that the optimal digestion scheme for nickel iron was as follows:digestion power of 600 W,digestion acid HNO_(3)+H_(2)SO_(4)+H_(2)O_(2)ratio(mL)of 8+4+1,reaction temperature of 220℃,and holding time of 25 min.When using an ICP-AES spectrometer for measurement,there is no significant interference with the tested elements in nickel iron when the iron content is 0.05g.The interference of coexisting element nickel on phosphorus can be eliminated by IEC correction.The detection limit of the method is 0.0003-0.011.The linear relationship between nickel,silicon,chromium,cobalt,phosphorus,and copper in nickel iron is good,and the relative standard deviation(RSD)is less than 5%.The recovery rate is between 95.5%-104.5%.The precision and accuracy of this experimental method are good,and it is suitable for the detection of nickel silicon chromium cobalt phosphorus copper content in nickel iron.

关 键 词：微波消解 ICP-AES 镍铁 镍 硅 铬 钻 磷 铜 

分 类 号：TF644[冶金工程—钢铁冶金]