电感耦合等离子体原子发射光谱法测定铁镍基高温合金中痕量硅.pdfVIP

电感耦合等离子体原子发射光谱法测定铁镍基高温合金中痕量硅 ·1 · 电感耦合等离子体原子发射光谱法测定 铁镍基高温合金中痕量硅 杨国武 刘晓波 韩 美 刘庆斌 胡净宇 （中国钢研科技集团有限公司钢研纳克检测技术有限公司，北京 100081 ） 摘 要 电感耦合等离子体原子发射光谱对高温合金中的痕量硅进行测定。对高温合金样品的消解，标准曲线 的配制，分析谱线的选择，基体干扰的消除进行了较为深入的探讨。对普通的高温合金样品，使用比例为5:1 的盐 酸与硝酸进行消解，而对于铌、钽等元素含量较高的高温合金样品，还需使用氢氟酸进行消解。基体干扰通过使用 高温合金主成分打底配制标准曲线的方式进行消除。考察并确定了在紫外区常见干扰元素如硼、磷、硫等对硅元素 的两条谱线184.685 和185.005 测定无明显干扰，但硅元素的185.005 谱线受到钽元素的重叠干扰，而184.685 谱线 峰型不佳。实验表明，通过绘制钽的干扰曲线并计算干扰校正系数，进行数学校正后可得到准确的测定结果。硅元 素两条谱线184.685 和185.005 的加标回收率在87%~107%之间，相对标准偏差小于5%。 关键词 电感耦合等离子体原子发射光谱 铁基高温合金 镍基高温合金 钽 痕量硅 Determination of Trace Silicon in Nickel-base Superalloy and Iron-base Superalloy by ICP-AES Yang Guowu Liu Xiaobo Han Mei Liu Qingbin Hu Jingyu (NCS Testing Technology Co., Ltd., Beijing, 100081) Abstract A method was established for the determination of silicon in nickel-base superalloy and Iron-base superalloy by ICP-AES. The sample pre-treatment, preparation of calibration curve, analysis lines and matrix interference were discussed in detail. The samples were dissolved with a freshly prepared mixture of HCl and HNO in 5:1 by volume. If the samples 3 have not been dissolved completely, a few drops of HF should be added. In order to eliminate the matrix effects, the approximate amount of main components as to the superalloy samples should be added into the standard solution. If the silicon lines 184.685 and 185.005 were chosen as the analytical lines, there is no interference by boron, phosphorus and sulfur, which are the most common interferences. Howev