微波消解-电感耦合等离子体原子发射光谱法测定镍基合金中硅铬硼

镍基合金耐蚀性优良,但难以溶解。实验使用盐酸-硝酸-氢氟酸并采用微波消解法消解样品,选择Si 288.158 nm、Cr 267.716 nm、B 249.678 nm为分析谱线,选用基体匹配法消除基体效应的影响,采用自动匹配法校正谱线干扰,并稀释溶液从而扩大铬元素的测定范围,建立了微波消解-电感耦合等离子体原子发射光谱法(ICP-AES)测定镍基合金中硅、铬、硼的方法。硅在0.1%～2.0%(质量分数,下同)、铬在0.1%～2.0%、硼在0.01%～0.1%范围内,各元素发射强度与其质量分数呈线性关系,校准曲线的线性相关系数均不小于0.999 4,各元素检出限不大于0.000 2%。按照实验方法测定镍基合金样品中硅、铬、硼,结果的相对标准偏差(RSD,n=6)为0.70%～1.8%。方法应用于镍基合金标准样品的测定,测定结果与认定值相符。

Determination of silicon,chromium and boron in nickel-based alloy by microwave digestion-inductively coupled plasma atomic emission spectrometry

The corrosion resistance of nickel-based alloy is excellent,but it is difficult to be dissolved.The nickel-based alloy sample was decomposed with hydrochloric acid-nitric acid-hydrofluoric acid by microwave digestion.Si 288.158nm,Cr 267.716 nm and B 249.678 nm were selected as the analytical lines.The matrix matching method was used to eliminate the influence of matrix effect and the automatic matching method (FITTED) was used to correct the spectral line interference.By diluting the solution,the detection range of chromium element was expanded.Consequently,the determination method of silicon,chromium and boron in nickel-based alloy by microwave digestion-inductively coupled plasma atomic emission spectrometry (ICP-AES) was established.When the mass fraction of silicon,chromium and boron was 0.1%-2.0% (mass fraction,similarly hereinafter),0.1%-2.0% and 0.01%-0.1%,the emission intensity was linear to the corresponding mass fraction.The linear correlation coefficients of calibration curves were not less than 0.999 4,and the limits of detection were not more than 0.000 2%.The contents of silicon,chromium and boron in nickel-based alloy were determined according to the experimental method.The relative standard deviations (RSD,n=6) of determination results were between 0.70% and 1.8%.The proposed method was applied for the determination of certified reference materials of nickel-based alloy,and the found results were consistent with the certified values.