火花放电发射光谱法同时测定铍青铜中多种元素

为了满足铍青铜化学成分快速测定需求,开发了利用火花放电发射光谱法直接测定铍青铜中Be、Co、Pb、Fe、Al、Ni、Si 7种元素的方法。用120目(124μm)刚玉砂纸打磨样品表面,优化光源激发条件为:冲洗时间10s;预燃时间15s;积分时间10s;频率500Hz;预燃能量0.5;积分能量0.09;氩气流量9L/min;以Cu 296.1nm谱线作为参比线,优选各元素的线性和精密度均较好的谱线作为该元素的分析谱线。利用购买的标样与电感耦合等离子体原子发射光谱法(ICP-AES)和原子吸收光谱法(AAS)共同定值的内控样一起绘制校准曲线,各元素校准曲线线性相关系数R~2均在0.995以上。对样品进行精密度试验考察,各元素测定结果的相对标准偏差(RSD,n=11)在0.39%~1.5%之间。对铍青铜未知样品进行正确度考察,测定值与湿法结果一致。

Simultaneous determination of multi elements in beryllium bronze by spark source emission spectroscopy

In order to meet the rapid determination requirements for chemical components in beryllium bronze, the direct determination method of seven elements including Be, Co, Pb, Fe, Al, Ni and Si in beryllium bronze by spark source emission spectroscopy was developed. The sample surface was polished with 120 mesh (124μm) corundum sand paper. The spark excitation conditions were optimized as follows: flush time of 10s; pre-burning time of 15s; integral time of 10s; frequency of 500Hz; pre-burning energy of 0.5; integral energy of 0.09; argon flow of 9L/min. Cu 296.1nm was used as reference line, and the spectral lines of elements with good linearity and precision were selected as the analytical lines. The calibration curves were prepared with the purchased certified reference materials and the internal control sample whose values were defined by inductively coupled plasma atomic emission spectrometry (ICP-AES) coupled with atomic absorption spectrometry (AAS). The linear correlation coefficients (R²) of calibration curves of elements were all higher than 0.995. The precision tests were performed, and the relative standard deviation (RSD, n=11) of elements were between 0.39% and 1.5%. The unknown beryllium bronze sample was used for accuracy test. The results were consistent with those obtained by wet method.