介绍了火花源原子发射光谱在铁基非晶合金钢中Si、B元素含量测定方面的研究。通过对非晶合金钢中Si和B分析谱线强度稳定性的试验比较,确定了Si的分析谱线为212.41 nm ,B的分析谱线为345.14 nm ;通过预燃试验确立了分析Si、B的最佳预燃时间为13 s 。采用部分国际标样和研制的内控样品绘制Si和B的校准曲线,在扣除了元素干扰后进行了曲线拟合。用Si 212.41 nm分析谱线绘制高含量Si(质量分数3.15%~7.04%)的校准曲线,使原有软件中曲线范围拓宽为0.003%~7.04%;用B 345.14 nm分析谱线绘制高含量B (质量分数0.90%~3.31%)的校准曲线,使B校准曲线范围拓宽为0.0001%~3.31%。用实验方法测定非晶合金样品中的Si和B含量,测定结果的相对标准偏差(RSD ,n=10)均不超过1.0%;准确度试验结果表明实验方法的测定值与电感耦合等离子体原子发射光谱法(ICP‐AES)的测定值具有较好的一致性。
T he determination of Si and B content in Fe‐based amorphous alloy steel by spark source atomic emission spectrometry was studied .The stability of analytical line strength of Si and B in amorphous alloy steel was tested and compared .Si 212.41 nm and B 345.14 nm were selected as analytical lines .The opti‐mal pre‐ignition time for Si and B analysis was 13 s .The calibration curves of Si and B were prepared using some international standard samples and self‐developed internal control samples .Then ,the curve fitting was conducted after deducting the elemental interference .The calibration curve of high content Si (mass fraction of 3.15%‐7.04% ) was prepared using analytical line Si 212.41 nm ,and the curve range in original software was broadened to 0.003%‐7.04% .The calibration curve of high content B (mass fraction of 0.90%‐3.31% ) was prepared using analytical line B 345.14 nm ,and the curve range of B was broadened to 0.000 1%‐3.31% .The content of Si and B in amorphous alloy sample was determined according to the experimental method .The relative standard deviations (RSD ,n=10) were less than 1.0% .The accuracy test results indicated that the determination results of proposed method were consistent with those ob‐tained by inductively coupled plasma atomic emission spectrometry (ICP‐AES) .
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