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作 者:黄辉[1] 张树军[2] 巩琛 李本涛[1] 李颖[1] 赵华[1]
机构地区:[1]中国兵器工业集团第五三研究所,山东济南250031 [2]积成电子股份有限公司,山东济南250000
出 处:《冶金分析》2016年第1期79-83,共5页Metallurgical Analysis
摘 要:以盐酸和硝酸作为消解试剂,采取高压密闭微波加热方法对低合金钢样品进行消解。通过考察低合金钢中常见元素以及铁基体对硼各灵敏线的干扰情况,确定B208.959nm作为分析线,建立了非线性干扰等效浓度校正一电感耦合等离子体原子发射光谱法(ICP-AES)测定低合金钢中硼的方法。通过考察铁基体对硼产生的干扰等效浓度与自身质量浓度之间的非线性关系,建立校准曲线。为了确保无需稀释可以直接测定铁基体含量,选择灵敏度较低的Fe218.719nm作为分析线并建立铁校准曲线。考察了不同质量浓度铁在波长B208.959nm处对硼产生的干扰等效浓度,利用多项式拟合铁质量浓度与产生硼的干扰等效浓度之间的校准曲线为y=(0.01225+0.00008ρ)/(1+0.0000410)。将实验方法用于某不锈钢标准样品中硼的测定,结果与参考值相吻合,测定结果的相对标准偏差(RSD,n=6)在3.7%~5.3%之间。The hydrochloric acid and nitric acid were used to digest the low alloy steel sample by microwave heating at high pressure in a closed system. The interference of common elements in low alloy steel and i- ron matrix with the sensitive lines of boron was investigated. B 208. 959 nm was selected as the analytical line. The determination method of boron in low alloy steel by inductively coupled plasma atomic emission spectrometry (ICP-AES) with non-linear interference equivalent concentration correction was established. The calibration curve was prepared by studying the non-linear relationship between the interference equiva- lent concentration of boron caused by iron matrix and the mass concentration itself; In order to determine the content of iron matrix directly without dilution, Fe 218. 719 nm with relatively low sensitivity was used as analytical line. Then, the calibration curve of iron was established. The interference equivalent concen- tration of boron caused by iron with different mass concentrations was investigated at wavelength of B 208. 959 nm. The calibration curve between the mass concentration of iron and interference equivalent concentration of boron was obtained by polynomial fitting, i. e. , y = (0. 012 25 +0. 000 08ρ)/(1 +0. 000 04 ρ). The proposed method was applied to the determination of boron in one standard sample of stainless steel. The found results were consistent with the reference values. The relative standard deviations (RSD, n=6) were between 3.7% and 5.3%.
关 键 词:非线性干扰等效浓度校正法 电感耦合等离子体原子发射光谱法 低合金钢 硼
分 类 号:TG115.33[金属学及工艺—物理冶金]
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