电感耦合等离子体原子发射光谱法测定铝合金中硼

发布时间：2018-06-06 08:05

本文选题：电感耦合等离子体原子发射光谱法 + 萃取　；参考：《冶金分析》2015年08期

【摘要】：铝合金样品采用氢氧化钠溶液和过氧化氢溶解,稀硫酸酸化,然后置于分液漏斗中,pH 3时溶液中硼酸和一定量的苯羟乙酸及孔雀石绿缔合成三元络合物,用苯定量萃取,萃取液直接进入有机进样系统的电感耦合等离子体原子发射光谱仪(ICP-AES),选择分析谱线B 249.678nm测定铝合金中硼。通过样品溶解方法、萃取剂、萃取方法及条件(时间和酸度)的选择,采用基体匹配法消除物理干扰。方法中硼的质量浓度在1.00mg/L以内与其发射强度呈线性关系,校准曲线的线性相关系数r=0.999 3,硼的检出限为0.001mg/L。按照实验方法对标准样品和自备样品分别测定,标准样品的测定值和认定值基本吻合;自备样品测定结果的相对标准偏差(RSD,n=10)小于5%,加标回收率为80%~100%,方法可检测铝合金中质量分数最低为0.000 1%的硼。
[Abstract]:Aluminum alloy samples were dissolved in sodium hydroxide solution and hydrogen peroxide and acidified with dilute sulfuric acid. Boric acid and a certain amount of phenylglycolic acid and malachite green were synthesized in the solution of pH 3 in the funnel and extracted quantitatively by benzene. An inductively coupled plasma atomic emission spectrometer (ICP-AES-) for the determination of boron in aluminum alloy was developed. The analytical line B 249.678nm was selected for the determination of boron in aluminum alloy. The physical interference was eliminated by matrix matching method through the selection of sample dissolution method, extractant, extraction method and conditions (time and acidity). The linear correlation coefficient of calibration curve is 0.999 3 and the detection limit of boron is 0.001 mg / L. According to the experimental method, the standard sample and the self-provided sample were determined, and the measured value of the standard sample was basically consistent with the determined value. The relative standard deviation (RSD) of the determination results of self-provided samples is less than 5. The recovery rate of the added standard is 80 and 100. The method can be used to detect boron with the lowest mass fraction of 0.000 in aluminum alloy.
【作者单位】：重庆工业职业技术学院;重庆市计量质量检测研究院铝镁中心;中原特钢股份有限公司;
【分类号】：TG115.33;TG146.21

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