电感耦合等离子体原子发射光谱法测定铝合金中硼

Determination of boron in aluminium alloy by inductively coupled plasma atomic emission spectrometry

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，pH3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（ICPAES），选择分析谱线B249．678nm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=0．9993，硼的捡出限为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0．0001％的硼。

The aluminium alloy sample was dissolved with sodium hydroxide solution followed by acidification with dilute sulfuric acid.The solution was transferred into separating funnel.The boric acid in solution could react with certain amount of mandelic acid and malachite green to form ternary complex,which could be quantitatively extracted with benzene.The extract liquor was directly injected into the organic sampling system of inductively coupled plasma atomic emission spectrometer(ICP-AES).The content of boron in ammonium alloy was determined using B 249.678 nm as analytical line.The sample dissolution method,the extracting reagent,the extraction method and conditions(time and acidity)were selected.The physical interference was eliminated by matrix matching method.The mass fraction of boron below1.00mg/L was linear to the emission intensity.The linear correlation coefficient of calibration curve was r=0.999 3.The detection limit of boron was 0.001mg/L.The standard sample and owned sample were determined according to the experimental method.The found results of standard sample were consistent with the certified values.The relative standard deviation(RSD,n=10)of determination results of owned sample was less than 5%.The recoveries were between 80% and 100%.The proposed method was applicable for the detection of boron in aluminium alloy with minimum mass fraction of 0.000 1%.