电感耦合等离子体原子发射光谱法测定铝基复合造渣剂中金属铝

Determination of metallic aluminum in aluminum matrix composite slagging agent by inductively coupled plasma atomic emission spectrometry

利用三氧化二铝不溶于三氯化铁溶液的特性,用50mL 50g/L三氯化铁溶液浸取铝基复合造渣剂样品中金属铝,使用磁力搅拌器搅拌溶解60min,经过滤并使用盐酸(2+98)洗涤沉淀,基体匹配法配制校准曲线消除基体效应的影响,采用Al 308.215nm和Al 396.152nm作为分析谱线,用电感耦合等离子体原子发射光谱法(ICP-AES)测定铝基复合造渣剂中金属铝。试验考察了样品中共存元素的影响,结果表明,样品中w(CaO、SiO2)≤40%、w(MgO)≤30%、w(MnO)≤15%、w(P2O5、BaO)≤10%、w(V、Mo)≤5%、w(Ti)≤3%、w(Ni、Nb)≤1%、w(Cr、Cu)≤0.2%时,不干扰金属铝的测定。当铝基复合造渣剂样品中金属铝质量分数小于2%时,采用Al 396.152nm作为分析线,校准曲线线性回归方程为y=275 00 x+669.1,相关系数r=0.999 4;当金属铝质量分数不小于2%时,使用Al 308.215nm作为分析谱线,校准曲线线性回归方程为y=4 502 x+56.1,相关系数r=0.999 9。方法中金属铝的检出限为0.001%(质量分数)。按照实验方法测定铝基复合造渣剂样品中金属铝,结果的相对标准偏差(RSD,n=8)小于2%,测定值与三氯化铁浸取-氟盐取代EDTA滴定法的测定结果相吻合。

The aluminum oxide could not be dissolved in iron trichloride solution.According to this character,the metallic aluminum in aluminum matrix composite slagging agent sample was leached with 50 mL of50g/L iron trichloride solution.The sample was dissolved for 60 min under the stirring by magnetic stirrer.After filtration,the precipitate was washed with hydrochloric acid(2+98).The calibration curve was prepared by matrix matching method to eliminate the influence of matrix effect.The Al 308.215 nm and Al396.152 nm were selected as the analytical lines.The metallic aluminum in aluminum matrix composite slagging agent was determined by the inductively coupled plasma atomic emission spectrometry(ICPAES).The influence of coexisting elements in sample was investigated by experiments.The results showed that the determination of metallic aluminum was not interfered under the follow conditions:w(CaO,SiO2)≤40%,w(MgO)≤30%,w(MnO)≤15%,w(P2O5,BaO)≤10%,w(V,Mo)≤5%,w(Ti)≤3%,w(Ni,Nb)≤1% and w(Cr,Cu)≤0.2%.When the mass fraction of metallic aluminum in aluminum matrix composite slagging agent sample was less than 2%,Al 396.152 nm was selected as the analytical line,and the linear regression equation of calibration curve was y=27 500 x+669.1with correlation coefficient of r=0.999 4.When the mass fraction of metallic aluminum in aluminum matrix composite slagging agent sample was not less than 2%,Al 308.215 nm was selected as the analytical line,and the linear regression equation of calibration curve was y=4 502 x+56.1with correlation coefficient of r=0.999 9.The detection limit of metallic aluminum in this method was 0.001%(mass fraction).The content of metallic aluminum in aluminum matrix composite slagging agent sample was determined according to the experimental method.The relative standard deviations(RSD,n=8)were less than 2%.The found results were consistent with those obtained by iron trichloride leaching-fluoride replacement EDTA titration method.