电感耦合等离子体原子发射光谱法测定高铝高钙改质剂中金属铝、三氧化二铝和氧化钙  

Determination of metallic aluminum,aluminum oxide and calcium oxide in high-aluminum high-calcium modifier by inductively coupled plasma atomic emission spectrometry

作　　者：李静 张春花 杨忠梅 柴烨 LI Jing;ZHANG Chunhua;YANG Zhongmei;CHAI Ye(HBlS Group Tangsteel Company,Tangshan 063611,China)

机构地区：[1]河钢集团唐钢公司,河北唐山063611

出　　处：《冶金分析》2022年第3期72-77,共6页Metallurgical Analysis

摘　　要：对高铝高钙改质剂中金属铝、三氧化二铝、氧化钙含量的准确测定可指导配料精细冶炼,控制成本,又可客观评价进厂物料质量。由于高铝高钙改质剂是粉末状和屑状混合的物料,所以将样品过0.125 mm样筛,筛上样品和筛下样品分别采用三氯化铁溶液在电磁搅拌下溶解,滤上样品经灰化、熔融、酸化、定容,滤下样品溶液直接定容,再选择Al 394.401 nm、Ca 317.933 nm为分析谱线,使用电感耦合等离子体原子发射光谱法(ICP-AES)分别测定筛上样品溶液和筛下样品溶液中铝和钙。根据校准曲线分别计算出高铝高钙改质剂中滤上和滤下样品溶液中金属铝、三氧化二铝和氧化钙含量,经加权平均法计算样品中金属铝、三氧化二铝和氧化钙总量。按照实验方法测定高铝高钙改质剂实际样品中金属铝、三氧化二铝和氧化钙并进行加标回收试验,结果的相对标准偏差在(RSD,n=8)为0.25%~6.1%,回收率为91%~106%。采用实验方法和X射线荧光光谱法进行方法比对试验,二者测定结果相符。The accurate determination of metallic aluminum,aluminum oxide and calcium oxide in high-aluminum high-calcium modifier could guide the fine smelting,control the cost,and evaluate the material quality objectively.Since the high-aluminum high-calcium modifier was a kind of mixture of powder and crumb materials,the sample was screened with 0.125 mm sieve.The samples on the screen and under the screen were dissolved by ferric chloride solution with electromagnetic stirring,respectively.After filtration,the sample on the filter paper was ashed,melted,acidified,and diluted to the mark.The filtrate solution was directly diluted to the certain volume.Al 394.401 nm and Ca 317.933 nm were selected as the analytical line.The contents of aluminum and calcium in the solution of sample on the screen and under the screen were determined by inductively coupled plasma atomic emission spectrometry(ICP-AES).According to calibration curves,the contents of metallic aluminum,aluminum oxide and calcium oxide in sample solution of high-aluminum high-calcium modifier were calculated.The total amount of metallic aluminum,aluminum oxide and calcium oxide in sample was calculated by weighted average method.The proposed method was applied for determination of metallic aluminum,aluminum oxide and calcium oxide in high-aluminum high-calcium modifier samples,and the recovery tests was conducted.The relative standard deviations(RSD,n=8) of the determination results were between 0.25% and 6.1%.The recoveries were between 91% and 106%.The method comparison test was conducted with the proposed method and X-ray fluorescence spectrometry,and the results were consistent.

关 键 词：高铝高钙改质剂 金属铝 三氧化二铝 氧化钙 电感耦合等离子体原子发射光谱法(ICP-AES) 

分 类 号：O657.31[理学—分析化学] TG115.33[理学—化学] TF111[金属学及工艺—物理冶金]