材料期刊网

采用氢氧化钾在700 ℃熔融20 min,经盐酸酸化、稀释10倍后,选取Si 251.611 nm、Al 396.153 nm、Ca 317.933 nm、Mg 285.213 nm、Ba 233.527 nm、P 334.940 nm、Cu 213.617 nm、Fe 327.393 nm、Sr 407.771 nm为分析线,使用电感耦合等离子体原子发射光谱法(ICP-AES)同时测定Si、Al、Ca、Mg、Ba、P、Cu、Fe、Sr,从而建立了炼钢用脱氧剂中9种主、次量元素的测定方法.结果表明,与酸溶方式相比,采用碱熔前处理对常见的各类脱氧剂可以避免分解不彻底的问题.当称样量为0.1 g时,加入2.0 g氢氧化钾熔剂可以使样品熔解完全.采用基体匹配法绘制校准曲线可以有效消除基体效应的影响,各元素质量浓度在一定范围内与其发射强度呈线性,校准曲线的线性相关系数r≥0.999 8,各元素的检出限在0.001 6%~0.012%之间.按照实验方法测定脱氧剂样品中Si、Al、Ca、Mg、Ba、P、Cu、Fe、Sr,结果的相对标准偏差(RSD,n=11)在0.81%~4.5%之间.实验方法用于测定4个脱氧剂标准样品(E511d、YSB 14609-2001、YSB 14606-2001、YSB 14607-2001)中Si、Al、Ca、Mg、Ba、P、Cu、Fe、Sr,测定值与认定值吻合较好,相对误差在0.25%~7.14%之间.

The deoxidizing agent samples were fused with potassium hydroxide at 700 ℃ for 20 min.After acidification with HCl, the solution was diluted by 10 times.Then, the content of Si, Al, Ca, Mg, Ba, P, Cu, Fe and Sr was simultaneously determined by inductively coupled plasma optical emission spectrometry (ICP-AES) using Si 251.611 nm, Al 396.153 nm, Ca 317.933 nm, Mg 285.213 nm, Ba 233.527 nm, P 334.940 nm, Cu 213.617 nm, Fe 327.393 nm and Sr 407.771 nm as the analytical lines.The method for determination of nine elements in deoxidizing agent samples for steel making was established.Compared to the acid dissolution process, the results showed that the alkali fusion method could avoid the problems of incomplete decomposition for various common deoxidizing agents.0.1 g of sample could be fully fused with 2.0 g of potassium hydroxide.The influence of matrix effect could be effectively eliminated by preparing the calibration curves using matrix matching method.The mass concentration of each element in certain range showed linear relationship with the corresponding emission intensity.The linear correlation coefficients of calibration curves were r≥0.999 8.The detection limits of elements were between 0.001 6% and 0.012%.The content of Si, Al, Ca, Mg, Ba, P, Cu, Fe and Sr in deoxidizing agent samples was determined according to the experimental method, and the relative standard deviations (RSD, n=11) were between 0.81% and 4.5%.The proposed method was applied to the determination of Si, Al, Ca, Mg, Ba, P, Cu, Fe and Sr in four standard samples (E511d, YSB 14609-2001, YSB 14606-2001 and YSB 14607-2001).The found results were consistent with the certified values.The relative errors were between 0.25% and 7.14%.