通过硝酸-氢氟酸-盐酸分解试样,高氯酸冒烟驱走硅和氟,最后用盐酸溶解盐类,选择Al 396.152 nm、Ca 315.887 nm、Ba 233.527 nm、Mn 257.610 nm、Zr 339.197 nm作为分析线,电感耦合等离子体原子发射光谱法(ICP-AES)测定硅锰锆孕育剂中铝、钙、钡、锰、锆.通过对试液分取稀释,降低和避免了铁离子共存体系中基体效应和光谱干扰对待测元素测定的影响.铝、钙、钡、锰、锆质量浓度在0.50~4.00μg/mL 时与其发射强度呈线性,校准曲线的线性相关系数均大于0.9999;方法中铝钙、钡、锰、锆的检出限为0.60 ~ 1.1 μg/g.按照实验方法测定硅锰锆孕育剂中铝、钙、钡、锰、锆,结果的相对标准偏差(RSD ,n = 10)为1.6% ~3.0% ,并与其他方法测定结果基本一致.
The sample was decomposed with nitric acid-hydrofluoric acid-hydrochloric acid.After removing silicon and fluorine by perchloric acid smoking, the salts were finally dissolved with hydrochloric acid.Al 396.152 nm, Ca 315.887 nm, Ba 233.527 nm, Mn 257.610 nm and Zr 339.197 nm were selected as analytical lines to determine aluminum, calcium, barium, manganese and zirconium in silicon-manganese-zirconium inoculant by inductively coupled plasma atomic emission spectrometry (ICP-AES).The influence of matrix effect and spectral interference on determination caused by coexisting ion irons was reduced and avoided via sample solution dilution.The mass concentration of aluminum, calcium, barium, manganese and zirconium in range of 0.50-4.00 μg/mL was linear to its corresponding emission intensity.The linear correlation coefficients of calibration curves were higher than 0.999 9.The detection limit of aluminum, calcium, barium, manganese and zirconium was between 0.60 μg/g and 1.1 μg/g.The relative standard deviations (RSD, n=10) of determination results for aluminum, calcium, barium, manganese and zirconium in silicon-manganese-zirconium inoculant according to experimental method were between 1.6% and 3.0%.The results were consistent with those obtained by other methods.
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