电感耦合等离子体原子发射光谱法测定硅铁钡孕育剂中9种元素
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摘要
采用硝酸和氢氟酸溶解样品,高氯酸冒烟驱尽硝酸-氢氟酸,盐酸溶解盐类,选择Ba233.527nm、Fe 259.940nm、Ca 317.933nm、Mn 257.610nm、Cr 267.716nm、Al 394.401nm、Ni231.604nm、Cu 327.396nm、P 178.284nm为分析线,使用电感耦合等离子体原子发射光谱法(ICP-AES)测定钡、铁、钙、锰、铬、铝、镍、铜、磷,从而建立了硅铁钡孕育剂中钡、铁、钙、锰、铬、铝、镍、铜、磷等9种元素的测定方法。各元素校准曲线的相关系数均大于0.999 5;方法中各元素检出限为0.000 06%~0.000 69%。按照实验方法测定标准样品GSB03-1607-2003中钡、铁、钙、锰、铬、铝、镍、铜、磷,结果的相对标准偏差(RSD,n=11)为0.63%~3.4%。实验方法用于测定标准样品GSB03-1607-2003和YSB14607-2001中钡、铁、钙、锰、铬、铝、镍、铜、磷,测定值与认定值基本相符。
The sample was dissolved with nitric acid and hydrofluoric acid.Then nitric acid and hydrofluoric acid were removed by perchloric acid fuming.The salts were dissolved with hydrochloric acid.Ba 233.527 nm,Fe259.940 nm,Ca 317.933 nm,Mn 257.610 nm,Cr 267.716 nm,Al 394.401 nm,Ni 231.604 nm,Cu327.396 nm and P 178.284 nm were selected as analytical lines.The contents of barium,iron,calcium,manganese,chromium,aluminum,nickel,copper and phosphorus were determined by inductively coupled plasma atomic emission spectrometry(ICP-AES).Thus the determination method of nine elements in silicon-iron-barium inoculant(including barium,iron,calcium,manganese,chromium,aluminum,nickel,copper and phosphorus)was established.The correlation coefficients of calibration curves of elements were all higher than 0.999 5.The detection limits of method were between 0.000 06% and 0.000 69%.The content of barium,iron,calcium,manganese,chromium,aluminum,nickel,copper and phosphorus in standard sample GSB03-1607-2003 was determined according to the experimental method.The relative standard deviations(RSD,n=11)of determination results ranged from 0.63% to 3.4%.The proposed method was applied for the determination of barium,iron,calcium,manganese,chromium,aluminum,nickel,copper and phosphorus in standard sample GSB03-1607-2003 and YSB14607-2001,and the found results were basically consistent with the certified values.
The sample was dissolved with nitric acid and hydrofluoric acid.Then nitric acid and hydrofluoric acid were removed by perchloric acid fuming.The salts were dissolved with hydrochloric acid.Ba 233.527 nm,Fe259.940 nm,Ca 317.933 nm,Mn 257.610 nm,Cr 267.716 nm,Al 394.401 nm,Ni 231.604 nm,Cu327.396 nm and P 178.284 nm were selected as analytical lines.The contents of barium,iron,calcium,manganese,chromium,aluminum,nickel,copper and phosphorus were determined by inductively coupled plasma atomic emission spectrometry(ICP-AES).Thus the determination method of nine elements in silicon-iron-barium inoculant(including barium,iron,calcium,manganese,chromium,aluminum,nickel,copper and phosphorus)was established.The correlation coefficients of calibration curves of elements were all higher than 0.999 5.The detection limits of method were between 0.000 06% and 0.000 69%.The content of barium,iron,calcium,manganese,chromium,aluminum,nickel,copper and phosphorus in standard sample GSB03-1607-2003 was determined according to the experimental method.The relative standard deviations(RSD,n=11)of determination results ranged from 0.63% to 3.4%.The proposed method was applied for the determination of barium,iron,calcium,manganese,chromium,aluminum,nickel,copper and phosphorus in standard sample GSB03-1607-2003 and YSB14607-2001,and the found results were basically consistent with the certified values.
引文
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[3]李存根,陈延昌,支国瑞,等.硫酸钡重量法测定硅铝钙钡合金中钡的改进[J].冶金分析,2005,25(5):92-93.LI Cun-gen,CHEN Yan-chang,ZHI Guo-rui,et al.Improvement of barium in determination of Si-Al-Ca-Ba alloy by barium sulfate gravimetric method[J].Metallurgical Analysis,2005,25(5):92-93.
[4]焦风菊,郭英英.硅钡孕育剂中钡、钙的测定[J].铸造技术,2011(8):1187-1188.JIAO Feng-ju,GUO Ying-ying.Determination of barium and calcium in Si-Ba inoculant[J].Foundry Technology,2011(8):1187-1188.
[5]谭小菊,邬景荣.硅铁中铁含量的测定[J].大众科技,2013,15(4):80-82.TAN Xiao-ju,WU Jing-rong.Determination of iron in ferrosilicon[J].Popular Science&Technology,2013,15(4):80-82.
[6]黄仁彬.硅铝钡合金中硅、钙、铝的测定[J].冶金分析,2004,24(6):80-81.HUANG Ren-bin.Determination of silicon calcium aluminum in Si-Al-Ba alloy[J].Metallurgical Analysis,2004,24(6):80-81.
[7]李杰,李洁,于录军,等.二苯碳酰二肼分光光度法测定氮化硅铁中铬[J].冶金分析,2016,36(12):69-73.LI Jie,LI Jie,YU Lu-jun,et al.Determination of chromium in ferrosilicon nitride by diphenylcarbonhy drazide spectrophotonetry[J].Metallurgical Analysis,2016,36(12):69-73.
[8]孙宝莲,董岐,周恺,等.火焰原子吸收光谱法测定铜磁铁矿中铜[J].冶金分析,2017,37(3):44-47.SUN Bao-lian,DONG Qi,ZHOU Kai,et al.Determination of copper in copper magnetite by flame atomic absorption spectrometry[J].Metallurgical Analysis,2017,37(3):44-47.
[9]朱国忠,徐艳燕,庞燕,等.连续光源火焰原子吸收光谱法同时测定氢氧化钴中镍铜锰铁钙镁钠镉[J].湿法冶金,2017,36(4):346-349.ZHU Guo-zhong,XU Yan-yan,PANG Yan,et al.Simultaneous determination of nickel,copper,manganese,iron,calcium,magnesium,sodium and cadmiun in cobalt hydroxide by continuous light souce flame atomic absorption spectrometry[J].Hydrometallurgy of China,2017,36(4):346-349.
[10]叶晨亮,胡家明.电感耦合等离子体原子发射光谱法测定地质样品中镉[J].冶金分析,2016,36(6):35-39.YE Chen-liang,HU Jia-ming.Determination of cadmium in geological samples by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2016,36(6):35-39.
[11]陶锐,高舸.电感耦合等离子体光发射光谱分析中无机酸基体效应研究(I)无机酸基体效应及其机理[J].理化检验:化学分册,2005,41(1):67-71.TAO Rui,GAO Ge.Matrix effect of inorganic acids in icp-oes analysis(I)matrix effect of inorganic acids and its mechanism[J].Chinese Journal of Analytical Chemistry,2005,41(1):67-71.