介绍了利用电感耦合等离子体原子发射光谱(ICP-AES)测定钢铁合金中全硅的方法。样品用盐酸和硝酸溶解,不溶物经过滤、干燥、灰化和灼烧后,在950 ℃温度下用碳酸钠和硼酸混合熔剂熔融,熔块溶解于滤液中,在优化的工作条件下采用ICP-AES法测定溶液中全硅量。大量的铁、钠、硼产生基体干扰,但可以用标准加入法消除。本法已用于含硅量不同的标准样品的测定,得到的测定值与认定值相符,用于钢铁样品中全硅的测定,其结果与国家标准方法-还原型硅钼酸盐分光光度法的测定结果相符。
Abstract
This paper introduced the determination of total Si in steel and iron with inductively coupled plasma atomic emission spectrometry(ICP-AES). After the sample was dissolved with HCl and HNO3, the undissolved substance was fused with sodium carbonate and boric acid at 950 ℃after treatment of filtration, drying, incineration and ignition. The fused blocks were dissolved in the filtrate. The content of total silicon was then determined with ICP-AES under the optimal working conditions. A large amount of Fe, Na and B would generate interference, but the interference was removed by standard addition method. The proposed method has been applied to the determination of certified reference material containing different amount of silicon. The found values are consistent with the certified values. The method was also employed to determine total silicon in steel samples, and the results agreed with the reduced molybdosilicate spectrophotometry(National Standards).
关键词
钢铁 /
全硅 /
标准加入法 /
电感耦合等离子体原子发射光谱法
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Key words
iron and steel /
total silicon /
inductively coupled plasma atomic emission spectrometry
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中图分类号:
O657.31
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参考文献
[1] 王海燕.钢铁中硅的测定[J],贵州化工(Guizhou Chemical industry),2009,34(02):39-41.
[2]GB/T 20125-2006 低合金钢 多元素含量的测定 电感耦合等离子体原子发射光谱法[s].
[3]GB/T 223.5-2008 钢铁 酸溶硅和全硅含量的测定 还原型硅钼酸盐分光光度法[s].
[4]GB/T 223.60-1997钢铁及合金化学分析方法 高氯酸脱水重量法测定硅含量[s].
[5] 梁述忠, 许崇礼, 张珈铭,等.利用氟离子选择性电极间接测定钢铁中硅含量[J],冶金分析(Metallurgical Analysis),2008 ,28 (8):36-39.
[6] 侯曼玲,邓飞跃,鲁统娟,等. 硼氢化钾还原-硅钼蓝分光光度法测定钢铁中硅[J ] . 冶金分析(Metallurgical Analysis) ,2004 ,24 (1) :39-41
[7] 辛仁轩 等离子体发射光谱分析[M] 北京:化学工业出版社,2005 : 183,155.
[8] 程键.电感耦合等离子体原子发射光谱法测定锌精矿及焙砂中10 种杂质元素[J], 冶金分析,2007,27(11):65-68.
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脚注
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