作者：庞振兴, 王贵玉, 金伟, 腰瑞雪, 杜士毅

作者单位：首钢股份公司迁安钢铁公司, 河北 迁安 064400

关键词：电感耦合等离子体质谱法;硅铁;碰撞/反应池;铌;砷;锑

摘要：

在高锰酸钾存在下，采用硝酸-氢氟酸溶解样品，建立电感耦合等离子体质谱法（ICP-MS）测定硅铁中铌、砷、锑含量的方法。根据丰度高和无干扰的原则来选择93Nb、75As、121Sb为测量同位素；对仪器工作条件进行优化，确定功率为1 300 W，载气流量为1.00 L/min，采样深度为1.3104 m；以钇、铑、铟为内标元素对仪器信号漂移和基体效应进行校正试验，选择10 ng/mL铑为内标。在标准模式下与碰撞/反应池（CCT）模式下砷的测定结果一致，该方法标准模式下测定砷没有受到56Fe19F的干扰。该方法铌、砷、锑的检出限分别为0.087，0.313，0.069 ng/mL；测定下限分别为0.291，1.042，0.229 ng/mL。可作为测定硅铁中痕量铌、砷、锑元素含量的分析方法。

Determination of trace niobium, arsenic and stibonium in ferrosilicon by ICP-MS

PANG Zhenxing, WANG Guiyu, JIN Wei, YAO Ruixue, DU Shiyi

Shougang Co., Ltd., Qian'an Steel Corp, Qian'an 064400, China

Abstract: In the presence of Potassium Permanganate, the method of determining the content of niobium, arsenic and stibonium in silicon iron by ICP-MS was established by using nitric acid-hydrofluoric acid solution sample. According to the principle of high abundance and non-interference, ⁹³Nb, ⁷⁵As and ¹²¹Sb were selected to measure isotopes. The instrument operation condition was optimized to determine the power was 1 300 W, the carrier gas flow rate was 1.00 L/min, and the sampling depth was 1.3×10⁴ μm. Yttrium, rhodium and indium are used as the internal standard elements to calibrate the instrument signal drift and matrix effect, and 10 ng/mL rhodium solution is selected as the internal standard. Under the standard model, the determination of arsenic in the model was consistent with the collision/reaction cell technology(CCT) model. Under the standard model, there was no interference with ⁵⁶Fe¹⁹F in the determination of arsenic. The detection limits of niobium, arsenic and antimony were 0.087 ng/mL, 0.313 ng/mL and 0.069 ng/mL, respectively, and the lower limits were 0.291 ng/mL, 1.042 ng/mL and 0.229 ng/mL, respectively. It could be used as an analytical method for the determination of trace amounts of niobium, arsenic and antimony in ferrosilicon.

Keywords: inductively coupled plasma mass spectrometry(ICP-MS);ferrosilicon;CCT;niobium;arsenic;stibonium

2018, 44(5): 49-52  收稿日期: 2017-12-19;收到修改稿日期: 2018-01-15

基金项目: 

作者简介: 庞振兴(1987-),男,河南安阳市人,工程师,主要从事铁合金、耐火材料的检测及研究。

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