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1.3×104μm;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。
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 acidhydrofluoric acid solution sample. According to the principle of high abundance and non-interference,93 Nb,75 As and121 Sb were selected to measure isotopes. The instrument operation condition was optimized to determine the power was 1300 W, the carrier gas flow rate was 1.00 L/min,and the sampling depth was 1.3 ×104μm. 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 with56 Fe19 F 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.
作者
庞振兴
王贵玉
金伟
腰瑞雪
杜士毅
PANG Zhenxing, WANG Guiyu, JIN Wei, YAO Ruixue, DU Shiyi(Shougang Co., Ltd., Qian＇an Steel Corp, Qian＇an 064400, Chin)
出处
《中国测试》
CAS
北大核心
2018年第5期49-52,共4页
China Measurement & Test
关键词
电感耦合等离子体质谱法
硅铁
碰撞/反应池
铌
砷
锑
inductively coupled plasma mass spectrometry （ICP-MS）
ferrosilicon
CCT
niobium
arsenic
stibonium
