电感耦合等离子体原子发射光谱法测定钛铁中硅和磷
Determination of silicon and phosphorus in ferrotitanium by inductively coupled plasma atomic emission spectrometry
田玉伟 1孙卓 1于丽泓1
作者信息
- 1. 本钢板材质检计量中心,辽宁本溪 117000
- 折叠
摘要
采用国标GB/T 4701测定钛铁中硅和磷,耗时长且操作繁琐.实验采用硝酸-盐酸-氢氟酸的酸溶体系溶解样品,选择Si 212.412 nm、P 185.924 nm作为硅、磷元素的分析谱线,用钛铁标准物质/样品绘制校准曲线消除基体效应的影响,建立了电感耦合等离子体原子发射光谱法(ICP-AES)测定钛铁中硅和磷的方法.硅和磷校准曲线的线性相关系数均不小于0.999 5;方法中硅和磷的检出限为0.001 5％和0.000 5％,定量限为0.004 9％和0.001 7％.按照实验方法测定3个钛铁样品中硅和磷,结果的相对标准偏差(RSD,n=11)小于2％;钛铁标准物质/样品中硅和磷的测定结果与认定值/标准值相符.分别使用实验方法与国标方法GB/T 4701测定钛铁实际样品中硅和磷,结果未超规定的允许差.
Abstract
The determination method of silicon and phosphorus in ferrotitanium by GB/T 4701 is time-con-suming with complicated operation.In this study,the sample was dissolved using an acid soluble system composed of nitric acid,hydrochloric acid and hydrofluoric acid.Si 212.412 nm and P 185.924 nm were se-lected as the analytical line for silicon and phosphorus,respectively.Ferrotitanium reference materials/samples were used to draw calibration curves to eliminate the influence of matrix effect.A method for the determination of silicon and phosphorus in ferrotitanium by inductively coupled plasma atomic emission spectrometry(ICP-AES)was established.The linear correlation coefficients of calibration curves for sili-con and phosphorus were not less than 0.999 5.The limits of detection for silicon and phosphorus were 0.001 5％and 0.000 5％,and the limits of quantification were 0.004 9％and 0.001 7％,respectively.The contents of silicon and phosphorus in three ferrotitanium samples were determined according to the ex-perimental method,and the relative standard deviations(RSD,n=11)of the results were less than 2％.The determination results of ferrotitanium reference materials/samples were consistent with the certified values/standard values.The contents of silicon and phosphorus in ferrotitanium samples were determined according to the experimental method and national standard method GB/T 4701,and the found results did not exceed the specified allowable deviation.
关键词
钛铁/电感耦合等离子体原子发射光谱法(ICP-AES)/硅/磷Key words
ferrotitanium/inductively coupled plasma atomic emission spectrometry(ICP-AES)/silicon/phosphorus引用本文复制引用
出版年
2024
NETL
NSTL
万方数据