电感耦合等离子体原子发射光谱法测定高碳锰铁中硅含量  

Determination of silicon content in high-carbon ferromanganses by inductively coupled plasma atonmic emission spectrometry

作　　者：王李鑫 WANG Lixin(Zenith Steel Group Company Limited,Changzhou 213000,Jiangsu,China)

机构地区：[1]中天钢铁集团有限公司,江苏常州213000

出　　处：《四川冶金》2021年第4期55-58,共4页Sichuan Metallurgy

摘　　要：电感耦合等离子体发射光谱法测高碳锰铁中硅含量是较为准确的方法,因高碳锰铁中碳含量一般在7%以上,所以样品的前处理普遍借助微波消解仪进行高温高压消解,未配备微波消解仪的实验室无法便捷地对样品进行前处理。实验使用硝酸与氢氟酸在常温下溶解样品,建立了电感耦合等离子体发射光谱法检测高碳锰铁中硅含量的分析方法。采用国家标准物质绘制检测曲线,通过实验确定:称样量0.1000 g时用20 ml(1+1)硝酸和5 ml氢氟酸溶解样品后过滤定容;在仪器设定的参数条件下,在推荐分析谱线212.412 nm处可得准确测定结果。实验结果显示:硅含量在0.073%~2.38%(质量分数)范围内,硅的检测强度与对应的质量分数呈线性关系,校准曲线的线性相关系数r为0.9999。按照实验方法测定高碳锰铁合金有证标准物质中硅,测定值与标准值的误差均符合国家标准要求。有效解决了高碳锰铁样品前处理依赖微波消解仪的问题,可用于高碳锰铁中硅含量的快速测定。Inductively coupled plasma emission spectroscopy is a more accurate method for the determination of silicon content in ferromanganese with high carbon.Because the carbon content in ferromanganese with high carbon is generally more than 7%,the pretreatment of samples is generally carried out by microwave digestion instrument at high temperature and high pressure.A method for the determination of silicon content in ferromanganese with high carbon by inductively coupled plasma emission spectrometry(ICPES)was established.Using the national standard material to draw the test curve,through the experiment to determine:weighing 0.1000 g with 20 ml(1+1)nitric acid and 5 ml hydrofluoric acid dissolved samples were filtered and fixed volume.Under the condition of parameters set by the instrument,line 212.412 nm under the condition of the parameters set by the instrument.The experimental results show that in the range of 0.073~2.38%(mass fraction),the detection intensity of silicon is linearly related to the corresponding mass fraction,and the linear correlation coefficient of calibration curve is r 0.9999.According to the experimental method,the silicon in the certified standard material of high carbon manganese ferroalloy is determined,and the error between the measured value and the standard value is in accordance with the requirements of the national standard.It effectively solves the problem that the pretreatment of high carbon ferromanganese sample depends on microwave digestion instrument,and can be used for the rapid determination of silicon content in high carbon ferromanganese.

关 键 词：高碳锰铁 硅含量测定 电感耦合等离子体发射光谱法 样品前处理 

分 类 号：TG115.3[金属学及工艺—物理冶金] O657.31[金属学及工艺—金属学]