电感耦合等离子体原子发射光谱法测定钴铬钨合金中钨镍铁钒

摘要

采用盐酸、硝酸溶解样品,再加硫磷混酸冒烟,冒烟期间滴加硝酸使碳化物完全溶解,采用基体匹配法配制标准溶液系列消除基体效应的影响,选择 W 207.911 nm、Ni 231.604 nm、Fe 259.940 nm、V 311.071 nm为分析线,使用电感耦合等离子体原子发射光谱法(ICP-A ES)测定钴铬钨合金中钨、镍、铁、钒.钨的质量分数在0.1% ~30% 范围内,镍、铁、钒的质量分数在0.1% ~10% 范围内各元素质量分数与对应的发射强度呈线性,校准曲线线性相关系数不小于0.9997;方法中各元素检出限为0.0008% ~0.0033%(质量分数).按照实验方法测定两个钴铬钨合金中钨、镍、铁、钒,结果的相对标准偏差(RSD,n=6)为1.0% ~1.9%;并与微波消解-电感耦合等离子体原子发射光谱法的测定结果进行对比,测定结果基本一致.%The sample was dissolved with hydrochloric acid and nitric acid.Then the mixture of sulfuric acid and phosphoric acid was added.During fuming,nitric acid was dripped to completely dissolve the car-bides.The standard solution series were prepared by matrix matching method to eliminate the influence of matrix effect.W 207.911 nm,Ni 231.604 nm,Fe 259.940 nm and V 311.071 nm were selected as analytical lines for the determination of tungsten,nickel,iron and vanadium in cobalt chromium tungsten alloy by inductively coupled plasma atomic emission spectrometry(ICP-AES).When the mass fraction of tungsten was in range of 0.1%-30%,and the mass fraction of nickel,iron and vanadium was in range of 0.1%-10%,the mass concentration of each element showed good linearity to the corresponding emission intensity.The linear correlation coefficients of calibration curves were higher than 0.9997.The detection limits of elements in this method were between 0.0008% and 0.0033%(mass fraction).The proposed method was applied for the determination of tungsten,nickel,iron and vanadium in two cobalt chromium tungsten alloy samples.The relative standard deviations(RSD,n=6)of determination results were be-tween 1.0% and 1.9%.The samples were also determined by microwave digestion-inductively coupled plasma atomic emission spectrometry for comparison,and the found results were basically consistent.