电感耦合等离子体原子发射光谱法测定钴铬钨系合金粉末中钨含量的不确定度评定  

Uncertainty evaluation during determination of tungsten content in cobalt-chromium-tungsten alloy powder by inductively coupled plasma atomic emission spectrometry

作　　者：罗海霞 LUO Haixia(BGRIMM MTC Technology Technical Co.,Ltd.,Beijing 102628,China;Bejing Key Lab of Mineral Resource Evaluation&Analysis,Beijing 102628,China)

机构地区：[1]北矿检测技术股份有限公司,北京102628 [2]金属矿产资源评价与分析检测北京市重点实验室,北京102628

出　　处：《冶金分析》2023年第11期90-96,共7页Metallurgical Analysis

基　　金：国家重点研发计划(战略性矿产选冶关键分析检测技术和标准体系研究2021YFC2903101)。

摘　　要：采用微波消解-电感耦合等离子体原子发射光谱法(ICP-AES)测定钴铬钨系合金粉末样品中钨含量,并建立了该方法的定量数学模型并推导出不确定度计算公式,找出了该检测过程中的不确定度的主要来源,主要有标准溶液配制过程、称量过程、溶液定容过程、试液稀释过程、校准曲线拟合过程、重复测量等引入的不确定度分量。按照JJF 1059.1—2012《测量不确定度评定与表示》的规定逐一分析了影响不确定度的主要因素,并对各种不确定度分量进行量化计算,最后得出合成标准不确定度和扩展不确定度,给出测试结果。结果表明:标准溶液配制过程、校准曲线的拟合过程及重复测量是不确定度的主要来源,ICP-AES用于测定钴铬钨系合金粉末样品中钨的结果令人满意,同时为ICP-AES测定钨元素的不确定度评价提供了一定的参考价值。The content of tungsten in cobalt-chromium-tungsten alloy powder samples was determined by microwave digestion-inductively coupled plasma emission spectrometry(ICP-AES).The quantitative mathematical model of this method was established,and the calculation formula of uncertainty was deduced.The main source of uncertainty in the detection process was found out,which mainly included the uncertainty components introduced in the preparation process of standard solution,the weighing process,the constant volume process of solution,the fitting process of calibration curve,and the process of repeated measurement.According to JJF 1059.1-2012 Evaluation and expression of uncertainty in measurement,the main factors affecting the uncertainty were analyzed one by one.Each uncertainty component was quantitatively calculated.Finally,the synthetic standard uncertainty and extended uncertainty were obtained,and the measurement results were provided.The results showed that the preparation process of standard solution,the fitting process of calibration curve,and the process of repeated measurement were main sources of uncertainty.The determination results of tungsten in cobalt-chromium-tungsten alloy powder by ICP-AES were satisfactory.This method provided certain reference for the uncertainty evaluation during determination of tungsten by ICP-AES.

关 键 词：微波消解 电感耦合等离子体原子发射光谱法(ICP-AES) 不确定度 扩展不确定度 合成标准不确定度 

分 类 号：O657.31[理学—分析化学] TF03[理学—化学]