电感耦合等离子体发射光谱法测定石灰岩样品中氧化钾、氧化钠的方法改进  

Improvement of inductively coupled plasma Emission Spectrometry for Determination of Potassium Oxide and Sodium Oxide in Limestone Samples

作　　者：陈丽春[1] Chen Li-chun(Laboratory Testing Center of Fujian Province Geological Brigade 121,Longyan,Fujian 364000,China)

机构地区：[1]福建省121地质大队化验测试中心,福建龙岩364000

出　　处：《福建分析测试》2023年第6期55-59,共5页Fujian Analysis & Testing

摘　　要：本文根据本实验室测试要求,依据检测方法《岩石矿物分析》2011年16.38.2.2对石灰岩样品中氧化钾、氧化钠进行测试遇到的问题,作出相应的方法改进。由于石灰岩样品中主要成分为氧化钙、氧化镁,在使用电感耦合等离子体发射光谱法测试钾钠等元素值时,其信号值会受到高含量CaO(可达45%以上)和MgO(可达5%以上)的显著干扰,使测试值远高于真实值,从而无法获得准确的待测元素含量。为解决这一问题,本文通过实验探寻测试中的主要干扰因素,确定相应的校正方法,并对样品前处理及仪器参数进行了优化,从而减小K、Na及其氧化物的测试误差。对GBW07120、GBW03107、GBW070149三个石灰岩国家一级标准物质进行验证,测定结果均在标准误差范围内,准确度精密度均符合要求,值得推广应用。This article is based on the testing requirements of our laboratory,and according to the testing method"Rock Min⁃eral Analysis"(16.38.2,2011),the problems encountered in the testing of potassium oxide and sodium oxide in limestone samples are analyzed,and corresponding method improvements are made.Since the limestone samples are mainly com⁃posed of calcium oxide and magnesium oxide,when using inductively coupled plasma emission spectrometry to test the val⁃ues of other elements,their signal values will be significantly interfered by the high content of CaO(up to 45%)and MgO(up to 5%),making the test values far higher than the true values,so it is impossible to obtain accurate content of the ele⁃ments to be measured.To address this issue,this article explores the main interference factors in testing through experi⁃ments,determines corresponding calibration methods,and optimizes sample pretreatment and instrument parameters to re⁃duce the testing errors of K,Na,and their oxides.The validation of three national first-class standard materials for lime⁃stone,GBW07120,GBW03107,and GBW070149,showed that the measurement results were all within the standard error range,with high accuracy and good precision,which is worth promoting and applying.

关 键 词：电感耦合等离子体发射光谱 石灰岩 氧化钾 氧化钠 

分 类 号：O657.31[理学—分析化学]