旋转圆盘电极原子发射光谱法检测变压器油中金属及污染物元素含量及其不确定度评估  

Determination of mental and pollutant element content in transformer oilby rotating disk electrode atomic emission spectrometry and itsuncertainty evaluation

作　　者：邹梦 赵举 韩丹丹 张亮 李国斌 王瑞英 ZOU Meng;ZHAO Ju;HAN Dandan;ZHANG Liang;LI Guobin;WANG Ruiying(Electric Power Research Institute of State Grid Xinjiang Electric Power Co.,Ltd.,Urumqi 830011,China)

机构地区：[1]国网新疆电力有限公司电力科学研究院,新疆乌鲁木齐830011

出　　处：《绝缘材料》2024年第3期102-107,共6页Insulating Materials

摘　　要：本文采用旋转圆盘电极原子发射光谱法(RDE-AES)测定变压器绝缘油中银、铝、钡等21种金属及污染物元素含量,考察了圆盘电极浸油深度以及油样均匀化方式对检测结果的影响,并用标准油和绝缘油样品对实验方法进行了验证。结果表明:当选择圆盘电极浸油深度为其直径的1/3时,超声3 min且用力摇匀后检测,检测结果相对误差较小。各元素检出限为0~1.07μg/g,相对标准偏差(RSD,n=6)为0.7%~2.9%,除V元素外,其他20种元素加标回收率为96.64%~110.01%。对绝缘油中P元素含量进行A类和B类不确定度评定,并对各分量不确定度进行合成和扩展,得到不确定度为(8.34±1.06)μg/g(k=2),此不确定度主要来源于工作曲线的标准油样、测量重复性和日常标准化过程。In this paper,the rotating disc electrode atomic emission spectrometry(RDE-AES)was used to determine the content of 21 mental and pollution elements such as silver,aluminum,and barium and other pollutants in transformer insulating oil.The influences of the immersion depth of disk electrode and the homogenization method of oil sample on the test results were investigated,and the test method was verified with the standard oil and insulating oil samples.The results show that when the immersion depth of disk electrode is 1/3 of its diameter,the relative error of the detection results is small after 3 min of ultrasound and vigorous shaking.The detection limits of each elements is 0−1.07μg/g,the relative standard deviations(RSD,n=6)are 0.7%−2.9%,and except for element V,the recoveries of the other 20 elements are 96.64%−110.01%.The element P content in insulating oil was used to evaluate the class A and class B uncertainties,and the uncertainty of each component was synthesized and expanded to obtain an uncertainty of(8.34±1.06)μg/g,(k=2).The uncertainty mainly comes from the standard oil,measurement repeatability,and daily standardization processes.

关 键 词：绝缘油 旋转圆盘电极 发射光谱 元素含量 不确定度 

分 类 号：TM214[一般工业技术—材料科学与工程]