压水堆核电机组一回路腐蚀产物样品前处理及测量方法研究  

Study on the Pretreatment and Detection Method for Primary Corrosion Products in PWR Nuclear Power Plants

作　　者：吕传君 梁维江 伊海龙 LYU Chuanjun;LIANG Weijiang;YI Hailong(Daya Bay Nuclear Power Operations and Management Co.,Ltd.Shenzhen of Guangdong Prov.518000,China)

机构地区：[1]大亚湾核电运营管理有限公司,广东深圳518000

出　　处：《核科学与工程》2024年第1期135-141,共7页Nuclear Science and Engineering

摘　　要：本研究通过实验室方法探测和现场检测验证进行压水堆核电机组一回路腐蚀产物样品前处理及测量方法研究,方法研究过程中考察样品前处理和测量方法两个维度对测量结果的影响。其中,方法研究过程分别考查样品前处理加酸种类(分别为硝酸和王水)和加酸后静置时间(分别静置1 h、4 h、24 h)对测量结果精密度、准确度和检出限的影响。综合火焰原子吸收光谱法、石墨炉原子吸收光谱法、电感耦合等离子体发射光谱法、电感耦合等离子体质谱法和离子色谱法这几种检测方法的检出限、适用测试样品性质及国内核电厂仪器资源配置,本文选择电感耦合等离子体发射光谱法作为样品检测方法,并用石墨炉原子吸收光谱法辅助验证。结果表明一回路腐蚀产物样品前处理过程采用硝酸酸化,加酸量控制在1%,加酸后24 h内完成测量,采用电感耦合等离子体发射光谱法(ICP-OES)作为样品检测方法,是一种检出限低(检出限低于1μg/kg)、精密度高(相对标准偏差值介于6.54%~14.07%)和准确度高(加标回收率在99.2%~104.4%)的测量方法。The laboratory test and the onsite sample test confirmation were carried out to study the pretreatment and detection method for primary corrosion products pretreatment and detection method in PWR nuclear power plants.The effect of the sample pre-treatment and analysis method selection were considered in the whole process.The influence of different type of the acid(nitric acid and aqua regia,respectively)used in the pr-treatment process and the standing time for acidified samples(1 h,4 h,24 h)on the precision,accuracy and detection limit of analysis results were discussed.The detection methods considered in this paper include the flame atomic absorption,graphite furnace atomic absorption spectrometer,inductively coupled plasma-optical emission spectrometer,inductively coupled plasma emission mass spectrometer and ion chromatography.Based on the detection limit,the applicable objects and the PWR unit instrument configuration,the inductively coupled plasma-optical emission spectrometer was selected as the detection method and the graphite furnace atomic absorption spectrometer was supported verified.The study result shows that the corrosion product acidified with the nitric acid while the volume of nitric acid added controlled at 1%,and the acidified sample was analyzed in 24 hours after the acidified process.The inductively coupled plasma-optical emission spectrometer used as the nickel analysis method was proved to be a measurement method with lower detection limit(the detection limit below 1μg/kg),high precision(the relative standard deviation between 6.54%and 14.07%)and high accuracy(the recovery rate between 99.2%and 104.4%).

关 键 词：压水堆核电厂 一回路注锌 腐蚀产物 镍元素 

分 类 号：TL48[核科学技术—核技术及应用]