擦拭检验法在测定核电设备表面氟氯铅和硫酸根中的应用  

Application of wipe test in determination of fluorine,chlorine,lead and sulfate on the surface of nuclear power equipment

作　　者：王楠 魏占超 冶金辉 WANG Nan;WEI Zhanchao;YE Jinhui(Harbin Electric Corporation(QHD)Heavy Equipment Company Limited,Qinhuangdao 066206,China)

机构地区：[1]哈电集团(秦皇岛)重型装备有限公司,河北秦皇岛066206

出　　处：《冶金分析》2024年第5期25-30,共6页Metallurgical Analysis

摘　　要：核电设备表面残留的氟、氯、硫和低熔点金属离子可能会导致材料表面的腐蚀失效,直接影响核反应堆系统的服役寿命和运行安全,因此准确检测核电设备表面的F^(—)、Cl^(—)、Pb^(2+)、SO_(4)^(2-)含量尤为重要。本文建立了一种可以定量检测核电设备表面F^(—)、Cl^(—)、Pb^(2+)、SO_(4)^(2-)含量的新型检验方法:擦拭检验法,共包括样品收集、样品处理和样品检测3个步骤。利用沸水处理后的纱布对核电设备表面进行擦拭,一块纱布擦拭面积一般为20 dm^(2);将擦拭后的纱布和未经擦拭的纱布分别放入烧杯中,加水后在电热板上加热至90~100℃微沸30 min,用不含卤化物的0.45μm滤纸过滤,得到待检测样品和对比样品;用离子色谱法(IC)测定F^(—)、Cl^(—)、SO_(4)^(2-)和石墨炉原子吸收光谱法(GF-AAS)测定Pb^(2+),从而计算出单位面积各离子的含量,实现了对核电设备表面F^(—)、Cl^(—)、SO_(4)^(2-)、Pb^(2+)的准确测定。在优化的实验条件下,F^(—)、Cl^(—)、SO_(4)^(2-)、Pb^(2+)的方法检出限分别为0.01、0.02、0.05、0.001μg/mL。按照实验方法对不锈钢堆焊层表面F^(—)、Cl^(—)、SO_(4)^(2-)、Pb^(2+)进行测定,结果的相对标准偏差(RSD,n=6)为3.6%~5.3%;向样品溶液中加入4种离子的标准溶液进行加标回收试验,回收率为99%~116%。The fluoride,chloride,sulfide and low melting point metal ions on the surface of nuclear power equipment may cause the corrosion failure of material surface,which directly affects the service life and operation safety of nuclear reactor system.Therefore,it is very important to detect the contents of F^(-),Cl^(-),Pb^(2+)and SO^(2-)_(4)on the surface of nuclear power equipment.In this paper,a new detection method,i.e.,wipe test method,for the quantitative determination of F^(-),Cl^(-),Pb^(2+)and SO^(2-)_(4)on the surface of nuclear power equipment was established.This method included three steps:sample collection,sample treatment and sample analysis.The gauze after treatment in boiling water was used to wipe the surface of nuclear power equipment.The wiping area of each gauze was usually 20 dm^(2).The wiped and unwiped gauze samples were put into beakers separately.After adding water,the beaker was heated to slight boiling at 90-100℃for 30 min.Then the solution was filtrated with halide-free 0.45μm filter paper,and the test sample and the contrast sample were obtained.The contents of F^(-),Cl^(-)and SO^(2-)_(4)were determined by ion chromatography(IC),while the content of Pb^(2+)was determined by graphite furnace atomic absorption spectrometry(GF^(-)AAS).Consequently,the content of each ion in unit area could be calculated,realizing the accurate determination of F^(-),Cl^(-),Pb^(2+)and SO^(2-)_(4)on the surface of nuclear power equipment.Under the optimized experimental conditions,the limit of detection of F^(-),Cl^(-),Pb^(2+)and SO^(2-)_(4)in this method was 0.01μg/mL,0.02μg/mL,0.05μg/mL and 0.001μg/mL,respectively.The contents of F^(-),Cl^(-),Pb^(2+)and SO^(2-)_(4)on the surface of stainless-steel welding layer were determined according to the experimental method,and the relative standard deviations(RSD,n=6)of the determination results were between 3.6%and 5.3%.The standard solution of four irons were added into the sample solution for standard recovery tests.The spiked recoveries were between 99%and 116%.

关 键 词：擦拭检验 纱布 核电设备 氟 氯 硫酸根 铅 离子色谱法(IC) 石墨炉原子吸收光谱法(GF-AAS) 

分 类 号：O657.31[理学—分析化学] O657.7[理学—化学] TL28[核科学技术—核燃料循环与材料]