Abstract：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-, Pb2+ and SO2-4 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-, Pb2+ and SO2-4 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 dm2. 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 0.45 μm filter paper, and the test sample and the contrast sample were obtained. The contents of F-, Cl- and SO2-4 were determined by ion chromatography (IC), while the content of Pb2+ 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-, Pb2+ and SO2-4 on the surface of nuclear power equipment. Under the optimized experimental conditions, the limit of detection of F-, Cl-, Pb2+ and SO2-4 in this method was 0.01 μg/mL, 0.02 μg/mL, 0.05 μg/mL and 0.001 μg/mL, respectively. The contents of F-, Cl-, Pb2+ and SO2-4 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%.
王楠, 魏占超, 冶金辉. 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[J]. 冶金分析, 2024, 44(5): 25-30.
WANG Nan, WEI Zhanchao, YE Jinhui. Application of wipe test in determination of fluorine,chlorine,lead and sulfate on the surface of nuclear power equipment. , 2024, 44(5): 25-30.
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