铅铋合金蒸馏捕集物中痕量Te的测定

    Determination of Trace Tellurium in Lead-Bismuth Eutectic Distilled Catch

    • 摘要: 采用高温蒸馏捕集技术能有效提取铅铋冷却剂中大量的210Po,用Te替代210Po能高效研究210Po提取工艺,测量蒸馏捕集物中痕量Te能为210Po提取工艺提供有力支持。硝酸浸取蒸馏捕集片上的Te,717强碱性阴离子树脂对浸取液中的Te进行分离,以排除杂质离子的干扰;SnCl2在HCl介质中将Te4+还原为Te单质,于分光光度计上测量吸光度,得到样品中痕量Te的含量。探究了浸取液中干扰离子对Te测量值的影响;研究了上柱液酸度、洗脱剂浓度及用量、淋洗速率对Te分离效果的影响;建立了铅铋冷却剂蒸馏捕集物中痕量Te的分光光度测定方法。结果表明:室温下,淋洗液HCl浓度为4 mol/L,超纯水为洗脱剂,淋洗速率2 mL/min,717强碱性阴离子树脂对Te的分离效果理想;在Te质量浓度0~10 mg/L范围内,吸光度与Te的浓度呈良好的线性关系,相关系数r2= 0.999 9,测量相对标准偏差为0.3%~2.7%(测量次数n=6),重加回收率为96.0%~101.9%,测定方法满足210Po提取工艺研究要求。

       

      Abstract: Lead-bismuth coolant in nuclear reactors generates and accumulates 210Po during operation, which has strong toxicity and high volatility. When the coolant leaks or the reactor is opened, some of the 210Po on the surface of the coolant and in the covering gas will diffuse out of the main system if not properly handled and released into the environment, posing a potential serious threat to the ecological environment and human health. The high-temperature distillation capture technology can effectively extract large amounts of 210Po from the lead-bismuth coolant. Since 210Po is an extremely toxic radioactive isotope with no stable isotope, and to facilitate the experimental study of the capture process, this study ultimately chose its isotopic cousin, Te, as a substitute for 210Po for experimental research. Measuring the trace amount of Te in the distillation capture product can provide strong support for the 210Po extraction process. In the experiment, Te was extracted from the distillation capture film using nitric acid, and the 717 strong basic anion resin was used to separate Te from the extraction solution to eliminate the interference of impurity ions. SnCl2 reduced Te4+ to Te in HCl medium, and the absorbance was measured on a spectrophotometer to obtain the content of trace Te in the sample. The influence of interfering ions in the extraction solution on the measurement value of Te was investigated; the effects of the pH of the column liquid, the concentration and amount of the elution agent, and the washing rate on the separation of Te were explored; and a spectrophotometric method for the determination of trace Te in the distillation capture product of lead-bismuth coolant was established. The results show that at room temperature, the HCl concentration of the column liquid is 4 mol/L, the eluent is ultrapure water, the washing rate is 2 mL/min. The 717 strong basic anion resin demonstrates excellent separation performance for Te across a concentration range of 0 to 10 mg/L, where the absorbance shows a strong linear correlation with Te concentration. The correlation coefficient is r2=0.999 9, with a relative standard deviation of measurement ranging from 0.3% to 2.7%(n=6). The recovery rate is between 96.0% and 101.9%. This measurement method satisfies the requirements for researching the 210Po extraction process.

       

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