程序升温-称量法测定1AW溶液中总氧化物含量  

Determinations of total oxide content in 1AW liquid waste by temperature-programmed gravimetric method

作　　者：康晓燕 梁馨月 罗中艳[1] 朱海巧[1] 应浙聪[1] 李定明[1] 左臣[1] KANG Xiaoyan;LIANG Xinyue;LUO Zhongyan;ZHU Haiqiao;YING Zhecong;LI Dingming;ZUO Chen(China Institute of Atomic Energy,Department of Radiochemistry,Beijing 102413,China)

机构地区：[1]中国原子能科学研究院,放射化学研究所,北京102413

出　　处：《化学分析计量》2023年第4期52-58,共7页Chemical Analysis And Meterage

摘　　要：建立了程序升温-称量法测定1AW溶液中总氧化物含量的分析方法。利用热重分析方法和拉曼光谱分析方法对1AW溶液中关键核素的分解行为进行系统性研究,最终优选出1AW溶液的煅烧温度,并筛选样品盒材质和优化两步法升温程序的温度参数。该方法取样体积为20~70μL,样品加热时长约130 min,总氧化物含量的测量相对标准偏差为5.1%(n=6),氧化锆测定结果的相对误差为-3.7%~3.7%,精密度、准确度满足工艺分析需求。An analytical method of determining the total oxide content in 1AW liquid waste by temperature-programmed gravimetric method was established.A systematic study was conducted on the decomposition behavior of key nuclides in 1AW solution using thermogravimetric analysis and Raman spectroscopy.The calcination temperature of the 1AW solution was optimized,the sample cell was selected,and the temperature parameters was optimized in two-step temperature program.By using this method,the sampling volume is 20-70μL and the sample is heated for about 130 minutes,the relative standard deviation(RSD)of the total oxide content was 5.1%(n=6),and the relative error of ZrO 2 were-3.7%to 3.7%,meeting the analysis requirement of the reprocessing process.

关 键 词：1AW溶液 总氧化物 称重法 热重分析 

分 类 号：O657.99[理学—分析化学]