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联用扫描电子显微镜-能谱法和电感耦合等离子体质谱法核取证表征铀矿石浓缩物
Determination of Nuclear Forensic Signatures in Uranium Ore Concentrates by Combining SEM-EDS with ICP-MS
【摘要】 该研究建立了联合扫描电子显微镜-能谱法(SEM-EDS)、全溶/电感耦合等离子体质谱法(ICP-MS)和萃淋去铀电感耦合等离子体质谱法(CL-TBP/ICP-MS)鉴别铀矿石浓缩物(UOC)中60余种杂质元素种类和含量的方法。通过SEM-EDS得到5种UOC的表面微观形貌,并结合ICP-MS得到的N、O、S、K和Cl等基体元素的含量信息,可初步判断不同UOC的生产方式及其化学组成。全溶/ICP-MS方法可快速测定Na、Ca、Fe等含量较高的基体元素,特别在测量W、Sn等易吸附或水解元素含量方面具有优势。CL-TBP/ICP-MS方法的优势在于可获得包含极低含量目标元素在内的60种元素的种类和浓度,对重点关注的稀土元素的检出限可达10-9 g/g量级。根据稀土元素含量及其分布模式信息,可有效鉴别不同来源的UOC,并初步推测其成矿类型。该方法操作简便、结果准确、重现性好,可为铀矿石浓缩物和其他铀基体材料的核取证表征、解析溯源、数据库建设等提供参考和技术支持。
【Abstract】 Scanning electron microscopy-energy dispersive spectrometer(SEM-EDS),inductively coupled plasma mass spectrometry(ICP-MS) and ICP-MS with CL-TBP resin column(CL-TBP/ICP-MS) have been combined to determine the elemental signatures of uranium ore concentrate(UOC) samples. Analysis of the 5 UOCs at the microscopic level showed that the microstructures(particle size,shape,surface texture) of the UOC Bayanwula and UOC Tianshan are different from those of the UOC Jinyuan and UOC Tongliao. It seems that UOCs from precipitation may exist crystal on the surface. The SEM-EDS is a fast and flexible methodology for the determination of N,O,S,K and Cl,which are hard to be measured by ICP-MS. The results obtained from the SEM-EDS preliminari-ly showed the production process and chemical compositon of different UOCs. The matrix elements Na,Ca and Fe were analyzed in solution mode/ICP-MS,as well as W and Sn,which are easily ab-sorbed or hydrolyzed. The measurements of trace elements for UOCs were conducted by CL-TBP/ICP-MS,which can detect more than sixty elements and those concentrations. Moreover,the detec-tion of rare earth elements(REEs) of CL-TBP/ICP-MS is 10-9 g/g. As a result,this method is espe-cially suit for REE patterns,from which each UOC was categorized from each other. Therefore,ef-fective nuclear forensic investigations of 5 UOCs were proposed rely on combining SEM-EDS with ICP-MS. The method is convenient,accurate and reproducible,giving a powerful tool for the nucle-ar forensic analysis and databases development of UOCs and other uranium materials.
【Key words】 nuclear forensic; uranium ore concentrates; material morphology; matrix elements; trace elemental impurities; REE pattern;
- 【文献出处】 分析测试学报 ,Journal of Instrumental Analysis , 编辑部邮箱 ,2024年10期
- 【分类号】TL212;O657.63
- 【下载频次】77