氢化物发生-电感耦合等离子体质谱法测定砂岩型铀矿样品中痕量镉  

Determination of trace cadmium in sandstone type uranium ore samples by hydride generation inductively coupled plasma mass spectrometry

作　　者：张良圣[1] 常阳[1] 谢灵扬 赵国英 张琪[1] 张建新 梁潇 张彦辉[1] ZHANG Liangsheng;CHANG Yang;XIE Lingyang;ZHAO Guoying;ZHANG Qi;ZHANG Jianxin;LIANG Xiao;ZHANG Yanhui(Beijing Research Institute of Uranium Geology,Beijing 100029,China;Haiyan County Food and Drug Inspection and Testing Center,Haiyan 314300,China)

机构地区：[1]核工业北京地质研究院,北京100029 [2]海盐县食品药品检验检测中心,浙江海盐314300

出　　处：《世界核地质科学》2024年第1期63-72,共10页World Nuclear Geoscience

基　　金：国防科技工业局项目(编号:JSJL2020201A003)资助。

摘　　要：在砂岩型铀矿样品中,被测元素镉含量较低,每个质量丰度都存在不同类型的质谱干扰,而且各干扰元素的含量也存在较大差异,对电感耦合等离子体质谱法准确测量痕量镉造成比较大的困难。因此为了准确测量砂岩型铀矿样品中镉的含量,需要克服样品中不同类型的质谱干扰。采用氢化物发生-电感耦合等离子体质谱联用技术,被测镉元素气化后进入质谱仪中进行测量,可以有效解决测量元素镉的质谱干扰问题,同时提高了元素镉的灵敏度。建立了微波消解样品,连续流动注射进样氢化物发生-电感耦合等离子体质谱法准确测定砂岩型铀矿样品中痕量镉的方法。以盐酸溶液为介质,加入硫脲、亚铁氰化钾掩蔽剂溶液,以磷酸氢二铵、锶离子为增敏剂,优化了介质选择及浓度、硼氢化钾浓度、镉增敏剂的选择与用量等条件,并且有效解决了共存离子的干扰问题。研究表明:建立的连续流动注射氢化物发生-电感耦合等离子体质谱法测定砂岩型铀矿样品中痕量镉的方法,具有检出限低,正确度高,精密度好和适用范围宽等特点。方法检出限为0.001µg·g^(-1),精密度优于8.80%(以多次测量的相对标准偏差RSD来表征)。In sandstone type uranium ore samples,the cadmium content to be measured is low,and there are different types of mass spectra interference for each mass abundance.Moreover,the content of interfering elements also differs greatly,which brings significant challenges to the accurate measurement of trace cadmium using inductively coupled plasma mass spectrometry.In order to accurately measure the cadmium content in sandstone type uranium ore samples,it is necessary to overcome the different types of mass spectral interference in the samples.The hydride generation inductively coupled plasma mass spectrometry technique was used,in which the measured cadmium element was vaporized and measured in the mass spectrometer,which effectively overcame the issue of mass spectral interference for cadmium measurement and improve the sensitivity of cadmium.A method for accurately determining trace cadmium in sandstone type uranium ore samples using microwave digestion and continuous flow injection hydride generation-inductively coupled plasma mass spectrometry was established.Hydrochloric acid solution was used as the medium,and a thiourea-ferrocyanide masking solution was added.Ammonium dihydrogen phosphate and strontium ions were used as sensitizers.The selection and concentration of the medium,concentration of potassium borohydride,selection,and quantity of cadmium sensitizer were optimized,which effectively solved the problem of interference from coexisting ions.The method established for determining trace cadmium in sandstone type uranium ore samples using continuous flow injection hydride generation-inductively coupled plasma mass spectrometry has the characteristics of low detection limit,high accuracy,good precision,and wide applicability.The detection limit of the method is 0.001µg·g^(-1),and the precision is better than 8.80%(characterized by the relative standard deviation RSD from multiple measurements).

关 键 词：砂岩型铀矿 痕量镉 氢化物发生 电感耦合等离子体质谱 质谱干扰 

分 类 号：O657.63[理学—分析化学]