盐湖卤水中微量钒的浓度测定  

Determining the Concentration of Trace Vanadium in Natural Saline Lake Brines

作　　者：初剑 黄清钢 高瑞勤 王卫平[4] 殷小杰[1] 吴晓蕾[1] 田伟[1] 李莎 秦芝[1] 白静[1] CHU Jian;HUANG Qinggang;GAO Ruiqin;WANG Weiping;YIN Xiaojie;WU Xiaolei;TIAN Wei;LI Sha;QIN Zhi;BAI Jing(Institute of Modern Physics,Chinese Academy of Sciences,Lanzhou 730000,China;School of Nuclear Science and Technology,Lanzhou University,Lanzhou 730000,China;School of Nuclear Science and Technology,University of Chinese Academy of Sciences,Beijing 100049,China;Department of Chemistry,University of Science and Technology of China,Hefei 230026,China;Department of Chemistry,Tianjin Normal University,Tianjin,300387,China)

机构地区：[1]中国科学院近代物理研究所,兰州730000 [2]兰州大学核科学与技术学院,兰州730000 [3]中国科学院大学核科学与技术学院,北京100049 [4]中国科学技术大学化学学院,合肥230026 [5]天津师范大学化学学院,天津300387

出　　处：《原子核物理评论》2022年第2期238-244,共7页Nuclear Physics Review

基　　金：National Natural Science Foundation of China(U1932142,11575260,12005272,11905266,11505250);West Light Foundation of Chinese Academy of Sciences。

摘　　要：为了测定盐湖卤水中微量钒的浓度,开发了一个钒的分离纯化流程来降低大量的共存离子的基质效应。该分离纯化流程包括萃取和反萃两个步骤。详细地研究了影响钒纯化效率的各种因素,得到钒的最佳分离纯化条件为:以正己烷为稀释剂,有机相中D2EHPA和TBP的体积百分比分别为30%及20%,在pH为3.0时萃取30 min;然后用3 mol/L H_(2)SO_(4)反萃10 min。基于此分离纯化流程,将两个实际盐湖卤水样品中的微量钒纯化后,再用电感耦合等离子体质谱仪(ICP-MS)测定其浓度,该ICP-MS对^(51)V的检测灵敏度和检测限别为53171 cps/(μg/L)和1.88ng/L。所得实际盐湖卤水钒测定结果的加标回收率接近100%而相对标准偏差低于0.6%,表明该方法可用于实际复杂体系中微量钒的浓度测定,例如海水和盐湖卤水。To determine the concentration of trace vanadium in saline lake brines,a vanadium pre-purification process is established to reduce the matrix effect of the huge coexisting ions.Two steps,extraction and stripping,are included in the process.The factors affecting the vanadium purification efficiencies are investigated in detail and the optimum conditions are determined to be:vanadium in the solutions was extracted by the organic phase containing 30%D2 EHPA(v/v),20%TBP(v/v)in n-hexane for 30 min at pH 3.0,and then stripped with 3 mol/L H_(2)SO_(4)for 10 min.Trace vanadium in two natural brine samples are pre-purified using this process and their concentrations are determined by inductively coupled plasma-mass spectrometry(ICP-MS)with sensitivity and limit of detection(LOD)for^(51)V are 53171 cps/(μg/L)and 1.88 ng/L,respectively.The standard addition recoveries of the brine samples are~100%but with small relative standard deviations(RSD<0.6%),indicating that the method can be used to measure the concentration of trace vanadium in natural complicated waters,such as seawater and saline lake brines.

关 键 词：钒 测定 萃取 盐湖卤水 纯化 

分 类 号：X125[环境科学与工程—环境科学]