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微波消解-离子选择电极法测定植物样品中氟离子的实验条件优化
引用本文:韩张雄,马娅妮,刘琦,王曦婕,雒虹.微波消解-离子选择电极法测定植物样品中氟离子的实验条件优化[J].岩矿测试,2016,35(4):397-401.
作者姓名:韩张雄  马娅妮  刘琦  王曦婕  雒虹
作者单位:中国地质科学院岩溶地质研究所, 广西 桂林 541004,中国地质科学院岩溶地质研究所, 广西 桂林 541004,中国地质科学院岩溶地质研究所, 广西 桂林 541004,中国地质科学院岩溶地质研究所, 广西 桂林 541004,中国地质科学院岩溶地质研究所, 广西 桂林 541004,中国地质科学院岩溶地质研究所, 广西 桂林 541004
基金项目:国土资源部公益性行业专项(21411075-03);国家自然科学基金面上项目(41572234)
摘    要:准确检测植物体内的氟含量有助于预测氟化物的生态环境效应。植物中的氟含量低,通常不超过300μg/g,应用离子选择电极法测量氟需选择样品分解效率高的前处理方法使氟不受到损失,获得离子成分简单、空白低的溶液,同时加入适量的缓冲液增强氟离子的强度和掩蔽干扰。本文采用微波消解法处理植物样品,离子选择电极法测定氟的含量,通过优化实验条件确定了缓冲液的浓度。结果表明,在25℃、p H=6.5的样品溶液中加入147 g/L总离子强度缓冲溶液(TISAB)10 m L,避免了溶液中的阳离子与氟离子生成稳定的不溶絮状物,显著降低了沉淀物的产生。本方法检出限为0.242μg/g,精密度(RSD)小于8.5%,回收率为92.0%~108%,能满足地球化学样品分析中对植物样品中低含量氟的检测要求。

关 键 词:天然水    固体聚合膜电解浓集法  淬灭效应  pH值  电导率
收稿时间:6/2/2015 12:00:00 AM
修稿时间:2016/7/15 0:00:00

Optimal Conditions for Determination of Fluoride in Plant Samples by Microwave Digestion Coupled with Ion Selective Electrode Method
HAN Zhang-xiong,MA Ya-ni,LIU Qi,WANG Xi-jie and LUO Hong.Optimal Conditions for Determination of Fluoride in Plant Samples by Microwave Digestion Coupled with Ion Selective Electrode Method[J].Rock and Mineral Analysis,2016,35(4):397-401.
Authors:HAN Zhang-xiong  MA Ya-ni  LIU Qi  WANG Xi-jie and LUO Hong
Institution:Institute of Karst Geology, Chinese Academy of Geological Sciences, Guilin 541004, China,Institute of Karst Geology, Chinese Academy of Geological Sciences, Guilin 541004, China,Institute of Karst Geology, Chinese Academy of Geological Sciences, Guilin 541004, China,Institute of Karst Geology, Chinese Academy of Geological Sciences, Guilin 541004, China,Institute of Karst Geology, Chinese Academy of Geological Sciences, Guilin 541004, China and Institute of Karst Geology, Chinese Academy of Geological Sciences, Guilin 541004, China
Abstract:Tritium content is very low in most of the natural water, and it is necessary to be concentrated before measurement. Polymerization (SPE) membrane electrolysis enrichment method is important in the concentration of low level tritium content for natural water samples. But impurity ions concentrate from water samples and SPE device in the process of water samples treatment cause acidification, resulting in the colour quenching in the mixture of concentrated liquid and liquid scintillation. Consequently, the radioactive activity of tritium will be lower than the reference value. Experimental for Solid polymer electrolyte method,study the impurity ions concentrate from water samples failed to remove completely and the aging of SPE device,the acidification pH and the electrical conductivity of samples in the process of samples treatment on the influence of the quenching. Use the ion and acid-base hybrid exchange resin column separate impurity ions once again for high electrical conductivity and acidification pH samples; adjust the pH value to the neutral after the concentration of the electrolyte with Ammonia to effectively reduce the quenching cause by impurity ions from the aging of SPE device, avoid quenching significantly reduced the low tritium natural water samples counting.
Keywords:natural water  tritium  solid polymer electrolyte method  quenching effect  pH  electrical conductivity
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