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首页> 外文期刊>The Analyst: The Analytical Journal of the Royal Society of Chemistry: A Monthly International Publication Dealing with All Branches of Analytical Chemistry >A novel flow-through microdialysis separation unit with integrated differential potentiometric detection fro the determination of chloride in soil samples
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A novel flow-through microdialysis separation unit with integrated differential potentiometric detection fro the determination of chloride in soil samples

机译：一种新型的集成微分电位检测的流通式微透析分离装置，用于测定土壤样品中的氯

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In this paper,a novel and miniaturised flow-through dialysis-based potentiometric detector is proposed for the determinationof chloride in soil smaples.The outstanding feature of the designed unit is the integration of analyte isolation from matrix constituents via membrane separation with differential potentiometric detection.Two identical tubular all-solid-state Ag/AgCl ion selective electrodes(ISEs) were assembled respectively at the inlet and outlet of the acceptor channel.Thus,as a consequence of the continuous forward flow of solutions through the microdialyser the outlet tube becomes the indicator electrode for the analyte diffusate while the nested tube at the entrance serves as reference electrode.The effect o fphysical and chemicalpameters on the mass transfer efficiency is discussed in detail and compared with conventional configurations involving downstream detection.The membrane morphology for optimum dialysis performance is also thoroughly evaluated in terms of thickness,porosity and molecular weight cut-off.Higher dialysis efficiency and reduction of dilution factors up to a value of 5 were attained by halting th erecipient stream temporarily.Under the optimised conidtions,a dynamic working range of 5-5000 mgl`-1 chloride with a linear interval between 10 and 5000 mgl~-1 (for 1 min stopped-flow and 200mul sample volume),a repeatability better than 3.0% and a 3omicron_blank detection limit of 1.2 mg l~-1 chloride were the analytical figures of merit of the devised configuratonl.The potentionmetric dialysis sensor features exstreme tolerance to high molecular weight interfering matrix compounds (>1000 mg l~-1 humic acid),which makes it specially suited for the interference-free potentiometrixc determination of chloride in soils containing high levels of organic matter.Themniature size,low-reagent consumptionand high analytical throughpu(25-40h~-1) also warrant its applicability to in-field monitoring or screening schemes.The accuracy fo the measurements was assessed using ion-chromatography as an external reference method.A mean t-test showed no statistical differences between both methodologies at the 95% confidence level.
机译：本文提出了一种新型的基于流通孔透析的微型电位计，用于测定土壤中的氯。设计单元的突出特点是通过膜分离与差动电位检测相结合，将分析物从基质成分中分离出来。两个相同的管状全固态Ag / AgCl离子选择性电极（ISE）分别在受体通道的入口和出口处组装。因此，由于溶液不断流过微透析器，因此出口管变成了用于分析物的指示电极扩散，而在入口处的嵌套管用作参比电极。详细讨论了物理和化学参数对传质效率的影响，并与涉及下游检测的常规配置进行了比较。还对厚度进行了全面评估，通过暂时停止受液流，可获得更高的透析效率和降低的稀释因子，将稀释因子降低至5。在优化的条件下，5-5000 mgl-1氯化物的动态工作范围为分析的优点是，线性范围在10和5000 mgl〜-1之间（对于1分钟的停止流量和200mul样品体积），重复性优于3.0％，氯的3omicron_blank检测极限为1.2 mg l〜-1。电位透析传感器具有对高分子量干扰基质化合物（> 1000 mg l〜-1腐殖酸）的极高耐受性，使其特别适用于高干扰量土壤中氯化物的无干扰电位测定。其体积大，试剂消耗低，分析通量高（25-40h〜-1）也保证了其在现场监测或筛选方案中的适用性。测量的准确性使用离子色谱法作为外部参考方法进行评估。平均t检验显示两种方法在95％置信水平下均无统计学差异。

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