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首页> 外文期刊>Analytica chimica acta >Flow-through solid-solid-phase based optical sensor for the multisyringe flow injection trace determination of orthophosphate in waters with chemiluminescence detection
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Flow-through solid-solid-phase based optical sensor for the multisyringe flow injection trace determination of orthophosphate in waters with chemiluminescence detection

机译：基于流-固-固相的光学传感器，用于化学发光检测，用于多注射器流动注射痕量测定水中的正磷酸盐

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摘要

In this work,a novel flow-through solid-phase based chemiluminescence(CL)opticalsesor is described for the trace detmrination of orthophosphate in watersexploiting the multisyringe flow injeciton analysis(MSFIA) concept withmulticommutation.The proposed time-basedinjection flow system relies upon the in-line derivatisation of the analyte with ammonium molybdate in the presence of vanadate,and the transient immobilisaition of the resulting hetropolyacid in a N-vinylpyrrolidone/divingylbenzene copolymer packed spiral shape flow-through cell located in front of the window of a photomultiplier tube.The simultaneous injection of well-defined slugs of luminol in alkalien medium and methanol solution towards the packed reactor is afterwards performed by proper switching of the solenoidvalves.then,the light emisisonform the luminol oxidationby the oxidant species retained onto the sorbent material is readily detected.At the same time,the generatedmolybdenum-blue compound is eluted by the minute amount of injected methanol,rendering the system prepared for a new measureing cycle.Therefore,the devised sensor enables the integratonof th esolid-phase CL reacton with elution and deteciton o fthe emitted light without the typical drawbacks of the molybdenum-blue based spectrophotometric procedures regarding the excess of molybdate anion,which causes high backgroun signals due to its self-reduction.The noteworthy features of the developed CL-MSFIA system are the feasibility to accommodate reactions with differetn pH requirements and the ability to detrmine trace levels of orthophosphate in high silicate content samples (Si/P ratios up to 500).Under the optimised conditions,a dynamic linear range form 5 to 50 mug P l~-1 for a 1.8 ml sample,repeatability bettter than 3.0% and a quantificaton limit of 4 mug Pl~-1 were attained.The flowing stream system handles 11 analysis h ~-1 and hasbeen successfully applied to the detrmination o ftrace levels of orthophojsphate in environmental samples such as mineral,ground,tap and pond watersas well as samples from a water-steam cycle of an incineration plant.The t-test comparison fo the means forth edeveloped optical sensor and the molybdenum-blue spectrophotometric APHA/AWWA/WPCF reference method revealed that there is no evidence of significant differences between the obtained results at the 95% confidence level.
机译：在这项工作中，描述了一种新颖的基于流动相的化学发光（CL）光学传感器，用于利用多交换多注射流注入分析（MSFIA）概念对水中的正磷酸盐进行痕量脱除。提出的基于时间的注射流系统依赖于在钒酸盐存在下，用钼酸铵在线分析物进行线性衍生化，并将生成的杂多酸瞬时固定在位于光电倍增管窗口前的N-乙烯基吡咯烷酮/二乙烯基苯共聚物填充的螺旋形流通池中。之后，通过适当切换电磁阀，将碱性介质和甲醇溶液中定义良好的鲁米诺团块同时注入电磁阀，然后将其充填到反应器中。然后，可以很容易地检测到形成鲁米诺醇的光是由吸附在吸附剂材料上的氧化剂所氧化的。同时，生成的钼蓝化合物被洗脱液洗脱注入的甲醇量很大，使系统为新的测量周期做好了准备。因此，该设计的传感器可对固相CL反应物进行积分并洗脱和检测发射光，而没有基于钼蓝的分光光度法的典型缺点关于过量的钼酸根阴离子，由于其自​​身还原而导致高背景信号。发达的CL-MSFIA系统的显着特点是可适应不同pH要求的反应的可行性以及在高pH值下去除微量正磷酸的能力。硅酸盐含量的样品（Si / P比例高达500）。在优化的条件下，动态线性范围为1.8 ml样品的5至50杯P l〜-1，重复性大于3.0％，定量限为4杯达到Pl〜-1。流动系统处理11〜h〜-1，已成功应用于环境中正磷酸盐的痕量去除。诸如矿泉水，矿井水，自来水和池塘水的样品，以及焚化厂水蒸气循环的样品。t检验比较了开发的光学传感器和钼蓝分光光度法APHA / AWWA / WPCF参考方法的方法结果表明，在95％的置信水平下，没有证据表明所得结果之间存在显着差异。

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