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Ratiometric detection of total bromine in E-waste polymers by colloidal gold-based headspace single-drop microextraction and microvolume spectrophotometry
Sensors and Actuators B: Chemical ( IF 8.4 ) Pub Date : 2018-01-11 , DOI: 10.1016/j.snb.2018.01.107
Francisco Pena-Pereira , Adrián García-Figueroa , Isela Lavilla , Carlos Bendicho

A ratiometric analysis method for total bromine determination in E-waste polymers based on the significant effect of molecular bromine in the UV–vis spectra of gold nanoparticles (AuNPs) is presented herein. The proposed method involves alkaline fusion of polymeric samples, in situ conversion of resulting bromide ions into molecular bromine and exposure of a microdrop of AuNPs to the evolved volatile prior to microvolume UV–vis spectrophotometric analysis. Experimental parameters affecting the trapping/sensing of molecular bromine by the colloidal solution were optimized by a two-stage multivariate optimization approach involving Placket-Burman and central composite designs for screening and optimization, respectively. Under optimal conditions, the method yielded limits of detection (LOD) and quantification (LOQ) of 8.8 and 29.4 ng/mL Br, respectively, corresponding to 17.0 and 56.7 μg/g Br, respectively. The repeatability, expressed as relative standard deviation (RSD), was found to be 4.8% (n = 10). The proposed method was validated against two certified reference materials (BCR-681 Trace elements in polyethylene (low level) and ERM®-EC680 m low-density polyethylene), and applied to the determination of total bromine in plastics from E-wastes. The results obtained with the proposed method were in good agreement with those obtained by ion chromatography (paired t-test, α 0.05, 2 tails).



中文翻译:

胶态金基顶空单滴微萃取和微分光光度法按比例检测电子废物中的总溴

本文介绍了一种比例分析方法,用于确定电子废物聚合物中的总溴,该方法基于分子溴在金纳米颗粒(AuNPs)的UV-vis光谱中的显着影响。拟议的方法涉及就地对聚合物样品进行碱熔在进行微体积紫外可见分光光度法分析之前,将所得的溴离子转变为分子溴,并将一滴AuNPs暴露于所释放的挥发物。通过两阶段多变量优化方法(包括Placket-Burman和中央复合设计分别用于筛选和优化),优化了影响胶体溶液对分子溴的捕集/传感的实验参数。在最佳条件下,该方法的检测限(LOD)和定量限(LOQ)分别为8.8和29.4 ng / mL Br,分别对应于17.0和56.7μg/ g Br。发现以相对标准偏差(RSD)表示的重复性为4.8%(n = 10)。® -EC680 m低密度聚乙烯),用于测定电子废物中塑料中的总溴。所提方法得到的结果与离子色谱法(配对t检验,α0.05,2尾)相吻合。

更新日期:2018-01-11
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