Maya Fernando, Estela José Manuel, Cerdà Víctor
Department of Chemistry, Faculty of Sciences, University of the Balearic Islands, Carretera de Valldemossa km 7.5, E-07122 Palma de Mallorca, Illes Balears, Spain.
Anal Chem. 2008 Aug 1;80(15):5799-805. doi: 10.1021/ac8004633. Epub 2008 Jun 26.
A new, multisyringe flow injection setup was designed to develop the first completely automated flow methodology for the expeditious, accurate in-line determination of halogenated organic compounds (HOCs) in water. The target compounds are preconcentrated and isolated by solid-phase extraction. Following elution, previously organically bound halogens are released as free hydrogen halides by the combined action of UV light and a chemical oxidant for their subsequent spectrophotometric determination by reaction with Hg(SCN) 2 and Fe(3+). Optimizing the major hydrodynamic and chemical variables resulted in improved performance. Recovery of various HOCs was assessed, and potential interferents were examined. Under the selected operating conditions, the proposed method exhibits variable analytical performance depending on the particular sample volume used (e.g., a sample volume of 5 mL provides a linear working range of 140-2000 microg L(-1), a LOD of 100 microg L(-1), and a throughput of 9 samples h(-1)). The method was successfully used to determine total adsorbable organic halogens (AOX) in well water and leachates, and the results validated against an AOX reference method. The role of the proposed system in the environmental analytical field is critically discussed.
设计了一种新型多注射器流动注射装置,以开发首个完全自动化的流动方法,用于快速、准确地在线测定水中的卤代有机化合物(HOCs)。目标化合物通过固相萃取进行预浓缩和分离。洗脱后,先前与有机物结合的卤素通过紫外光和化学氧化剂的联合作用以游离卤化氢的形式释放出来,随后通过与Hg(SCN)₂和Fe(3+)反应进行分光光度测定。对主要的流体动力学和化学变量进行优化可提高性能。评估了各种HOCs的回收率,并检测了潜在干扰物。在选定的操作条件下,所提出的方法根据所使用的特定样品体积表现出不同的分析性能(例如,5 mL的样品体积提供140 - 2000 μg L⁻¹的线性工作范围、100 μg L⁻¹的检测限和每小时9个样品的通量)。该方法成功用于测定井水和渗滤液中的总可吸附有机卤素(AOX),并与AOX参考方法验证了结果。对所提出的系统在环境分析领域中的作用进行了批判性讨论。