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首页> 外文期刊>International journal of environmental analytical chemistry >Determination of lead in complex sample matrices by atomic fluorescence spectrometry: optimisation of online hydride generation
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Determination of lead in complex sample matrices by atomic fluorescence spectrometry: optimisation of online hydride generation

机译：原子荧光光谱法测定复杂样品中的铅：在线氢化物生成的优化

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摘要

Lead hydride or plumbane (PbH4) generation was optimised by exploiting a simple flow-injection method coupled to atomic fluorescence spectrometry (HG-AFS), and allowing ultra-trace lead determination. Plumbane was generated through two methods: (1) 5% (v/v) H2O2 was employed as oxidant with 1.5% (m/v) KBH4 as a reducing agent and 1.5% (v/v) HCl solution; (2) with 1.5% (m/v) K-3[Fe(CN)(6)] as an oxidant/sensitiser, 1% (m/v) KBH4 as a reducing agent and 1.5% (v/v) HCl. Variables such as reagent concentrations, flow rates and sample and reagent volumes were tested and critically compared. The best results were obtained with potassium ferricyanide K-3[Fe(CN)(6)], achieving a detection limit of 0.03 mu g PbL-1 and a relative standard deviation (RSD) of 1.1%. The selected method was validated by analysis of certified reference materials such as SRM-2976 (mussel tissue) and BCR-610 (groundwater), with good agreement with the certified values. The developed methodology was successfully applied to different environmental sample matrices, such as rain water, tap water, ground water, spring water and drinking water, and biological samples, i.e., human blood, plasma and serum.
机译：氢化铅或铅铅（PbH4）的产生通过利用一种简单的流动注射方法与原子荧光光谱法（HG-AFS）结合使用，并允许超痕量铅的测定而得到优化。铅是通过两种方法生成的：（1）使用5％（v​​ / v）的H2O2作为氧化剂，使用1.5％（m / v）的KBH4作为还原剂和1.5％（v / v）的HCl溶液； （2）用1.5％（m / v）的K-3 [Fe（CN）（6）]作为氧化剂/敏化剂，1％（m / v）的KBH4作为还原剂和1.5％（v / v）的HCl 。测试并严格比较了诸如试剂浓度，流速，样品和试剂体积等变量。铁氰化钾K-3 [Fe（CN）（6）]可获得最佳结果，检出限为0.03微克PbL-1，相对标准偏差（RSD）为1.1％。通过分析经认证的参考物质（例如SRM-2976（贻贝组织）和BCR-610（地下水））验证了所选方法，并与认证值高度吻合。所开发的方法已成功地应用于不同的环境样品基质，例如雨水，自来水，地下水，泉水和饮用水，以及生物样品，即人体血液，血浆和血清。

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