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Determination Of Lead In Wine And Rum Samples By Flow Injection-hydride Generation-atomic Absorption Spectrometry

机译:流动注射氢化物发生-原子吸收光谱法测定葡萄酒和朗姆酒中的铅

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摘要

A method for direct determination of lead in wine and rum samples was developed, using a flow injection hydride generation system coupled to an atomic absorption spectrometer with flame-quartz atomizer (FI-HG-AAS). Lead hyride (PbH_4) was generated using potassium ferricyanide (K_3Fe(CN)_6), as oxidant and sodium tetrahydroborate (NaBH_4) as reductant. Samples were acidified to 0.40% (v/v) HCl for wine and to 0.30% (v/v) HCl for rum, which were then mixed on-line with 3% (m/v) K_3Fe(CN)_6 solution in 0.03% (v/v) HCl prior to reaction with 0.2% (m/v) alkaline NaBH_4 solution. Lead contents of a rum and two different red wine samples were determined by FI-HG-AAS agreed with those obtained by ICP-MS. The analytical figures of merit of method developed were determined. The calibration curve was linear up to 8.0 μg L~(-1) Pb with a regression coefficient of 0.998. The relative error was lower than 4.58%. The relative standard deviation (n = 7) was better than 12%. A detection limit of 0.16 μg L~(-1) was achieved for a sample volume of 170 μL.
机译:开发了一种直接测定葡萄酒和朗姆酒样品中铅的方法,该方法使用流动注射氢化物发生系统,该系统与带有火焰石英雾化器的原子吸收光谱仪(FI-HG-AAS)耦合。使用铁氰化钾(K_3Fe(CN)_6)作为氧化剂和四氢硼酸钠(NaBH_4)作为还原剂生成氢化铅(PbH_4)。对于葡萄酒,将样品酸化至0.40%(v / v)HCl,对于朗姆酒则酸化至0.30%(v / v)HCl,然后将其与3%(m / v)K_3Fe(CN)_6的0.03溶液在线混合在与0.2%(m / v)碱性NaBH_4溶液反应之前,先使用%(v / v)HCl。朗姆酒和两种不同的红酒样品中的铅含量由FI-HG-AAS确定,与ICP-MS一致。确定了所开发方法的分析价值。校准曲线在8.0μgL〜(-1)Pb时呈线性,回归系数为0.998。相对误差低于4.58%。相对标准偏差(n = 7)优于12%。对于170μL的样品量,检测限为0.16μgL〜(-1)。

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