Tokalioğlu Serife, Yilmaz Vedat, Kartal Senol
Department of Chemistry, Faculty of Arts and Sciences, Erciyes University, 38039, Kayseri, Turkey.
Environ Monit Assess. 2009 May;152(1-4):369-77. doi: 10.1007/s10661-008-0322-6. Epub 2008 May 17.
A new method for separation and preconcentration of trace amounts of Cu(II), Ni(II), Pb(II), Cd(II) and Mn(II) ions in various matrices was proposed. The method is based on the adsorption and chelation of the metal ions on a column containing Amberlite XAD-1180 resin impregnated with 1-(2-thiazolylazo)-2-naphthol (TAN) reagent prior to their determination by flame atomic absorption spectrometry (FAAS). The effect of pH, type, concentration and volume of eluent, sample volume, flow rates of sample and elution solutions, and interfering ions have been investigated. The optimum pH for simultaneous retention of all the metal ions was 9. Eluent for quantitative elution was 20 ml of 2 mol l(-1) HNO(3). The optimum sample and eluent flow rates were found as 4 ml min(-1), and also sample volume was 500 ml, except for Mn (87% recovery). The sorption capacity of the resin was found to be 0.77, 0.41, 0.57, and 0.30 mg g(-1) for Cu(II), Ni(II), Cd(II), and Mn(II), respectively. The preconcentration factor of the method was 200 for Cu(II), 150 for Pb(II), 100 for Cd(II) and Ni(II), and 50 for Mn(II). The recovery values for all of the metal ions were > or = 95% and relative standard deviations (RSDs) were < or = 5.1%. The detection limit values were in the range of 0.03 and 1.19 microg l(-1). The accuracy of the method was confirmed by analysing the certified reference materials (TMDA 54.4 fortified lake water and GBW 07605 tea samples) and the recovery studies. This procedure was applied to the determination of Cu(II), Ni(II), Pb(II), Cd(II) and Mn(II) in waste water and lake water samples.
提出了一种分离和预富集各种基质中痕量铜（II）、镍（II）、铅（II）、镉（II）和锰（II）离子的新方法。该方法基于在通过火焰原子吸收光谱法（FAAS）测定之前，金属离子在装有浸渍1-（2-噻唑基偶氮）-2-萘酚（TAN）试剂的Amberlite XAD - 1180树脂的柱上进行吸附和螯合。研究了pH值、洗脱剂的类型、浓度和体积、样品体积、样品和洗脱溶液的流速以及干扰离子的影响。同时保留所有金属离子的最佳pH值为9。用于定量洗脱的洗脱剂是20 ml 2 mol l⁻¹的硝酸。除锰（回收率87%）外，最佳样品和洗脱剂流速为4 ml min⁻¹，样品体积为500 ml。树脂对铜（II）、镍（II）、镉（II）和锰（II）的吸附容量分别为0.77、0.41、0.57和0.30 mg g⁻¹。该方法对铜（II）的预富集因子为200，对铅（II）为150，对镉（II）和镍（II）为100，对锰（II）为50。所有金属离子的回收率≥95%，相对标准偏差（RSDs）≤5.1%。检测限在0.03至1.19 μg l⁻¹范围内。通过分析有证标准物质（TMDA 54.4强化湖水和GBW 07605茶叶样品）和回收率研究证实了该方法的准确性。该方法应用于废水和湖水样品中铜（II）、镍（II）、铅（II）、镉（II）和锰（II）的测定。
