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首页> 外文期刊>The Analyst: The Analytical Journal of the Royal Society of Chemistry: A Monthly International Publication Dealing with All Branches of Analytical Chemistry >Preconcentration and determination of trace elements with 2,6-diacetylpyridine functionalized amberlite XAD-4 by flow injection and atomic spectroscopy
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Preconcentration and determination of trace elements with 2,6-diacetylpyridine functionalized amberlite XAD-4 by flow injection and atomic spectroscopy

机译：流动注射和原子光谱法对2,6-二乙酰吡啶官能化Amberlite XAD-4进行痕量元素的富集和测定

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摘要

An on-line flow injection method for the direct determination of trace elements in environmental samples is described.A mini-column packed with 2,6-diacetylpyridine functionalized Amberlite XAD-4 was used to preconcentrate and separate 8 trace metals (Cd,Co,Cu,Mn,Ni,Pb,U and Zn) from water and extracts from solid samples.The metals were eluted with 0.1 M HNO_3 directly to the detection system (either inductively coupled plasma-mass spectrometry (ICP-MS) or flame atomic absorption spectrometry (FAAS)).As well as demonstrating that the resin could be used to preconcentrate ultra-trace analytes from natural waters,it was also shown to work well at a pH of 5.5.Therefore,after treatment of sample digests with sodium fluoride,samples that contain extremely large concentrations of iron may be analysed for trace analytes without the excess iron overloading the capacity of the resin.To this end,the analytes Cd,Co,Cu and Ni were preconcentrated from acid extracts of certified soil/sediment samples and then eluted with nitric acid to be determined on-line.Limits of detection (3sigma) of Cd = 0.33 mug l~(-1),Co = 0.094 mug l~(-1),Cu = 0.34 mug l~(-1),Mn = 0.32 mug l~(-1),Ni = 0.30 mug l~(-1),Pb = 0.43 mug l~(-1),U = 0.067 mug l~(-1) and Zn = 0.20 mug l~(-1) for the FI-ICP-MS system and Cd = 22 mug l~(-1),Co = 60 mug l~(-1),Cu = 10 mug l~(-1) and Ni = 4.8 mug l~(-1) for the FI-FAAS system were obtained.Analysis of certified reference materials showed good agreement with the certified values using the two methods.
机译：本文介绍了一种在线流动注射法直接测定环境样品中的痕量元素的方法。一个装有2,6-二乙酰基吡啶官能化的Amberlite XAD-4的微型柱用于预浓缩和分离8种痕量金属（Cd，Co，从水中和固体样品中提取铜，锰，镍，铅，铀和锌）。金属用0.1 M HNO_3直接洗脱到检测系统（电感耦合等离子体质谱法（ICP-MS）或火焰原子吸收法）并证明该树脂可用于对天然水中的超痕量分析物进行预浓缩，而且在pH为5.5时也能很好地工作。因此，在用氟化钠处理样品消化液后，可以分析包含极高铁含量的样品中的痕量分析物，而不会使过量的铁超载到树脂容量中。为此，分析物Cd，Co，Cu和Ni是从经认证的土壤/沉积物样品的酸提取物中进行预浓缩的。 es，然后用硝酸洗脱进行在线测定.Cd的检测极限（3sigma）= 0.33杯l〜（-1），Co = 0.094杯l〜（-1），Cu = 0.34杯l〜（-1） -1），Mn = 0.32杯l〜（-1），Ni = 0.30杯l〜（-1），Pb = 0.43杯l〜（-1），U = 0.067杯l〜（-1），Zn =用于FI-ICP-MS系统的0.20杯l〜（-1），Cd = 22杯l〜（-1），Co = 60杯l〜（-1），Cu = 10杯l〜（-1）和获得了用于FI-FAAS系统的Ni = 4.8杯l〜（-1）。两种标准方法对认证参考物质的分析均显示出与认证值的良好一致性。

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