キトサンキレート樹脂前処理法を用いる空気分節試料導入/誘導結合プラズマ質量分析法による天然水中の多元素同時定量

本法では,各種天然水中の極微量金属成分を同時定量する目的で空気分節試料導入/ICP-MSシステムを用いて,微少量試料(数十μl)を前処理せずにネブライザーに送り込み,多数の金属成分の定量が可能であった。共存主成分による質量干渉を受ける一部遷移金属や直接試料導入では感度の足りない元素については,イミノ二酢酸型キトサンキレート樹脂充填カラムによる分離·濃縮操作の併用によって更に信頼性の高いデータが得られることが分かった。前処理においては,体積1mlのミニカラムを用いて50mlの溶液試料から50倍濃縮を行い,試料·試薬·廃液すべてを少量化することができた。本ICP-MSシステムでは試料導入量は80μlで十分であり,1mlでも数回繰り返し測定が可能で,しかも多元素同時分析ができた。確立した分析法を用いて河川水や市販のミネラルウォーターに応用し,希土類を含め45種の微量元素の定量が可能となった。

Ultratrace elements in natural water samples were determined simultaneously by air-segmented flow-injection/inductively coupled plasma-mass spectrometry(SFI/ICP-MS).A small volume of the sample solutions(80μl) was introduced into a nebulizer by an air-segmented flow-injection(SFI) system, and a maximum of fifteen elements were measured during each run.A chitosan-based chelating resin containing functional groups of iminodiacetate was used to separate and enrich analyte metal ions.A 50-fold preconcentration using 50ml of sample solutions was achieved by the proposed method, where 1ml of 0.1M nitric acid was added to residues after drying the chelating column effluent.At pH6, several heavy metals(Fe, Ni, Co, Cu, Zn, Ag, Cd, Pb and U) and rare earth elements(REEs) were quantitatively retained on the chelating resin column, whereas alkali and alkaline earth metals were eluted from the column by rinsing with 5ml of a 0.2M ammonium acetate solution.Metals adsorbed on the chelating resin column were recovered by elution with 10ml of 1M nitric acid.The proposed method was applied to the determination of trace elements in several natural water samples, such as river water and mineral drinking water.