Preconcentaration/separation methods for the multi-elements analysis of trace metals.

用于痕量金属多元素分析的预富集/分离方法。

• 批准号: 10650791
• 负责人: AKATSUKA Kunihiko
• 金额: $ 2.24万
• 依托单位: Kitami Institute of Technology
• 依托单位国家: 日本
• 项目类别: Grant-in-Aid for Scientific Research (C)
• 财政年份: 1998
• 资助国家: 日本
• 起止时间: 1998 至 1999
• 项目状态: 已结题
• 来源: https://kaken.nii.ac.jp/grant/KAKENHI-PROJECT-10650791/
• 关键词: Preconcentration method; trace metals; solid phase extraction; water-soluble complexes; chemically-bonded silica gel; chelating resin; ICP-MS analysis; multi-elements analysis; エチレンジアミン3酢酸基; 分離濃縮; トレース・アナリシス; ICP質量分析法; キレート試薬; 共重合体ポリマー

Some methods are proposed for the analysis of ultra-trace metals in environmental samples by atomic spectrometry after preconcentration/separation with solid phase extraction. The one method is based on the formation of water-soluble complexes in an aqueous sample followed by adsorption onto a CィイD218ィエD2-bonded silica gel column. 2-(5-Bromo-2-pyridylazo)-5-(N-propyl-N-sulfopropylamino)phenol (5-Br-PAPS) was used as a water-soluble chelating reagent. By passage of water sample, added 5-Br-PAPS and adjusted the pH at 8.3, quantitative adsorption of trace metal complexes onto the column took place while the major matrix ions such as alkaline and alkaline earth metal ions, passed through the column. The metals were subsequently eluted with 4.0 ml of 1.0 M HNOィイD23ィエD2. Seven trace metals (Mn, Fe, Ni, Cu, Zn, Cd and Pb) were determined with an ordinal plasma ICP-MS. The ultratrace of Fe was determined by nitrogen-argon mixed gas plasma to reduce the isobaric interference by ィイD140ィエD1ArィイD … More 116ィエD1O on ィイD156ィエD1Fe. The precision and accuracy of the method were demonstrated by analyzing coastal and open-ocean seawater CRMs : CASS-2 and NASS-4 (NRC, Canada). Ethylenediaminetriacetate-bonded silica gel (ED3A-SG) is also proposed as a solid phase extractant in the other method. ED3A was synthesized by reacting silica gel with N-(trimethoxysilylpropyl)ethylenediaminetriacetate. Sixty ml of 5% aqueous solution of the silane coupler added to 18 g of dried silica gel and stirred for 3 h, then silica gel was filtered off and dried for 24 h. The metal uptake capacity of ED3A-SG thus obtained was 0.18 mM gィイD1-1ィエD1 and remained the capacity for at least 3 months when it was stored in a desiccator at room temperature. After rinse the ED3A-SG column with 1.0 M HNOィイD23ィエD2 and water, a definite volume of aqueous sample, the pH of which was adjusted with acetic acid or ammonia, was percolated through the column to concentrate trace metals. The metals collected onto the column was eluted with 5 ml of 1.0 M HNOィイD23ィエD2. The eluate was then analyzed by ICP-MS. More than 15 metals including Fe, Co, Ni. Cu. Zn. Cd and Pb were quantitatively collected onto the column between pH 3.5 and 4.5. Whereas major matrices such as alkaline and alkaline earth metals were not collected at this pH region. The proposed method was applied to determine trace metals in environmental water samples such as river waters, coastal seawater and tap water. Those methods proposed here achieved rapid and reliable preconcentration/separation of trace metals and elimination of matrix effects in the analysis of environmental water samples by ICP-MS. The procedures involve simple chemical separations with less contamination and provide improvements of the detection power necessary for trace metals in environmental waters. Less

提出了固相萃取富集分离原子光谱法测定环境样品中超痕量金属元素的方法。一种方法是基于在水性样品中形成水溶性络合物，然后吸附到C218-D218-键合硅胶柱上。以2-（5-溴-2-吡啶偶氮）-5-（N-丙基-N-磺丙基氨基）苯酚（5-Br-PAPS）为水溶性螯合剂。通过水样的过流，加入5-Br-PAPS，调节pH值为8.3，微量金属络合物在柱上发生定量吸附，而主要基质离子如碱金属和碱土金属离子则通过柱。随后用4.0 ml 1.0 M HNO 3-D23-D2洗脱金属。采用等离子体ICP-MS法测定Mn、Fe、Ni、Cu、Zn、Cd、Pb等7种痕量金属元素，其中Fe的超痕量采用氮氩混合气体等离子体测定，以消除D140等离子体D1 Ar等离子体D140等离子体的等压干扰 ...更多信息 116颗铯D1 O在铯D156颗铯D1 Fe上通过分析沿海和公海海水标准物质：卡斯-2和NASS-4（NRC，加拿大），证明了该方法的精密度和准确度。乙二胺三乙酸键合硅胶（ED 3A-SG）也被建议作为固相萃取剂在另一种方法中。用硅胶与N-（三甲氧基硅丙基）乙二胺三乙酸酯反应合成了乙二胺三乙酸酯（ED 3A）。将60毫升5%硅烷偶联剂水溶液加入到18克干燥硅胶中并搅拌3小时，然后滤出硅胶并干燥24小时。由此获得的ED 3A-SG的金属吸收能力为0.18mM g·kg-1·kg-用1.0 M HNO-23-D2和水冲洗ED 3A-SG柱后，取一定体积的水溶液样品，用乙酸或氨水调节其pH值，通过该柱以富集痕量金属。收集到柱上的金属用5 ml的1.0M HNO 3-D23-D2洗脱。然后用ICP-MS分析了样品中的铁、钴、镍等15种以上的金属。Cu. Zn.镉和铅定量收集到柱上的pH值为3.5和4.5之间。而主要基质如碱金属和碱土金属在该pH区域未被收集。该方法已应用于江河沃茨、近海海水和自来水等环境水样中痕量金属的测定。这些方法实现了环境水样中痕量金属的快速可靠的预富集/分离，消除了ICP-MS分析中的基体效应。该方法化学分离简单，污染少，提高了环境沃茨中痕量金属的检测能力。少