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一种新型的 N-羟乙基亚氨基二乙酸修饰的核壳硅胶固定相,用于螯合离子色谱法分离碱土、过渡和稀土元素。

A new N-hydroxyethyliminodiacetic acid modified core-shell silica phase for chelation ion chromatography of alkaline earth, transition and rare earth elements.

机构信息

Irish Separation Science Cluster (ISSC), National Centre for Sensor Research, Dublin City University, Dublin 9, Ireland.

出版信息

J Chromatogr A. 2013 Dec 20;1321:56-64. doi: 10.1016/j.chroma.2013.10.057. Epub 2013 Oct 25.

Abstract

Bare core-shell silica (1.7μm) has been modified with iminodiacetic acid functional groups via standard silane chemistry, forming a new N-hydroxyethyliminodiacetic acid (HEIDA) functionalised core-shell stationary phase. The column was applied in high-performance chelation ion chromatography and evaluated for the retention of alkaline earth, transition and heavy metal cations. The influence of nitric acid eluent concentration, addition of complexing agent dipicolinic acid, eluent pH and column temperature on the column performance was investigated. The efficiencies obtained for transition and heavy metal cations (and resultant separations) were comparable or better than those previously obtained for alternative fully porous silica based chelation stationary phases, and a similarly modified monolithic silica column, ranging from ∼15 to 56μm HETP. Increasing the ionic strength of the eluent with the addition of KNO3 (0.75M) and increasing the column temperature (70°C) facilitated the isocratic separation of a mixture of 14 lanthanides and yttrium in under 12min, with HETP averaging 18μm (7μm for Ce(III)).

摘要

裸核壳二氧化硅(1.7μm)已通过标准硅烷化学方法用亚氨基二乙酸官能团进行改性,形成了一种新的 N-羟乙基亚氨基二乙酸(HEIDA)官能化核壳固定相。该柱应用于高效螯合离子色谱中,并评估了其对碱性土、过渡金属和重金属阳离子的保留性能。考察了硝酸洗脱液浓度、络合剂吡啶二酸的添加、洗脱液 pH 值和柱温对柱性能的影响。与替代的全多孔硅胶基螯合固定相和类似改性的整体硅胶柱相比,过渡金属和重金属阳离子的效率(以及由此产生的分离)相当或更好,范围在约 15 到 56μm HETP 之间。通过添加 KNO3(0.75M)增加洗脱液的离子强度并升高柱温(70°C),可以在 12 分钟内实现 14 种镧系元素和钇的混合物的等度分离,HETP 平均为 18μm(Ce(III) 为 7μm)。

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