Pirogov Andrey V, Chernova Marina V, Nemtseva Dar'ya S, Shpigun Oleg A
Chemistry Department, Moscow State University, GPS-2, Lenin Hills, 119992, Moscow, Russia.
Anal Bioanal Chem. 2003 Jul;376(5):745-52. doi: 10.1007/s00216-003-1953-7. Epub 2003 May 16.
Three different types of cation exchangers were produced from four basic poly(styrene-divinylbenzene) substrates with different properties. Porous PS-DVB resin beads were functionalized by sulfonation and sulfoacylation under various conditions to produce sulfonated resins with exchange capacities of 0.03-1.80 mM g(-1). The matrix with 50% of cross-linking is most suitable for updating by the proposed technique. Sulfuric and chlorosulfonic acids were used as the reagents for sulfonation. The sulfonating conditions, capacities, and the technique of the synthesis are given. The effects of parameters of the sulfonation reaction and the composition of the reactionary mixture on ion-exchange capacity of the sorbents were investigated. Selectivity and efficiency of the separation of some inorganic cations and derivatives of amines and hydrazines on the resins obtained are compared by ion chromatography with conductometric detection. As a result, the sulfoacylated resin was proved more efficient for the separation of these analytes. The resolution of the analytes strongly depends on the degree of functionalization. The best performance about 19,000 plates m(-1) was obtained using the sulfopropionylated beads with an ion-exchange capacity of 0.3 mM g(-1). The prepared sulfoacylated cation exchanger was compared with the commercially available Dionex CS-12 packing material. It was found that the separation of alkaline ions and 1,1-dimethylhydrazine (UDMH) were much better that those for the commercial material.
由四种具有不同性质的基本聚(苯乙烯 - 二乙烯基苯)底物制备了三种不同类型的阳离子交换剂。多孔聚苯乙烯 - 二乙烯基苯树脂珠在各种条件下通过磺化和磺酰化进行功能化,以制备交换容量为0.03 - 1.80 mM g(-1)的磺化树脂。交联度为50%的基质最适合用所提出的技术进行更新。硫酸和氯磺酸用作磺化试剂。给出了磺化条件、容量和合成技术。研究了磺化反应参数和反应混合物组成对吸附剂离子交换容量的影响。通过离子色谱法和电导检测比较了所获得的树脂对一些无机阳离子以及胺和肼衍生物的分离选择性和效率。结果表明,磺酰化树脂对这些分析物的分离更有效。分析物的分离度强烈依赖于功能化程度。使用离子交换容量为0.3 mM g(-1)的磺丙酰化珠获得了约19,000块板每米(-1)的最佳性能。将制备的磺酰化阳离子交换剂与市售的戴安CS - 12填充材料进行了比较。发现碱性离子和1,1 - 二甲基肼(UDMH)的分离效果比市售材料好得多。