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无机酸在弱酸性阳离子交换树脂柱上的空穴离子排斥色谱法。

Vacancy ion-exclusion chromatography of inorganic acids on a weakly acidic cation-exchange resin column.

作者信息

Mori Masanobu, Itabashi Hideyuki, Helaleh Murad I H, Kaczmarski Krzysztof, Głód Bronisław, Kowalska Teresa, Xu Qun, Ikedo Mikaru, Hu Wenzhi, Tanaka Kazuhiko

机构信息

Faculty of Engineering, Gunma University, Kiryu, Gunma, Japan.

出版信息

J Chromatogr A. 2006 Jun 16;1118(1):41-5. doi: 10.1016/j.chroma.2006.01.017. Epub 2006 Feb 2.

Abstract

Vacancy ion-exclusion chromatography (VIEC) for inorganic acids such as H(2)SO(4), HCl, H(3)PO(4), HNO(3), HI and HF is tested on a polymethacrylate-based weakly acidic cation-exchange resin column in the H(+)-form. That is, mixture of inorganic acids in the mobile phase is adsorbed to the resin phase passing through the separation column, and each vacant peak induced by injecting water is determined. Retention times are dependent on the degrees of retention for each analyte in the resin phase. In VIEC, well-shaped peaks of inorganic acids are produced, leading to efficient separations. However, retention behaviors of inorganic acids were strongly affected by the concentrations of the acids in the mobile phase. Sulfosalicylic acid was mixed with inorganic acids in the mobile phase prior to the introduction of a separation column in order to obtain the well-resolutions in the lower concentrations of the acids. By using this method, the separations of inorganic acids could be achieved in the range of 0.01-1 mM, and the linear ranges could be extended over two-orders of magnitude. This is considered since the protonated carboxylic groups fixed on the resin phase were increased with increasing the acid concentrations in the mobile phase, and the penetration effects for the acids to the resin phase were thus enhanced. The detection limits (S/N=3) were below 1.0 microM for all analyte acids. Precision values for retention times were below 0.32% and for peak area were below 0.91%.

摘要

在以H⁺形式存在的基于聚甲基丙烯酸酯的弱酸性阳离子交换树脂柱上,对H₂SO₄、HCl、H₃PO₄、HNO₃、HI和HF等无机酸进行了空位离子排斥色谱(VIEC)测试。也就是说,流动相中的无机酸混合物在通过分离柱时被吸附到树脂相上,然后测定注入水所诱导的每个空穴峰。保留时间取决于每种分析物在树脂相中的保留程度。在VIEC中,无机酸会产生形状良好的峰,从而实现高效分离。然而,无机酸的保留行为受到流动相中酸浓度的强烈影响。在引入分离柱之前,将磺基水杨酸与流动相中的无机酸混合,以便在较低酸浓度下获得良好的分离效果。通过使用这种方法,可以在0.01 - 1 mM的范围内实现无机酸的分离,并且线性范围可以扩展两个数量级。这是因为固定在树脂相上的质子化羧基随着流动相中酸浓度的增加而增加,从而增强了酸对树脂相的渗透作用。所有分析物酸的检测限(S/N = 3)均低于1.0 μM。保留时间的精密度值低于0.32%,峰面积的精密度值低于0.91%。

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