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脂肪族羧酸和苯羧酸在以含各种醇的硫酸为洗脱剂的磺化苯乙烯 - 二乙烯基苯共聚物树脂柱上的离子排斥色谱行为。

Ion-exclusion chromatographic behavior of aliphatic carboxylic acids and benzenecarboxylic acids on a sulfonated styrene--divinylbenzene co-polymer resin column with sulfuric acid containing various alcohols as eluent.

作者信息

Ohta Kazutoku, Towata Atsuya, Ohashi Masayoshi

机构信息

Ceramics Research Institute, National Institute of Advanced Industrial Science and Technology, 2266-98 Anagahora, Simoshidami, Moriyama-ku, Nagoya 463-8560, Japan.

出版信息

J Chromatogr A. 2003 May 16;997(1-2):95-106. doi: 10.1016/s0021-9673(03)00079-7.

Abstract

The addition of C1-C7 alcohols (methanol, ethanol, propanol, butanol, heptanol, hexanol and heptanol) to dilute sulfuric acid as eluent in ion-exclusion chromatography using a highly sulfonated styrene-divinylbenzene co-polymer resin (TSKgel SCX) in the H+ form as the stationary phase was carried out for the simultaneous separations of both (a) C1-C7 aliphatic carboxylic acids (formic, acetic, propionic, isobutyric, butyric, isovaleric, valeric, 2-methylvaleric, isocaproic, caproic, 2,2-dimethyl-n-valeric, 2-methylhexanoic, 5-methylhexanoic and heptanoic acids) and (b) benzenecarboxylic acids (pyromellitic, hemimellitic, trimellitic, o-phthalic, m-phthalic, p-phthalic, benzoic and salicylic acids and phenol). Heptanol was the most effective modifier in ion-exclusion chromatography for the improvement of peak shapes and a reduction in retention volumes for higher aliphatic carboxylic acids and benzenecarboxylic acids. Excellent simultaneous separation and relatively highly sensitive conductimetric detection for these C1-C7 aliphatic carboxylic acids were achieved on the TSKgel SCX column (150 x 6 mm I.D.) in 30 min using 0.5 mM sulfuric acid containing 0.025% heptanol as eluent. Excellent simultaneous separation and highly sensitive UV detection at 200 nm for these benzenecarboxylic acids were also achieved on the TSKgel SCX column in 30 min using 5 mM sulfuric acid containing 0.075% heptanol as eluent.

摘要

在离子排斥色谱中,使用H⁺形式的高度磺化苯乙烯 - 二乙烯基苯共聚物树脂(TSKgel SCX)作为固定相,将C1 - C7醇(甲醇、乙醇、丙醇、丁醇、己醇和庚醇)添加到稀硫酸中作为洗脱剂,用于同时分离(a)C1 - C7脂肪族羧酸(甲酸、乙酸、丙酸、异丁酸、丁酸、异戊酸、戊酸、2 - 甲基戊酸、异己酸、己酸、2,2 - 二甲基 - n - 戊酸、2 - 甲基己酸、5 - 甲基己酸和庚酸)和(b)苯羧酸(均苯四甲酸、偏苯三酸、苯三甲酸、邻苯二甲酸、间苯二甲酸、对苯二甲酸、苯甲酸和水杨酸以及苯酚)。庚醇是离子排斥色谱中最有效的改性剂,可改善较高脂肪族羧酸和苯羧酸的峰形并降低保留体积。使用含0.025%庚醇的0.5 mM硫酸作为洗脱剂,在TSKgel SCX柱(内径150×6 mm)上30分钟内实现了对这些C1 - C7脂肪族羧酸的出色同时分离和相对高灵敏度的电导检测。使用含0.075%庚醇的5 mM硫酸作为洗脱剂,在TSKgel SCX柱上30分钟内也实现了对这些苯羧酸的出色同时分离和在200 nm处的高灵敏度紫外检测。

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