Bord N, Crétier G, Rocca J-L, Bailly C, Souchez J-P
Laboratoire des Sciences Analytiques, Equipe Séparation, CNRS UMR 5180, Université Claude Bernard Lyon 1, Bât. CPE (308), Villeurbanne, France.
J Chromatogr A. 2005 Dec 30;1100(2):223-9. doi: 10.1016/j.chroma.2005.09.024. Epub 2005 Sep 30.
A new CE method has been developed for the simultaneous determination of selected inorganic anions (bromide, chloride, thiosulfate, nitrite, nitrate, sulfate, thiocyanate, fluoride and phosphate) and organic acids (oxalic, malonic, formic, tartric, acetic, glycolic, propionic, butyric and cyclohexanoic) in amine solutions from sour gas treatment units. An electrolyte composed of 10 mM trimellitic acid, 200 mM Tris (pH 9.0), 0.1% polyvinyl alcohol provides a satisfactory separation of all analytes of interest. The electroosmotic flow is reversed by using hexadimethrine bromide as a semi-permanent positively charged coating, making the electrolyte free of additive. Indirect UV detection at 240 nm is used because of the weak absorbing properties of most of analytes. The addition of 1% diethanolamine in standard mixtures permits to better preserve them, inhibiting potential degradation processes, especially for thiosulfate. The quantification is performed using internal standardization, by which molybdate is used as internal standard. Moreover, the use of relative migration times and the excellent repeatabilities obtained allow unambiguous identification of analytes in real samples by comparison with standard mixture. It has been shown that no significant matrix effect came from the presence of 30% diethanolamine in amine solution samples and the developed method was characterized in terms of calibration linearity and accuracy using recovery tests. In short, the developed method allows the simultaneous and rapid determination, in difficult matrices, of numerous inorganic anions and organic acids characterized by a large range of electrophoretic mobilities.
已开发出一种新的毛细管电泳方法,用于同时测定来自酸性气体处理装置的胺溶液中的特定无机阴离子(溴化物、氯化物、硫代硫酸盐、亚硝酸盐、硝酸盐、硫酸盐、硫氰酸盐、氟化物和磷酸盐)和有机酸(草酸、丙二酸、甲酸、酒石酸、乙酸、乙醇酸、丙酸、丁酸和环己酸)。由10 mM偏苯三酸、200 mM三(羟甲基)氨基甲烷(pH 9.0)、0.1%聚乙烯醇组成的电解质能使所有目标分析物得到令人满意的分离。通过使用溴化己二甲铵作为半永久性带正电荷涂层使电渗流反向,从而使电解质无需添加其他物质。由于大多数分析物的吸收特性较弱,因此采用240 nm的间接紫外检测。在标准混合物中添加1%二乙醇胺可以更好地保存它们,抑制潜在的降解过程,尤其是对硫代硫酸盐。定量采用内标法进行,其中钼酸盐用作内标。此外,使用相对迁移时间以及所获得的出色重复性,通过与标准混合物比较可明确鉴定实际样品中的分析物。结果表明,胺溶液样品中30%二乙醇胺的存在不会产生显著的基质效应,并且通过回收率测试对所开发方法的校准线性和准确性进行了表征。简而言之,所开发的方法能够在复杂基质中同时快速测定多种具有大范围电泳迁移率的无机阴离子和有机酸。