首页> 外文期刊>The Analyst: The Analytical Journal of the Royal Society of Chemistry: A Monthly International Publication Dealing with All Branches of Analytical Chemistry >Determination of carbonyl compounds in waters using triazine-based hydrazine reagents and liquid chromatography
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Determination of carbonyl compounds in waters using triazine-based hydrazine reagents and liquid chromatography

机译:使用三嗪基肼试剂和液相色谱法测定水中的羰基化合物

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Triazine-based hydrazine reagents hae been developed and applied for the determination of aldehydes in waters. N-Methyl-4-N',N'-dimethylamino-6-(4'-methoxy-1'-naphthyl)-1,3,5-triazine-2-hydrazine (MDMNTH) and 4-N,N-dimethylamino-6-(4'methoxy-1'-naphthyl)-1,3,5-triazine-2- hydrazine (DMNTH) react with these carbonyl compounds with very high yields under the formation of the respective hydrazones, which are separated by reversed-phase liquid chromatography with binary gradients of acetonitrile and water. Organic modifiers are added to obtain improved peak shapes. UV/vis as well as fluorescence detection has been applied successfully to quantify the hydrazones. The derivatization of aqueous solutions of the aldehydes has been optimized. Limits of detection are in the range between 0.1 #mu#M and 1.0#mu#M depending on the analyte and the reagent used for derivatization. Although calibration via external standards is possible for higher analyte concentrations, best results are obtained by calibration via the derivatization reactionl. Compared to the US EPA method 8315A, the newly developed method is characterized by very easy sample prepartion, lower limits of detection without enrichment and excellent reproducibility with an average RSD of 1.5% with DMNTH as reagent and 3.5% with MDMNTH as reagent for a formaldehyde concentration of 1.0 X 10~(-5) mol L~(-1). Aldehyde-spiked mineral water samples were analyzed successfully with the new method.
机译:已经开发了基于三嗪的肼试剂,并将其用于测定水中的醛。 N-甲基-4-N',N'-二甲基氨基-6-(4'-甲氧基-1'-萘基)-1,3,5-三嗪-2-肼(MDMNTH)和4-N,N-二甲基氨基-6-(4'甲氧基-1'-萘基)-1,3,5-三嗪-2-肼(DMNTH)与这些羰基化合物反应时,在各自的形成下,它们的产率很高,并通过反向分离相液相色谱,用乙腈和水的二元梯度洗脱。添加有机改性剂以获得改善的峰形。紫外/可见光以及荧光检测已成功应用于定量azo。醛的水溶液的衍生化已被优化。检测限在0.1#mu#M和1.0#mu#M之间,具体取决于分析物和用于衍生的试剂。尽管可以通过外部标准品对更高的分析物浓度进行校准,但通过衍生化反应进行校准可以获得最佳结果。与美国EPA方法8315A相比,新开发的方法的特点是样品易于分离,不进行富集检测的下限低,重现性好,以DMNTH为试剂的平均RSD为1.5%,以MDMNTH为甲醛的试剂的平均RSD为3.5%浓度为1.0 X 10〜(-5)mol L〜(-1)。用新方法成功地分析了醛加标的矿泉水样品。

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