Simultaneous Analysis of Formaldehyde and Methanol Emissions During Curing Reactions of Polyester-melamine Coatings

IF 1.2 4区化学 Q4 BIOCHEMICAL RESEARCH METHODS

Chromatographia Pub Date : 2024-04-03 DOI:10.1007/s10337-024-04325-z

Elias Rippatha, Clemens Schwarzinger

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Abstract

This paper introduces a new derivatization agent for the simultaneous quantification of formaldehyde and methanol during curing reactions of complex organic coatings. Formaldehyde emitted from a polyester-melamine coating is derivatized in a gas phase reaction with unsymmetrical dimethylhydrazine (UDMH) to form formaldehyde dimethylhydrazone (FDMH). UDMH and FDMH tend to degrade at temperatures above 200 °C rather fast. The applicability of derivatization agent and analyte as well as their degradation products are therefore discussed thoroughly. In this method curing temperatures of 150 °C with incubation times between 0.1 and 60 min are used to trigger crosslinking reactions. The emissions of formaldehyde and methanol are continuously quantified with headspace gas chromatography to obtain an emission trend. While one of the main sources of formaldehyde is the demethylolation during crosslinking, methanol is produced via hexamethoxymethylmelamine (HMMM) deetherification and as a condensation byproduct. The emission monitoring shows a high potential for comparative and mechanistic investigations. Results show good repeatability with low standard deviations (< 7%) with a quantification limit of 2.09 µg for formaldehyde and 2.08 µg for methanol.

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同时分析聚酯-三聚氰胺涂料固化反应过程中的甲醛和甲醇释放量

本文介绍了一种新型衍生剂，用于同时定量复杂有机涂料固化反应过程中的甲醛和甲醇。聚酯-三聚氰胺涂层释放出的甲醛与不对称二甲基肼（UDMH）发生气相衍生反应，生成甲醛二甲基腙（FDMH）。UDMH 和 FDMH 在 200 °C 以上的温度下会迅速降解。因此，我们对衍生剂和分析物的适用性及其降解产物进行了深入讨论。该方法使用 150 °C 的固化温度和 0.1 至 60 分钟的孵育时间来引发交联反应。通过顶空气相色谱法对甲醛和甲醇的释放量进行连续定量，从而得出释放趋势。甲醛的主要来源之一是交联过程中的脱甲基作用，而甲醇则是通过六甲氧基甲基甲胺（HMMM）脱乙醚作用和作为缩合副产品产生的。排放监测显示了进行比较和机理研究的巨大潜力。结果表明，甲醛和甲醇的定量限分别为 2.09 微克和 2.08 微克，具有良好的重复性和较低的标准偏差（< 7%）。

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来源期刊

Chromatographia 化学-分析化学

CiteScore

3.40

自引率

5.90%

发文量

103

审稿时长

2.2 months

期刊介绍： Separation sciences, in all their various forms such as chromatography, field-flow fractionation, and electrophoresis, provide some of the most powerful techniques in analytical chemistry and are applied within a number of important application areas, including archaeology, biotechnology, clinical, environmental, food, medical, petroleum, pharmaceutical, polymer and biopolymer research. Beyond serving analytical purposes, separation techniques are also used for preparative and process-scale applications. The scope and power of separation sciences is significantly extended by combination with spectroscopic detection methods (e.g., laser-based approaches, nuclear-magnetic resonance, Raman, chemiluminescence) and particularly, mass spectrometry, to create hyphenated techniques. In addition to exciting new developments in chromatography, such as ultra high-pressure systems, multidimensional separations, and high-temperature approaches, there have also been great advances in hybrid methods combining chromatography and electro-based separations, especially on the micro- and nanoscale. Integrated biological procedures (e.g., enzymatic, immunological, receptor-based assays) can also be part of the overall analytical process.