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Preparation of gaseous standard mixtures: Methods for controlling the amount of components generated in the process of thermal decomposition of immobilized compounds [Review]

机译:制备气态标准混合物:控制固定化合物热分解过程中产生的组分数量的方法[综述]

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Gaseous standard mixtures play an important role in characterizing and checking the applicability of new analytical procedures. In this case gaseous standard mixtures can be treated as a special kind of reference material (validation process requires the use of so-called matrix reference materials). The selection of a method of generation of gaseous standard mixtures with the desired characteristics depends on the nature of the analyte and diluent gas, as well as on the required concentration of analytes in the mixture. Recently, dynamic methods of generation of gaseous standard mixtures are becoming more and more common. These include the method based on thermal decomposition of immobilized compounds. The generation of the measured component takes place as a result of heating of a sample of solid support with chemically modified surface. During a chemical reaction initiated by sufficiently high temperature, the immobilized compound undergoes decomposition or rearrangement accompanied by the release of a specific volatile compound. Various amounts of the analyte per unit time can be obtained by adjusting the conditions of the thermal decomposition process. This article describes the possibility of varying the amount of a measured component through the adjustment of conditions of drying the solid support or of the process of chemical modification of its surface. The principle of this technique is exemplified by the generation of a mixture containing ethene as the analyte. Porous glass was used as a solid support. The proposed technique was used for the generation of gaseous standard mixtures for the calibration of a thermal desorber-gas chromatograph-flame ionization detector (TD-GC-FID) system. [References: 29]
机译:气态标准混合物在表征和检查新分析程序的适用性方面起着重要作用。在这种情况下,气态标准混合物可以作为一种特殊的参考物质(验证过程需要使用所谓的基质参考物质)。产生具有所需特性的气态标准混合物的方法的选择取决于分析物和稀释气体的性质,以及混合物中分析物的所需浓度。最近,动态生成气态标准混合物的方法变得越来越普遍。这些包括基于固定化合物热分解的方法。被测组分的产生是通过加热具有化学修饰表面的固体载体样品而产生的。在足够高的温度引发的化学反应过程中,固定化的化合物会发生分解或重排,并释放出特定的挥发性化合物。通过调节热分解过程的条件,可以获得每单位时间各种量的分析物。本文介绍了通过调节干燥固相支持物的条件或对其表面进行化学改性的方法来改变被测组分的量的可能性。该技术的原理以生成包含乙烯作为分析物的混合物为例。多孔玻璃用作固体载体。所提出的技术用于生成气态标准混合物,用于热脱附器-气相色谱-火焰电离检测器(TD-GC-FID)系统的校准。 [参考:29]

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