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采用热解吸和气相色谱法,借助两种内标物分析气态羰基化合物。

A combined application of thermal desorber and gas chromatography to the analysis of gaseous carbonyls with the aid of two internal standards.

机构信息

Atmospheric Environment Laboratory, Department of Environment & Energy, Sejong University, Seoul, Korea.

出版信息

J Sep Sci. 2010 Nov;33(21):3354-64. doi: 10.1002/jssc.201000015.

Abstract

In this study, a series of GC calibration experiments were conducted to examine the feasibility of the thermal desorption approach for the quantification of five carbonyl compounds (acetaldehyde, propionaldehyde, butyraldehyde, isovaleraldehyde, and valeraldehyde) in conjunction with two internal standard compounds. The gaseous working standards of carbonyls were calibrated with the aid of thermal desorption as a function of standard concentration and of loading volume. The detection properties were then compared against two types of external calibration data sets derived by fixed standard volume and fixed standard concentration approach. According to this comparison, the fixed standard volume-based calibration of carbonyls should be more sensitive and reliable than its fixed standard concentration counterpart. Moreover, the use of internal standard can improve the analytical reliability of aromatics and some carbonyls to a considerable extent. Our preliminary test on real samples, however, indicates that the performance of internal calibration, when tested using samples of varying dilution ranges, can be moderately different from that derivable from standard gases. It thus suggests that the reliability of calibration approaches should be examined carefully with the considerations on the interactive relationships between the compound-specific properties and the operation conditions of the instrumental setups.

摘要

在这项研究中,进行了一系列的 GC 校准实验,以检验热解吸方法在结合两种内标化合物的情况下定量测定五种羰基化合物(乙醛、丙醛、丁醛、异戊醛和戊醛)的可行性。通过热解吸,对羰基的气态工作标准进行了标准浓度和加载体积的函数校准。然后将检测性能与通过固定标准体积和固定标准浓度方法得到的两种类型的外部校准数据集进行了比较。根据这一比较,基于固定标准体积的羰基校准应该比其固定标准浓度对应物更灵敏和可靠。此外,内标物的使用可以在很大程度上提高芳烃和一些羰基化合物的分析可靠性。然而,我们对实际样品的初步测试表明,在使用不同稀释范围的样品进行内标校准时,其性能可能与标准气体得出的结果略有不同。因此,建议应仔细检查校准方法的可靠性,同时考虑化合物特定性质与仪器设备操作条件之间的相互关系。

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