Dipartimento di Chimica, Università degli Studi di Milano, Milan, Italy.
Anal Bioanal Chem. 2013 Jan;405(2-3):1123-32. doi: 10.1007/s00216-012-6433-5. Epub 2012 Sep 30.
In the last decade, our research group set up and optimised analytical techniques for the characterisation of the major components of atmospheric aerosol (i.e. secondary inorganic ions and carbonaceous material) and source markers (e.g. levoglucosan, carbonates). In this study, we present a complete overview on the most problematic aspects that can be encountered during the quantification of the two main components of aerosol, i.e. the ionic and carbonaceous fractions. More in detail, different liquid chromatographic approaches were set up for main ions and anhydrosugars determination. Quality assurance procedures (i.e. tests on data reliability) were applied during the set-up phase and they are presented in this work. As regards the carbonaceous component characterisation, two evolved gas analysis techniques were set up and applied: the thermogravimetric technique coupled to the Fourier transformed infrared spectroscopy (TGA/FTIR) and the thermal-optical transmittance method (TOT). A suitable protocol for organic and elemental carbon separation was set up for the TGA/FTIR system and a comparison with the results obtained by the TOT method was carried out. Studies on the impact of filter load, field blanks, and sample composition on OC/EC quantification by the TOT method were performed. Moreover, approaches for carbonate carbon quantification on different kinds of filters were developed. It was demonstrated that this approach allows to reach the ionic balance in samples impacted by carbonate compounds. The optimised methods have been applied for the analysis of thousands of PM filters allowing the obtainment of reliable results.
在过去的十年中,我们的研究小组建立并优化了分析技术,用于大气气溶胶主要成分(即二次无机离子和含碳物质)和源标记物(如左旋葡聚糖、碳酸盐)的特征描述。在本研究中,我们全面介绍了在气溶胶两种主要成分(即离子和含碳部分)定量过程中可能遇到的最具挑战性的问题。更详细地说,我们建立了不同的液相色谱方法来测定主要离子和无水糖。在建立阶段应用了质量保证程序(即数据可靠性测试),并在本文中进行了介绍。关于含碳成分的特征描述,我们建立并应用了两种热解气分析技术:热重分析结合傅里叶变换红外光谱(TGA/FTIR)和热光学透射法(TOT)。为 TGA/FTIR 系统建立了一种适合有机碳和元素碳分离的方案,并与 TOT 方法的结果进行了比较。还对 TOT 方法中 OC/EC 定量的滤膜负载、现场空白和样品组成的影响进行了研究。此外,我们还开发了在不同类型滤膜上定量碳酸盐碳的方法。结果表明,这种方法可以使受碳酸盐化合物影响的样品达到离子平衡。优化后的方法已应用于数千个 PM 滤膜的分析,得到了可靠的结果。