Analytical Spectroscopy and Sensors Group, Institute of Environmental Sciences, University of Zaragoza, Pedro Cerbuna, 12, 50009 Zaragoza, Spain.
Anal Chim Acta. 2010 Feb 28;661(2):206-14. doi: 10.1016/j.aca.2009.12.021. Epub 2009 Dec 22.
A methodological approach based on the size characterization of environmental microparticles (size larger than 1 microm), nanocolloids (1 microm to 15 nm) and macromolecules (lower than 1000 kDa) by asymmetrical flow field-flow fractionation (AsFlFFF), taking advantage of both normal and steric elution modes, is presented. The procedure was optimized to minimize the potential alteration of the size distribution and metal associations of the species characterized. Prior to separation by AsFlFFF, samples are subjected to gravitational settling of the solid suspension, followed by a centrifugation of the settled sample. The comparison between the fractograms of the settled and the centrifuged samples allows the characterization of the microparticles, which are eluted in steric mode in the AsFlFFF system. The characterization of nanocolloids and macromolecules is carried out on the centrifuged sample by applying different operational conditions under normal mode in the AsFlFFF system. A comparison with the conventional frontal filtration through 0.45 microm pore size membranes have shown that filtration removes particles below their nominal pore size, modifying the size distribution of the samples respect to the centrifugation. The methodology proposed has been applied to the size characterization of compost leachates. The contribution of these three differentiated fractions to the mobilization of metals has been determined by coupling the AsFlFFF system to an inductively coupled plasma mass spectrometer (ICP-MS).
提出了一种基于环境微粒(尺寸大于 1 微米)、纳米胶体(1 微米至 15 纳米)和大分子(低于 1000 kDa)的尺寸特征化的方法学方法,该方法利用不对称流场流分离(AsFlFFF)的正常和空间排阻洗脱模式。该程序经过优化,可最大程度地减少所描述物种的尺寸分布和金属缔合的潜在变化。在通过 AsFlFFF 分离之前,样品经过固体悬浮液的重力沉降,然后对沉降样品进行离心。沉降和离心样品的 fractogram 之间的比较允许对以空间排阻模式洗脱的 AsFlFFF 系统中的微粒进行特征化。通过在 AsFlFFF 系统中的正常模式下应用不同的操作条件,对纳米胶体和大分子进行离心样品的特征化。与通过 0.45 微米孔径膜的常规前端过滤的比较表明,过滤会去除小于其名义孔径的颗粒,从而改变样品相对于离心的尺寸分布。所提出的方法已应用于堆肥浸出液的尺寸特征化。通过将 AsFlFFF 系统与电感耦合等离子体质谱仪(ICP-MS)耦合,确定了这三个不同分数对金属迁移的贡献。