Graphite Furnace Atomic Absorption Spectrometry for Sizing Nanoparticles

石墨炉原子吸收光谱法测定纳米颗粒尺寸

• 批准号: 431441727
• 负责人: Professorin Dr. Kerstin Leopold
• 金额: --
• 依托单位: Institut für Analytische und Bioanalytische Chemie
• 依托单位国家: 德国
• 项目类别: Research Grants
• 财政年份: 2019
• 资助国家: 德国
• 起止时间: 2018-12-31 至 2023-12-31
• 项目状态: 已结题
• 来源: https://gepris.dfg.de/gepris/projekt/431441727?language=en
• 关键词: Graphite; Furnace; Atomic; Absorption; Spectrometry

The aim of the project is the development of a robust, direct and rapid method for the size determination of metal nanoparticles using graphite furnace atomic absorption spectrometry (GFAAS). The new method will provide reliable results on the size and size distribution of nanoparticles (NPs) in polydisperse suspensions, particularly for the lower nanoparticle size range. The focus is therefore on the development of a reproducible method for size detection and simultaneous concentration determination by means of GFAAS. Here, three crucial aspects will be addressed: 1. Investigation and optimization of the atomization of NPs in the graphite furnace; 2. The development of calibration strategies for size and concentration correlation; and 3. Investigation of the robustness of the method on the basis of complex, real samples. For the first sub-goal, it is important to investigate the kinetics and thermodynamics of the atomization of NPs as a function of concentration and size. For this purpose, the actual temperature curve in the graphite furnace will be recorded in-situ during the atomization phase. Thereby, amongst other parameters the so-called "appearance temperature" of the signals can be determined, from which activation energies can be calculated and the kinetic order of the atomization can be derived. These theoretical findings then serve the second sub-goal, the development of an optimal analytical calibration strategy for both particle size determination and metal concentration. Furthermore, a mathematical method for the deconvolution of signals from polydisperse suspensions will be developed and optimized in order to obtain a rapid method for the size distribution of metal nanoparticles in suspensions. In the third part of the project, more complex samples as well as real samples are to be investigated in which both a heterogeneous size distribution and heteroaggregates may occur. The robustness and possibly limits of the method are determined. The successfully developed and validated method will allow a direct, simple and fast sizing of even very small nanoparticles of real samples, which is difficult or impossible to access with other methods. In addition, the method is based on a different physical principle compared to the techniques of NP analysis proposed in the literature, such as single-particle mass spectrometry or light scattering methods. Thus, the successful project will also make a significant contribution to the analytical quality assurance of nanoparticle analysis on the way to reliable and standardized methods.

该项目的目的是开发使用石墨炉原子吸收光谱法（GFAAS）来确定金属纳米颗粒的尺寸来开发金属纳米颗粒的尺寸。新方法将为多分散悬浮液的纳米颗粒（NP）的尺寸和大小分布提供可靠的结果，特别是对于下纳米颗粒尺寸范围。因此，重点是开发可重复的方法，用于通过GFAA进行大小检测和同时浓度确定。在这里，将解决三个关键方面：1。石墨炉中NP雾化的研究和优化； 2。开发规模和浓度相关的校准策略；和3。根据复杂的真实样品研究该方法的鲁棒性。对于第一个亚目标，重要的是研究NP的雾化的动力学和热力学作为浓度和大小的函数。为此，将在雾化阶段记录石墨炉中的实际温度曲线。因此，在其他参数中，可以确定信号的所谓“外观温度”，可以从中计算激活能，并可以得出雾化的动力学顺序。然后，这些理论发现是第二个亚目标，即用于粒度确定和金属浓度的最佳分析校准策略的发展。此外，将开发和优化来自多分散悬浮液信号的数学方法，以获得悬浮液中金属纳米颗粒的尺寸分布的快速方法。在项目的第三部分中，将要研究更复杂的样本以及实际样品，其中可能会发生异质大小分布和杂聚集物。确定该方法的鲁棒性和可能的​​限制。成功开发和验证的方法将允许直接，简单，快速的尺寸，即使很小的真实样品的纳米颗粒，这很难或无法使用其他方法访问。另外，该方法基于与文献中提出的NP分析技术相比，例如单粒子质谱法或光散射方法。因此，成功的项目还将为纳米颗粒分析的分析质量保证做出重大贡献，以实现可靠和标准化方法的方式。