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.

该项目的目标是开发一种稳健、直接和快速的方法，使用石墨炉原子吸收光谱法 (GFAAS) 测定金属纳米颗粒的尺寸。新方法将为多分散悬浮液中纳米颗粒（NP）的尺寸和尺寸分布提供可靠的结果，特别是对于较低的纳米颗粒尺寸范围。因此，重点是开发一种可重复的方法，通过 GFAAS 进行尺寸检测和同时测定浓度。在这里，将讨论三个关键方面：1.石墨炉中纳米颗粒雾化的研究和优化； 2. 尺寸和浓度相关性校准策略的开发； 3. 基于复杂的真实样品研究该方法的稳健性。对于第一个子目标，重要的是研究纳米粒子原子化的动力学和热力学作为浓度和尺寸的函数。为此，将在原子化阶段现场记录石墨炉内的实际温度曲线。由此，除了其他参数之外，还可以确定信号的所谓“出现温度”，由此可以计算活化能并且可以导出原子化的动力学级数。这些理论发现随后服务于第二个子目标，即开发用于粒度测定和金属浓度的最佳分析校准策略。此外，还将开发和优化多分散悬浮液信号反卷积的数学方法，以获得悬浮液中金属纳米颗粒尺寸分布的快速方法。在该项目的第三部分中，将研究更复杂的样品以及真实样品，其中可能出现异质尺寸分布和异聚集体。确定该方法的稳健性和可能的​​限制。成功开发和验证的方法将允许直接、简单和快速地测定真实样品中甚至非常小的纳米颗粒的尺寸，这是其他方法很难或不可能实现的。此外，与文献中提出的 NP 分析技术（例如单粒子质谱法或光散射法）相比，该方法基于不同的物理原理。因此，该项目的成功也将为纳米颗粒分析的分析质量保证以及可靠和标准化方法的发展做出重大贡献。