Thermogravimetric Analysis Combined with Calorimetry and Gas-Chromatography/Mass Spectrometry

热重分析与量热法和气相色谱/质谱联用

• 批准号: 530331787
• 金额: --
• 依托单位: Friedrich-Alexander-Universität Erlangen-Nürnberg
• 依托单位国家: 德国
• 项目类别: Major Research Instrumentation
• 财政年份: 2023
• 资助国家: 德国
• 起止时间: 2022-12-31 至 无数据
• 项目状态: 未结题
• 来源: https://gepris.dfg.de/gepris/projekt/530331787?language=en
• 关键词: Thermogravimetric; Analysis; Combined; Calorimetry; Gas

In the present application, the procurement of a combined thermogravimetric analysis/differential scanning calorimeter (TGA-DSC) coupled to gas chromatography/mass spectrometry (GC/MS) for the simultaneous investigation and characterization of ionic liquids (ILs) is kindly requested. The system will be installed in the Chair of Inorganic and General Chemistry at the Friedrich-Alexander-Universität Erlangen-Nürnberg (FAU) and represents a central infrastructure component of the newly established Collaborative Research Center SFB 1452 “Catalysis at Liquid Interfaces” (CLINT). In close collaboration with working groups from chemistry, physics, theory, chemical engineering, and material science, the instrument will enable the characterization of the thermal and thermodynamic properties of task-specific (TS) ILs. The newly developed and synthesized ILs are of vital importance for interface-enhanced “Supported Ionic Liquid Processes” (ie-SILP) and “Solid Catalysts with Ionic Liquid Layer” (SCILL) systems in connection with (electro-)catalytic processes at gas/liquid and liquid/solid interfaces within CLINT. The focus is on the idea of using the anisotropic reaction environment at the interface to tailor active sites with unique reactivity. Thus, the device will play a central role in studying interface-enhanced SILP and SCILL, concepts that use custom-tailored ILs to control (electro-)catalytic reactions in which interface-enhanced molecular complexes generate the catalytic properties. Several specific requirements for the device result from the envisioned application areas. Custom-tailored TS-ILs with different thermal and chemical properties must be developed, synthesized, and fully characterized with regard to their thermal stability and sub¬stance properties; thus, leading the way to potential applications. Accordingly, we will have to install an apparatus that allows for the simultaneous thermal analysis (STA) combined with gas-chromatography and mass spectrometry (STA-GC-MS), which combines four standard characterization methods (DSC, TGA, GC, and MS) in a single instru¬ment. With only one sample required, the results of the thermal analyses are exceptionally comparable due to perfectly identical measuring conditions, such as atmosphere, gas flow rate, vapor pressure, heating rate, and thermal contact with the sensor. Thus, it is less time-consuming and reduces the expenses for high-cost materials and elaborate syntheses. Due to wider operating temperature windows (–150 to 1600 °C) of STA instruments – compared to common TGA instruments – temperature-sensitive samples can be examined regarding their thermal properties. Additionally, the in-situ attached GC-MS unit can clearly separate and detect the complex product and pyrolysis mixtures, providing insights into the constitution of the reaction and decomposition products. This gives access to a variety of information on material properties, composition, and stability.

在介绍应用中，请求与气相色谱/质谱（GC/MS）相连的热重分析/差分扫描量热计（TGA-DSC）的采购，以简单投资和表征离子液体（IL）的表征。该系统将安装在Friedrich-Alexander-UniversitätErlangen-Nürnberg（FAU）的无机和通用化学主席中，并代表了新成立的合作研究中心SFB 1452 SFB 1452的中心基础设施成分（Clint）。与化学，物理，理论，化学工程和材料科学的工作组密切合作，该仪器将能够表征任务特异性（TS）ILS的热力学和热力学特性。新开发和合成的IL对于接口增强的“支撑的离子液体过程”（IE-SILP）和“具有离子液体层的固体催化剂”（丝网膜液层）（scill）系统至关重要。重点是在界面上使用各向异性反应环境来量身定制具有独特反应性的活动位点的想法。这是该设备在研究界面增强的SILP和刺激中起着核心作用，这些概念使用定制的IL来控制（电 - ）催化反应，其中界面增强的分子复合物会产生催化性能。该设备的几个特定要求来自设想的应用领域。必须开发，合成和完全表征具有不同热和化学特性的量身定制的TS-IL，以其热稳定性和子质特性进行全面表征；因此，引导潜在应用。彼此之间，我们将必须安装一种允许同时进行热分析（STA）与气体色谱和质谱（STA-GC-MS）结合的设备，该设备结合了单个仪器中的四种标准表征方法（DSC，TGA，GC和MS）。仅需要一个样品，由于完全相同的测量条件，例如大气，气流流速，蒸气压，加热速率和与传感器的热接触，热分析的结果非常可比。这是较少的时间，减少了高成本材料和精心制作的合成费用。由于与常见的TGA仪器相比，由于宽阔的工作温度窗口（–150至1600°C），因此可以检查对温度敏感的样品的热性能。此外，原位附着的GC-MS单元可以清楚地分离并检测复杂的产物和热解混合物，从而洞悉反应和分解产物的构型。这样可以访问有关材料属性，组成和稳定性的各种信息。