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

在本申请中，请采购热重分析/差示扫描量热计（TGA-DSC）与气相色谱/质谱（GC/MS）相结合的组合热重分析/差示扫描量热计，用于同时研究和表征离子液体（ILs）。该系统将安装在Friedrich-Alexander-Universität erlangen - n<s:1> rnberg （FAU）无机和普通化学系主任的办公室，并代表新成立的SFB 1452“液体界面催化”（CLINT）合作研究中心的核心基础设施组成部分。通过与来自化学、物理、理论、化学工程和材料科学的工作组的密切合作，该仪器将能够表征特定任务（TS） ILs的热学和热力学特性。新开发和合成的ILs对于界面增强的“负载离子液体过程”（- silp）和“离子液体层固体催化剂”（SCILL）系统在CLINT中与气/液和液/固界面（电）催化过程相关的催化过程至关重要。重点是利用界面上的各向异性反应环境来定制具有独特反应活性的活性位点。因此，该装置将在研究界面增强型SILP和SCILL方面发挥核心作用，这些概念使用定制的il来控制（电）催化反应，其中界面增强型分子复合物产生催化性能。对设备的几个特定要求来自于预期的应用领域。必须开发、合成具有不同热、化学性质的定制化ts - il，并对其热稳定性和物质性质进行充分表征；因此，引领了潜在应用的道路。因此，我们必须安装一套设备，允许同时热分析（STA）结合气相色谱和质谱（STA-GC-MS），它结合了四种标准的表征方法（DSC， TGA， GC和MS）在一个仪器。只需要一个样品，由于完全相同的测量条件，如大气、气体流速、蒸汽压力、加热速率和与传感器的热接触，热分析的结果具有特别的可比性。因此，它更节省时间，减少了高成本材料和复杂合成的费用。与普通TGA仪器相比，STA仪器的工作温度窗口（- 150°C至1600°C）更宽，因此可以检查温度敏感样品的热性能。此外，原位附着的GC-MS单元可以清晰地分离和检测复杂产物和热解混合物，从而深入了解反应和分解产物的组成。这样就可以获得关于材料性质、成分和稳定性的各种信息。

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.