Specialized Characterization Methods at the ITC – New Perspectives Through Unique Measurement Techniques:
XAS/XES-Spectrometer
easyXAFS 300+:
With our in-house laboratory XAS/XES spectrometer, we can perform X-ray absorption and emission measurements on the elements Ti-Mo and Te-U. These measurements provide insights into oxidation state, coordination geometry, and – thanks to EXAFS measurements – also information about neighboring atoms such as atomic distance, number, and type. In the future, in-situ measurements for solid and liquid samples will also be possible in electrochemical and heterogeneous in-situ XAS reactors.
Solid State NMR
Bruker Avance III 400WB & AvanceNEO 500WB:
The ITC has got a Bruker Avance III 400 WB 9,4 T solid state NMR spectrometer with 4 mm and 7 mm MAS probe heads. These allow to gain important structural information about solids, e.g. the chemical environment or coordination, which are otherwise inaccessible in liquid NMR. This is achieved by measuring many different nuclei and pulse sequences – from a simple direct excitation to more advanced sequences like cp (cross polarization), TRAPDOR, or 2D experiments. The focus herein lies on the investigation of porous heterogeneous catalysts, e.g. bulk measurements of aluminosilicates via 27Al or 29Si MAS NMR. Furthermore, the acid sites of catalysts can be measured both qualitatively and quantitatively, either via 1H MAS NMR directly or with the help of additional probe molecules like ammonia.
Explore our equipment and learn how we turn science into measurable results:
- 3D-Printing
- Prusa i3 MK3S & Prusa MINI 3D-printer: 3D printing enables the production of precise and custom-made components directly at the Institute. Complex reactor designs for electrochemical applications can be realized with high geometric flexibility. This approach allows prototypes to be created fast and adapt quickly to research needs.
- Auto Column
- Biotage Isolera One Flash Chromatography: The Isolera One Flash Chromatography Instrument from Biotage® enables rapid purification of compounds (milligram to 75 g samples) using a UV-VIS detector and automatic separation of fractions. The versatile settings (gradient of the mobile phase mixture, flow rate 1-200 mL/min, pressure up to 10 bar) allow challenging separation problems to be solved.
- Chemisorption
- Quantachrome Autosorb-1
- Differential Scanning Calorimetry
- Netzsch STA 449 F5: The STA 449-F5 allows simultaneous application of Thermogravimetry (TG, TGA) and Differential Thermal Analysis (DTA) or Differential Scanning Calorimetry (DSC) to the same sample in one instrument. In the STA, the test conditions are identical for the TGA and DTA/DSC signals (same atmosphere, gas flow rate, heating rate, thermal contact to the sample crucible and sensor, etc.). The DSC allows for measuring e.g. the melting/crystallization behavior or glass transitions of samples, while the TGA allows for measuring e.g. mass changes (loss of water), temperature stability and oxidation/reduction behavior. Heating rates up to 50 K/min (RT to 1600°C) and up to 3 different gases (1 inert, 2 for purging) allows the application of a wide range of experimental conditions.
- Elemental Analysis ICP-OES
- PerkinElmer Avio200
- FT-IR DRIFTS
- Harrick Praying Mantis
- FT-IR-Spectrometer
- ThermoFisher iS50: The Thermo Scientific Nicolet 6700 FT-IR spectrometer is a Fourier-transform infrared (FT-IR) spectrometer designed for routine analysis and research applications. It offers a broad spectral range (standard range: 350–7800 cm⁻¹), enabling the precise chemical identification of materials based on their infrared spectra. Interchangeable accessories are available for transmission, ATR (attenuated total reflectance; ITR ATR Diamond), and HATR (horizontal attenuated total reflectance; X700 Smart Ark) measurements. Measurements are performed on KBr pellets under ambient atmospheric conditions. The spectrometer is therefore suitable for the analysis of samples that are stable in air and resistant to moisture.
- Gas Chromatography & GC-MS & Micro-GC
- Agilent 7890A (various other models) & 7890B + 5977B & 490 Mikro-GC
- Glovebox
- Jacomey P(BOX), M-Braun Labstar (2- und 3-armig) with solvent system (M-Braun SPS-5)
- HPLC (offline & online)
- Agilent 1260 with DAD + RID & Agilent 1260 Infinity II with RID: At the ITC, three modular HPLC systems with autosamplers are available for offline analysis of liquid samples. Due to the wide range of available columns, eluents (aqueous or organic) and the possibility to adjust the injection volume, column and detector temperature, a large number of analytical challenges can be solved. A typical example is the quantitative analysis of liquid products of the electrochemical CO2 reduction like organic acids (e.g. formic acid, acetic acid) and alcohols (e.g. ethanol, propanol) in the electrolyte. Another example would be the quantification of liquid samples from the cyclohexane oxidation on a reversed-phase column.
- IR-Spectrometer
- Bruker Alpha 2
- Particle Size Analyzer
- Horiba LB-500
- Physisorption
- Quantachrome Autosorb-3B: Nitrogen adsorption at 77 K on solid sample surfaces, combined with advanced evaluation methods such as the Brunauer–Emmett–Teller (BET) and Barrett–Joyner–Halenda (BJH) models as well as density functional theory (DFT) simulations, enables the determination of key properties including specific surface area, pore volume, pore size, and their distribution.
- Planetary Mill
- Fritsch Pulverisette 7 Premium-Linie
- Potentiostats
- Gamry Reference 3000 & Interface 1010E & Booster & Origalys Electrochemical Workstation
- Raman-Spectrometer
- Ocean Optics Ventana 532
- Ring Disc Electrode
- Gamry RxE 10k Rotating Electrode, Pine Research RDE Tip
- Solid State NMR
- Bruker Avance III 400WB & AvanceNEO 500WB: The ITC has got a Bruker Avance III 400 WB 9,4 T solid state NMR spectrometer with 4 mm and 7 mm MAS probe heads. These allow to gain important structural information about solids, e.g. the chemical environment or coordination, which are otherwise inaccessible in liquid NMR. This is achieved by measuring many different nuclei and pulse sequences – from a simple direct excitation to more advanced sequences like cp (cross polarization), TRAPDOR, or 2D experiments. The focus herein lies on the investigation of porous heterogeneous catalysts, e.g. bulk measurements of aluminosilicates via 27Al or 29Si MAS NMR. Furthermore, the acid sites of catalysts can be measured both qualitatively and quantitatively, either via 1H MAS NMR directly or with the help of additional probe molecules like ammonia.
- Thermal Gravimetric Analysis
- Setaram SETSYS 16/18
- TPx
- Quantachrome Autosorb iQ TPx: The Autosorb 6300 is a multi-purpose Device for physisorption and chemisorption measurements of solids to characterize their properties (e.g. BET surface, redox activity). The measurements can be done under static or dynamic conditions (flow cells). It is equipped with a mass spectrometer (Co. Pfeiffer) which allows the qualitative analysis of desorbing gaseous molecules during dynamic measurements. Physisorption measurements like multi-point BET can be done with liquid N2 or Ar to measure the specific surface or pore size distributions even for microporous solids like zeolites. A Dewar kit allows measurements at controlled temperatures (e.g. -20°C – 100°C) to determine the gas adsorption capacities of CO2 or H2O in single or multicomponent gases. For temperature programmed methods (desorption, reduction, oxidation etc.) a tube furnace can be applied. The Autosorb 6300 is a high-vacuum system designed for physisorption and chemisorption studies, enabling accurate determination of BET surface area, active surface sites, and pore size distribution. In addition, temperature programmed reactions (TPX) including techniques such as temperature programmed desorption (TPD), reduction (TPR), and oxidation (TPO), provide valuable insights into surface properties, adsorption strength, and catalytic behavior by monitoring gas-solid interactions as a function of temperature. Together, these capabilities make the Autosorb 6300 a versatile and reliable analytical equipment for advanced materials characterization in the catalytic research at the Institute of Technical Chemistry.
- Ultrasonic Spray Coater
- Nadetech ND-SP Mini-Ultrasonic
- UV/VIS-Spectrometer
- Agilent Cary 60 UV/VIS-Spectrophotometer (with DR-Adapter): Wavelength range: 190 - 1100 nm UV/VIS absorption spectra can be recorded in customary transmission mode. With a remote diffuse reflection probe VideoBarrelinoTM designed for the Cary 50 and 60, used for true diffuse reflection mode (no specular reflection from sample) with a small sampling spot size, UV/VIS spectra of solid materials can be measured.
- X-ray Powder Diffraction
- Bruker D8
- XAS/XES-Spectrometer
- easyXAFS 300+: With our in-house laboratory XAS/XES spectrometer, we can perform X-ray absorption and emission measurements on the elements Ti-Mo and Te-U. These measurements provide insights into oxidation state, coordination geometry, and – thanks to EXAFS measurements – also information about neighboring atoms such as atomic distance, number, and type. In the future, in-situ measurements for solid and liquid samples will also be possible in electrochemical and heterogeneous in-situ XAS reactors.