Instrumentation of the Department of Structure and Dynamics in Catalysis

A: Major Equipment - Preparation

1) 500 MHz MAS NMR spectrometer Bruker Avance III HD 500 WB/US NMR (upgrade 2013)

  • 7-mm N-P/H probehead
  • 4-mm N-P/H-F probehead
  • 4-mm X/Y/H probehead
  • 3.2-mm N-P/H-F probehead
  • 2.5-mm N-P/F-H probehead

2) Equipment for liquid phase synthesis 

  • Autoclave 0.55 l, 20 - 220 °C, 0 - 150 bar, Stainless steel DIN WNr. 1.4571/1.4404 (AISI 316Ti/316L)
  • Autoclave 0.55 l, 20 - 220 °C, 0 - 150 bar, Hastelloy C22
  • Autoclave 2.2 l, 20 - 250 °C, 0 - 200 bar, Stainless steel
  • Autoclave 3.2 l, 20 - 220 °C, 0 - 150 bar, Stainless steel
  • Speedwave four for synthesis of nanomaterials - Microwave digestion system with built-in, non-contact temperature and pressure measurements

3) UV-Vis-NIR spectrometer Perkin-Elmer Lambda 950 

  • Two integrating sphere attachments for diffuse-reflectance measurements at UV-Vis-NIR with spectralon coating
  • Integrating sphere attachment for diffuse-reflectance measurements at NIR with coating by gold
  • Harrick through flow cell for elevated temperatures for measurements with praying mantis
  • Home-made through flow cell for elevated temperatures for measurements with integrating sphere

4) Three FTIR spectrometers Nexus 670 e.s.p. (Thermo Nicolet Co.) 

  • MKS detectors
  • DTGS KBr
  • ATR and reflectance accessories
  • High-low pressure IR reactor In-Situ Research - Instruments, USA equipped by AvaSpec-2048FT Fast Trigger Fiber Optic UV-Vis Spectrometer Avantes and MS gas analysis.

5) Catalytic apparatuses

  • Computerized catalytic reactors for hydrocarbon transformations equipped with gas chromatograph with GC (HP 5890, HP 6890, HP 5971A, HP 6850, Finnigan 9001 with GC-FID, TCD, MSD) and MS detection (GC-MS spectrometer Agilent, Quadrupole mass spectrometers QMA 125, QMG 421C, QMG 420)
  • Computerized Microactivity-Reference catalytic reactors PIDENG&TECH with gas chromatography detection
  • Computerized catalytic reactors for N2O/NO/NO2 abatement reactions with NO/NOx chemoluminescence analyzers VAMET, Analyzer Advanced Optima 200/Limas 11HW ABB, N2O analytical system Advance Optima Hartmann & Brown and GC detection

6) Photocatalytic apparatuses

  • Liquid phase testing using UV or visible light
  • Gas phase testing using UV or visible light

7) QUV Accelerated Weathering Tester and Q-Sun Xenon Test Chamber 

  • QUV Overview: Solar Eye Irradiance Control, Lamps: UVA-340, UV-B, Water spray system, ISO calibration
  • Q-Sun Overview: Full-spectrum xenon arc lamps, The Solar Eye Irradiance Control System, Optical filters (Daylight, Window, Extended UV), A choice of irradiance set points (340 nm, 420 nm or TUV), ISO, ASTM &SAE compliance

B: Available Methods

1) Liquid phase bath synthesis 

  • Synthesis in 100 ml - 2.2 l autoclaves 
  • Acid or base corrosive environment
  • Hydrothermal synthesis and preparation of inorganic materials including zeolites
  • Modification of catalysts forms (acid, base, redox) by ion exchanges and impregnations
  • Basic characterization of products (XRD, SEM, N2 adsorption)

2) Characterization of catalytic activity of acid and base heterogeneous catalysts

  • Through-flow catalytic experiments, including elevated pressure
  • Batch catalysts and kinetic testing (100 ml - 2.2 l autoclaves)
  • GC and MAS spectroscopy analysis of products

3) Characterization of acid and base heterogeneous inorganic catalysts

  • Characterization of acidic properties by TPD and FTIR spectroscopy of adsorbed probes
  • Characterization of redox properties by TPR, FTIR spectroscopy and UV-Vis spectroscopy
  • Characterization of sorption properties of catalysts, XRD, SEM

4) NMR spectroscopy of inorganic solids

  • 500 MHZ MAS NMR spectrometer, N-P/H and Al/Si/H experiments
  • Setup for treatment/evacuation of samples & sealing prior spectra measurement

5) UV-Vis-NIR spectroscopy in transition and diffuse-reflectance mode

  • Measurement of liquids, powders, turbid media
  • Measurement in transmission, reflection and diffuse reflection mode
  • Harric and home-made through-flow cells for measurement at elevated temperatures and different gases

6) FTIR spectroscopy in transition and diffuse-reflectance mode

  • Measurement in transmission and diffuse reflectance mode
  • Home-made cells for measurement in different atmospheres and treatment of sampúles at elevated temperatures
  • Through flow cell for in situ measurement at elevated temperatures

7) Separation of nanoparticles 

  • Gradient separations, in which the tubes are filled from top to bottom with an increasing concentration of a dense substance in solution.
  • Determination of particle size distribution of solid particles, emulsions and bubbles
  • Determination of the zeta potential of particles

8) Preparation of thin layers by dipcoating 

  • Coating of flat supports in controlled atmosphere
  • Coating of tube supports up to 80 cm in length and 10 cm in diameter

9) Testing the photocatalytic performance of powders and layers

  • Degradation of aqueous pollutants
  • Degradation of gaseous pollutants according to ISO standards

10) Accelerated weathering testing of solid materials

  • Testing the durability of bulk materials or layers and coatings on different substrates
  • Test according to ISO, CEN, DIN and other standards

11) Determination of the texture and sorption properties of solids

  • Determination of porosity of micro- and mesoporous materials
  • Determination of surface area of thin films

12) Scanning electron microscopy

C: Auxiliary equipment

1) Ultracentrifuge Optima XPN-100 (Beckman Coulter)

  • Maximum speed: 100,000 rpm, Maximum RCF (x g): 802,400, Speed control: ± 2 rpm of set speed (above 1,000rpm), Set temperature: 0 to 40°C,Ambient operating range: 10 to 35°C, Accel/decal: 10/11, Drive cooling: air-cooled

2) Analyzer of the particle size and zeta potential ZetaSizer NanoS, model ZEN1600 (Malvern)

  • Cell for the measurement of the zeta potential of surfaces

3) Dip Coater 5

  • Uniform deposition of layers on plates and similar objects by dipping and dragging into bath with solution.

4) Sorption apparatus ASAP 2010 (Micromeritics)

  • Microporous option with three transducers
  • Low-pressure system

5) Laboratory electric superkanthal furnace Model 2017S (Clasic CZ) 

  • Preparation and heat treatment of ceramics, glass phases and metals/metal alloys up to 1700°C under air or an inert atmosphere.

6) Extruder Multi-Gran, Model MG-55 ( FUJI PAUDAL CO)

  • Manufacturing granules of ceramics, organic materials, polymers/biopolymers in form of cylinders of the diameter 1 to 3 mm adjusted by the selection of a die with proper openings

7) Planet laboratory mill Pulverisette 6 (Ilabo) 

  • for the milling of powders up to 500 g in weight.

8) Fiber Optic UV-Vis Spectrometers 

  • Two UV-Vis spectrometers AvaSpec-2048FT Fast Trigger Avantes
  • UV-Vis spectrophotometer VWR

9) Scanning electron microscope Jeol JSM-5500 LV

10) TPD/TPR AMI-200 catalyst characterization system Altamira Instruments

11) Universal apparatus of in-house construction for studies of transport and reaction processes in inorganic membranes

Department of Structure and Dynamics in Catalysis

Deputy Head