Instrumentation of the Department of Structure and Dynamics in Catalysis | J. Heyrovsky Institute of Physical Chemistry

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)