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Department of Synthesis and Catalysis

 Department of Theoretical Chemistry    Department of Spectroscopy    Department of Biophysical Chemistry     Department of Structure and Dynamics in Catalysis     Department of Synthesis and Catalysis     Department of Electrochemical Materials    Department of Molecular Electrochemistry    Department of Chemistry of Ions in Gaseous Phase    Department of Dynamics of Molecules and Clusters    Department of Low-dimensional Systems  

Instrumentation of Department of Synthesis and Catalysis

A: Major Equipment

1) Micromeritics ASAP 2020, ASAP 2020
- Static volumetric aparatus with two independent parts (sample preparation and sample analysis)
- Micromeritics'patented isothermal jackets for sample tube allowing stable thermal profile along the full length of the sample
- Three pressure transduceres: 133 Pa, 1.33 kPa, 133 kPa
- Degas system allows temperature up to 450 °C

2) Micromeritics Gemini II 2370
- Allows determining the surface area of solid materials
- Minimum resolvable pressure (p/p0) 10-4

3) FlowPrep060 instrument for sample degassing befor adsorption measurements
- With working temperature range of 10-400 °C

4) Thermo Scientific iCAP-7600 inductively coupled plasma optical emission spectrometr
- 4-channel, mini peristaltic pump with a drain sensor
- Free-running 27.12 MHz solid state RF plasma generator
- Charge injection device detector (CID86) with the range of 166 - 847 nm
- Duo plasma viewing (radial and axial)
- CETAC ASX 520 autosampler

5) Bruker AXSD8 Advanced diffractometer
- With Vantec-1 detector in the Bragg-Brentano geometry using Cu Kα radiation

6) Nicolet 6700 FTIR spectrometer
- Equipped with MCT/B and DTGS detectors

7) Berghof Speed wave MWS-3+ microwave digestion system
- 8 durable Berhof digestion vessels made of isostatically molded TFMTM PTFE material with the volume 100 ml ( max. pressure 100 bar, max. temperature 230 °C) allowing to use HF, HNO3 and HCl
- Frequency of magnetron 2450 MHz
- With built-in, non-contact temperature measurement

8) Agilent gas chromatographs
Agilent GC 6890 Plus
- Equipped with 100 position 7683 Series Injector autosampler
Agilent 7890 A
- Equipped with unique high pressure liquid injection device
Two Agilent 6850
- Equipped with 27 position injector autosampler
Agilent 7820A
- Equipped with 50 position injector autosampler

9) Microactivity Reference flow catalytic reactor
- Automated laboratory system for measurement of catalytic activity and for the study of the yield and kinetics on chemical reactions in liquid or gas phase at atmospheric - tubular reactor with 2 µm porous plate used up to 700 °C, thermocouple in catalytic bed
- Reactive system integrated within hot box with temperature up to 170 °C
- 6-port VICI valve for reactor bypass
- 6 control devices for mass flow controllers
- Dosing by two Gilson 307 HPLC pumps in streams ranging between 0,01 and 5 ml/min and pressures of up to 600 bar

10) HF X-Cube flow catalytic aparatus
- High pressure, continuous-flow reactor capable of reaching temperatures and pressures up to 200 °C and 150 bar respectively
- Two built-in conventional HPLC pumps deliver reagent to a stainless steel, packed cartidge (CatCartTM) surrounded by aluminum heating block
- Product mixture is air-cooled before being collected in a vial or flask.

11) Nicolet iS10 FTIR spectrometer
- DTGS detector with spectral resolution of 4 cm-1
-ATR accessory
- 400-4000 cm-1, KBr optics

12) Heidolph Synthesis 1 instrument
- Catalytic experiments in liquid phase, 16 parallel reactions
- 25 ml reaction glass vessels with PTFE caps
- 4 heating zones with individual heat control
- Condensation zone allows for refluxing of solvents using chiller

13) NMR spectrometer Varian Mercury 300.
- Gradient module Performa I for pulsed field gradient experiments.
- Probes for liquid NMR: ASW PFG 4 nuclear or broad-band operation (1H, 19F, 15N-31P), ID PFG (1H, 15N-31P).

14) 250 mL BĂĽchi glass double-jacketed polymerization autoclave equipped with a magnetic stirrer.
- The consumption of ethylene is recorded during the polymerization by a calibrated mass flow meter (Bronkhorst, EL-FLOW) which was controlled by a Bronkhorst High-Tech modular digital readout and control system.

15) 100 mL high pressure picoclave BĂĽchi reactors equipped with cyclone 075 agitator with integrated magnetic coupling.
- Steel vessel with heating jacket and bottom opening 100 ml, 60 bar, 250 °C.

16) Argon-vacuum lines and high-vacuum lines.
- Lines are equipped for manipulations with air- and moisture-sensitive compounds using standard Schlenk techniques and all sealed ampoules.

17) Labmaster 130 glovebox (mBraun).
- Oxygen and water vapour concentrations below 2.0 ppm

18) Solvent purification system (PureSolv MD 7; Innovative Technology, Inc.)

 

B: Available Methods

1) Adsorption of N2, CO2, Ar and other gases
2) Elemental analysis of mineralized samples (ICP-OES)
3) X-ray diffraction patterns (XRD)
4) Fourier transform infrared spectroscopy (FTIR)
5) Gas chromatography (GC)
6) EPR spectrometer MiniScope MS400(Magnettech)
- Spectrometer with high measurement sensitivity 8*109 Spins/0,1mT and magnetic field stability 1,5ÎĽT/min.
- Microwave power range standard 100ÎĽW - 50mW.
- Ultra fast automatic frequency control (AFC).
- Allows irradiation of samples in the resonator during the measurement using a parallel beam.
- Microwave frequency counter model FC400.
7) Nicolet Avatar FT IR spectrometer
- Air-protecting cuvette on a in the range 400-4000 cm-1
- Attenuated Total Reflectance (ATR) accessory with Si and ZnSe crystals.
8) UV-near IR spectrometer Varian Cary 17D spectrometer.
- Measuring in the range 300-2000 nm in all-sealed quartz cells (Hellma).
9) Thermo Focus DSQ GC-MS analyser.
- Equipped with a capillary column Thermo TR-5MS (15 m x 0.25 mm x ID 0.25 ÎĽm).


C: Auxiliary equipment

1) Autoclave Parr
- 1 l, 2 l PTFE liners
- Maximum working pressure 131 bar
- Temperature range -10-350 °C
- Parr reactor controller 4848 taking control of temperature and stirring

2) Autoclaves for the synthesis
- 20 ml, 90 ml, 500 ml teflon liners
- Maximum pressure 50 bar, maximum temperature 200 °C

3) Hettich EBA 200 centrifuge
- 8 positions rotor with maximum RPM 6000
- 10 ml flasks

4) Trigon-Plus C3i centrifuge
- 4 position rotor Jouan T40 with maximum load 3,7 kg and maximum RPM of 4300
- 250 ml flasks


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