Instrumentation of Department of Molecular Electrochemistry 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 Büchi 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 Büchi 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 1,5μT/min.
- Microwave power range standard 100μW - 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 μm).

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

Department of Molecular Electrochemistry and Catalysis