Instrumentation of Department of Structure and Dynamics in Catalysis

A: Major Equipment

1) 500 MHz MAS NMR spectrometer Bruker Avance III HD 500 WB/US NMR (upgrade 2013, in the Joint Laboratory of ss-NMR Spectroscopy of Institute of Macromolecular Chemistry ASCR and JHIPC)

  • 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) 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

3) Four FTIR spectrometers Nexus 670 e.s.p. (Thermo Nicolet Co.)

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

4) 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 GC 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

B: Available Methods

1) Preparation of heterogeneous catalysts and sorbents

  • Hydrothermal synthesis and preparation of inorganic materials including zeolites in 50 ml - 2.2 l autoclaves
  • Modification of catalysts forms (acid, base, redox) by ion exchanges and impregnations
  • Basic characterization of products (XRD, SEM)

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, Mössbauer spectroscopy and UV-Vis spectroscopy
  • Characterization of catalysts by XRD, SEM, TEM

4) NMR spectroscopy of inorganic solids

  • 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
  • Measurement at elevated temperatures and different gases

6) FTIR spectroscopy in transition and diffuse-reflectance mode

  • Home-made cells for measurement in different atmospheres and treatment of samples at elevated temperatures
  • Through flow cell for in situ measurement at elevated temperatures

C: Auxiliary equipment

1) TPD/TPR catalyst characterization system AutoChemHP Micrometric

Department of Structure and Dynamics in Catalysis