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Centre for Sustainable Chemical Processes

Integrated Chemical Reaction Facility (ICRF)

Resources

 

Instrumentation

CSCP’s recently established Integrated Chemical Reaction Facility (ICRF) brings together Durham Chemistry Department’s unique high pressure laboratory and highly reactive/toxic gas handling laboratory facilities, together with state-of-the-art equipment and instrumentation, to create a world-class laboratory for the development and exploitation of interdisciplinary sustainable, efficient chemical reactions and energy-related research projects. An overview of the varied facilities available through the ICRF is given below.

 

(1) Gas Chromatography

  • BRUKER SCION 456 GC with flame ionisation detector (FID) and thermal conductivity detector (TCD) - used to analyse a wide range of liquid and gas samples on an analytical scale to identify and quantify complex mixtures as well as being a valuable tool in testing compound purity. 

 

Figure 1. Bruker GC (left) and Peak Scientific H2 generator (right).

  • Agilent GC/MS (7820A GC/5977E MSD) provides low detection limits in complex mixtures. It features electron ionisation (EI) source, single gold quartz quadrupole with 1050 u mass range, and synchronous Selected Ion Monitoring (SIM)/Scan mode, which allows selective monitoring of ions of interest at high sensitivity, while simultaneously acquiring spectra within a specified mass range. Additionally, both MSD ChemStation and MassHunter software are available for data analysis.

 

Figure 2. Agilent GC/MS.

(2) CDS Pyroprobe 5200 with a fast filament heating rate (up to 20 °C ms−1) and precise temperature control (max. temperature 1400 °C) is configured to permit pyrolysis of samples in different modes, such as with/without reactant gas and/or a catalyst, or under steam gasification conditions. Pyrolysis products are analysed online with Agilent GC/MS, which are injected via a heated transfer line (max. temperature 350 °C). Gas phase is analysed with CDS 5500 Fixed Gas Analyser.

Figure 3. Pyrolysis unit.

 

 

Figure 4. Instrument setup.

 

(3) Synthesis workstation METTLER-TOLEDO Optimax 1001 can be easily operated from - 40 to 180 °C with precise and programmable temperature control. An experimental configuration can be chosen from a wide range of different size reactors (250 ml, 500 ml and 1 L) and stirrers for process scalability. ReactIR 15, a real-time, in situ mid-infrared based system designed to study reaction progression and provide specific information about reaction initiation, conversion, intermediates and endpoint, is coupled with the synthesis workstation for in situ monitoring to track concentration changes of key reactive and transient organic species to understand mechanism pathway, determine kinetics and detect major reaction events. It is ideal for real-time process optimization. 

 

Figure 5. Optimax 1001

(4) Micromeritics ASAP (Accelerated Surface Area and Porosimetry System) 2020 is equipped with two independent vacuum systems - one for sample preparation and one for sample analysis. Having two separate systems, as well as separate preparation ports, allows sample preparation and sample analysis to occur concurrently. Inline cold traps are located between the vacuum pump and the manifold in both the analysis and the degas systems.

Figure 6. Micromeritics ASAP 2020

(5) Rayonet Photochemical Reactor RPR-208 completes with eight 254 nm or 300 nm U-shaped lamps. It has a 12” diameter centre opening in the top and bottom – vessels up to 12 inches in diameter can be used. The reactor can be used in vertical or horizontal position.

Figure 7. Rayonet Photochemical Reactor RPR-208

(6) Büchiglasuster - Jacketed pressure vessels, 5.0 L, max. 3 bar @200 °C with thermostat and stirrer drive (motor with speed transmission).

Figure 8. Büchiglasuster - Jacketed pressure vessels

(7) Two fume cupboards are configured with compressed air, low pressure N2, high pressure (60 bar) N2, H2, O2, CO and ethylene (others possible) gas lines. The open door gateways facilitate wheel-in/-out equipment for performing various experiments.

Figure 9. Fume cupboards configured with pressure control panels.

(8) Dedicated facilities for fluorine reactions, and handling facilities for cobalt trifluoride, sulphur tetrafluoride, hydrogen fluoride, etc..

Figure 10. Fume cupboards configured with F2 storage tanks for fluorination reactions.

(9) Dedicated high pressure laboratory comprising separate control room and 4 independent blast cells allows for the safe operation of high pressure vessels up to 5 L / 300 bar. The configured gas lines include high pressure N2, ethylene, H2/CO, and H2 (others possible). This facility has available a diverse range of pressure vessels, which permit, stirring, agitation, sampling and different construction materials.

Figure 11. Blast cell (left) and the control room (right).

Figure 12. Selection of high pressure vessels and sample cylinders available.

(10) General Support Facilities

Durham Chemistry Department has a wide variety of unique specialised and general research facilities (https://www.dur.ac.uk/chemistry/research/facilities/). These may be accessed through collaboration with CSCP. For further details and information please email Professor Andy Whiting(andy.whiting@durham.ac.uk) or Dr Phil Dyer (p.w.dyer@durham.ac.uk).

To contact ICRF for further information about its activities, possible collaborations, or access to research facilities, please email Dr Li Li at li.li2@durham.ac.uk.