Facilities

The newly refurbished £1,000,000 laboratory has eight fume-cupboards paired in four bays, two of which are walk-in. There is ample bench and storage space with each fume-cupboard and additional bench top space running the entire length of the lab. The fume-cupboard bays have ventilated gas cylinder cabinets with a capacity for five L size gas cylinders. The rear of the lab has a well equipped workspace for such tasks as reactor assembly and disassembly and basic metalworking. Deionised water is available on demand. For safety, gas alarms for carbon monoxide, hydrogen and methane are also fitted. The laboratory is prepared for a huge variety of tasks. Our range of equipment includes:

  • Microreactor Mass Spectrometer System (Hiden CatLab)
  • Electrochemical Measurement Apparatus
  • Gas Analysis Equipment
  • Surface Area and Porosimetry Measurement Apparatus
  • High Temperature Furnaces
  • Apparatus for Pulse Isotopic Exchange (PIE) Measurements
  • Automatic Press
  • Gas Flow Control
  • Reactor Systems

Hiden CATLAB
    A fully automated microreactor-mass spectrometer system from Hiden, designed for the testing of catalysts at temperatures up to 1000°C under flowing gas conditions.  The system has an online mass spectrometer (QIC-20) to constantly monitor changes in the gas composition in real time.  The software allows for the programming of large numbers of sequences of experimental conditions i.e. temperature changes, variable gas compositions and gas flow rates so that kinetic data and complicated TPD, TPO and TPR cycles can be performed. For more information from the manufacturer click here.
     

 

 Potentiostat/Galvanostats

 

 

 

For in-situ solid-state electrochemistry measurements, four sets of potentiastat galvanostat and frequency response analysers- (PGSTAT-FRA) systems are available. These are provided by Ivium (Compactstat) and Amel (7050 PGSTAT). These system allows us to conduct different electrochemical experiments, such open-circuit voltage (OCV) measurements, solid electrolyte cyclic voltammetry (SECV), current-voltage (I-V) curves and AC impedance spectrometry. They are software driven and the collected data can be exported into other plotting software as required. Combined with the analytical equipment available in the lab the electrochemical equipment available is a very powerful tool for work on electrocatalysis and Solid Oxide Fuel Cells.

For more information from the manufacturers click here (Ivium) and here (AMEL).

 

Gas analysis

Our work mostly involves  gas phase reactions and inlet and outlet analysis of light hydrocarbon, carbon and nitrogen oxides and permanent gases is routinely performed. Our lab is equipped with five gas chromatographs (GC), four mass spectrometers (MS), two CO/CO2 infra-red analysers, one low concentration quantum cascade laser CO2 analyser, one NOx analyser and four hygrometers.

 Gas chromatography

 

 

 

The laboratory is equipped with three Varian (now Agilent) CP-3800 and two Varian CP-3900 GCs. The systems are automated and data is collected using Varian’s GC Star software. Two of the units (CP-3800) have series-bypass capability and are equipped with molecular sieve 5A and Haysep Q columns, two detectors, thermal conductivity (TCD) and flame ionisation (FID) are installed. The other units are simpler, it has one column (molsieve 5A, or Shincarbon) and a TCD.  GC calibration is done using standards supplied by STG gasses.  Click here for more information from the manufacturer.

 

 Mass Spectrometry

 

 

Two Cirrus quadrupole mass spec’ portable bench top unit from MKS is ranged to 200 atomic mass units. The unit is sensitive, with a detection limit down to 100 ppb and a maximum data collection speed of 150 points per second. The units are fully automated and driven by Process Eye Professional™ software. For more information, click here. In addition, we have two Hiden quadrupole MS Units, a QIC-20 and a QGA. Both units are controlled by the MasSoft software. For more information from the manufacturer, click here.

 

Continuous single-gas analysis

We have a Rosemount BINOS 100 dual channel infra-red detector to detect carbon dioxide (0 to 1%) and carbon monoxide (0 to 10%). The channels are calibrated using single component carbon dioxide (1%) and carbon monoxide (10%) gasses. We also have two Emerson X-tream continuous gas analysers, one for CO2 analysis (0-1%) and one for NOx (NO 0-3000ppm, NO2 0-500ppm and N2O 0-3000ppm) analysis. The output from these analysers can be monitored in real time over long periods of time. The data is recorded by a data logger interfaced with a PC. These instruments are often used in conjunction with a GC. For more information, click here.

Quantum Cascade Laser CO2 Analyser

A CO2 sensor based upon a quantum cascade, built in Manchester University is available in the lab. The CO2 sensor has been developed for measurements of CO2 concentrations in gas flows and based upon direct absorption spectroscopy with a single-pass 54.2-cm long optical cell and a thermoelectrically cooled distributed feedback quantum cascade laser (QCL) (LC0246, Hamamatsu) emitting at 2305 - 2310 cm–1. Typical CO2 limit of detection (signal-to-noise ratio = 1) is about 36 – 42 ppb for averaging within 0.1 s. CO2 minimum precision of 24-26 ppb was demonstrated at 4-10 averaging of successive CO2 measurements in 2-12 ppm CO2 gas flows. This sensor was developed in Manchester University as part of a collaborative project on ‘Spillover processes on micro- and nano-structured catalysts

Hygrometer

For accurate determination of the water content in the product gas stream a chilled mirror hygrometer, model CMH-1, supplied by Alpha Moisture Systems is employed. The unit has a three-stage flow through dew point sensors allowing accurate water content detection from -75°C to 100°C with an accuracy of ±0.5% of the full scale pressure. Our laboratory is also equipped with a further three HMT337 Vaisala hygrometers. The dew-point temperature range for these units is -75-100 °C.

 BET apparatus

 

 

 

The laboratory is fitted with a specific surface area, pore size and pore volume measurements equipment supplied by COULTER. The gas sorption method is used by the analyzer. Nitrogen and other inert gas may be used. The method may be defined as the physical characterisation of material structures using a process where gas molecule of known size are condensed or adsorbed on unknown samples surfaces. The BET calculation is the model used for the determination of the sample specific surface area, while BJH calculation yields the pore size distribution.

 Furnaces

 The mixed metal oxide powders are formed into disc membranes by afully automated Atlas T25 uniaxial press and densification achieved by sintering in a Lenton tube furnace rated to 1600°C. The furnace has an eight segment Eurotherm 2416 controller for temperature programming. The lab has an array of tube furnaces of different sizes made by Vecstar furnaces and Lenton to meet the needs for the particular reactor system. All are equipped with eight segment Eurotherm 2416 controllers and rated to 1200°C. Three of the furnaces are split to allow easy placement and removal of particularly cumbersome reactors. There are also two box furnaces rated to 1200°C and 1600°C with a larger heating cavity for heat treating bulkier samples.

   

 

 

 

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