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    10
    Isobutane Dehydrogenation Activity Measure-
    ments. The isobutane dehydrogenation activity of the
    13.5CrAl catalyst was measured in a continuous flow
    reaction system consisting of a fixed-bed microreactor
    along with a Fourier transform infrared (FTIR) gas
    analyzer and a gas chromatograph (GC) for on-line
    product analysis. The activity measurements were car-
    ried out at 580 °C under atmospheric pressure. The
    catalyst was heated to the reaction temperature under
    5% O2/N2 (AGA, air 99.99%, N2 99.999%). Nitrogen used
    in the experiments was purified with Oxisorb (Messer
    Griesheim GmbH).
    In the dehydrogenation experiments aimed to com-
    pare the behavior of calcined and prereduced chromia/
    alumina, the reduction of the catalyst (0.2 g) was
    accomplished either during the first minutes on isobu-
    tane stream or during a 30 min prereduction with 10%
    H2/N2 (H2, AGA 99.999%) or 5% CO/N2 (CO, Messer
    Griesheim GmbH, 99.997%). Dehydrogenation was car-
    ried out for 15 min using isobutane feed (AGA 99.95%)
    with a weight hourly space velocity (WHSV) of 5 h 1
    and diluted with nitrogen at a molar ratio of 1:9. After
    the dehydrogenation, the catalyst was flushed with
    nitrogen and regenerated with diluted air. The reduc-
    tion and regeneration productsscarbon oxides and
    waterswere measured by FTIR. The dehydrogenation
    products were monitored by FTIR for the first 6 min on
    stream, a GC sample was taken after 10 min, and the
    FTIR analysis was then continued. In selected measure-
    ments the catalyst was regenerated directly after the
    prereduction without implementing the dehydrogena-
    tion stage.
    The amount of coke as a function of time on isobutane
    stream was measured for a hydrogen-prereduced cata-
    lyst (0.1 g, 15-min prereduction with 10% H2/N2). The
    isobutane flow with a WHSV of 30 h 1 was diluted with
    nitrogen at a molar ratio of 1:1. Dehydrogenation was
    carried out for 2, 5, 10, or 15 min and was followed with
    the FTIR. The amount of coke deposited on the catalyst
    during dehydrogenation was calculated from the amounts
    of carbon oxides measured by FTIR during regeneration.
    The gaseous products were analyzed on-line with a
    Gasmet FTIR gas analyzer (Temet Instruments Ltd.)
    equipped with a Peltier-cooled mercury cadmium
    telluride detector and with an HP 6890 gas chromato-
    graph equipped with an HP PLOT/Al2O3 “M” column
    and a flame ionization detector. The FTIR spectra were
    recorded in the wavenumber range of 4000 850 cm 1
    with a resolution of 8 cm 1 and a scanning rate of 10
    scans/s. The analysis cuvette (9 cm3) was maintained
    at constant temperature (180 °C) and pressure (103
    kPa). The spectra were measured every 2 s during the
    first 2 min on stream, every 5 s during the next 2 min,
    and thereafter every 30 or 60 s. Further details of the
    FTIR gas analysis method and of the determination of
    the product distribution based on the measured spectra
    can be found elsewhere.
    9,17 The conversions, selectivi-
    ties, and yields were calculated on a molar basis.
    In Situ DRIFTS-MSMeasurements. The formation
    of hydroxyl and carbon-containing species during cata-
    lyst reduction and isobutane dehydrogenation was
    studied by in situ DRIFTS combined with MS. The
    DRIFTS measurements were performed using a Nicolet
    Nexus FTIR spectrometer and a Spectra-Tech high-
    temperature/high-pressure reaction chamber. Gaseous
    products were monitored on-line by a Pfeiffer Vacuum
    OmniStar mass spectrometer. Nitrogen used in the
    measurements was purified with Oxisorb (Messer-
    Griesheim GmbH).
    Isobutane dehydrogenation was investigated as a
    function of time on stream at 580 °C for the three
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