Fourier transform infrared sample compartment

Figure 20-29 Fourier transform infrared spectrum of polystyrene film. The Fourier transform of the background interferogram gives a spectrum determined by the source intensity, beamsplitter efficiency, detector response, and absorption by traces of H20 and C02 in the atmosphere. The sample compartment is purged with dry N2 to reduce the levels of H20 and C02. The transform of the sample interferogram is a measure of all the instrumental factors, plus absorption by the sample. The transmission spectrum is obtained by dividing the sample transform by the background transform.

The next class of VCD instruments to be developed was centered around a Fourier transform infrared (FT-IR) spectrometer. The idea was to design the sample compartment to be the same as in a dispersive VCD instrument, including a photoelastic modulator. To measure VCD, the detector signal is first sent to a lock-in amplifier to demodulate the high-frequency polarization modulation. The output of the lock-in is a VCD interferogram which is Fourier transformed in much the same way as the ordinary transmission interferogram. 

All activity measurements were conducted in an in-situ infrared reactor cell placed in the sample compartment of a DIGILAB 15C Fourier Transform Infrared (FTIR) Spectrometer. The reactor, described in detail elsewhere [11], consisted of two aluminum flanges with CaF2 IR transparent windows, a gas inlet and outlet, and two foil fast response thermocouples which were placed in direct contat with the catalyst. The reactor temperature was maintained constant by external heaters controlled by a temperature programmed controller. A Teflon coated recycle pump permitted to maintain near isothermal conditions and improve the mixing in the reactor. The reactor and associated lines were tested for activity at the highest temperature used, and it was found to have negligible activity. 

In many studies, particularly those related to materials and forensic science, it is frequently necessary to measure a mid-infrared spectrum from a trace amount of a sample or a sample of small size. In some circumstances, this may be accomplished by using a beam-condenser accessory within the conventional sample compartment of a Fourier-transform infrared (FT-IR) spectrometer. Perhaps today though, it is more convenient to use infrared microspectrometry (often commonly referred to as infrared microspectroscopy or even infrared microscopy). Based on an optical microscope (or infrared microscope) coupled to an FT-IR spectrometer, it is one of the most useful methods for structural analysis of such samples and can often be undertaken in a non-destructive manner [1, 2]. 

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