Infrared spectrometer detectors

In the most general temis, an infrared spectrometer consists of a light source, a dispersmg element, a sample compartment and a detector. Of course, there is tremendous variability depending on the application. 

As in all Fourier transform methods in spectroscopy, the FTIR spectrometer benefits greatly from the multiplex, or Fellgett, advantage of detecting a broad band of radiation (a wide wavenumber range) all the time. By comparison, a spectrometer that disperses the radiation with a prism or diffraction grating detects, at any instant, only that narrow band of radiation that the orientation of the prism or grating allows to fall on the detector, as in the type of infrared spectrometer described in Section 3.6. 

One cm3 of the reactant/product/catalyst mixture was sampled periodically during the reaction for the transmission infrared analysis (Nicolet Magna 550 Series II infrared spectrometer with a MCT detector). The concentrations of reactants and products were obtained by multiplying integrated absorbance of each species by its molar extinction coefficient. The molar extinction coefficient was determined from the slope of a calibration curve, a plot of the peak area versus the number of moles of the reagent in the IR cell. The reaction on each catalyst was repeated and the relative error for the carbamate yield measured by IR is within 5%. 

Olsen, E. Serially interfaced gas chromatography/Fourier Transform infrared spectrometer/ion trap detector. Finnigan MAT IDT 35. 

We discussed the fundamentals of mass spectrometry in Chapter 10 and infrared spectrometry in Chapter 8. The quadrupole mass spectrometer and the Fourier transform infrared spectrometer have been adapted to and used with GC equipment as detectors with great success. Gas chromatography-mass spectrometry (GC-MS) and gas chromatography-infrared spectrometry (GC-IR) are very powerful tools for qualitative analysis in GC because not only do they give retention time information, but, due to their inherent speed, they are also able to measure and record the mass spectrum or infrared (IR) spectrum of the individual sample components as they elute from the GC column. It is like taking a photograph of each component as it elutes. See Figure 12.14. Coupled with the computer banks of mass and IR spectra, a component s identity is an easy chore for such a detector. It seems the only real... 

Both the GC-MS and GC-IR instruments obviously require that the column effluent be fed into the spectrometer detection path. For the IR instrument, this means that the IR cell, often referred to as a light pipe, be situated just outside the interferometer (Chapter 8) in the path of the light, of course, but it must also have a connection to the GC column and an exit tube where the sample may possibly be collected. The infrared detector is nondestructive. With the mass spectrometer detector, we have the problem of the low pressure of the mass spectrometry unit coupled with the ambient pressure of the GC column outlet. A special method is used to eliminate carrier gas while retaining sufficient amounts of the mixture components so that they are measurable with the mass spectrometer. 

Most standard infrared spectrometers currently operating in the mid-IR spectral region feature single element detectors. Exceptions are analyzers that are equipped with multiple detectors dedicated to single wave-... 

For qualitative analysis, two detectors that can identify compounds are the mass spectrometer (Section 22-4) and the Fourier transform infrared spectrometer (Section 20-5). A peak can be identified by comparing its spectrum with a library of spectra recorded in a computer. For mass spectral identification, sometimes two prominent peaks are selected in the electron ionization spectrum. The quantitation ion is used for quantitative analysis. The confinnation ion is used for qualitative identification. For example, the confirmation ion might be expected to be 65% as abundant as the quantitation ion. If the observed abundance is not close to 65%, then we suspect that the compound is misidentified. 

A mid-infrared absorption instrument generally consists of a Fourier transform design with the same basic components as noted above for the Fourier transform near-infrared spectrometers (broadband light source, Michelson interferometer, and detector optimized for the mid-infrared spectral region.)... 

A Fourier transform infrared spectrometer consists of an infrared source, an interference modulator (usually a scanning Michelson interferometer), a sample chamber and an infrared detector. Interference signals measured at the detector are usually amplified and then digitised. A digital computer initially records and then processes the interferogram and also allows the spectral data that result to be manipulated. Permanent records of spectral data are created using a plotter or other peripheral device. 

Principal component analysis is most easily explained by showing its application on a familiar type of data. In this chapter we show the application of PCA to chromatographic-spectroscopic data. These data sets are the kind produced by so-called hyphenated methods such as gas chromatography (GC) or high-performance liquid chromatography (HPLC) coupled to a multivariate detector such as a mass spectrometer (MS), Fourier transform infrared spectrometer (FTIR), or UV/visible spectrometer. Examples of some common hyphenated methods include GC-MS, GC-FTIR, HPLC-UV/Vis, and HLPC-MS. In all these types of data sets, a response in one dimension (e.g., chromatographic separation) modulates the response of a detector (e.g., a spectrum) in a second dimension. 

Auxiliary Instruments. Auxiliary instruments can be used on the fly as special detectors, or analytes can be trapped and taken to other instruments. Instruments that have been used with chromatography include the mass spectrometer (MS), the infrared spectrometer (IR), the nuclear magnetic resonance spectrometer (NMR), the polarograph, the fluorescence spectrophotometer, and the Raman spectrometer, among others. The two most popular ones are MS and IR, and they will be discussed in more detail in Chapter 11. In the beginning of this chapter we noted the utility iof GC/MS and LC/MS. 

Spectroscopic detectors measure partial or complete energy absorption, energy emission, or mass spectra in real-time as analytes are separated on a chromatography column. Spectroscopic data provide the strongest evidence to support the identifications of analytes. However, depending on the spectroscopic technique, other method attributes such as sensitivity and peak area measurement accuracy may be reduced compared to some nonselective and selective detectors. The mass spectrometer and Fourier transform infrared spectrometer are examples of spectroscopic detectors used online with GC and HPLC. The diode array detector, which can measure the UV-VIS spectra of eluting analytes is a... 

Fig. 7.1. Layout of the infrared spectrometer showing the Michelson Interferometer Optical System. An FTIR spectrometer s optical system requires two mirrors, an infrared light source, an infrared detector and a beamsplitter. The beamsplitter reflects about 50% of an incident light beam and transmits the remaining 50%. One part of this split light beam travels to a moving interferometer mirror, while the other part travels to the interferometer s stationary mirror. Both beams are reflected back to the beamsplitter where they recombine. Half of the recombined light is transmitted to the detector and half is reflected to the infrared source.

The method used to observe the infrared spectra of the deposits is relatively simple. The optics of a single-beam infrared spectrometer have been modified so that light from the Nernst filament is incident nearly normally on the drum and the light that is reflected directly from the surface of the drum is focused on the slit of the spectrometer. Because of the nature of the optics and the detector it is not feasible to divide the deposit into two bands as for the ultraviolet and visible spectra. Thus a blank run in which no alkali metal is deposited has to be made to provide a reference spectrum. 

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