Fourier transform IR instruments

In a Fourier transform IR instrument the principles are the same except that the monochromator is replaced by an interferometer. An interferometer uses a moving mirror to displace part of the radiation produced by a source (Fig. 5.4) thus producing an interferogram which can be transformed using an equation called the Fourier transform in order to extract the spectrum from a series of overlapping frequencies. The advantage of this technique is that a full spectral scan can be acquired in about 1 s compared to the 2-3 min required for a dispersive instrument... 

Fourier transform IR instruments contain no dispersing element, and all wavelengths are detected and measured simultaneously. Instead of a monochromator, an interferometer is used to produce interference patterns that contain the infrared spectral information. The. same types of sources used in dispersive instruments are used in FTIR spectrometers. Transducers are typically triglycine sulfate—a pyroelectric transducer—or mercury cadmium telluride—a photoconductive trans-... 

What are the major advantages of Fourier transform IR instruments over dispersive IR instruments ... 

There are a number of advantages to Fourier Transform IR instrumentation relative to dispersive IR instrumentation including ... 

Most modem IR facilities will use a Fourier Transform IR Spectrometer (FTIR), rather than a dispersive instrument. The essential feature is that all of the light from the source falls on to the detector at any instant, which thus leads to increased signal levels, thereby automatically improving the signal-to-noise ratio at all points on the spectrum. 

Different experimental approaches were applied in the past [6, 45] and in recent years [23, 46] to study the nature of the organic residue. But the results or their interpretation have been contradictory. Even at present, the application of modem analytical techniques and optimized electrochemical instruments have led to different results and all three particles given above, namely HCO, COH and CO, have been recently discussed as possible methanol intermediates [14,15,23,46,47]. We shall present here the results of recent investigations on the electrochemical oxidation of methanol by application of electrochemical thermal desorption mass spectroscopy (ECTDMS) on-line mass spectroscopy, and Fourier Transform IR-reflection-absorption spectroscopy (SNIFTIRS). 

The pharmaceutical industry comprises the largest segment, roughly 15 to 20%, of the infrared (IR) market. Modern mid-infrared instrumentation consists almost exclusively of Fourier transform (FT) instruments. Because of its ability to identify molecular species, FT-IR is routinely used as an identification assay for raw materials, intermediates, drug substances, and excipients. However, the traditional IR sample preparation techniques such as alkali halide disks, mulls, and thin films, are time-consuming and not always adequate for quantitative analysis. 

Figure 10.12—Sequence of events necessary to obtain a pseudo-double beam spectrum with a Fourier transform IR spectrometer. The instrument records and stores in its memory two spectra representing the variation of lu (blank) and / (sample) as a function of wavenumber (emission spectra 1 and 2 above). Then, it calculates the conventional spectrum, which is identical to that obtained on a double beam instrument, by calculating the ratio T — /// — f(A) for each wavenumber. Atmospheric absorption (CO2 and H20) is thus eliminated. The figure illustrates the spectrum of a polystyrene film.

One of the major advances in the past decade has been the maturation of the electronic revolution. This has had its effect on surface spectroscopy, with regard to instrumentation for transmission IR, but particularly for sensitivity gains that have made reflectance techniques the preferred alternative for fundamental studies. In the transmission mode, the commercial development of the Fourier transform IR spectrometer has led to significant advantages in the determination of the vibrational spectra of adsorbed species. This is covered in the chapter by Bell. 

Theories and instrumentation of Fourier transform IR spectroscopy and electron spectroscopy for chemical analysis are briefly reviewed. The possibility of using these techniques in detection and analysis of acid impurities distributed at surfaces of paper documents produced during the period from 1790 to 1983 is demonstrated. Results show that all of the papers tested contained carboxylic groups. The carboxylic acids found in the paper of 1790 are the results of oxidation and aging. Acids in other papers are due to fiber oxidation as well as the presence of rosin acids. These techniques show promise as nondestructive methods for elucidating chemical characteristics of surfaces of paper documents. 

Important to quality control are the comparison and confirmation of drug substance identity, excipients, and packaging components. Techniques such as Fourier transform IR (FTIR), attenuated total reflectance (ATR), NIR, Raman spectroscopy are used with increased regularity. The detection of foreign metal contaminants is essential with inductively coupled plasma spectroscopy (ICP), atomic absorption (AA), and X-ray fluorescence. Also notable is the increased attention to analysis of chiral compounds, as in the synthesis of drug substances. Optical rotation, ORD, and CD are currently the preferred instruments for this practice. The analytical techniques commonly used in the preformulation study are discussed in the following. 

The Fourier transform IR spectra were obtained on a Dlgllab Model 15B (Company or trade names are given for Information purposes only and their use does not Imply that the USDA recommends those products over others that may also be suitable.) with a Nova 3 computer, a TGS (trlglyclne sulfate) detector, a globar source and a KBr beam splitter. The Instrument was continuously purged with dry nitrogen. The following parameters were used to collect the... 

Nowadays, many analytical laboratories are equipped with an infrared (IR) and a Raman spectrometer, be it a dispersive device or a Fourier transform (FT) instrument. Raman and IR spectra provide images of molecular vibrations that complement each other and thus both spectroscopic techniques together are also called vibrational spectroscopy. The concerted evaluation of both spectra gives more information about the molecular structure than when they are evaluated separately. 

The history of investigation of the molecular surface chemistry of silica can be divided into three time periods. The period between 1960 and 1970 saw the introduction of IR spectroscopy and the use of chemical reactivity to follow reactions on a silica surface at a molecular level. The period between 1970 and 1980 was less active, but the advances in computer instrumentation that occurred in that decade (in particular Fourier transform IR and NMR spectroscopy) have led to the current revitalization of the subject. The chapters that follow will question some old interpretations and will reinterpret some old ideas. 

The most important metal-containing heat stabilizers in PVC can also be identified through IR-spectroscopy (see Section 8.2). Characteristic absorption bands for the salts of carboxylic acids are the bands of the ionized carboxy group in the region from 1590 to 1490 cm and from 1410 to 1370 cm Since the exact position of the absorption bands depends mainly on the metal counterions of the carboxy group, the IR-spectra provide a first identification of these metals. Tin stabilizers also show characteristic bands in these regions of the IR-spectrum. To determine the spectra, one uses pressed pellets made by finely grinding the sample material with potassium bromide. The identification of the metal becomes even more certain if an FT-IR (Fourier Transform/Infrared) instrument is available. With such an instrument, it is possible to subtract the spectrum of an additive-free... 

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