Fourier transform infrared spectroscopic detector

Detection in SFC can be achieved in the condensed phase using optical detectors similar to those used in liquid chromatography or in the gas phase using detectors similar to those used in gas chromatography. Spectroscopic detectors, such as mass spectrometry and Fourier transform infrared spectroscopy, are relatively easily interfaced to SFC compared to the problems observed with liquid mobile phases (see Chapter 9). The range of available detectors for SFC is considered one of its strengths. 

Miniaturized chemical analysis systems have been developed for most macroscopic counterparts (Dittrich et al. 2006). The availability of optical fibers, light sources, and detectors in the visible UV and near-infrared (NIR) wavelengths makes it possible to integrate spectroscopic measurements in microreactors (Lobbecke et al. 2005). Fourier transform infrared spectroscopy (FTIR) is an efficient, broadly applicable... 

Several researchers have combined the separating power of supercritical fluid chromatography (SFC) with more informative spectroscopic detectors. For example, Pinkston et. al. combined SFC with a quadrupole mass spectrometer operated in the chemical ionization mode to analyze poly(dimethylsiloxanes) and derivatized oligosaccharides (7). Fourier Transform infrared spectroscopy (FTIR) provides a nondestructive universal detector and can be interfaced to SFC. Taylor has successfully employed supercritical fluid extraction (SFE)/SFC with FTIR dectection to examine propellants (8). SFC was shown to be superior over conventional gas or liquid chromatographic methods. Furthermore, SFE was reported to have several advantages over conventional liquid solvent extraction (8). Griffiths has published several... 

It is clear that the introduction of the IR FPA detector has brought Fourier transform infrared (FTIR) microscopy with a thermal source to a new and exciting stage of development. This is illustrated in the other chapters of this volume. Our purpose in this chapter is to address how IR FPA technology could be combined with the synchrotron source to advance IR spectroscopic imaging in ways that would prove quite difficult with a conventional thermal source. To address this question, we will need to understand the detailed nature of the synchrotron IR source, the optical... 

An integrated GC/IR/MS instrument is a powerful tool for rapid identification of thermally generated aroma compounds. Fourier transform infrared spectroscopy (GC/IR) provides a complementary technique to mass spectrometry (MS) for the characterization of volatile flavor components in complex mixtures. Recent improvements in GC/IR instruments have made it possible to construct an integrated GC/IR/HS system in which the sensitivity of the two spectroscopic detectors is roughly equal. The combined system offers direct correlation of IR and MS chromatograms, functional group analysis, substantial time savings, and the potential for an expert systems approach to identification of flavor components. Performance of the technique is illustrated with applications to the analysis of volatile flavor components in charbroiled chicken. 

The ultimate selectivity of gas chromatography is determined by the detector. The most selective detectors are spectroscopic, such as Fourier-Transform Infrared or Mass Spectrometer. Automated systems can employ chemometric algorithms to discriminate unresolved chromatographic peaks. These combinations are expensive and require significant computer support. As such, they are more likely to be used in a laboratory for confirmation. Efforts to convert this approach to field units are still under development. The MiniCAMS described above, based on a FPD is a reliable monitor but requires 3-5 min to make a determination. Gas chromatographs also require a source of purified gas for operation and the flame detector requires additional hydrogen and air for operation. This device will have the fewest false positives and the most... 

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. 

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... 

Improvements in column technology, detector sensitivity and the development of new detection systems, have made possible the routine separation of picomole quantities of nucleic acid components in complex physiological matrices. The very sensitivity of most LC systems, however, which is invaluable in the analysis of biological samples, is often the limiting factor because of inadequate or ambiguous identification methods. Although tremendous advances have been made in the on-line combination of HPLC with spectroscopic techniques [e.g., mass spectrometry, Fourier transform infrared (FT/IR), nuclear magnetic resonance], their application has not become routine in most biochemical and biomedical laboratories. 

Spectroscopic methods, such as fluorescence recovery and quenching, Fourier-transform infrared spectroscopy (FT-IR), and light reflection technique have been used for studies of adsorbed proteins (for example Burghardt Axelrod 1981, Thompson et al. 1981, van Wagenen et al. 1982), and surfactant adsorption layers (for example Ldsche et al. 1983, L6sche Mohwald 1989, Daillant et al. 1991, Henon Meunier 1992, Mohwald 1993). Considerable progress has been made in recent years with respect to the sensitivity of detectors and the efficiency of computers, so that the power of these methods has increased remarkably. 

Infrared spectroscopy is probably the most widespread analytical spectroscopic technique for identification and characterization of organic compounds. Because of this identification capability infrared spectroscopy is desirable as a detection technique for chromatographic separations. With the advent of Fourier transform infrared spectroscopy/ the speed and sensitivity of infrared detection is greatly enhanced making such applications feasible. FT-IR detection has been widely accepted as a detector for gas chromatography (GC/FT-IR) (1) and has been applied with limited success to liquid chromatography (LC/FT-IR) (2)/ and more recently to supercritical fluid chromatography (SFC/FT-IR) (3). The recent review articles cited here provide excellent introduction and references to current state-of-the-art in these areas. 

The selective detectors discussed in the previous sections often do not provide enough information to elucidate with 100% probability the nature of the eluting solutes. For this reason, data with selective detectors can be erratic. The future in this respect definitely belongs to the spectroscopic detectors that allow. selective recognition of the separated compounds. Today, the hyphenated techniques CGC-mass spectroscopy (CGC-MS), CGC-Fourier transform infrared spectroscopy (CGC-FTIR), and CGC-atomic emission detection (CGC - AED) are the most powerful analytical techniques available. They provide sensitive and selective quantitation of target compounds and structural elucidation or identification of unknowns. The applicability and ease of use of the hyphenated techniques were greatly increased by the introduction of fused silica wall coaled open tubular columns. The main reason for this is that because of the low flows of capillary columns, no special interfaces are required and columns are connected directly to the different spectrometers. The introduction of relatively inexpensive benchtop hyphenated systems has enabled many laboratories to acquire such instrumentation, which in turn has expanded their applicability ever further. 

Spectroscopic techniques used in essential oil analysis comprise ultraviolet and visible spectrophotometry, infrared spectrophotometry (IR), mass spectrometry (MS), and nuclear magnetic resonance spectroscopy (NMR), including the following H-NMR, C-NMR, and site-specific natural isotope fractionation NMR. Combined techniques (hyphenated techniques) employed in essential oil analysis are GC/MS, liquid chromatography/mass spectrometry, gas chromatography/Fourier transform infrared spectrophotometry (GC/FT-IR), GC/FT-IR/MS, GC/atomic emission detector, GC/isotope ratio mass spectrometry, multidimensional GC/MS. 

Lewis, E. N., Treado, R J., Reeder, R. C. et al. (1995) Fourier transform spectroscopic imaging using an infrared focal-plane array detector. Anal. Chem. 67, 3377-81. 

Bhargava, R. and Levin, I.W. (2005) Fourier transform mid-infrared spectroscopic imaging, Ch. 1 in Spectrochemical Analysis Using Infrared Multichannel Detectors (eds R. Bhargava and I.W. Levin), Blackwell Publishing Ltd, Oxford, UK, pp. 1-24. 

Fourier transform mid-infrared (FTIR), near-infrared (FTNIR), and Raman (FT-Raman) spectroscopy were used for discrimination among 10 different edible oils and fats, and for comparing the performance of these spectroscopic methods in edible oil/fat studies. The FTIR apparatus was equipped with a deuterated triglycine sulfate (DTGS) detector, while the same spectrometer was also used for FT-NIR and FT-Raman measurements with additional accessories and detectors. The spectral features of edible oils and fats were studied and the unsaturation bond (C=C) in IR and Raman spectra was identified and used for the discriminant analysis. Linear discriminant analysis (LDA) and canonical variate analysis (CVA) were used for the disaimination and classification of different edible oils and fats based on spectral data. FTIR spectroscopy measurements in conjunction with CVA yielded about 98% classification accuracy of oils and fats followed by FT-Raman (94%) and FTNIR (93%) methods however, the number of factors was much higher for the FT-Raman and FT-NIR methods. 

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