Fourier transform near-infrared spectrometer

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.)... 

Fourier transform near-infrared (FT-NIR) spectrometers produce reflection spectra by moving mirrors. Once plagued by noise, modern FT-NIR spectrometers boast noise levels equivalent to grating-based instruments. FT-NIR spectrometers are full-spectrum instruments. 

Fourier Transform-Near infrared (FT-NiR). Only within the last 20 years has FT-NIR instrumentation (Fig. 4.1.14) become available. Even then, the first commercial instmments had a distinct disadvantage compared to grating-based scanning instruments. FT-NIR spectrometers employ an entirely different method for producing spectra. There is no dispersion involved. Energy patterns set up by an interaction with a sample and a reference and moving mirrors (or other optical components) produce sample and reference interferograms that are used to calculate the absorbance spectrum of the sample. 

Figure 4.1.14. The Bruker Matrix-E, a Fourier transform near-infrared (FT-NIR) spectrometer (Bruker Optics Inc., 19 Fortune Drive, Manning Park, BiUerica, MA 01821-3991) (A) illustrating the noncontact measuring concept and (B) mounted for analyzing sugarcane pulp passing underneath.

NIR reflectance spectra were collected using a Laser Precision PCM 4000 Fourier transform near-infrared (FT-NIR) spectrometer, equipped with CaF beam splitters and a thermoelectrically cooled PbSe detector. An Axiom difftise/specular reflectance attachment, set at 15" C, was used to collect the reflectance spectrum from each sample coupon. Each sample spectrum was the result of a 5 scan... 

An alternative approach for NIR hyperspectral imaging to the one described earlier is to use a Fourier transform near-infrared (FT-NIR) spectrometer. Since the design of FT-NIR microspectrometer is more similar to that of instruments... 

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. 

For radiofrequency and microwave radiation there are detectors which can respond sufficiently quickly to the low frequencies (<100 GHz) involved and record the time domain specttum directly. For infrared, visible and ultraviolet radiation the frequencies involved are so high (>600 GHz) that this is no longer possible. Instead, an interferometer is used and the specttum is recorded in the length domain rather than the frequency domain. Because the technique has been used mostly in the far-, mid- and near-infrared regions of the spectmm the instmment used is usually called a Fourier transform infrared (FTIR) spectrometer although it can be modified to operate in the visible and ultraviolet regions. 

Principles and Characteristics Both mid-IR (2.5-50 p.m) and near-IR (0.8-2.5 p.m) may be used in combination to TLC, but both with lower sensitivity than UV/VIS measurements. The infrared region of the spectrum was largely ignored when the only spectrometers available were the dispersive types. Fourier-transform instruments have changed all that. Combination of TLC and FTIR is commonly approached in two modes ... 

Fig. 26 Fourier transform spectrum of v2 of ammonia. Trace (a) is a section of the infrared absorption spectrum of ammonia recorded on a Digilab Fourier transform spectrometer at a nominal resolution of 0.125 cm-1. In this section of the spectrum near 848 cm-1 the sidelobes of the sine response function partially cancel, but the spectrum exhibits negative absorption and some sidelobes. Trace (b) is the same section of the ammonia spectrum using triangular apodiza-tion to produce a sine-squared transfer function. Trace (c) is the deconvolution of the sine-squared data using a Jansson-type weight constraint.

D Commercial COTS controlled by external computer Hybrid systems such as automated dissolution workstation with high-performance liquid chromatography (HPLC) or ultraviolet-visible (UV-Vis) interface Liquid chromatographs, gas chromatographs, UV/Vis spectrophotometers, Fourier transform infrared (FTIR) spectrophotometers, near-infrared (NIR) spectrophotometers, mass spectrometers, atomic absorption spectrometers, thermal gravimetric analyzers, COTS automation workstations... 

Infrared analyses are conducted on dispersive (scanning) and Fourier transform spectrometers. Non-dispersive industrial infrared analysers are also available. These are used to conduct specialised analyses on predetermined compounds (e.g. gases) and also for process control allowing continuous analysis on production lines. The use of Fourier transform has significantly enhanced the possibilities of conventional infrared by allowing spectral treatment and analysis of microsamples (infrared microanalysis). Although the near infrared does not contain any specific absorption that yields structural information on the compound studied, it is an important method for quantitative applications. One of the key factors in its present use is the sensitivity of the detectors. Use of the far infrared is still confined to the research laboratory. 

Advantages of Fourier transform infrared spectrometers are so great that it is nearly impossible to purchase a dispersive infrared spectrometer. Fourier transform visible and ultraviolet spectrometers are not commercially available, because of the requirement to sample the interferometer at intervals of S = l/(2Av). For visible spectroscopy, Av could be 25 000 cm 1 (corresponding to 400 nm), giving S = 0.2 im and a mirror movement of 0.1 xm between data points. Such fine control over significant ranges of mirror motion is not feasible. 

Near-infrared spectra were collected with a Nicolet 670 Nexus Fourier transform (FT) spectrometer.6 Solutions were thermally equilibrated at 37.0 0.1 °C prior to collecting spectra. The following two unique sets of near-infrared spectra were collected (1) first-overtone spectra (6500-5500 cm-1) with a 7.5 mm optical path length and (2) combination spectra (5000-4000 cm-1) with a 1.5 mm optical path length. Single-beam spectra were collected in triplicate as 256 coadded interfero-grams that were Fourier transformed to produce spectra with 1.94 cm-1 point spacing. 

The photograph presented in Figure 13.10 shows a typical interface used to collect these noninvasive spectra. Light is incident on one side of the skinfold and a fraction of the transmitted light is collected directly from across the input fiber. Bundles of low-hydroxy silica fibers are used to deliver and collect the near-infrared radiation for the measurement. For the experiments described here, the noninvasive spectra were collected with a Fourier transform spectrometer set for a resolution of 16 cm-1 and 128 coadded interferograms. Each recorded spectrum required approximately 60 s to acquire and save. A total of 370 spectra were collected over a period of nearly 7h while in vivo glucose concentrations varied from 6 to 33 mM (108-594 mg/dL). 

Automation 6 [A 6] Micro Fabricated Near-infrared Fourier Transform Spectrometer... 

A miniaturized Fourier transform spectrometer for near-infrared measurements (FTIR, 2500-8330 nm) was developed at the Forschungszentrum Karlsruhe [120], Near-infrared measurements give information, for example, about the oil, water and protein content of liquids or solids. The dimensions of the detector chip are 11.5 x 9.4 mm, the device is essentially a miniaturized Michelson interferometer and it consists of a micro optical bench with beamsplitter, ball lenses, mirrors and the detector chip. The light beam is coupled in via a glass-fiber and an electromagnetic actuator. The signal is derived from the signal response of the detector by Fourier transformation. 

There is a real chance of a breakthrough of Raman spectroscopy in routine analytics. Excitation of Raman spectra by near-infrared radiation and recording with interferometers, followed by the Fourier transformation of the interferogram into a spectrum -the so-called NIR-FT-Raman technique - has made it possible to obtain Raman spectra of most samples uninhibited by fluorescence. In addition, the introduction of dispersive spectrometers with multi-channel detectors and the development of several varieties of Raman spectroscopy has made it possible to combine infrared and Raman spectroscopy whenever this appears to be advantageous. 

The Raman spectrum of gases can now also be recorded with Fourier-Transform Raman spectrometers with near infrared excitation (Dyer and Hendra, 1992). Fig. 4.3-19 shows a survey spectrum of air obtained in 4 hours of sampling time (Bruker, 1993). The region of the rotational spectrum is presented on an expanded scale in Fig. 4.3-20, it can be compared with Fig. 4.3-18. The intensities of the lines below about 80 cm are weakened by the Rayleigh line suppression filter and the resolution is limited to 1 cm", mainly by the laser used for excitation. 

Major technological and scientific innovation in the past 10 to 15 years has significantly broadened the applicability of Raman spectroscopy, particularly in chemical analysis. Fourier transform (FT)-Raman, charge-coupled device (CCD) detectors, compact spectrographs, effective laser rejection filters, near-infrared lasers, and small computers have contributed to a revolution in Raman instrumentation and made routine analytical applications possible. An increase in instrumental sensitivity by factors as large as 10, plus decreases in both interferences and noise resulted from this revolution. The number of vendors of Raman spectrometers increased from 3 to 12 over a 10-year period, and integrated commercial spectrometers led to turnkey operation and robust reliability. 

The most attractive sensors now being developed are the Fourier transform infrared spectrometer (FTIR) and the near-infrared (NIR) spectrometer for the on-line measurement of composition changes in complex media during cultivation. The FTIR measurements are based on the type and quantities of infrared radiation that a molecule absorbs. The NIR measurements are based on the absorption spectra following the multi-regression analyses. These sensors are not yet available for fermentation processes. 

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