Diffuse reflectance FT-IR spectroscopy

Hartauer KJ, Guilroy JK. A comparison of diffuse reflectance FT-IR spectroscopy and DSC in the characterization of a drug-excipient interaction. Drug Dev Ind Pharm 1991 17 617-630. 

IR spectroscopy has been utilized to measure methocarbamol and ethoxybenzamide in pharmaceutical preparations15 and diffuse reflectance FT-IR for direct analysis of methocarbamol tablets16. 

This study was prompted by a report on the rapid determination of lignocellulose by diffuse reflectance Fourier transform infrared reflectance (FT/IR) spectroscopy [1]. Although the results of that study were good, the claims by the promoters of near-infrared (NIR) instrumentation suggested that the latter might produce equally good results in less time and with less sample preparation. 

However, the improved sensitivity of FT-IR allows one to obtain better sensitivity using the conventional sampling accessories and expand the range of sampling techniques. Emission, diffuse reflectance and photoacoustic spectroscopy represent new areas where FT-IR reduces the difficulty of the techniques considerably. Greatly improved results are also achievable from reflection spectroscopy. Special effects such as vibrational circular dichroism can be observed using FT-IR instrumentation. 

The direct measurement of the various important parameters of foam films (thickness, capillary pressure, contact angles, etc.) makes it possible to derive information about the thermodynamic and kinetic properties of films (disjoining pressure isotherms, potential of the diffuse electric layer, molecular characteristics of foam bilayer, such as binding energy of molecules, linear tension, etc.). Along with it certain techniques employed to reveal foam film structure, being of particular importance for black foam films, are also considered here. These are FT-IR Spectroscopy, Fluorescence Recovery after Photobleaching (FRAP), X-ray reflectivity, measurement of the lateral electrical conductivity, measurement of foam film permeability, etc. 

Binary copper-based catalysts were prepared by coprecipitation method and some components were added as promoters into the binary catalysts. The methanol synthesis reaction was carried out in a continuous flow microreactor operated at 22 atm and at various temperatures. Reaction pathway of the methanol synthesis was investigated through FT-IR spectroscopy. For the catalyst with a copper content over 15wt%, the diffuse reflectance method (DRIFT) was applied, but for fee catalyst wife a copper content of 7wt%, the transmission teclmique was used. For more information about intermediates, TPD of adsorbed methanol was carried out and the products were analyzed using mass spectrometer. 

We therefore here describe the realisation of our development of diffuse reflectance/absorbance FT-IR spectroscopy as a quantitative tool for the rapid analysis of all samples of biotechnological and other interest, specifically by exploiting the ability of modem, supervised learning methods to take multivariate spectral inputs and map them directly to the concentration of one or more target determinands (see above and [70]), using as before [46] mainly mixtures of ampicillin and E. coli as a model system. 

Surface composition and morphology of copolymeric systems and blends are usually studied by contact angle (wettability) and surface tension measurements and more recently by x-ray photoelectron spectroscopy (XPS or ESCA). Other techniques that are also used include surface sensitive FT-IR (e.g., Attenuated Total Reflectance, ATR, and Diffuse Reflectance, DR) and EDAX. Due to the nature of each of these techniques, they provide information on varying surface thicknesses, ranging from 5 to 50 A (contact angle and ESCA) to 20,000-30,000 A (ATR-IR and EDAX). Therefore, they can be used together to complement each other in studying the depth profiles of polymer surfaces. 

Figure 5.11 Diffuse Reflectance Absorbance Spectroscopy Taking In Chemometiics (DRASTIC), a FT-IR-based method for rapid screening for metabohtes. Different concentrations of ampicillin (ranging from 0 to 5 mg/mL) were mixed with a constant amount E. coli cells, dried and analyzed by FT-IR (Winson et at, 1997).

All of the usual sampling techniques used in infrared spectroscopy can be used with FT-IR instrumentation. The optics of the sampling chamber of commercial FT-IR instruments are the same as the traditional dispersive instruments so the accessories can be used without modification for the most part. To make full use of the larger aperature of the FT-IR instrument, some accessories should be modified to accomodate the larger beam. The instrumental advantages of FT-IR allow one to use a number of sampling techniques which are not effective using dispersive instrumentation. Transmission, diffuse reflectance and internal reflectance techniques are most often used in the study of epoxy resins. 

Abstract—This study extends previous work on silanized kaolin clays to other substrates, such as aluminum hydroxide. It will also show that high precision quantitative Fourier Transform Infrared Spectroscopy (FT-IR) diffuse reflectance measurements can be performed on this vinyl silanized substrate and predict that other silanized finely divided powders can be analyzed using these techniques. 

FT-IR diffuse reflectance measurements have been used to quantitatively determine the amount of silane deposited on a substrate. The advantages of FT-IR are speed and sensitivity, the latter relating to the ultimate analytical precision or the smallest amount of the analyte one can determine. Other classical uses of infrared spectroscopy are as a qualitative identification or structure elucidation tool. 

The feasibility of diffuse reflectance NIR, Fourier transform mid-IR and FT-Raman spectroscopy in combination with multivariate data analysis for in/ on-line compositional analysis of binary polymer blends found in household and industrial recyclates has been reported [121, 122]. In addition, a thorough chemometric analysis of the Raman spectral data was performed. 

There are several major areas of interfacial phenomena to which infrared spectroscopy has been applied that are not treated extensively in this volume. Most of these areas have established bodies of literature of their own. In many of these areas, the replacement of dispersive spectrometers by FT instruments has resulted in continued improvement in sensitivity, and in the interpretation of phenomena at the molecular level. Among these areas are the characterization of polymer surfaces with ATR (127-129) and diffuse reflectance (130) sampling techniques transmission IR studies of the surfaces of powdered samples with adsorbed gases (131-136) alumina(137.138). silica (139). and catalyst (140) surfaces diffuse reflectance studies of organo- modified mineral and glass fiber surfaces (141-143) metal overlayer enhanced ATR (144) and spectroelectrochemistry (145-149). 

Kell DB, Winson MK, Goodacre R, Woodward AM, Alsberg BK, Jones A, Timmins EM, Rowland JJ (1998) DRASTIC (Diffuse Reflectance Absorbance Spectroscopy Taking In Chemometrics). A novel, rapid, hyperspectral, FT-IR-based approach to screening for biocatalytic activity and metabolite overproduction. In Kieslich K (ed) New Frontiers in Screening for Microbial Biocatalysts. Elsevier Science B. V., The Netherlands, p 61... 

T. Chopin and E. Whalen, A new and rapid method for carrageenan identification by FT IR diffuse reflectance spectroscopy directly on dried, ground algal material, Carbohydr. Res., 246 (1993) 51-59. 

Diffuse Reflectance Infrared Fourier Transform Spectroscopy (DR I FT). When IR radiation is directed onto the surface of a solid sample, two types of energy reflectance can occur specular and diffuse. The specular component is the radiation that reflects directly off the sample surface (i.e., not absorbed by the sample). Diffuse reflectance is the radiation that penetrates into the sample and then emerges. Diffuse reflectance accessories are designed to optimize the diffuse reflected energy and suppress the specular component. The optics therefore selectively directs the scattered radiation to the IR detector. 

Fourier transform infrared spectroscopy (FT-IR) is useful for identifying organic and inorganic compounds by comparison with library references. Perkin Elmer System 2000 offers near IR, mid IR, far IR 15,000-15,030 cm, transmittance (T), specular reflectance (SR Ref. 6) and diffuse reflectance (DR), horizontal and vertical attenuated total reflectance (ATR) microscope (>10-gm spot, 10,000-10,580 cmy ... 

After introduction of chromium on AIF3, FT-IR spectrum did not show substantial changes relative to the single support on the other hand these spectra have been obtained in transmittance with use of KBr pellets. This technique allows the characterization of the bulk, but it is very difficult to characterize the chromium species on the surface. The characterization of the samples obtained after the various preparation steps of the catalyst through UV-Vis spectroscopy in diffuse reflectance is reported in Fig. 2. 

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