Diffuse-reflectance spectroscopy

DETERMINATION ORGANIC COMPOUNDS BY DIFFUSE REFLECTION SPECTROSCOPY... 

The application of diffuse reflectance spectroscopy to the chemistry of transition metal coordination compounds. E. L. Simmons, Coord. Chem. Rev., 1974,14,181-196 (81). 

W.F. McClure, A. Hamid, F.G. Giesbrecht and W.W, Weeks, Fourier analysis enhances NIR diffuse reflectance spectroscopy. Appl. Spectrosc., 38 (1988) 322-329. 

Ean Q, Pu C, Ley KL, Smotkin ES. 1996. In situ FTIR-diffuse reflectance spectroscopy of the anode surface in a direct methanol fuel cell. J Electrochem Soc 143 L21-L23. 

In situ UV-Vis Diffuse Reflectance Spectroscopy was performed under reactive atmosphere ( -butane/oxygen). These experiments confirmed that submitting the catalyst to the reaction mixture favors the development of a more oxidized active surface, and that the extent of transformation depends on the reaction temperature and on the catalyst P/V ratio. For instance, catalyst P/V 1.06 was less oxidized than catalyst P/V 1.00 at a temperature lower than 340°C. X-ray Photoelectron spectra of catalysts recorded after reaction at 380°C confirmed that catalyst P/V 1.00 was considerably more oxidized (average oxidation state for surface V 4.23) than the P/V 1.06 catalyst (average oxidation state 4.03). 

The problems discussed above may be circumvented by eliminating the mobile phase before measuring the spectra of the eluites, as first demonstrated by Shafer et al. [379] for pSFC-FTIR. Each eluite was deposited on a moving glass plate, on which a layer of powdered KC1 or KBr had been laid down from methanol slurry for diffuse reflectance spectroscopy (SFC-DRIFTS). Solvent elimination SFC-FTIR after deposition of the eluites on to a moving ZnSe substrate is quite straightforward the window is moved to the... 

Dedecek, J., Kaucky, D. and Wichterlova, B. (2000) Co2+ ion siting in pentasil-containing zeolites, part 3. Co2+ ion sites and their occupation in ZSM-5 A VIS diffuse reflectance spectroscopy study, Microporous Mesoporous Mater., 35-6, 483. 

Colombo DP, Bowman RM (1995) Femtosecond diffuse reflectance spectroscopy of Ti02 powder. J Phys Chem 99 11752e6... 

Danzer K, Fischbacher C, Jagemann K-U, Reichelt KJ (1998) Near-infrared diffuse reflection spectroscopy for non-invasive blood-glucose monitoring. LEOS Newslett 12(2) 9... 

Atomic Absorption and Fluorescence Spectroscopy Diffuse Reflectance Spectroscopy Vol. 5 Emission Spectroscopy... 

The metal content analysis of the samples was effected by Inductively Coupled Plasma Atomic Emission Spectroscopy (ICP-AES Varian Liberty II Instrument) after microwaves assisted mineralisation in hydrofluoric/hydrochloric acid mixture. Ultraviolet and visible diffuse reflectance spectroscopy (UV-Vis DRS) was carried out in the 200-900 nm range with a Lambda 40 Perkin Elmer spectrophotometer with a BaS04 reflection sphere. HF was used as a reference. Data processing was carried out with Microcal Origin 7.1 software. 

Malin S.F., Ruchti T.L., Blank T.B., Thennadil S.N., Monfre S.L., Noninvasive prediction of glucose by near-infrared diffuse reflectance spectroscopy, Clin. Chem. 1999 45 (9) 1651-1658. 

Various optical detection methods have been used to measure pH in vivo. Fluorescence ratio imaging microscopy using an inverted microscope was used to determine intracellular pH in tumor cells [5], NMR spectroscopy was used to continuously monitor temperature-induced pH changes in fish to study the role of intracellular pH in the maintenance of protein function [27], Additionally, NMR spectroscopy was used to map in-vivo extracellular pH in rat brain gliomas [3], Electron spin resonance (ESR), which is operated at a lower resonance, has been adapted for in-vivo pH measurements because it provides a sufficient RF penetration for deep body organs [28], The non-destructive determination of tissue pH using near-infrared diffuse reflectance spectroscopy (NIRS) has been employed for pH measurements in the muscle during... 

Until quite recently the very initial stages of metal deposition were difficult to characterize in detail by structure- and morphology-sensitive techniques. As a consequence and for practical purposes - multilayers were more useful for applications than monolayers - the main interest was focussed onto thick deposits. Optical and electron microscopy, ellipsometry and specular or diffuse reflectance spectroscopy were the classic tools, by which the emerging shape of the deposit was monitored [4-7],... 

Connors and Jozwiakowski have used diffuse reflectance spectroscopy to study the adsorption of spiropyrans onto pharmaceutically relevant solids [12]. The particular adsorbants studied were interesting in that the spectral characteristics of the binary system depended strongly on the amount of material bound. As an example of this behavior, selected reflectance spectra obtained for the adsorption of indolinonaphthospiropyran onto silica gel are shown in Fig. 1. At low concentrations, the pyran sorbant exhibited its main absorption band around 550 nm. As the degree of coverage was increased the 550 nm band was still observed, but a much more intense absorption band at 470 nm became prominent. This secondary effect is most likely due to the presence of pyran-pyran interactions, which become more important as the concentration of sorbant is increased. 

R. W. Frei and J. D. MacNeil, Diffuse Reflectance Spectroscopy in Environmental Problem Solving, CRC Press, Cleveland, Ohio, 1973. 

V. APPLICATIONS OF DIFFUSE REFLECTANCE SPECTROSCOPY TO THE STUDY OF PHARMACEUTICAL SOLIDS 42... 

Diffuse reflectance spectroscopy was used to screen the possible interactions between a large number of adjuvants and several dyes [23]. It was concluded that supposedly inert excipients (such as starch or lactose) were capable of undergoing significant reactions with the dyes investigated (Red No. 3, Blue No. 1, and Yellow No. 5). For adjuvants containing metal ions (zinc oxide, or calcium, magnesium, and aluminum hydroxides), the degree of interaction could be considerable. It was concluded from these studies that dye-excipient interactions could also be responsible for the lack of color stability in certain tablet formulations. 

It was recognized very early that diffuse reflectance spectroscopy could be used to study the interactions of various compounds in a formulation, and the technique has been particularly useful in the characterization of solid state reactions [24]. Lach concluded that diffuse reflectance spectroscopy could also be used to verify the potency of a drug in its formulation. In addition, studies conducted under stress conditions would be useful in the study of drug-excipient interactions, drug degradation pathways, and alterations in bioavailability owing to chemisorption of the drug onto other components in the formulation [24]. 

The reaction of a primary amine with lactose is accompanied by a browning of the solids, and the path of such reactions is easily following by means of diffuse reflectance spectroscopy. For instance, the reaction of isonicotinic acid hydrazide (Isoniazid) with lactose could be followed through changes in the reflectance spectrum [31]. As may be seen in Fig. 4, a steady decrease in reflectance was noted as the sample was heated for increasing amounts of time. The spectral data were used to deduce the rate constants for the browning reaction at various heating temperatures, and these rates could be correlated with those... 

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