Spheres diffusely reflecting

Diffuse reflectance accessory based on an integrating sphere Diffuse reflectance accessory based on a collection mirror... 

Diffuse reflectance UV-Vis spectra were obtained with a Shimadzu UV-2401PC UV-Vis spectrometer equipped with an integration sphere diffuse reflectance attachment. The samples were used as powders and a halon white (PTFE) reflectance standard used to record the baseline. The reflectance spectra were taken over the range 200 to 800 nm and converted into Kubelka-Munk function F(R). 

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. 

The nature and the distribution of different types of Fe species in calcined (C) and steamed (S) samples were investigated by means of UV-vis spectroscopy. UV-vis spectra of Fe species were monitored on UV-vis spectrometer GBS CINTRA 303 equipped with a diffuse reflectance attachment with an integrating sphere coated with BaS04 and BaS04 as a reference. The absorption intensity was expressed using the Schuster-Kubelka-Munk equation. 

Fig. 1 Schematic diagram of the integrating sphere portion of a diffuse reflectance spectrometer, illustrating the key elements of the optical train. Although the detecto has been placed in the plane of the sample and reference materials, in common practice it would be mounted orthogonal to the plane created by the intersection of the optica beams.

The overall tumbling of a protein molecule in solution is the dominant source of NH-bond reorientations with respect to the laboratory frame, and hence is the major contribution to 15N relaxation. Adequate treatment of this motion and its separation from the local motion is therefore critical for accurate analysis of protein dynamics in solution [46]. This task is not trivial because (i) the overall and internal dynamics could be coupled (e. g. in the presence of significant segmental motion), and (ii) the anisotropy of the overall rotational diffusion, reflecting the shape of the molecule, which in general case deviates from a perfect sphere, significantly complicates the analysis. Here we assume that the overall and local motions are independent of each other, and thus we will focus on the effect of the rotational overall anisotropy. 

Figure 8.11. Diffuse reflectance absorption spectra of a strongly fluorescent sample (1,6-diphenylhexatriene adsorbed on porous alumina) (a) conventional measurement w ith monochromatic irradiation and detection via an integrating sphere (b) measurement in a fluorimeter with two monochromators. Reaction spectra during Irons - cis photoisomerization are also given (adapted from Ref. 26).

Three analytical expressions for the spin-echo intensity as a function of the gradient in a pulsed field gradient NMR experiment for spins diffusing in a sphere with reflecting walls are reinvestigated. It is found that none of the published formulas are completely correct. By numerical comparisons the correct formula is found. 

Since the Murday-Cotts paper in 1968 much progress has been made toward the theoretical description of the spin-echo intensity E g, A) for spins diffusing in well-defined geometries. Tanner and Stejskal derived already in 1968 the exact expression of ii(g. A) for spins diffusing in a rectangular box. The derivation of an exact expression for E g, A) for diffusion in a sphere with reflecting walls is not a trivial mathematical problem and it took between 1992 and 1994 when three expressions were published. All three expressions are only valid in the short-gradient-pulse approximation (see below). 

When we wanted to numerically fit experimental PFGE data of water diffusion in a water-in-oil emulsion, we found that for a beginner in this field the literature is quite confusing. First, all three expressions for diffusion in a sphere with reflecting walls are somewhat different and lead to very different fitting results, especially when the formulas are combined with a radius distribution function. Since the derivation of the published expressions needs some tedious algebra (which has not been published), it is not trivial to check the derivation in order to establish which expression is the correct one. Here we use a numerical approach to decide which expression is correct. 

In the diffuse reflectance technique (Fig. 14.2d), light scattered by a thick layer of particles is directed by the integrating sphere to a detector. Absorption... 

To collect scattered transmission and correct for diffuse reflectance, a spectrophotometer with an integrating sphere should be used. This is important if films are not very transparent. 

When light is directed onto a sample it may either be transmitted or reflected. Hence, one can obtain the spectra by either transmission or reflection. Since some of the light is absorbed and the remainder is reflected, study of the diffuse reflected light can be used to measure the amount absorbed. However, the low efficiency of this diffuse reflectance process makes it extremely difficult to measure 120) and it was speculated that infrared diffuse reflection measurements would be futile 120). Initially, an integrating sphere was used to capture all of the reflected light121) but more recently improved diffuse reflectance cells have been designed which allow the measurement of diffuse reflectance spectra using FT-IR instrumentation 122). 

UV-VIS-NIR diffuse reflectance (DR) spectra were measured using a Perkin-Elmer UV-VIS-NIR spectrometer Lambda 19 equipped with a diffuse reflectance attachment with an integrating sphere coated by BaS04. Spectra of sample in 5 mm thick silica cell were recorded in a differential mode with the parent zeolite treated at the same conditions as a reference. For details see Ref. [5], The absorption intensity was calculated from the Schuster-Kubelka-Munk equation F(R ,) = (l-R< )2/2Roo, where R is the diffuse reflectance from a semi-infinite layer and F(R00) is proportional to the absorption coefficient. 

The strict solution for the problem of the resistance to the motion of a small sphere moving through gas has been obtained by Baines et al. (1965). They considered both specular and diffuse reflection of the molecules at the surface of the sphere mass of which is large in comparison with the mean mass of gas molecules and the radius to be small compared with the mean free path of gas molecules. All these assumptions are applicable for circumstellar outflows. Fadeyev and Henning (1987) used these solutions for calculation of momentum transfer from silicate dust grains to gas molecules in cool 0-rich red giants... 

For some typical modes of scattering from large spherical particles (f >5), simple formulations of phase functions can be obtained. These modes include scattering from a specularly reflecting sphere, scattering from a diffuse reflection sphere, and scattering by diffraction from a sphere. 

Figure 4.5b. Scattering phase function for a diffuse reflecting sphere which is large compared with the wavelength of incident radiation and with constant reflectivity (from Siegel and Howell, 1981).

All ground state diffuse reflectance spectra were recorded using a Phillips PU8800 UV-Visible spectrophotometer equipped with an integrating sphere, interfaced to an Elonex PC-386SX computer. These ground state diffuse reflectance spectra were measured relative to a BaSC>4 white reflectance standard (Eastman Kodak Ltd.). 

Reflectance spectra are usually measured using a diffuse reflectance accessory with an integrating sphere attached to a spectrophotometer. Spectra are referenced against a reflectance standard, such as smoked MgO, barite or Halon powder. The latter is a commercial fluorocarbon that does not absorb water or suffer radiation damage as does MgO. Each of these standards is virtually free of spectral features in the wavelength range 0.3 to 2.5 pm. 

Surprisingly TPA could not be detected by FTIR, either on the outer surface, in the diffuse reflection mode, or in flakes from the interior of the gel spheres in the transmission mode. 

Diffuse Reflectance Spectroscopy Using Integrating Spheres... 

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