Diffuse reflectance sample

Fig. 4 Schematic representation of the diffuse reflectance sampling accessory. Key A, blocker device to eliminate specular reflectance B, path of IR beam.

Depth profiling of a solid sample may be performed by varying the interferometer moving-mirror velocity (modulated IR radiation). By increasing the mirror velocity, the sampling depth varies, and surface studies may be performed. Limitations do exist, but the technique has proven to be quite effective for solid samples [21]. In addition, unlike diffuse reflectance sampling techniques, particle size has a minimal effect upon the photoacoustic measurement. 

The light-path length / between the two modulators is varied, and the relative intensity as a function of / is determined. Data are collected for both a diffusely reflecting sample and for the fluorescent sample. 

The X-ray powder diffraction pattern was collected (Philips, PW 1840) with a Cu target and Ni filter (AcuKa = 0.15418 nm). The IR spectra were collected with a FTIR spectrometer (Bruker, Equinox 55) equipped with a diffuse reflectance sampling stage (Praying Mantis, Flarrick) utilizing the ambient chamber. The samples were analyzed by an UNI-SPECS ESCA system with a... 

Fig. 18. A Schematic representation of a diffuse reflectance spectrometer. For (i) nondiffuse dispersed illumination the source at the left and the detector at the integrating sphere are used. For (ii) diffuse nondisperse illumination (in the case of fluorescent samples) a source directly attached to the sphere and the detectors on the left upper side are applied. B Temperature-regulated and evacuable diffuse reflectance sample cell according to [32]. Reprinted from [32] with permission of Academic Press, Inc...

Figure 1. Theoretical (Monte Carlo modelling) and experimental (integrating sphere) (a, c) collimated transmittance T and (h, d) diffuse reflectance visible spectra of the human sclera. MC 1 mm-thickness, 120 nm-mean fihril diameter, 285 nm-mean separation between fibrils, fibril refractive index, = 1.47, and interfibrillar refractive index is under control 1) o = 1-35, 2) 1.37, 3) 1.39, 4) 1.41, 5) 1.43, and 6) 1.45. Experiment The sclera was carefully purified fiom ciliary body and retina, washed, and cut into pieces of area 10x10 mm. (c) Collimated transmittance, sample thickness, 0.6 mm (b) diffusion reflection, sample thickness, 0.7 mm. Samples were measured for different time intervals of administration of Trazograph-60 (x-ray contrast agent - a derivative of 2,4,6-triiodobenzene acid with molecular weight of about 500, n=1.437) in a bath. Spectra 1 were measured 1 min after the samples were immersed in solution, and spectra...

Fig. 5. (a) ATR sampling system for infrared spectrometry, p) Diffuse reflectance sampling for infrared spectrometry. 

Several factors affect the bandshapes observed ia drifts of bulk materials, and hence the magnitude of the diffuse reflectance response. Particle size is extremely important, siace as particle size decreases, spectral bandwidths generally decrease. Therefore, it is desirable to uniformly grind the samples to particle sizes of <50 fim. Sample homogeneity is also important as is the need for dilute concentrations ia the aoaabsorbiag matrix. 

Diffuse reflection iavolves reflecting the iafrared beam off of a soHd sample, as ia specular reflectioa, but it is the aoaspecular portioa of the reflected radiatioa that is coUected. Whea an ftir spectrometer is used, diffuse reflection is caUed DRIFTS (diffuse reflectance iafrared Fourier-transform... 

A solvent free, fast and environmentally friendly near infrared-based methodology was developed for the determination and quality control of 11 pesticides in commercially available formulations. This methodology was based on the direct measurement of the diffuse reflectance spectra of solid samples inside glass vials and a multivariate calibration model to determine the active principle concentration in agrochemicals. The proposed PLS model was made using 11 known commercial and 22 doped samples (11 under and 11 over dosed) for calibration and 22 different formulations as the validation set. For Buprofezin, Chlorsulfuron, Cyromazine, Daminozide, Diuron and Iprodione determination, the information in the spectral range between 1618 and 2630 nm of the reflectance spectra was employed. On the other hand, for Bensulfuron, Fenoxycarb, Metalaxyl, Procymidone and Tricyclazole determination, the first order derivative spectra in the range between 1618 and 2630 nm was used. In both cases, a linear remove correction was applied. Mean accuracy errors between 0.5 and 3.1% were obtained for the validation set. 

Ultraviolet-visible (UV-vis) diffuse reflectance spectra of supported WOx samples and standard W compounds were obtained with a Varian (Cary 5E) spectrophotometer using polytetrafluoroethylene as a reference. The Kubelka-Munk function was used to convert reflectance measurements into equivalent absorption spectra [12]. Spectral features of surface WOx species were isolated by subtracting from the W0x-Zr02 spectra that of pure Z1O2 with equivalent tetragonal content. All samples were equilibrated with atmospheric humidity before UV-vis measurements. 

The quantification of the extra-framework titanium species in titanium silicalites of MFI structure, TS-1, was performed using either XANES at the Ti K-edge or XPS Ti (2p) photolines. In addition, two different framework sites, [Ti(OH)(OSi)3] and [Ti(OSi)4], were characterized in dehydrated samples using Diffuse Reflectance UV-visible, multiple scattering analysis of EXAFS, H and Si NMR spectroscopies. 

Characterization. In-situ diffuse reflectance FTIR (DRIFT) experiments were carried out with undiluted samples of the zeolites in a Spectratech DRIFT cell and a Nicolet Magna 550 spectrometer. Most experiments were carried out in a flow mode, passing 0.84 ml/s of a gas mixture containing inert (He, Ar or N2) and N2O, NO, CO or mixtures of these gases continuously through the cell at atmospheric pressure. Each spectrum was recorded by addition of 256 scans and a resolution of 8 cm. ... 

This simple relationship between incident and transmitted light is well known as the Boguert-Lambert-Beer law. This expression renders positive values for Ij < Iq. In case of scattering material like TLC plates, a part of the scattered light is emitted as reflectance J from the plate surface to the top. For the hrst approximation of a parallel incident light beam with the intensity /g, some radiation may be scattered inside the layer and some radiation may be absorbed either by the sample or by the layer itself. According to the Schuster equations and with the abbreviation R (the diffuse reflectance of an infinitely thick layer). 

FTIR instrumentation is mature. A typical routine mid-IR spectrometer has KBr optics, best resolution of around 1cm-1, and a room temperature DTGS detector. Noise levels below 0.1 % T peak-to-peak can be achieved in a few seconds. The sample compartment will accommodate a variety of sampling accessories such as those for ATR (attenuated total reflection) and diffuse reflection. At present, IR spectra can be obtained with fast and very fast FTIR interferometers with microscopes, in reflection and microreflection, in diffusion, at very low or very high temperatures, in dilute solutions, etc. Hyphenated IR techniques such as PyFTIR, TG-FTIR, GC-FTIR, HPLC-FTIR and SEC-FTIR (Chapter 7) can simplify many problems and streamline the selection process by doing multiple analyses with one sampling. Solvent absorbance limits flow-through IR spectroscopy cells so as to make them impractical for polymer analysis. Advanced FTIR... 

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