Glass sample preparation

Experiments were also performed on dry samples in order to avoid interference from solution dye. A dry glass sample, prepared from the same wet sample which gave the results at the top of Table 1, had = 0.60 ns, T2 = 3.1 ns, and = 0.22. This is typical of results from dry glass samples prepared with 10 M solutions The dry sample always had slightly shorter than the original wet sample, Tj = 3.1 ns, and A < 0.25. The... 

Figure 6.16 presents absorption and emission spectra of BP-codoped GGKBD glass samples prepared at different MTs. As expected, the enhanced emissions from both BP and Dy ions are observed with decreasing MTs [Fig. 6.16b], which correspond well to the markedly raised absorption baselines [Fig. 6.16a). As shown above, the BP-Dy codoping displays mutually enhanced emissions therefore, the increasing LVB ions with the decreasing MTs simultaneously enhance the emission from Dy at 1,310 nm. Most strikingly, the intensity ratio of BP to Dy emissions increases with the decreasing MTs pronouncedly, demonstrating that the MT effect works more effectively on BP instead of on Dy ions. In particular, the much enhanced broadband emissions with an FWHM of over 200 nm are realized from the BP-Dy codoped sample melted at 860°C.

Sample preparation is straightforward for a scattering process such as Raman spectroscopy. Sample containers can be of glass or quartz, which are weak Raman scatterers, and aqueous solutions pose no problems. Raman microprobes have a spatial resolution of - 1 //m, much better than the diffraction limit imposed on ir microscopes (213). Eiber-optic probes can be used in process monitoring (214). 

As-polymerized PVDC does not have a well-defined glass-transition temperature because of its high crystallinity. However, a sample can be melted at 210°C and quenched rapidly to an amorphous state at <—20°C. The amorphous polymer has a glass-transition temperature of — 17°C as shown by dilatometry (70). Glass-transition temperature values of —19 to — 11°C, depending on both method of measurement and sample preparation, have been determined. 

Glass-Transition Temperature. The T of PVP is sensitive to residual moisture (75) and unreacted monomer. It is even sensitive to how the polymer was prepared, suggesting that MWD, branching, and cross-linking may play a part (76). Polymers presumably with the same molecular weight prepared by bulk polymerization exhibit lower T s compared to samples prepared by aqueous solution polymerization, lending credence to an example, in this case, of branching caused by chain-transfer to monomer. 

Artifacts introduced through sample preparation are common materials these may be bits of facial tissue, wax, epithelial cells, hair, or dried stain, all inadvertently introduced by the microscopist. Detergent residues on so-called precleaned microscope slides and broken glass are common artifacts, as are knife marks and chatter marks from sectioning with a faulty blade, or scratch marks from grinding and polishing. 

In a study of dental silicate cements, Kent, Fletcher Wilson (1970) used electron probe analysis to study the fully set material. Their method of sample preparation varied slightly from the general one described above, in that they embedded their set cement in epoxy resin, polished the surface to flatness, and then coated it with a 2-nm carbon layer to provide electrical conductivity. They analysed the various areas of the cement for calcium, silicon, aluminium and phosphorus, and found that the cement comprised a matrix containing phosphorus, aluminium and calcium, but not silicon. The aluminosilicate glass was assumed to develop into a gel which was relatively depleted in calcium. 

As microwave sample preparation has evolved, standard microwave procedures have been developed and approved by numerous standard methods organisations (ASTM, AOAC International, EPA, etc.), see ref. [64]. Examples are standard test methods for carbon black/ash content (ASTM Method D 1506-97), lead analysis in direct paint samples (ASTM Method E 1645-94), etc. Table 8.15 shows some microwave ashing references (detection weight). A French AFNOR method utilises the atmospheric pressure single-mode microwave method as an alternative sample preparation procedure for Kjeldahl nitrogen determination [84], The performance of a microwave-assisted decomposition for rapid determination of glass fibre content in plastics for QC has been described [85]. 

Sample Preparation. Liquid crystalline phases, i.e. cubic and lamellar phases, were prepared by weighing the components in stoppered test tubes or into glass ampoules (which were flame-sealed). Water soluble substances were added to the system as water solutions. The hydrophobic substances were dissolved in ethanol together with MO, and the ethanol was then removed under reduced pressure. The mixing of water and MO solutions were made at about 40 C, by adding the MO solution dropwise. The samples for the in vivo study were made under aseptic conditions. The tubes and ampoules were allowed to equilibrate for typically five days in the dark at room temperature. The phases formed were examined by visual inspection using crossed polarizers. The compositions for all the samples used in this work are given in Tables II and III. 

XRD analyses were performed on oriented samples prepared by spreading of the sample suspension on a glass slide, followed by drying at room temperature. The XRD patterns were obtained with a PW 1130/00/60 Philips diffractometer using CuKa radiation (/, = 1,5405 A). Chemical analysis was carried out on a Perkin Elmer 3100 atomic absorption spectrometer after dissolution of the sample with several acids (HF, HCIO4, HC1) for 24h, and HN03 in a second time. 

In all microscopic methods, sample preparation is key. Powder particles are normally dispersed in a mounting medium on a glass slide. Allen [7] has recommended that the particles not be mixed using glass rods or metal spatulas, as this may lead to fracturing a small camel-hair brush is preferable. A variety of mounting fluids with different viscosities and refractive indices are available a more viscous fluid may be preferred to minimize Brownian motion of the particles. Care must be taken, however, that the refractive indices of sample and fluid do not coincide, as this will make the particles invisible. Selection of the appropriate mounting medium will also depend on the solubility of the analyte [9]. After the sample is well dispersed in the fluid, a cover slip is placed on top... 

Boylan and Tripp [76] determined hydrocarbons in seawater extracts of crude oil and crude oil fractions. Samples of polluted seawater and the aqueous phases of simulated samples (prepared by agitation of oil-kerosene mixtures and unpolluted seawater to various degrees) were extracted with pentane. Each extract was subjected to gas chromatography on a column (8 ft x 0.06 in) packed with 0.2% of Apiezon L on glass beads (80-100 mesh) and temperatures programmed from 60 °C to 220 °C at 4°C per minute. The components were identified by means of ultraviolet and mass spectra. Polar aromatic compounds in the samples were extracted with methanol-dichlorome-thane (1 3). 

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