High vacuum

Surface defects (Section VII-4C) are also influenced by the history of the sample. Such imperfections may to some extent be reversibly affected by processes such as adsorption so that it is not safe to regard even a refractory solid as having fixed surface actions. Finally, solid surfaces are very easily contaminated detection of contamination is aided by ultra-high-vacuum techniques and associated cleaning protocols [24]. 

A number of methods that provide information about the structure of a solid surface, its composition, and the oxidation states present have come into use. The recent explosion of activity in scanning probe microscopy has resulted in investigation of a wide variety of surface structures under a range of conditions. In addition, spectroscopic interrogation of the solid-high-vacuum interface elucidates structure and other atomic processes. 

The course of a surface reaction can in principle be followed directly with the use of various surface spectroscopic techniques plus equipment allowing the rapid transfer of the surface from reaction to high-vacuum conditions see Campbell [232]. More often, however, the experimental observables are the changes with time of the concentrations of reactants and products in the gas phase. The rate law in terms of surface concentrations might be called the true rate law and the one analogous to that for a homogeneous system. What is observed, however, is an apparent rate law giving the dependence of the rate on the various gas pressures. The true and the apparent rate laws can be related if one assumes that adsorption equilibrium is rapid compared to the surface reaction. 

Soriaga M P 1992 Ultra-high vacuum techniques in the study of single-crystal electrode surfaces Prog. Surf. Sc/. 39 325... 

As a special development in recent years, SEMs have been designed which no longer necessitate high vacuum (enviromnental SEM, ESEM variable pressure SEM, VPSEM). This development is important for the imaging of samples with a residual vapour pressure, such as aqueous biological or medical samples, but also samples in materials science (wet rock) or organic chemistry (polymers). 

Ultra-high vacuum (UHV) surface science methods allow preparation and characterization of perfectly clean, well ordered surfaces of single crystalline materials. By preparing pairs of such surfaces it is possible to fonn interfaces under highly controlled conditions. Furthennore, thin films of adsorbed species can be produced and characterized using a wide variety of methods. Surface science methods have been coupled with UHV measurements of macroscopic friction forces. Such measurements have demonstrated that adsorbate film thicknesses of a few monolayers are sufficient to lubricate metal surfaces [12, 181. 

McFadden C F and Geiiman A J 1995 Ultra-high vacuum boundary lubrication of the Cu-Cu interface by 2,2,2-trifluoroethanol Langmuir 273-80... 

Apart from the sheer complexity of the static stmctures of biomolecules, they are also rather labile. On the one hand this means that especial consideration must be given to the fact (for example in electron microscopy) that samples have to be dried, possibly stained, and then measured in high vacuum, which may introduce artifacts into the observed images [5]. On the other, apart from the vexing question of whether a protein in a crystal has the same stmcture as one freely diffusing in solution, the static stmcture resulting from an x-ray diffraction experiment gives few clues to the molecular motions on which operation of an enzyme depends [6]. 

The spatial arrangement of atoms in two-dimensional protein arrays can be detennined using high-resolution transmission electron microscopy [20]. The measurements have to be carried out in high vacuum, but since tire metliod is used above all for investigating membrane proteins, it may be supposed tliat tire presence of tire lipid bilayer ensures tliat tire protein remains essentially in its native configuration. 

Mercury is extensively used in various pieces of scientific apparatus, such as thermometers, barometers, high vacuum pumps, mercury lamps, standard cells (for example the Weston cell), and so on. The metal is used as the cathode in the Kellner-Solvay cell (p. 130). 

When constructing a manometer of the type shown in Fig. 12(c), it is impor tant to apply a very high vacuum (e.g., with a Hy-Vac pump) to the manometer while the mercury in the left-hand (sealed) limb is heated until it boils unless this is done, traces of air will remain in this limb and cause inaccurate readings. During a distillation, the tap I should be kept closed except when a pressure reading is being taken if it is left open indefinitely, a sudden default by the distillation apparatus or by the pump may cause the mercury in the sealed limb of G to fly back and fracture the top of the limb. 

In filling the tube R, one tap is inserted after being carefully greased with a high-vacuum or silicone grease. The taps are provided with scored grooves (that run completely around them near their outer end) which act as a trap to prevent... 

A particularly good metal pump, which operates on a comparatively small head of water is made by Edwards High Vacuum Ltd. 

This is sometimes made of mirror glass in order to eliminate the error due to parallax, t Manufactured by Edwards High Vacuum Ltd. This is essentially a form of McLeod gauge. 

Supplied by The Emil Greiner Co. of New York and by Edwards High Vacuum Ltd. an all.metal Cartesian manostat is also marketed. 

Some simple apparatus, suitable for high vacuum distillation, are collected in Figs. 11, 26, 1-4. Fig. 11, 26, 1 represents an apparatus, which is particularly well adapted for solids the ground glass joint must be lubricated with a grease of negligible vapour pressure. Hickman s vacuum still is shown in Fig. 11, 26, 2 it is about 60 mm. in diameter. 

The distinguishiag features are (i) the special stopcock is constructed to turn easily under a high vacuum (ii) a moulded arrow on the stopcock indicates the open position, euid a quarter turn from this position closes the desiccator and (iii) a special liquid container of the non-spill type. 

Europium is now prepared by mixing EU2O3 with a 10%-excess of lanthanum metal and heating the mixture in a tantalum crucible under high vacuum. The element is collected as a silvery-white metallic deposit on the walls of the crucible. 

High vacuum distillation gave a crystalline product, containing small amounts of impurities, inter alia some 2-butynoic acid. Crystallization from a 3 1 mixture of pentane and diethyl ether at low temperature gave the pure acid, m.p. 77°C, in 38-45 yields. 

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