Apparatus spectrometer

X-ray spectrometer An apparatus used in the X-ray study of crystals in which a fine beam of monochromatic X-rays impinges at a measured angle on the face of a crystal mounted in its path, and in which the intensity of the X-rays diffracted in various directions by the crystal is measured with an ionization chamber mounted on an arm of the spectrometer table, or is recorded photographically. 

In essence, a guided-ion beam is a double mass spectrometer. Figure A3.5.9 shows a schematic diagram of a griided-ion beam apparatus [104]. Ions are created and extracted from an ion source. Many types of source have been used and the choice depends upon the application. Combining a flow tube such as that described in this chapter has proven to be versatile and it ensures the ions are thennalized [105]. After extraction, the ions are mass selected. Many types of mass spectrometer can be used a Wien ExB filter is shown. The ions are then injected into an octopole ion trap. The octopole consists of eight parallel rods arranged on a circle. An RF... 

A single magnetic sector can be used as a mass filter for other apparatus. However, much more infonnation of the simple mass spectrum of a species can be obtained using the tandem mass spectrometer. 

Probably the simplest mass spectrometer is the time-of-fiight (TOP) instrument [36]. Aside from magnetic deflection instruments, these were among the first mass spectrometers developed. The mass range is theoretically infinite, though in practice there are upper limits that are governed by electronics and ion source considerations. In chemical physics and physical chemistry, TOP instniments often are operated at lower resolving power than analytical instniments. Because of their simplicity, they have been used in many spectroscopic apparatus as detectors for electrons and ions. Many of these teclmiques are included as chapters unto themselves in this book, and they will only be briefly described here. 

These limitations have recently been eliminated using solid-state sources of femtosecond pulses. Most of the femtosecond dye laser teclmology that was in wide use in the late 1980s [11] has been rendered obsolete by tliree teclmical developments the self-mode-locked Ti-sapphire oscillator [23, 24, 25, 26 and 27], the chirped-pulse, solid-state amplifier (CPA) [28, 29, 30 and 31], and the non-collinearly pumped optical parametric amplifier (OPA) [32, 33 and 34]- Moreover, although a number of investigators still construct home-built systems with narrowly chosen capabilities, it is now possible to obtain versatile, nearly state-of-the-art apparatus of the type described below Ifom commercial sources. Just as home-built NMR spectrometers capable of multidimensional or solid-state spectroscopies were still being home built in the late 1970s and now are almost exclusively based on commercially prepared apparatus, it is reasonable to expect that ultrafast spectroscopy in the next decade will be conducted almost exclusively with apparatus ifom conmiercial sources based around entirely solid-state systems. 

It is difficult to observe tliese surface processes directly in CVD and MOCVD apparatus because tliey operate at pressures incompatible witli most teclmiques for surface analysis. Consequently, most fundamental studies have selected one or more of tliese steps for examination by molecular beam scattering, or in simplified model reactors from which samples can be transferred into UHV surface spectrometers witliout air exposure. Reference [4] describes many such studies. Additional tliemes and examples, illustrating botli progress achieved and remaining questions, are presented in section C2.18.4. 

The use of more complex or more costly articles of equipment, such as catalytic hydrogenation apparatus, autoclaves, polari-meters, ultraviolet absorption spectrometers, etc., has not been described, because the type of such apparatus employed indifferent laboratories varies considerably, and students must be taught the use of their own laboratory equipment. 

These thin wires are supported on a special carrier that can be inserted into the ion source of the mass spectrometer after first growing the whiskers in a separate apparatus. Although the wires are very fragile, they last for some time and are easily renewed. They are often referred to as emitter electrodes (ion emitters). 

The apparatus as modified for x-ray emission spectrograph is also shown in Figure 11-1. The proportional counter may be used alone (pulse-height analysis Section 2.13) or a curved-crystal spectrometer can be employed to achieve better resolution. Analytical results were comparable to those quoted above, but localization of the area analyzed was considerably less sharp than the micron-diameter spot achieved in differential absorptiometry. 

Vapor pressures of phases in these systems were measured by the Knudsen effusion technique. Use of mass spectrometer-target collection apparatus to perform thermodynamic studies is discussed. The prominent sublimation reactions for these phases below 2000 K was shown to involve formation of elemental plutonium vapor. Thermodynamic properties determined in this study were correlated with corresponding values obtained from theoretical predictions and from previous measurements on analogous intermetallics. 

Equilibrium vapor pressures were measured in this study by means of a mass spectrometer/target collection apparatus. Analysis of the temperature dependence of the pressure of each intermetallic yielded heats and entropies of sublimation. Combination of these measured values with corresponding parameters for sublimation of elemental Pu enabled calculation of thermodynamic properties of formation of each condensed phase. Previ ly reported results on the subornation of the PuRu phase and the Pu-Pt and Pu-Ru systems are correlated with current research on the PuOs and Pulr compounds. Thermodynamic properties determined for these Pu-intermetallics are compared to analogous parameters of other actinide compounds in order to establish bonding trends and to test theoretical predictions. 

Maier (50) also investigated the charge exchange between Xe + and C2H4. These reactions were studied previously by Tal roze et al. (29, 30, 31, 32) in a perpendicular type apparatus in which the geometry seems to result in a smaller discrimination in the second mass spectrometer than in the Stockholm apparatus. Finally, the same reactions were observed in Stockholm by Szabo (19) during a detailed investiga-... 

The apparatus used, as described previously (7), has modifications as described by Maier (16). A description also appears in this volume (15). A mass spectrometer of special design with 2-inch round poles, using 90° deflection with 1-inch magnetic radius, provides momentum-selected beams of low energy ions. These ions proceed at full energy... 

Fig. 14—A sketch of surface force apparatus. (1) cantilever, (2) samples, (3) supporter and driver for lateral motion, (4) chamber, (5) supporter and driver for normal displacement, (6) lens, (7) prism, (8) spectrometer, (9) computer for data collection.

The spectrometer is fitted with a skimmed c.w. supersonic molecular beam source. Many chiral species of interest are of low volatility, so a heated nozzle-reservoir assembly is used to generate, in a small chamber behind a 70-pm pinhole, a sample vapor pressure that is then seeded in a He carrier gas as it expands through the nozzle [103], Further details of this apparatus are given elsewhere [36, 102, 104],... 

ATP apparatus equipped with a mass spectrometer. Right-hand side TPR patterns of silica-supported Rh, Fe, and Fe-Rh catalysts, which had been previously calcined to ensure that all metals are oxidized at the start of the measurement. [Adapted from J.W. Niemantsverdriet, Spectroscopy in Catalysis, An Introduction (2000), Wiley-VCH, Weinheim, and H.F.J. van t Blik and J.W. Niemantsverdriet, Appl. Cota/. 10 (1984) 155.]... 

The apparatuses used for the studies of both ammonia synthesis emd hydrodesulfurization were almost identical, consisting of a UHV chamber pumped by both ion and oil diffusion pumps to base pressures of 1 x10 " Torr. Each chamber was equipped with Low Energy Electron Diffraction optics used to determine the orientation of the surfaces and to ascertain that the surfaces were indeed well-ordered. The LEED optics doubled as retarding field analyzers used for Auger Electron Spectroscopy. In addition, each chamber was equipped with a UTI 100C quadrupole mass spectrometer used for analysis of background gases and for Thermal Desorption Spectroscopy studies. 

The samples were characterized by chemical analysis induced coupled plasma and atomic absorption techniques apparatus), nitrogen adsorption isotherms (at 77 K), XRD patterns ( Siemens diffractometer and (3uKa radiation), SEM observations (Hitachi S800 apparatus of the University C. Bernard, Lyon I) and TGA-DTA (Setaram 92-12 apparatus). The IR spectra were recorded with a Bruker IPS 48 FTIR spectrometer. 

The chemical compositions of the isolated Au SR clusters were investigated by mass spectrometry [15,16,18, 22,32-35]. TEM was used to confirm that the species detected by the mass spectrometer represents the clusters in the sample. Figure 3a is a schematic representation of the top view of the mass spectrometer, which consists of five stages of differentially pumped vacuum chambers. The apparatus accommodates two t5 pes of ion sources, electrospray ionization (ESI) and laser-desorption ionization (EDI), and a time-of-flight (TOE) mass spectrometer with a reflectron. Details of the apparatus and the measurement protocols are described below. 

Figure 3. Mass spectrometer (a) whole apparatus, (b) LDI source, and (c) ESI source. (Adapted with permission from Ref [16], 2005, American Chemical Society.)...

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