Spectrometer description

The basic principles of fast-atom bombardment (FAB) and liquid-phase secondary ion mass spectrometry (LSIMS) are discussed only briefly here because a fuller description appears in Chapter 4. This chapter focuses on the use of FAB/LSIMS as part of an interface between a liquid chromatograph (LC) and a mass spectrometer (MS), although some theory is presented. 

The quadrupole mass spectrometer has been found to be particularly suitable for EGA in thermal analysis. Published reports include descriptions of the various systems used [153—155] and applications in studies of the pyrolysis of polymers [155], minerals [156] and many inorganic solids [157—159]. 

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... 

Mgssbauer Spectroscopy. All details of the Mdssbauer spectroscopy studies are described elsewhere (25,27). This includes descriptions of the spectrometer, situ cells, and the computer program used to analyze the MCssbauer spectra. 

It is only since 1980 that in situ spectroscopic techniques have been developed to obtain identification of the adsorbed intermediates and hence of reliable reaction mechanisms. These new infrared spectroscopic in situ techniques, such as electrochemically modulated infrared reflectance spectroscopy (EMIRS), which uses a dispersive spectrometer, Fourier transform infrared reflectance spectroscopy, or a subtractively normalized interfacial Fourier transform infrared reflectance spectroscopy (SNIFTIRS), have provided definitive proof for the presence of strongly adsorbed species (mainly adsorbed carbon monoxide) acting as catalytic poisons. " " Even though this chapter is not devoted to the description of in situ infrared techniques, it is useful to briefly note the advantages and limitations of such spectroscopic methods. 

The present description is based on previous publications from this laboratory56-59 and the interested reader will find additional details and references in that work. Two different ion-source reaction chambers are used. One of these sources which operates at room temperature is shown in Figure 4. The second source, a variable temperature source will also be described. The electrospray generator and the ion-source reaction chamber are shown in Figure 4, while the mounting of the ion source and the front end of the mass spectrometer are shown in Figure 5. 

This chapter concludes with a brief description of one advanced technique, Electron Nuclear Double Resonance (ENDOR), the capabilities for which, unlike pulsed methods, may be added as a relatively minor modification to commercial CW ESR spectrometers. 

This chapter is a guided tour of the standard EPR spectrometer. The goal is not to give a rigorous description of the underlying physics, but to develop a feel for basic parts and principles sufficient to make you an independent, intelligent operator of any X-band machine. 

A mass spectrometer is often indispensable for a complete analysis of low-pressure gases, but a description of the various types of spectrometers is beyond the purpose of this book, but see, for example, ref. [18]. We simply remind that a mass spectrometer consists of three parts an ion source where the neutral gas is ionized (usually by electron bombardment) an analyser where ions are selected according to their mass to charge ratio and a collector with an amplifier to measure the weak ion current. 

Field desorption (FD) was introduced by Beckey in 1969 [76]. FD was the first soft ionization method that could generate intact ions from nonvolatile compounds, such as small peptides [77]. The principal difference between FD and FI is the sample injection. Rather than being in the gas phase as in FI, analytes in FD are placed onto the emitter and desorbed from its surface. Application of the analyte onto the emitter can be performed by just dipping the activated emitter in a solution. The emitter is then introduced into the ion source of the spectrometer. The positioning of the emitter is cmcial for a successful experiment, and so is the temperature setting. In general, FI and FD are now replaced by more efficient ionization methods, such as MALDI and ESI. For a description of FD (and FI), see Reference 78. 

A simple convention for description of peptide fragments formed in the mass spectrometer was proposed by Roepstorff and Fohlman in 1984 [1] and further modified by Johnson in 1987 [2]. Fragment ions are described by single lower-case letters with additional indexes (Fig. 6.5). If we consider fragmentation of a peptide backbone only, six ion series can be formed due to fragmentation at ... 

Description of several types of mass spectrometers used as detectors for GC. 

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