Cyclotron, types

The most widely used type of trap for the study of ion-molecule reactivity is the ion-cyclotron-resonance (ICR) [99] mass spectrometer and its successor, the Fourier-transfomi mass spectrometer (FTMS) [100, 101]. Figure A3.5.8 shows the cubic trapping cell used in many FTMS instmments [101]. Ions are created in or injected into a cubic cell in a vacuum of 10 Pa or lower. A magnetic field, B, confines the motion in the x-y... 

In the other types of mass spectrometer discussed in this chapter, ions are detected by having them hit a detector such as an electron multiplier. In early ICR instruments, the same approach was taken, but FT-ICR uses a very different teclmique. If an RF potential is applied to the excitation plates of the trapping cell (figure B 1.7.18(b)) equal to the cyclotron frequency of a particular ion m/z ratio, resonant excitation of the ion trajectories takes place (without changing the cyclotron frequency). The result is ion trajectories of higher... 

The reactivity of size-selected transition-metal cluster ions has been studied witli various types of mass spectrometric teclmiques [1 ]. Fourier-transfonn ion cyclotron resonance (FT-ICR) is a particularly powerful teclmique in which a cluster ion can be stored and cooled before experimentation. Thus, multiple reaction steps can be followed in FT-ICR, in addition to its high sensitivity and mass resolution. Many chemical reaction studies of transition-metal clusters witli simple reactants and hydrocarbons have been carried out using FT-ICR [49, 58]. 

Gr. technetos, artificial) Element 43 was predicted on the basis of the periodic table, and was erroneously reported as having been discovered in 1925, at which time it was named masurium. The element was actually discovered by Perrier and Segre in Italy in 1937. It was found in a sample of molybdenum, which was bombarded by deuterons in the Berkeley cyclotron, and which E. Eawrence sent to these investigators. Technetium was the first element to be produced artificially. Since its discovery, searches for the element in terrestrial material have been made. Finally in 1962, technetium-99 was isolated and identified in African pitchblende (a uranium rich ore) in extremely minute quantities as a spontaneous fission product of uranium-238 by B.T. Kenna and P.K. Kuroda. If it does exist, the concentration must be very small. Technetium has been found in the spectrum of S-, M-, and N-type stars, and its presence in stellar matter is leading to new theories of the production of heavy elements in the stars. 

Other types of mass spectrometer may use point, array, or both types of collector. The time-of-flight (TOF) instrument uses a special multichannel plate collector an ion trap can record ion arrivals either sequentially in time or all at once a Fourier-transform ion cyclotron resonance (FTICR) instrument can record ion arrivals in either time or frequency domains which are interconvertible (by the Fourier-transform technique). 

Other types of mass spectrometer can use point, array, or both types of ion detection. Ion trap mass spectrometers can detect ions sequentially or simultaneously and in some cases, as with ion cyclotron resonance (ICR), may not use a formal electron multiplier type of ion collector at all the ions can be detected by their different electric field frequencies in flight. 

Plasmas can be used in CVD reactors to activate and partially decompose the precursor species and perhaps form new chemical species. This allows deposition at a temperature lower than thermal CVD. The process is called plasma-enhanced CVD (PECVD) (12). The plasmas are generated by direct-current, radio-frequency (r-f), or electron-cyclotron-resonance (ECR) techniques. Eigure 15 shows a parallel-plate CVD reactor that uses r-f power to generate the plasma. This type of PECVD reactor is in common use in the semiconductor industry to deposit siUcon nitride, Si N and glass (PSG) encapsulating layers a few micrometers-thick at deposition rates of 5—100 nm /min. 

Instruments are available that can perform MS/MS type experiments using a single analyzer. These instruments trap and manipulate ions in a trapping cell, which also serves as the mass analyzer. The ion trap and fourier transform ion cyclotron resonance (FT-ICR) mass spectrometers are examples. 

To check the identity and purity of the products obtained in the above reactions it is not sufficient to analyze for the sulfur content since a mixture may incidentally have the same S content. Either X-ray diffraction on single crystals or Raman spectra of powder-like or crystalline samples will help to identify the anion(s) present in the product. However, the most convincing information comes from laser desorption Fourier transform ion cyclotron resonance (FTICR) mass spectra in the negative ion mode (LD mass spectra). It has been demonstrated that pure samples of K2S3 and K2S5 show peaks originating from S radical anions which are of the same size as the dianions in the particular sample no fragment ions of this type were observed [28]. 

CsFeo.72Agi.28Te2,1053 and Cs2Ag2ZrTe4. The latter has a structure that comprises 2D slabs of Ag- and Zr-centered tetrahedral separated by Cs+ cations.1054 Gas-phase silver chalcogenide ions of the type [Ag2 i E ] (E = S, Se, Te) with < 14 have been investigated by laser-ablation Fourier transform ion cyclotron resonance mass spectrometry.1055... 

In anticipation of the development to operational status of the ion or direct counting systems, it would be helpful if we could compare these values with projected counting errors for the two types of direct counting systems being developed. Table 4 lists projections for the Rochester Van de Graaff facility [49] and the University of California Lawrence Berkeley cyclotron system employing an external ion source [31,50]. Table 4 also lists the sample sizes and approximate measurement periods for both systems. This data illustrates the potential extention in dating... 

Mass analyzers interrogate and resolve ions produced by an ion source based on their m/z ratios. Several types of mass analyzers are utilized for proteomic analysis including time-of-flight (TOF) quadrupoles, ion traps, and Fourier transform ion cyclotron resonance (FTICR). Mass analyzers may be assembled in hybrid configurations. MS instruments such as quadrupole TOF and quadra-pole ion trap-FTICR facilitate diversified applications and achieved great success. 

There are two kinds of Type (2) ion trap mass spectrometers the quadrupole ion trap and the ion cyclotron resonance instruments. 

Usually, concentration is measured as a pressure and may differ widely according to the type of mass spectrometer used. The triple quadrupole mass spectrometer may operate with pressures up to 1 x 10 1 Pa in the reaction region. At the other extreme, ion cyclotron resonance mass spectrometers operate poorly at pressures >1 X 10 4 Pa. A pressure of 1 x 10 4 Pa may be regarded as fairly high pressure for FT-ICR measurements. Converting the pressure into a more normal value of concentration means that reactions are carried out at concentrations < 10 9M (often several orders of magnitude < 10 0 M). 

The first report of this new type of kinetic isotope effect in a Menshutkin reaction was published by Matsson and coworkers in 198744. In this study, the alpha carbon kll/ku kinetic isotope effect was measured for the Menshutkin reaction between N,N-dimethyl-para-toluidine and labelled methyl iodide in methanol at 30 °C (equation 35). The carbon-11 labelled methyl iodide required for this study was prepared from the nC atoms produced in the cyclotron in three steps45 (equation 37). 

From its very beginnings to the present almost any physical principle ranging from time-of-flight to cyclotron motion has been employed to construct mass-analyzing devices (Fig 4.1). Some of them became extremely successful at the time they were invented, for others it took decades until their potential had fully been recognized. The basic types of mass analyzers employed for analytical mass spectrometry are summarized below (Tab. 4.1). 

The instruments used for the experimental work detailed in this review are several high-pressure mass spectrometers (HPMS) and a Fourier transform ion cyclotron resonance spectrometer (FTICR). Each of the instruments was constructed, to a considerable degree, in-house at the University of Waterloo, and each contains features unique to its type of apparatus. The instruments in general and the unique features of the Waterloo apparatus in particular are described below. 

BGeingeld and Nibbering et al. have shown that the intermediacy of such adducts can be demonstrated through the use of a double-resonance type of technique in which the transient [AB ] is continuously irradiated at its cyclotron frequency throughout the entire reaction time, even though it is not detectable in the ordinary mass spectrum. An overall decrease in the intensity of the product ion was then... 

Plutonium is produced from natural uranium which is a mixture of nonfis-sionable uranium-238 (99.3%) and fissionable uranium-235(0.7%). The first synthesis of this element was in a cyclotron generating plutonium in microgram quantities. The isotope Pu-239 can be produced in much larger quantities in a nuclear reactor, either a conventional thermal reactor or a breeder type reactor by neutron bombardment of uranium- 238. The nuclear reactions are shown below. 

The most commonly used mass separators are quadrupoles, ions traps and time-of-flight analyzers, for which the principle of mass separation is discussed below. Additionally, other types such as magnetic sector field or Fourier-trans-form cyclotron-resonance instruments are available. 

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