Mass Spectrometry 3

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PLATINblue MSQ Plus Hardware Guide V6950A UHPLC/HPLC Mass spectrometry 3 Content Preface . 8 Safety . 8 Fuses . 8 Lab regulations . 8 LC Solvents and Mobile Phase Additives . 8 LC Solvents . 8 Protective measures . 9 Safety precautions . 9 Solvent and Gas Purity Requirements . 11 Contacting Us . 11 To contact Technical Support or Customer Service for ordering information . 11 To suggest changes to documentation or to Help . 11 Introduction . 12 Overview . 12 Ion Polarity Modes . 13 Ionization Techniques . 14 Electrospray Ionization (ESI) . 14 Ion Desolvation Mechanism . 14 Spectral Characteristics . 15 Atmospheric Pressure Chemical Ionization (APCI) . 16 Ion Generation Mechanism . 16 Spectral Characteristics . 18 Scan Types . 18 Full Scan . 18 Selected Ion Monitoring (SIM) . 18 Data Types . 19 Profile Data Type . 19 Centroid Data Type . 20 MCA Data Type . 21 Functional Description. 22 Liquid Chromatograph . 23 To open the Instrument Configuration application . 23 Reference Inlet System . 25 Mass Detector . 27 Front Panel Status Indicator . 28 Rear Panel Controls and Connections . 29 Connection Between LC and Mass Detector . 31 API Sources . 31 V6950A 4 Electrospray Ionization (ESI) . 31 Atmospheric Pressure Chemical Ionization (APCI) . 33 RF/dc Prefilter . 34 Mass Analyzer . 35 RF and DC Fields Applied to the Quadrupoles . 35 Mass Analysis . 36 Ion Detection System . 37 Vacuum System . 39 Vacuum Manifold . 40 Turbomolecular Pump . 40 Forepump . 41 Pirani Gauge . 41 Vent Valve . 41 Inlet Gas Hardware . 42 Cone Wash System . 45 Data System . 46 Computer Hardware . 46 Xcalibur Software . 47 MSQ Plus Mass Detector Server . 49 Tune Window . 50 Title Bar . 51 Menu Bar . 51 Toolbar . 51 Comms Indicator . 51 Scan Events Table . 52 Per Method Parameters Table . 52 Peak Display . 52 Status Bar . 52 Printer . 52 Daily Operation . 53 Before Operating the Mass Detector . 53 Checking the Nitrogen Supply . 53 Checking the Disk Space . 53 To determine the amount of available disk space . 53 Checking the Oil Level in the Oil Mist Filter . 54 After Operating the Mass Detector . 54 Flushing the API Probes . 54 To flush the capillary of the API probe . 55 Placing the System in the Off Mode . 55 Draining the Oil Mist Filter and Purging the Pump Oil . 55 To drain the oil mist filter and purge volatile contaminants from the oil in the forepump . 56 Emptying the Solvent Waste Bottles . ..

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Mass Spectrometer Detectors
Mass Spectrometer Detectors www.sge.com Ion Detectors for Virtually all Mass Spectrometry Applications Electron multipliers are used in a wide range of applications to Figure 2. Secondary Electron Emission detect and measure small signals of ions, electrons or photons. One of the main applications for an electron multiplier is for 6 the detection of ions in a mass spectrometer. ACTIVE FILM Multipliers manufactured by ETP ( a division of SGE Group 5 of Companies) are the result of 15 years experience in 4 supplying high performance electron multipliers for use in mass spectrometry applications. The performance of this 3 unique type of ion detector has seen it become widely used in almost all fields of mass spectrometry (including ICP-MS, 2 GC-MS, LC-MS, TOF and SIMS). 1 An electron multiplier is used to detect the presence of ion Secondary Electron Emissions signals emerging from the mass analyser of a mass 0 spectrometer. It is essentially the "eyes" of the instrument (see 0 100 200 300 400 500 Figure 1). The task of the electron multiplier is to detect Incident Electron Energy (eV) every ion of the selected mass passed by the mass filter. How The average number of secondary electrons emitted from the efficiently the electron multiplier carries out this task surface of an ETP electron multiplier plotted against the represents a potentially limiting factor on the overall system energy of the incident primary electron. sensitivity. Consequently the performance of the electron multiplier can have a major influence on the overall (often referred to as a channel electron multiplier or CEM).
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Microchannel Plate Detectors
Reprinted from Nuclear Instruments and Methods, Vol. 162, 1979, pages 587 to 601 MICROCHANNEL PLATE DETECTORS JOSEPH LADISLAS WIZA 1. Introduction typical. Originally developed as an amplification element for A microchannel plate (MCP) is an array of 104-107 image intensification devices, MCPs have direct sensitivity miniature electron multipliers oriented parallel to one to charged particles and energetic photons which has another (fig. 1); typical channel diameters are in the range extended their usefulness to such diverse fields as X-ray1) 10-100 µm and have length to diameter ratios (α) between and E.U.V.2) astronomy, e-beam fusion studies3) and of 40 and 100. Channel axes are typically normal to, or biased course, nuclear science, where to date most applications at a small angle (~8°) to the MCP input surface. The have capitalized on the superior MCP time resolution channel matrix is usually fabricated from a lead glass, characteristics4-6). treated in such a way as to optimize the secondary emission The MCP is the result of a fortuitous convergence of characteristics of each channel and to render the channel technologies. The continuous dynode electron multiplier walls semiconducting so as to allow charge replenishment was suggested by Farnsworth7) in 1930. Actual from an external voltage source. Thus each channel can be implementation, however, was delayed until the 1960s considered to be a continuous dynode structure which acts when experimental work by Oschepkov et al.8) from the as its own dynode resistor chain. Parallel electrical contact USSR, Goodrich and Wiley9) at the Bendix Research to each channel is provided by the deposition of a metallic Laboratories in the USA, and Adams and Manley10-11) at coating, usually Nichrome or Inconel, on the front and rear the Mullard Research Laboratories in the U.K.
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Characterization of Morphological and Chemical Properties of Scandium Containing
Characterization of Morphological and Chemical Properties of Scandium Containing Cathode Materials A dissertation presented to the faculty of the College of Arts and Sciences of Ohio University In partial fulfillment of the requirements for the degree Doctor of Philosophy Michael V. Mroz May 2020 © 2020 Michael V. Mroz. All Rights Reserved. 2 This dissertation titled Characterization of Morphological and Chemical Properties of Scandium Containing Cathode Materials by MICHAEL V. MROZ has been approved for the Department of Physics and Astronomy and the College of Arts and Sciences by Martin E. Kordesch Professor of Physics and Astronomy Florenz Plassmann Dean, College of Arts and Sciences 3 ABSTRACT MROZ, MICHAEL V., Ph.D., May 2020, Physics and Astronomy Characterization of Morphological and Chemical Properties of Scandium Containing Cathode Materials Director of Dissertation: Martin E. Kordesch Understanding thermionic cathodes is crucial for the future development of communication technologies operating at the terahertz frequency. Model cathode systems were characterized using multiple experimental techniques. These included Low Energy Electron Microscopy, X-Ray Photoemission Spectroscopy, and Auger Electron Spectroscopy. This was done to determine the mechanisms by which tungsten, barium, scandium, and oxygen may combine in order to achieve high current densities via thermionic emission. Barium and scandium films are found to dewet from the tungsten surfaces studied, and not diffuse out from bulk sources. The dewetted droplets were found to contribute the most to thermal emission. Barium oxide and scandium oxide are also found to react desorb from the emitting surface at lower temperatures then the metals themselves. The function of scandium in scandate cathodes was determined to act as an inhibitor to oxide formation.
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Modern Mass Spectrometry
Modern Mass Spectrometry MacMillan Group Meeting 2005 Sandra Lee Key References: E. Uggerud, S. Petrie, D. K. Bohme, F. Turecek, D. Schröder, H. Schwarz, D. Plattner, T. Wyttenbach, M. T. Bowers, P. B. Armentrout, S. A. Truger, T. Junker, G. Suizdak, Mark Brönstrup. Topics in Current Chemistry: Modern Mass Spectroscopy, pp. 1-302, 225. Springer-Verlag, Berlin, 2003. Current Topics in Organic Chemistry 2003, 15, 1503-1624 1 The Basics of Mass Spectroscopy ! Purpose Mass spectrometers use the difference in mass-to-charge ratio (m/z) of ionized atoms or molecules to separate them. Therefore, mass spectroscopy allows quantitation of atoms or molecules and provides structural information by the identification of distinctive fragmentation patterns. The general operation of a mass spectrometer is: "1. " create gas-phase ions "2. " separate the ions in space or time based on their mass-to-charge ratio "3. " measure the quantity of ions of each mass-to-charge ratio Ionization sources ! Instrumentation Chemical Ionisation (CI) Atmospheric Pressure CI!(APCI) Electron Impact!(EI) Electrospray Ionization!(ESI) SORTING DETECTION IONIZATION OF IONS OF IONS Fast Atom Bombardment (FAB) Field Desorption/Field Ionisation (FD/FI) Matrix Assisted Laser Desorption gaseous mass ion Ionisation!(MALDI) ion source analyzer transducer Thermospray Ionisation (TI) Analyzers quadrupoles vacuum signal Time-of-Flight (TOF) pump processor magnetic sectors 10-5– 10-8 torr Fourier transform and quadrupole ion traps inlet Detectors mass electron multiplier spectrum Faraday cup Ionization Sources: Classical Methods ! Electron Impact Ionization A beam of electrons passes through a gas-phase sample and collides with neutral analyte molcules (M) to produce a positively charged ion or a fragment ion.
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Joseph Ladislas Wiza, Microchannel Plate Detectors
Reprinted from Nuclear Instruments and Methods, Vol. 162, 1979, pages 587 to 601 MICROCHANNEL PLATE DETECTORS JOSEPH LADISLAS WIZA 1. Introduction only by the channel dimensions and spacings; 12 mm diameter channels with 15 mm center-to-center spacings are A microchannel plate (MCP) is an array of 104-107 typical. miniature electron multipliers oriented parallel to one Originally developed as an amplification element for another (fig. 1); typical channel diameters are in the range image intensification devices, MCPs have direct sensitivity 10-100 mm and have length to diameter ratios (a) between to charged particles and energetic photons which has 40 and 100. Channel axes are typically normal to, or biased extended their usefulness to such diverse fields as X-ray1) at a small angle (~8°) to the MCP input surface. The and E.U.V.2) astronomy, e-beam fusion studies3) and of channel matrix is usually fabricated from a lead glass, course, nuclear science, where to date most applications treated in such a way as to optimize the secondary emission have capitalized on the superior MCP time resolution characteristics of each channel and to render the channel characteristics4-6). walls semiconducting so as to allow charge replenishment The MCP is the result of a fortuitous convergence of from an external voltage source. Thus each channel can be technologies. The continuous dynode electron multiplier considered to be a continuous dynode structure which acts was suggested by Farnsworth7) in 1930. Actual as its own dynode resistor chain. Parallel electrical contact implementation, however, was delayed until the 1960s to each channel is provided by the deposition of a metallic when experimental work by Oschepkov et al.8) from the coating, usually Nichrome or Inconel, on the front and rear USSR, Goodrich and Wiley9) at the Bendix Research surfaces of the MCP, which then serve as input and output Laboratories in the USA, and Adams and Manley10-11) at electrodes, respectively.
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Mass Spectrometry
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Electron Transfer Dissociation and Collision-Induced Dissociation
ELECTRON TRANSFER DISSOCIATION AND COLLISION-INDUCED DISSOCIATION MASS SPECTROMETRY OF METALLATED OLIGOSACCHARIDES by RANELLE MARIE SCHALLER-DUKE CAROLYN J. CASSADY, COMMITTEE CHAIR JOHN B. VINCENT SHANE C. STREET ŁUKASZ CIEŚLA SHANLIN PAN A DISSERTATION Submitted in partial fulfillment of the requirements for the degree of Doctor of Philosophy in the Department of Chemistry and Biochemistry in the Graduate School of The University of Alabama TUSCALOOSA, ALABAMA 2019 Copyright Ranelle Marie Schaller-Duke 2019 ALL RIGHTS RESERVED ABSTRACT Investigations of metallated glycans through tandem mass spectrometry (MS/MS) can further the field of glycomics, the sequencing of the human glycome. The field is hindered by the lack of an analytical technique that can determine all the stereo-diverse features of carbohydrates. In this dissertation, electron transfer dissociation (ETD) and collision-induced dissociation (CID) are utilized with metal-adducted oligosaccharides to explore the potential of these techniques to sequence glycans. The resulting mass spectra provide significant insight and information about the structure of oligosaccharides and how to distinguish between these complicated isomeric species. Using univalent, divalent, and trivalent transition metal adducts is valuable to glycan analysis. The ETD process requires multiply charged ions, which do not form via protonation for neutral glycans, and CID of protonated glycans produces uninformative glycosidic bond cleavage. The univalent and trivalent metals investigated did not produce ions sufficient for ETD studies, but CID of the trivalent metal adducts showed significant fragmentation. Dissociation of [M + Met]2+ from the divalent metals formed various fragment ions with ETD producing more cross-ring and internal cleavages, which are necessary for structural analysis.
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LTQ Series Hardware Manual
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Secondary Ion Mass Spectrometry (Sims)
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