Ion Collectors and Detectors
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Development of a Method for Xenon Determination in the Microstructure of High Burn-Up Nuclear Fuel
Diss. ETH No. 17527 Development of a Method for Xenon Determination in the Microstructure of High Burn-up Nuclear Fuel A dissertation submitted to the SWISS FEDERAL INSTITUTE OF TECHNOLOGY ZURICH for the degree of Dr. sc. ETH presented by MATTHIAS ISTVAN HORVATH Dipl. Phys. ETH born 24 August 1974 citizen of Châtillon (FR), Männedorf (ZH) - Switzerland citizen of Hungary accepted on the recommendation of Prof. Dr. D. Günther, examiner Prof. Dr. A. Wokaun, co-examiner Prof. Dr. Ch. Heinrich, co-examiner Dr. Ch. Hellwig, co-examiner 2008 II III Acknowledgements As many major work, this thesis could not have been performed and written, without the help and support of numerous people. This is especially true since this work was carried out at PSI and some experiments also at ETH combining different fields of research. I would like to send a special thank to my thesis advisor, Prof. Dr. Detlef Günther, and my supervisor Dr. Christian Hellwig for their support of my work at ETH and PSI. I am grateful to Dr. Marcel Guillong, with whom I got into the "world of LA-ICP-MS", and who’s experience was a great benefit. I would also to thank the members of the groups of Dr. Ines Günther-Leopold (Isotope and Element Analysis), Dr. Didier Gavillet (Surface and Solid State Materials), Daniel Kuster (Hot Cell Experiments), Dr. Johannes Bertsch (Core Safety Material Behavior) at PSI, and the trace element group of Prof. Dr. Detlef Günther at ETH. Without their support and the possibility using their infrastructure, this thesis could not be realized. -
Structural Amd Analytical Studies by Tandem Mass Spectrometry
STRUCTURAL AMD ANALYTICAL STUDIES BY TANDEM MASS SPECTROMETRY A Thesis submitted by TRACEY MADDEN for the degree of Doctor of Philosophy in the University of London Faculty of Science Department of Pharmaceutical Chemistry The School of Pharmacy University of London ProQuest Number: U556261 All rights reserved INFORMATION TO ALL USERS The quality of this reproduction is dependent upon the quality of the copy submitted. In the unlikely event that the author did not send a com plete manuscript and there are missing pages, these will be noted. Also, if material had to be removed, a note will indicate the deletion. uest ProQuest U556261 Published by ProQuest LLC(2017). Copyright of the Dissertation is held by the Author. All rights reserved. This work is protected against unauthorized copying under Title 17, United States C ode Microform Edition © ProQuest LLC. ProQuest LLC. 789 East Eisenhower Parkway P.O. Box 1346 Ann Arbor, Ml 48106- 1346 CONTENTS CHAPTER 1: INTRODUCTION 1.1 Tandem Mass Spectrometry ................... 1 REFERENCES ................................. 4 CHAPTER 2: THEORY 2.1 Mass Spectrometry ......................... 5 2.2 Formation of the Molecular Ion ............ 8 2.2.1 Vertical and Adiabatic Ionisation Potentials ......................... 9 2.2.2 Ionisation Efficiency Curve .......... 9 2.2.3 Appearance Energy ................... 10 2.3 Quasi Equilibrium Theory ................. 14 2.4 Fragmentation ............................ 16 2.4.1 Stevenson's Rule .................... 17 2.5 Rearrangement ............................ 19 2.6 Ion Stability ............................ 20 2.6.1 Stable Ions ......................... 20 2.6.2 Unstable Ions ....................... 21 2.6.3 Metastable Ions ..................... 21 2.6.3.1 Kinetic Energy Release ......... 22 2.6.3.2 Metastable Peak Shapes ....... -
20.5 Ion Detectors
20.5 Ion Detectors • the Faraday cup neutralizes ions to provide a high-precision measurement • the electron multiplier generates a pulse of current for each ion • the photon multiplier uses conversion dynodes to monitor both positive and negative ions • the two multipliers are capable of fast measurements, thus compatible with TOF or Fourier transform methods 20.5 : 1/4 Faraday Cup slit Ions exiting the analyzer are slowed by Faraday cup a positive potential and impact the ion + grounded electrode. At the electrode beam + they are __________ by electrons that RL travel through the load resistor. This ion suppressor causes a voltage across the load resistor that is measured by a high input impedance voltmeter. The impacted electrode is at an angle so that any secondary ions that are created are _____________ by the grounded wall. Of all ion detectors, the Faraday cup provides the most precise relationship between the number of ions exiting the analyzer and the electrical measurement. It is used in __________ experiments such as isotope dilution. Because very small currents are measured, the Faraday cup cannot be used for experiments involving rapid scanning. 20.5 : 2/4 Electron Multiplier ion beam An electron multiplier is constructed just like a photomultiplier but without 16e- 4e- 3 - a _______________. It has dynodes 10 e RL constructed from a Cu/Be alloy, which dynodes is a good secondary electron emitter. +V The dynode potentials are such that the first is grounded and each subsequent one is 100 V more positive. This makes the voltage measurement a little tricky because one end of the load resistor is connected to positive _____________. -
Copyrighted Material
Contents Preface................................................................................................... xix Acknowledgments .............................................................................. xxiii Chapter 1 Introduction......................................................................... 1 I. Introduction ..........................................................................................................3 1. The Tools and Data of Mass Spectrometry...............................................4 2. The Concept of Mass Spectrometry..........................................................4 II. History ...................................................................................................................9 III. Some Important Terminology Used In Mass Spectrometry...........................22 1. Introduction..............................................................................................22 2. Ions..........................................................................................................22 3. Peaks ......................................................................................................23 4. Resolution and Resolving Power.............................................................25 IV. Applications........................................................................................................28 1. Example 1-1: Interpretation of Fragmentation Patterns (Mass Spectra) to Distinguish Positional Isomers .........................................................................29 -
Lecture 15 Spring 2005
Geol. 655 Isotope Geochemistry Lecture 15 Spring 2005 ANALYTICAL METHODOLOGY THE MASS SPECTROMETER In most cases, isotopic abundances are measured by mass spectrometry. The exceptions are, as we have seen, short-lived radioactive isotopes, the abundances of which are determined by measuring their decay rate, and in fission track dating, where the abundance of 238U is measured, in effect, by in- ducing fission. (Another exception is spectroscopic measurement of isotope ratios in stars. Frequencies of electromagnetic emissions of the lightest elements are sufficiently dependent on nuclear mass that emissions from different isotopes can be resolved. We will discuss this when we consider stable iso- topes.) A mass spectrometer is simply a device that can separate atoms or molecules according to their mass. There are a number of different kinds of mass spectrometers operating on different principles. Undoubtedly the vast majority of mass spectrometers are used by chemists for qualitative or quantita- tive analysis of organic compounds. We will focus exclusively, however, on mass spectrometers used for isotope ratio determination. Most isotope ratio mass spectrometers are of a similar design, the magnetic-sector, or Nier mass spectrometer*, a schematic of which is shown in Figure 15.1. It consists of three essential parts: an ion source, a mass analyzer and a detector. There are, however, several variations on the design of the Nier mass spectrometer. Some of these modifications relate to the spe- cific task of the instrument; others are evolutionary improvements. We will first consider the Nier mass spectrometer, and then briefly consider a few other kinds of mass spectrometers. -
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. -
C7895 Mass Spectrometry of Biomolecules Schedule of Lectures
C7895 Mass Spectrometry of Biomolecules Schedule of lectures For schedule, please see a separate file with the course outline. Jan Preisler Consulting The last lecture. Please contact me in advance to make an appointment. Chemistry Dept. 312A14, tel.: 54949 6629, [email protected] This material is just an outline; students are advised to print this outline and write down notes durin the lectures. The material will be updated during The course is focused on mass spectrometry of biomolecules, i.e. ionization the semester. techniques MALDI and ESI, modern mass analyzers, such as time-of-flight MS or ion traps and bioanalytical applications. However, the course covers much broader area, including inorganic ionization techniques, virtually all Supporting study material: types of mass analyzers and hardware in mass spectrometry. • J. Gross, Mass Spectrometry, 3rd ed. Springer-Verlag, 2017 • J. Greaves, J. Roboz: Mass Spectrometry for the Novice, CRC Press, 2013 • Edmond de Hoffmann, Vincent Stroobant: Mass Spectrometry: Principles and Applications, 3rd Edition, John Wiley & Sons, 2007 Mass spectrometry of biomolecules 2018 1 Mass spectrometry of biomolecules 2018 2 1 2 Content I. Introduction 1 II. Ionization methods and sample introduction III. Mass analyzers IV. Biological applications of MS V. Example problems Introduction to Mass spectrometry. Brief History of MS. A Survey of Methods and Instrumentation. Basic Concepts in MS: Resolution, Sensitivity. Isotope patterns of organic molecules. Ionization Techniques and Sample Introductin. Electron Impact Mass spectrometry of biomolecules 2018 3 Ionization (EI). Chemical Ionization (CI) 3 4 I. Introduction Study Material • Information sources about mass spectrometry Lecture notes • Brief history of mass spectrometry, a survey of methods and Advice: please take notes, but do not copy the slides; the English slides will instrumentation be provided at the end of the semester. -
Article Is Available Ca
Geochronology, 2, 343–354, 2020 https://doi.org/10.5194/gchron-2-343-2020 © Author(s) 2020. This work is distributed under the Creative Commons Attribution 4.0 License. Expanding the limits of laser-ablation U–Pb calcite geochronology Andrew R. C. Kylander-Clark Department of Earth Science, University of California, Santa Barbara, CA 93106, USA Correspondence: Andrew R. C. Kylander-Clark ([email protected]) Received: 30 May 2020 – Discussion started: 30 June 2020 Accepted: 20 September 2020 – Published: 23 November 2020 Abstract. U–Pb geochronology of calcite by laser-ablation 1 Introduction inductively coupled plasma mass spectrometry (LA-ICPMS) is an emerging field with potential to solve a vast array Calcite U–Pb geochronology by laser-ablation inductively of geologic problems. Because of low levels of U and Pb, coupled plasma mass spectrometry (LA-ICPMS) is a rela- measurement by more sensitive instruments, such as those tively new technique with untapped potential for solving nu- with multiple collectors (MCs), is advantageous. However, merous geochronologic problems from the timing of faulting whereas measurement of traditional geochronometers (e.g., (e.g., Roberts and Walker, 2016; Nuriel et al., 2017; Good- zircon) by MC-ICPMS has been limited by detection of the fellow et al., 2017) and the age of ore deposits (Burisch daughter isotope, U–Pb dating of calcite can be limited by et al., 2017) to paleoclimate, sedimentation, and diagene- detection of the parent isotope if measured on a Faraday sis (e.g., Mangenot et al., 2018; Rasbury et al., 1997; Hoff detector. The Nu P3D MC-ICPMS employs a new detec- et al., 1995; Winter and Johnson, 1995; Wang et al., 1998; tor array to measure all isotopes of interest on Daly detec- Rasbury et al., 1998). -
Analytical Chemistry, Strategic Exercise: Organic Aerosol Analysis
WIR SCHAFFEN WISSEN –HEUTE FÜR MORGEN Analytical Chemistry, Strategic exercise: Organic aerosol analysis Urs Baltensperger Laboratory of Atmospheric Chemistry, Paul Scherrer Institute, Villigen , Switzerland ETHZ, HS 2020, 8.12.2020 Aerosol size distribution, and sources and sinks Chemical composition of PM1 in Zurich in winter Energiespiegel 19/2008 http://gabe.web.psi.ch/pdfs/Energiespiegel_19_e.pdf Today’s task: Organic aerosol analysis Page 4 The state of the art in 2009 Hallquist et al., ACP 2009 Traditional methods can identify only a fraction of organics Rogge et al., 1993 Most detailed analysis performed with off-line methods: More than 10‘000 different organic compounds isolated with GCxGC-TOF/MS Hamilton et al., 2004 NB: isolated ≠ identified…. Besides extraction, also thermal desorption is applied: TAG (Goldstein et al., 2008) Organic acids formed in the photooxidation of -pinene All acids found in aerosol phase. Some of them are highly volatile (e.g., formic, acetic acid) and not expected to be there. Probably hydrolysis of oligomers Fisseha et al., Anal. Chem. 2004 Developments since 2009 EESI CHARON‐ PTRMS FIGAERO -I-CIMS Adapted from Hallquist et al., 2009 9 Required for mass spectrometry: ionization of individual molecules • For gas phase: relatively easy (avoid fragmentation, clustering) • For aerosol particles: Much more difficult: either dissolution in a solvent or evaporation - Problem with dissolution: only the soluble fraction accessible - Problem with evaporation: fragmentation Page 10 What is Mass Spectrometry -
QMG 422 Analyzers
Operating Instructions Incl. Declaration of Conformity QMG 422 Analyzers BG 805 983 BE (0112) 1 Product Identification In all communications with Pfeiffer Vacuum, please specify the information on the product nameplate. For convenient reference copy that information into the space provided below. Pfeiffer Vacuum, D-35614 Asslar Typ: No: F-No: Validity This document applies to the QMA 400, QMA 410, QMA 430 with Faraday cup or 90° off-axis SEM and Faraday cup and with the ion sources described in this document. Illustrations If not indicated otherwise in the legends, the illustrations in this document corre- spond to the QMA 400 with 90° off-axis SEM. They apply to other types by analogy. Designations The short designation "QMA" is used for the QMA 400, QMA 410 and QMA 430. The short designation "QMH" is used for the QMH 400 and QMH 410. In contrast to the operating instructions for the QMG 422, these instructions follow the same conventions as the Pfeiffer QuadStar™ 422 operating instructions. The parameters are marked with quotation marks ("…") e.g. "Resolution". Technical changes We reserve the right to make technical changes without prior notice. Intended Use The QMA 400, QMA 410 and QMA 430 Analyzers are used for gas analysis in high vacuum. They are part of the QMG 422 mass spectrometer system and may only be used in connection with equipment belonging to that system. The operating instructions of all system components must be strictly followed. 2 BG 805 983 BE (0112) QMA4x0.oi Contents Product Identification 2 Validity 2 Intended -
Electron Microscopy Are the Beam Damaging Effects That Can Arise from Interactions Between the Primary High Energy Electron Beam and the Sample
Thermal in situ TEM experiment on nanoscale indium islands Estimation of Electron Beam Heating Effect Master’s thesis in Applied Physics REN QIU Department of Physics CHALMERS UNIVERSITY OF TECHNOLOGY Gothenburg, Sweden 2017 Master’s thesis 2017 Thermal in situ TEM experiment on nanoscale indium islands Estimation of Electron Beam Heating Effect REN QIU Department of Physics Eva Olsson Group Chalmers University of Technology Gothenburg, Sweden 2017 Thermal in situ TEM Experiment on Nanoscale Indium Islands Estimation of Electron Beam Heating Effect Master Thesis within the Masters Programme of Applied Physics © REN QIU, 2017. Supervisor: Eva Olsson, Norvik Voskanian, Lunjie Zeng, Department of Physics Examiner: Eva Olsson, Department of Physics Master’s Thesis 2017 Department of Physics Eva Olsson Group Chalmers University of Technology SE-412 96 Gothenburg Telephone + 46(0)73-732 4883 Cover: Top left: Indium islands segmentation by watershed algorithm based on the bright field TEM image. Top right: Dark field image of the in situ melting experiment where the indium islands with bright pixels are melted and the ones with dark pixels are in solid state. Bottom left: Nano-scale gold tip fabricated through electrochemical etching. Bottom right: A simple Faraday cup made on the gold tip by focus ion beam (FIB) method. Printed by Chalmers Reproservice Gothenburg, Sweden 2017 iv Thermal in situ TEM Experiment on Nanoscale Indium Islands Estimation of Electron Beam Heating Effect REN QIU Department of Physics Chalmers University of Technology Abstract One of the limitations of transmission electron microscopy are the beam damaging effects that can arise from interactions between the primary high energy electron beam and the sample. -
Mass Spectrometer Hardware for Analyzing Stable Isotope Ratios
Handbook of Stable Isotope Analytical Techniques, Volume-I P.A. de Groot (Editor) © 2004 Elsevier B.V. All rights reserved. CHAPTER 38 Mass Spectrometer Hardware for Analyzing Stable Isotope Ratios Willi A. Brand Max-Planck-Institute for Biogeochemistry, PO Box 100164, 07701 Jena, Germany e-mail: [email protected] Abstract Mass spectrometers and sample preparation techniques for stable isotope ratio measurements, originally developed and used by a small group of scientists, are now used in a wide range of fields. Instruments today are typically acquired from a manu- facturer rather than being custom built in the laboratory, as was once the case. In order to consistently generate measurements of high precision and reliability, an extensive knowledge of instrumental effects and their underlying causes is required. This con- tribution attempts to fill in the gaps that often characterize the instrumental knowl- edge of relative newcomers to the field. 38.1 Introduction Since the invention of mass spectrometry in 1910 by J.J. Thomson in the Cavendish laboratories in Cambridge(‘parabola spectrograph’; Thompson, 1910), this technique has provided a wealth of information about the microscopic world of atoms, mole- cules and ions. One of the first discoveries was the existence of stable isotopes, which were first seen in 1912 in neon (masses 20 and 22, with respective abundances of 91% and 9%; Thomson, 1913). Following this early work, F.W. Aston in the same laboratory set up a new instrument for which he coined the term ‘mass spectrograph’ which he used for checking almost all of the elements for the existence of isotopes.