1 Construction and Testing of an Atmospheric-Pressure
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Characterization of a Glow Discharge Ion Source for the Mass Spectrometric Analysis of Organic Compounds
Characterization of a Glow Discharge Ion Source for the Mass Spectrometric Analysis of Organic Compounds D. Carazzato and M. J. Bertrand Regional Center for Mass Spectrometry, Department of Chemistry, University of Montreal, Montreal, Canada A glow discharge ion source has been constructed for the mass spectrometric analysis of organic compounds. Characterization of the source has been made by studying the effect of pressure and discharge current on ionic distributions by anodic ion sampling along the discharge axis. Ion and electron densities and electronic temperatures have been calculated by using the single Langmuir probe technique to correlate the extraction efficiency with measured ion distributions and gain some insight into the ionization of organic molecules. The spectra obtained for several classes of organic compounds show that formation of parent-molecular ions by proton transfer, resulting partly from the background water molecules, is a major low energy process while charge transfer, Penning ionization, and electron ionization are probably responsible for the fragmentation observed. The spectra result from the simultaneous occurrence of high and low energy reactions, and their structural information content is very high, yielding both molecular and extensive fragment ion information. The glow discharge ion source has proved to be essentially maintenance-free, easy to operate, stable, and can be used at reasonable mass resolution (up to 7000). The source also provides picogram range detection limits and has a linear response range of about six orders of magnitude, which makes it an interesting ion source for routine analysis. Preliminary work conducted with chromatographic interfaces indicates that its use can be easily extended to both gas and liquid chromatography. -
Calibration Factors for Fast Flow Glow Discharge Mass Spectrometry (FF-GD-MS) in Continuous and Pulsed Mode
POSTER NOTE 30687 Calibration factors for Fast Flow Glow Discharge Mass Spectrometry (FF-GD-MS) in continuous and pulsed mode Authors: Torsten Lindemann, Joachim Hinrichs, Nicholas Lloyd, Thermo Fisher Scientific, Bremen, Germany Abstract The Thermo Scientific™ Element GD Plus™ GD-MS was used to measure a set of 13 iron based certified reference materials. Calibration factors for 29 elements were obtained in continuous and pulsed mode. In continuous mode operation, the calibration factors obtained confirm most of those factors previously used for semiquantitative analyses. However, significantly improved Introduction accuracy can be expected for Ti, V, Cr, and Zr with the Sector field glow discharge mass spectrometry is data obtained during this study. applied for the analysis of high purity bulk metals and alloys, semiconductors and ceramics, especially by the In pulsed mode operation, the calibration factors for many aerospace, electronics and photovoltaic industries. elements are similar to the ones in continuous mode. In detail though, some elements show lower calibration The Element GD Plus GD-MS features a fast flow glow factors. Therefore, a dedicated RSF table for pulsed mode discharge source that can be operated in continuous is recommended to support accurate routine operation for or pulsed mode. Continuous mode operation offers the semiquantitative analyses. advantage of high sputter rates to remove contaminated surface layers quickly. Also, the widely applied set of Most elements are analyzed within the accuracy range calibration factors (Standard RSF = general Relative of ±30 %, considered to be typical for semiquantitative Sensitivity Factors) is based on continuous mode operation. GD-MS analyses. For improved accuracy, the use of a dedicated set of calibration factors is advisable. -
The Use of Dc Glow Discharges As Undergraduate Educational Tools Stephanie A
The use of dc glow discharges as undergraduate educational tools Stephanie A. Wissel, Andrew Zwicker, Jerry Ross, and Sophia Gershman Citation: American Journal of Physics 81, 663 (2013); doi: 10.1119/1.4811435 View online: http://dx.doi.org/10.1119/1.4811435 View Table of Contents: http://scitation.aip.org/content/aapt/journal/ajp/81/9?ver=pdfcov Published by the American Association of Physics Teachers Articles you may be interested in Motivating Students to Do Homework Phys. Teach. 52, 295 (2014); 10.1119/1.4872413 Measuring the Effectiveness of Simulations in Preparing Students for the Laboratory Phys. Teach. 51, 113 (2013); 10.1119/1.4775536 New insights into student understanding of complete circuits and the conservation of current Am. J. Phys. 81, 134 (2013); 10.1119/1.4773293 Conductance quantization: A laboratory experiment in a senior-level nanoscale science and technology course Am. J. Phys. 81, 14 (2013); 10.1119/1.4765331 A low-cost spatial light modulator for use in undergraduate and graduate optics labs Am. J. Phys. 80, 211 (2012); 10.1119/1.3666834 This article is copyrighted as indicated in the article. Reuse of AAPT content is subject to the terms at: http://scitation.aip.org/termsconditions. Downloaded to IP: 198.35.1.48 On: Fri, 20 Jun 2014 16:13:40 The use of dc glow discharges as undergraduate educational tools Stephanie A. Wissela) and Andrew Zwickerb) Princeton Plasma Physics Laboratory, Princeton, New Jersey 08543 Jerry Ross Shawnee State University, Portsmouth, Ohio 45662 Sophia Gershman Advanced Research Innovation in Science Education (ARISE), Scotch Plains, New Jersey 07076 (Received 12 October 2012; accepted 4 June 2013) Plasmas have a beguiling way of getting students interested in physics. -
The Use of Glow Discharge Optical Emission Spectroscopy to Quantify Internal Carburization in Supercritical CO2
The 6th International Supercritical CO2 Power Cycles Symposium March 27 - 29, 2018, Pittsburgh, Pennsylvania The Use of Glow Discharge Optical Emission Spectroscopy to Quantify Internal Carburization in Supercritical CO2 Michael J. Lance Donovan N. Leonard Bruce A. Pint Senior R&D Staff Member R&D Staff Member Group Leader Oak Ridge National Laboratory Oak Ridge National Laboratory Oak Ridge National Laboratory Oak Ridge, TN 37831-6068 Oak Ridge, TN 37831-6064 Oak Ridge, TN 37831-6156 [email protected] [email protected] [email protected] Michael J. Lance is a Senior Research and Development Staff Member in Oak Ridge National Laboratory’s Materials Science and Technology Division. He received a B.S. in 1992 from Alfred University and an M.S. and PhD from Rutgers University in 1998 in Ceramic Science and Technology. He joined Oak Ridge National Laboratory as a staff member in 1998 and has been active in several research areas including emissions control technologies for diesel engines, high- temperature oxidation and heat exchanger fouling. Donovan N. Leonard is a Senior Technical Staff Member in the Materials Science & Technology Division at Oak Ridge National Laboratory. He received his Ph.D. in Materials Science & Engineering from North Carolina State University in 2002 and joined ORNL in 2007. Currently his research involves applying advanced microscopy and microanalysis methods to energy related materials at length scales from the atomic level to the macro scale. More specifically, aberration corrected STEM/EELS of quantum materials in addition to EPMA/WDS, EBSD and EDS analysis of materials for fossil, fusion and solar applications. Bruce A. -
Simultaneous Analysis of Drugs in Forensic Cases by Liquid Chromatography–High‑Resolution Orbitrap Mass Spectrometry
Chromatographia (2020) 83:53–64 https://doi.org/10.1007/s10337-019-03814-w ORIGINAL Simultaneous Analysis of Drugs in Forensic Cases by Liquid Chromatography–High‑Resolution Orbitrap Mass Spectrometry Siti U. Mokhtar1 · Chadin Kulsing2,3,4 · Jalal T. Althakafy2,5 · Alex Kotsos6 · Olaf H. Drummer6,7 · Philip J. Marriott2 Received: 10 May 2019 / Revised: 23 September 2019 / Accepted: 15 October 2019 / Published online: 31 October 2019 © Springer-Verlag GmbH Germany, part of Springer Nature 2019 Abstract In the present study, liquid chromatography coupled to an Orbitrap mass spectrometer (HPLC–Q-Orbitrap MS) was used as an approach for identifcation and quantifcation of 113 drugs simultaneously in biological samples (whole blood/plasma/ serum). Samples were prepared using liquid–liquid extraction conducted using a trizma/isopropanol/butyl chloride bufer system. Reversed-phase separation employing a column (50 × 2.1 mm) packed with 2.6-μm C18 particles was then performed under gradient elution with mobile phase composition consisting of acetic acid and aqueous-acetonitrile mixtures with the acetonitrile content ranging from 10 to 100% v/v. Compounds were detected with high-resolution MS operated in full scan mode having a mass accuracy < 5 ppm. In this study, isobaric compounds (same nominal mass) were easily distinguished and identifed by their diferent retention times. Extracted ion chromatograms (XICs) with narrow mass tolerance window (5 ppm) 2 provided analysis with acceptable linearity (r ) ranged from 0.9530 to 1, low limits of detection (LOD) (0.02–39 ng mL−1) and low limit of quantifcation (LOQ) (0.1–130 ng mL−1). The developed method was applied to successfully analyse drugs in 26 blood samples from positive forensic cases and proved that this technique was able to detect analytes at trace level. -
Multiplatform Investigation of Plasma and Tissue Lipid Signatures of Breast Cancer Using Mass Spectrometry Tools
International Journal of Molecular Sciences Article Multiplatform Investigation of Plasma and Tissue Lipid Signatures of Breast Cancer Using Mass Spectrometry Tools 1, 2, 2 3 Alex Ap. Rosini Silva y, Marcella R. Cardoso y , Luciana Montes Rezende , John Q. Lin , Fernando Guimaraes 2 , Geisilene R. Paiva Silva 4, Michael Murgu 5, Denise Gonçalves Priolli 1, Marcos N. Eberlin 6, Alessandra Tata 7, Livia S. Eberlin 3 , Sophie F. M. Derchain 2 and Andreia M. Porcari 1,* 1 Postgraduate Program of Health Sciences, São Francisco University, Bragança Paulista SP 12916-900, Brazil; [email protected] (A.A.R.S.); [email protected] (D.G.P.) 2 Department of Gynecological and Breast Oncology, Women’s Hospital (CAISM), Faculty of Medical Sciences, State University of Campinas (UNICAMP), Campinas SP 13083-881, Brazil; [email protected] (M.R.C.); [email protected] (L.M.R.); [email protected] (F.G.); [email protected] (S.F.M.D.) 3 Department of Chemistry, The University of Texas at Austin, Austin, TX 78712, USA; [email protected] (J.Q.L.); [email protected] (L.S.E.) 4 Laboratory of Molecular and Investigative Pathology—LAPE, Women’s Hospital (CAISM), Faculty of Medical Sciences, State University of Campinas (UNICAMP), Campinas SP 13083-881, Brazil; [email protected] 5 Waters Corporation, São Paulo, SP 13083-970, Brazil; [email protected] 6 School of Engineering, Mackenzie Presbyterian University, São Paulo SP 01302-907, Brazil; [email protected] 7 Laboratorio di Chimica Sperimentale, Istituto Zooprofilattico Sperimentale delle Venezie, Viale Fiume 78, 36100 Vicenza, Italy; [email protected] * Correspondence: [email protected]; Tel.: +55-11-2454-8047 These authors contributed equally to this work. -
Modern Real Mass Spectrometry
“Real” (Modern) Mass Spectrometry (Part I) Alex J. Roche 1 MS is fundamentally important • If you want to publish a new compound, 3 pieces of data are required: – relevant NMR (H, C, F, P, Pt, N, D, B, ...) – Mass Spectrometry (low resolution) – Elemental Analysis (CHN) or HRMS • Confirmation of a compound usually requires the 1st two • Industrially, GCMS / HPLCMS is the most common general Chemical Identification / Characterization tool • ACS accreditation guidelines state “instruments and equipment in a good undergraduate chemistry program include …gas chromatography mass spectrometry (GC-MS), and apparatus or instruments for Mass Spectrometry”. 2 Mass Spectrometry “What do you know about that ?” • Basic concept ? (what is it?) • What’s the point ? (what information does it provide?) • Underlying physics ? (why does it work?) • Underlying mechanics ? (how does it work?) 3 What we (I) teach Ions are generated, bent by magnetic field, and separated according to m/z ratio. → molecular weight information, and 4 structural information Agilent Quote (After significant bartering) $228,000 = Agilent Technologies Triple Quad HPLCMS with Multimode Source Instrument. MOST COMMON MODERN STANDARD MS INSTRUMENT 5 • Where is the triple quad ? • Where is the ESI or APCI? 6 • “...This type of ionization is compatible with triple quadrupole and ion-trap analyzers. Not so much with magnetic sector instruments (if you can still find one)...” 7 Photographic Mass Spec Trivia plate • 1803 Dalton “Mass consists of atoms...” • 1911 Thompson 1st mass spectrometer • 1940 Berry Electron Impact Ionization for organics • 1980 ESI, FAB, MALDI • Up to current day, MS fundamental characterization tool. • 2002 Nobel Prize MALDI / ESI (Tanaka / Fenn) •(4th MS area Nobel Prize) • Mass is measured in a.m.u. -
Mass Spectrometer Business Presentation Materials
Mass Spectrometer Business Presentation Materials Hiroto Itoi, Corporate Officer Deputy General Manager of the Analytical & Measuring Instruments Division Shimadzu Corporation Jul. 3, 2018 Contents I. Introduction • Expansion of Mass Spectrometry ………………………………………………………………… p.3 • History of Shimadzu's Growth in Mass Spectrometry …………………………………………… p.5 II. Overview of Mass Spectrometers • Operating Principle, Demand Trends, and Vendors ……………………………………………… p.9 • Mass Spectra ………………………………………………………………………………………… p.10 • Configuration of Mass Spectrometers …………………………………………………………… p.11 • Ionization …………………………………………………………………………………………… p.12 • Mass Separation …………………………………………………………………………………… p.14 III. Shimadzu's Mass Spectrometer Business • Product Type ………………………………………………………………………………………… p.17 • Application Software ………………………………………………………………………………… p.18 • Growth Strategy for Mass Spectrometer Business ……………………………………………… p.19 • Expand/Improve Product Lines …………………………………………………………………… p.20 • Measures to Expand Application Fields …………………………………………………………… p.24 • Measures to Automate Data Processing Using AI ……………………………………………… p.25 IV. Summary • Future Direction ……………………………………………………………………………………… p.26 July 2018 Mass Spectrometer Business Presentation Materials 2 I. Introduction Expansion of Mass Spectrometry (1) Why Mass Spectrometry? Mass spectrometry is able to analyze a wide variety of compounds with high accuracy and high efficiency (simultaneous multicomponent analysis). It offers superior characteristics that are especially beneficial in the following fields, -
Advantages of the LTQ Orbitrap for Protein Identification in Complex Digests
Application Note: 386 Advantages of the LTQ Orbitrap for Protein Identification in Complex Digests Rosa Viner, Terry Zhang, Scott Peterman, and Vlad Zabrouskov, Thermo Fisher Scientific, San Jose, CA, USA Introduction Materials and Methods Key Words Comprehensive, accurate identification of proteins in Sample Preparation • LTQ Orbitrap complex sample mixtures is an important fundamental capability for any proteomics research laboratory. Technology Ten µL of E. coli cell lysate diluted 20-fold with 6 M • Peptide advancements in both hardware and software continue to guanidine HCl in 50 mM ammonium bicarbonate (pH 8.0) Sequencing expand and refine our view of any proteomic system in was reduced with 5 mM DTT, alkylated with 25 mM iodoacetic acid and digested at 37 °C for 16 hours. • Protein terms of protein identities and their post-translational Identification modifications (PTMs). It has been suggested that the very HPLC recent ability to routinely obtain accurate mass measurements Column: C18 Packed tip, 75 µm x 75 mm (QSTAR Elite); • PTMs (< 5 ppm RMS) on precursor and MS/MS fragment ions C18 column, 75 µm x 100 mm (LTQ Orbitrap XL) in proteomic experiments should lead to unprecedented Mobile phase A: 0.1% Formic Acid in Water with accuracy in the ability to identify and characterize proteins.1 2% Acetonitrile This paper compares alternative approaches to this Mobile phase B: 0.1% Formic Acid in Acetonitrile challenging application using two high performance Flow Rate: 300 nL/min platforms for proteomics: a QqTOF instrument (QSTAR® Gradient: 5% B to 35% B in 90 min Elite from Applied Biosystems) and a hybrid linear ion trap- orbitrap instrument (Thermo Scientific LTQ Orbitrap XL). -
Electron Ionization
Chapter 6 Chapter 6 Electron Ionization I. Introduction ......................................................................................................317 II. Ionization Process............................................................................................317 III. Strategy for Data Interpretation......................................................................321 1. Assumptions 2. The Ionization Process IV. Types of Fragmentation Pathways.................................................................328 1. Sigma-Bond Cleavage 2. Homolytic or Radical-Site-Driven Cleavage 3. Heterolytic or Charge-Site-Driven Cleavage 4. Rearrangements A. Hydrogen-Shift Rearrangements B. Hydride-Shift Rearrangements V. Representative Fragmentations (Spectra) of Classes of Compounds.......... 344 1. Hydrocarbons A. Saturated Hydrocarbons 1) Straight-Chain Hydrocarbons 2) Branched Hydrocarbons 3) Cyclic Hydrocarbons B. Unsaturated C. Aromatic 2. Alkyl Halides 3. Oxygen-Containing Compounds A. Aliphatic Alcohols B. Aliphatic Ethers C. Aromatic Alcohols D. Cyclic Ethers E. Ketones and Aldehydes F. Aliphatic Acids and Esters G. Aromatic Acids and Esters 4. Nitrogen-Containing Compounds A. Aliphatic Amines B. Aromatic Compounds Containing Atoms of Nitrogen C. Heterocyclic Nitrogen-Containing Compounds D. Nitro Compounds E. Concluding Remarks on the Mass Spectra of Nitrogen-Containing Compounds 5. Multiple Heteroatoms or Heteroatoms and a Double Bond 6. Trimethylsilyl Derivative 7. Determining the Location of Double Bonds VI. Library -
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. -
Portable Mass Spectrometry
Food Analytical Methods https://doi.org/10.1007/s12161-019-01666-6 Potential of Recent Ambient Ionization Techniques for Future Food Contaminant Analysis Using (Trans)Portable Mass Spectrometry Marco H. Blokland1 & Arjen Gerssen1 & Paul W. Zoontjes1 & Janusz Pawliszyn2 & Michel W.F. Nielen1,3 Received: 3 June 2019 /Accepted: 31 October 2019 # The Author(s) 2019 Abstract In food analysis, a trend towards on-site testing of quality and safety parameters is emerging. So far, on-site testing has been mainly explored by miniaturized optical spectroscopy and ligand-binding assay approaches such as lateral flow immunoassays and biosensors. However, for the analysis of multiple parameters at regulatory levels, mass spectrometry (MS) is the method of choice in food testing laboratories. Thanks to recent developments in ambient ionization and upcoming miniaturization of mass analyzers, (trans)portable mass spectrometry may be added to the toolkit for on-site testing and eventually compete with multiplex immunoassays in mixture analysis. In this study, we preliminary evaluated a selection of recent ambient ionization techniques for their potential in simplified testing of selected food contaminants such as pesticides, veterinary drugs, and natural toxins, aiming for a minimum in sample preparation while maintaining acceptable sensitivity and robustness. Matrix-assisted inlet ionization (MAI), handheld desorption atmospheric pressure chemical ionization (DAPCI), transmission-mode direct analysis in real time (TM-DART), and coated blade spray (CBS) were coupled to both benchtop Orbitrap and compact quad- rupole single-stage mass analyzers, while CBS was also briefly studied on a benchtop triple-quadrupole MS. From the results, it can be concluded that for solid and liquid sample transmission configurations provide the highest sensitivity while upon addition ofastationaryphase,suchasinCBS,evenlowμg/L levels in urine samples can be achieved provided the additional selectivity of tandem mass spectrometry is exploited.