Ch 13. Basics of Mass Spectrometry (I) : Principles & Ionization Sources
|
|
- Sara Henry
- 5 years ago
- Views:
Transcription
1 Ch 13. Basics of Mass Spectrometry (I) : Principles & Ionization Sources Why should you be interested in mass spectrometry (MS)? - to identify unknown compounds - to quantify known materials - to elucidate the structural and chemical properties of molecules - detection of compounds at g, mole for a compound of mass 100 dalton 1 1. Where are MS used? Biotechnology: analysis of proteins, peptides, oligonucleotides Pharmaceutical Analysis: drugs discovery, combinatorial chemistry, pharmokinetics, drug metabolism Clinical Examination: neonatal screening, haemoglobin analysis, drug testing Environmental Analysis : water, food, air quality (PCBs etc) Geological Analysis : oil composition 2
2 1.1 Instrumental Design of Mass Spectrometer Ionization/ desorption Source Form ions (charged molecules) Mass Sorting Analyzer Sort Ions by Weight (m/z) Detection Ion Detection Detect ions Inlet Solid Liquid Vapor Sample Introduction Method to vaporize sample Mass Spectrum Data Analysis 3 Turbo pumps Diffusion Pumps Rough pumps Rotary pumps High Vacuum System Inlet Ion source Mass Filter Detector Data System HPLC Samle plate GC Solids probe DCI Electrospray MALDI FAB LSIMS EI CI TOF Quadrupole Ion Trap Magnetic Sector FT-ICR Microchannel Plate (MCP) Electron Multiplier 4
3 1.2 Vacuum Technology Pressure Gauges Gauge Pressure Range Typical Use (torr) Manometer systems near atm Thermocouple gauge monitoring mechanical pumps Ionization gauge high-vacuum systems Vacuum Pumps Pump Lowest Attainable Pressure Typical Use Mechanical pump roughing or backing pump Diffusion pump 10-6 vacuum lines Turbomolecular pump 10-9 high-vacuum systems Cryopump < ultrahigh-vacuum sys Reason for Vacuum in MS 10-6 to mid 10-5 Torr Increase sensitivity Avoid ion-molecule reactions Collision free ion trajectories Increase filament lifetime Avoid electric discharge Avoid background interference 6
4 2. Sample Introduction Techniques Direct Probe/Metal Targets Sample put onto the end of long probe and inserted into the MS Sample spotted with matrix onto a metal plate Gas chromatography: EI, CI, NCI - Sample must be volatile, thermally stable Liquid chromatography: PB, FAB, APCI, ESI Widely used in pharmaceutical industry LC/MS applicable to thermally labile, high MW compounds LC/MS suitable for proteins & peptides On-line technique 7 3. Ionization Methods Ionization Techniques Electron Impact (EI) Chemical Ionization (CI) Fast Atom Bombardment (FAB) ESI MALDI Hard Ionization Fragments Soft Ionization Intact 8
5 3.1 Electron Ionization (EI) M e - (70 ev) M (5 ev) 2e - (65 ev) Excess E (65eV) in the molecule leads to some degree of fragmentation M : molecular ions fragment ions neutral fragments M e - : M - (100 times less efficient) Energetic process. A heated filament emits electrons which are accelerated by a potential difference of usually 70eV into the sample chamber. Ionization of the sample occurs by removal of an electron from the molecule thus generating a positively charged ion with one unpaired electron. 9 1) Schematics of EI N M e - M. 2e - Fragmentation M. A B M. A B 10
6 2) Characteristics of EI Molecular ion AB e AB 2e Fragment ion AB e A B 2e Standard ionization methods in MS Vaporized sample bombards with high energy electrons (~ 70 ev) Hard ionization method leads to significant fragmentation Ionization is efficient but non-selective Widely used technique when coupled to GC Suitable for volatile organic compounds eg. hydrocarbons, oils, flavors, fragrances Not really coupled to LC today Produces M. radical cation giving molecular weight Produces abundant fragment ions Library searchable spectra 11 Electron Energy Profiles of Ionization Ionization efficiency 70 V Electron energy (ev) 70eV : strong enough to knock off an electron and initiate fragmentation. 12
7 EI Spectra 13 14
8 3.2 Chemical Ionization (CI) Positive Ion Chemical Ionization (PCI or CI) Negative Ion Chemical Ionization (NCI,NICI or ECNI) 1. Instrumentation for CI 2. Selection of Reagent Gas 3. Analytical Application 15 1) EI CI Comparison Source pressure Mean free path EI 10-6 torr -200 mm CI torr -2 x 10-4 torr High Energy process Odd E - ions formed Low Energy process (possess thermal energy) Even E - ions formed 16
9 2) Advantages and Disadvantages of CI Advantages of Chemical ionization: 1. Large (M1) ion identifies molecular weight (M) 2. Sensitivity is enhanced by - simple fragmentation (fewer peaks of higher abundance) - direct GC/MS interface 3. CI spectra complement EI spectra Disadvantages of Chemical ionization : 1. Simple fragmentation gives little structural information 2. Easy of ion source contamination 17 3) What happens in the CI source? Reactant ions are formed via EI/CI: CH 4 e - CH 4 2e - CH 4 e - CH 3 H 2e - CH 4 e - CH 2 H 2 2e - CH 4 CH 4 CH 5 CH 3 CH 3 CH 4 C 2 H 5 H 2 CH 2 2 CH 4 C 3 H 5 2H 2 H At 1 torr, the major ions are those at 17amu (CH 5 ), 29amu (C 2 H 5 ), 41amu (C 3 H 5 ) 18
10 Sample Ionization: 1. Proton transfer: higher proton affinity than that of reagent CH 5 RH CH 4 RH 2 (MH) C 2 H 5 RH C 2 H 4 RH 2 (MH) 2. Alkyl addition: C 2 H 5 RH RH C 2 H 5 (M29) C 3 H 5 RH RH C 3 H 5 (M41) 3. Hydride abstraction : lower PA molecules (M-1) CH 5 RH CH 4 H 2 R C 2 H 5 RH C 2 H 6 R 19 CI Mass spectra of reagent gas? 20
11 3.3 Fast Atom Bombardment (FAB) Ion Source 8000V or 1KV Cesium ion beam MH [ or MX ] Ion desorbed from matrix Matrix Comatrix Proton X : Na, K, Li Sample and Matrix Advantage Soft Ionization(MH, MNa... ) : little fragmentation Easy adaptation of HRMS : accurate mass measurement Matrix can be useful as ref. ion 21 1) Schematics of FAB Ion Source FAB gun 6~10 kev Primary atom or ion beam Probe Secondary ions Through Vacuum Lock Sample/Matrix To mass analyzer Xe Xe Xe Xe 0 ionization acceleration neutralization Slow atoms Slow ions Fast ions Fast atoms 22
12 2) Mechanism of ion formation Impact of a high-energy atom or ion formation of a high-temperature, high density gas in the cavity that is formed at the point of impact Generation of additional ions secondary electrons, radicals, and exited neutral species Mass Spectrom. Rev., 5, 191 (1986) 23 3) Basic setup of FAB MS Xe/Ar Xe/Ar ions ions are are generated generated by by Electron Electron Impact(EI) Impact(EI) Accelerating(3-8 Accelerating(3-8 kev) kev) and and Focusing Focusing Neutralization Neutralization by charge exchange by charge exchange with with neutral neutral gas gas in the collision cell in the collision cell (( X (fast) X (fast) X X X(fast) X(fast) X ) X ) or by Neutralizing metal such or by Neutralizing metal such as as Al Al Fast Fast atom atom beam beam hits hits the the drop drop of sample on the target of sample on the target Emerging Emerging secondary secondary ions ions Mass Mass analysis analysis 24
13 4) Matrix of FAB Ionization Successful ionization by FAB is deeply dependent on the matrix selection for the analysis. Matrix requirements - Dissolve the sample to be analyzed, (usually 1 mg/100 ml) - Facilitate in the ionization of the sample - low volatility - Not undergo a chemical reaction with the sample. - Constantly replenish the surface with new sample - Minimize sample damage from the high-energy particle beam - Reduce damage to the sample by absorbing the impact of the primary beam - Prolongs the sample ion current by constantly replenishing the upper layer with the fresh sample - Reduces the binding energy of the sample molecules Functions - proton donor(ve mode) - proton acceptor(-ve mode) - solvent - sample reservoir - reagent 25 Chemical Structures of Matrix 26
14 Matrix Selection of FAB MS Mol. Formula M/Z Glycerol C3H8O Best choice for polar compounds 1-thioglycerol C3H8O2S More volatile than glycerol, evaporates quickly 3-nitrobenzyl alcohol (NBA) C7H7NO Best choice for less polar compounds and many organometallics 2-nitrophenyl octyl ether (NPOE) C14H21NO Triethanolamine C6H15NO magic bullet C4H10S2O Matrix C24H38O4 dioctyl phthalate (DOP) [bis(2-ethylhexyl) phthalate] Characteristics Only FAB matrix with no reactive hydrogen Good matrix for negative-ion FAB Enhances [M-H]- formation Widespread contaminant in solvents, gives characteristic 149 peak in EI mass spectra Use care to avoid contaminating the mass spectrometer sulfuric acid H2SO4 Good for some inorganics and organometallics phthalocyanine) Corrosive, use care (e.g. copper 27 FAB MS Spectra by positive and negative ion modes Positive mode Negative mode M H [MH] M [M-H] H M Na [M Na] M Cl- [M Cl]- J. Agric. Food Chem.; 47(2); 588, (1999) 28
15 29 Applications of FAB MS Synthetic Peptides Recombinant DNA Proteins and Glycoproteins Carbohydrates Drug Metabolites (including intact congugates) Detergents (anionic, cationic, non-ionic, amphoteric) Biocides Petrochemicals Oil Additives Oil Field Chemicals Phospholipids 30
16 3.4 Matrix Assisted Laser Desorption Ionization (MALDI) Laser MH [ or MX ] Matrix Comatrix Proton X : Na, K, Li Sample & matrix Advantage High Sensitivity Soft Ionization(MH, MNa... ) Mixture Analysis Low Cost No Contamination 31 Selection of Matrix in MALDI Sinapinic Acid a-cyano-4-hydroxycinnamic acid 2,5 Dihydroxybenzoic acid Super DHB 3-Hydroxypicolinic acid HABA Proteins >10kDa Peptides<10kDa Neutral Carbohydrates, Synthetic Polymers Proteins, Glycosylated proteins Oligonucleotides Proteins, Oligosaccharides 32
17 Advantage High sensitivity, mass range Simple structure Easy operation & maintenance, low cost Fast acquisition and automation Disadvantage Accuracy, resolution [~10,000] delayed extraction, reflectron Different calibration for different mass range & experimental condition (laser, matrix) 33 MALDI/TOF 1. Sample is mixed with matrix & dried on target 4. Ions are accelerated by an electrical field to the same kinetic energy, and they drift (or fly) down a field free flight tube where they are separated in space kv Flight tube 5. Ions strike the detector at different times, depending on the mass to charge ratio of the ion. 2. Target is introduced into high vacuum of MS High vacuum High voltage 3. Sample spot is irradiated with laser, desorbing ions into the gas phase and starting the clock measuring the time of flight. Pulsed laser Tim e 6. A data system controls all instrument parameters, acquires the signal vs. time, and permits data processing. 34
18 Higher resolution Higher mass accuracy PSD(Post Source Decay) Reflector for TOF Second Detector Reflector (Ion mirror) First Detector Ion Gate Laser The reflector increases the overall path length for an ion and it corrects for minor variation in the energy spread of ions of the same mass. Both effects improve resolution. 35 Applications of MALDI/TOF-MS Molecular biology, biochemistry Biopolymer Characterization Protein & peptides [proteomics] Sequence Analysis DNA, RNA [genomics] In- Source Decay Exonuclease Sequencing Carbohydrate Lipid Pharmaceutical Industry Combinatorial Chemistry Chemical Industry Synthetic Polymer Characterization 36
19 3.5 Atmospheric Pressure Chemical Ionization (APCI) Pressure = 760 torr Sample Inlet Nozzle (Lower Voltage) N 2 Solvent Flow From HPLC MH MH MH MH MH Heat Heat applied to metal sheath Corona discharge needle 37 APCI Simple and efficient device for the LC/MS analysis of compounds Needle : 3-6kV potential creates a corona discharge Ionization : by CI Soft ionization which generates pseudo molecular ions MH, (MNH 4 ) etc. (M-H) -, (MCH 3 COO) -, (MCl) - etc Generates singly charged ions, in general Suitable for less polar compounds compared to ESI Same degradation may occur in case of labile compounds 38
20 Characteristics of APCI Both positive and negative ions can preferentially be formed in the APCI source using a corona discharge Ion molecule reaction Positive ion mode - the creation of reactant positive ions in ambient air (the proton hydrates, H 3 O [H 2 O] n ) - the major primary ions N 2, O 2, H 2 O and NO are formed by electron impact of corona-created electrons on the major neutral components in air - Proton transfer reaction H 3 O [H 2 O] n T TH (H 2 O) m (n-m1)h 2 O if the gas basicity (proton affinity) of T is greater than that of water TH (H 2 O) m TH by stripped off in the gas curtain and declustering lens region 39 In negative ion mode, - electron created by the corona are rapidly thermalized (lose excess energy) through collision with neutrals and captured by electronegative species such as O 2 to form O 2- and O -. - super oxide (O 2- ) and its hydrates (O 2- [H 2 O] n ) and cluster (O 2- [O 2 ] n ) Ion Molecule Reaction Charge transfer R T T R R - T T - R Proton transfer RH T TH R R - TH T - RH 40
21 APCI MS spectra of Phenylbutazones 41 APCI MS/MS spectra 42
22 3.6 Electrospray Ionization (ESI) 43 1) Characteristics of ESI Soft ionization, which generates pseudo molecular ions MH, (MNH 4 ), (MNa), (MK) etc. (M-H) -, (MCH 3 COO) -, (MCl) - etc. Applicable for wide range of compounds with relatively high sensitivity Up to 150 kda in case of proteins Middle to High polar compounds Thermally labile compounds Non covalently binding complex Generates multiply charged ions of biopolymers (MnH) n / (M-nH) n- 44
23 ESI Mass Spectra 1picomole Myoglobin MW: 16,939.4 amu LC/MS analysis m/z 1230 Heme dimer Second series protein Heme Synthetic DNA MW: amu Negative ion mode 45 Useful mass differences for interpretation of ESI-MS - Positive ion mode - (MH) (MNH 4 ) 17 (MNa) 22 5 (MK) 16 (MMeCNH)
M M e M M H M M H. Ion Sources
Ion Sources Overview of Various Ion Sources After introducing samples into a mass spectrometer, the next important step is the conversion of neutral molecules or compounds to gas phase ions. The ions could
More informationMolecular Mass Spectrometry
Molecular Mass Spectrometry Mass Spectrometry: capable of providing information about (1) Elemental composition of samples of matter: atomic mass (2) Structures of inorganic, organic, and biological molecules
More informationLecture 15: Introduction to mass spectrometry-i
Lecture 15: Introduction to mass spectrometry-i Mass spectrometry (MS) is an analytical technique that measures the mass/charge ratio of charged particles in vacuum. Mass spectrometry can determine masse/charge
More informationChemistry Instrumental Analysis Lecture 34. Chem 4631
Chemistry 4631 Instrumental Analysis Lecture 34 From molecular to elemental analysis there are three major techniques used for elemental analysis: Optical spectrometry Mass spectrometry X-ray spectrometry
More information20.2 Ion Sources. ions electrospray uses evaporation of a charged liquid stream to transfer high molecular mass compounds into the gas phase as MH n
20.2 Ion Sources electron ionization produces an M + ion and extensive fragmentation chemical ionization produces an M +, MH +, M +, or M - ion with minimal fragmentation MALDI uses laser ablation to transfer
More informationMass Spectrometry. Electron Ionization and Chemical Ionization
Mass Spectrometry Electron Ionization and Chemical Ionization Mass Spectrometer All Instruments Have: 1. Sample Inlet 2. Ion Source 3. Mass Analyzer 4. Detector 5. Data System http://www.asms.org Ionization
More informationTANDEM MASS SPECTROSCOPY
TANDEM MASS SPECTROSCOPY 1 MASS SPECTROMETER TYPES OF MASS SPECTROMETER PRINCIPLE TANDEM MASS SPECTROMETER INSTRUMENTATION QUADRAPOLE MASS ANALYZER TRIPLE QUADRAPOLE MASS ANALYZER TIME OF FLIGHT MASS ANALYSER
More informationLC-MS Based Metabolomics
LC-MS Based Metabolomics Analysing the METABOLOME 1. Metabolite Extraction 2. Metabolite detection (with or without separation) 3. Data analysis Metabolite Detection GC-MS: Naturally volatile or made volatile
More informationMolecular Mass Spectrometry
Molecular Mass Spectrometry Mass Spectrometry: capable of providing information about (1) Elemental composition of samples of matter: atomic mass (2) Structures of inorganic, organic, and biological molecules
More informationFundamentals of Mass Spectrometry. Fundamentals of Mass Spectrometry. Learning Objective. Proteomics
Mass spectrometry (MS) is the technique for protein identification and analysis by production of charged molecular species in vacuum, and their separation by magnetic and electric fields based on mass
More informationMass Spectrometry. General Principles
General Principles Mass Spectrometer: Converts molecules to ions Separates ions (usually positively charged) on the basis of their mass/charge (m/z) ratio Quantifies how many units of each ion are formed
More informationChemistry 311: Topic 3 - Mass Spectrometry
Mass Spectroscopy: A technique used to measure the mass-to-charge ratio of molecules and atoms. Often characteristic ions produced by an induced unimolecular dissociation of a molecule are measured. These
More informationMass Spectrometry for Chemists and Biochemists
Erasmus Intensive Program SYNAPS Univ. of Crete - Summer 2007 Mass Spectrometry for Chemists and Biochemists Spiros A. Pergantis Assistant Professor of Analytical Chemistry Department of Chemistry University
More information1) In what pressure range are mass spectrometers normally operated?
Exercises Ionization 1) In what pressure range are mass spectrometers normally operated? Mass spectrometers are usually operated in the high vacuum regime to ensure mean free paths significantly longer
More informationMass spectrometry gas phase transfer and instrumentation
Objectives of the Lecture spectrometry gas phase transfer and instrumentation Matt Renfrow January 15, 2014 1. Make ions 2. Separate/Analyze 3. Detect ions 4. What is mass resolution and mass accuracy?
More informationChemistry Instrumental Analysis Lecture 37. Chem 4631
Chemistry 4631 Instrumental Analysis Lecture 37 Most analytes separated by HPLC are thermally stable and non-volatile (liquids) (unlike in GC) so not ionized easily by EI or CI techniques. MS must be at
More informationMass Spectroscopy. Base peak. Molecular Ion peak. The positively charged fragments produced are separated, based on their mass/charge (m/z) ratio. M+.
Mass spectrometry is the study of systems causing the formation of gaseous ions, with or without fragmentation, which are then characteried by their mass to charge ratios (m/) and relative abundances.
More informationMS Goals and Applications. MS Goals and Applications
MS Goals and Applications 3 Several variations on a theme, three common steps Form gas-phase ions choice of ionization method depends on sample identity and information required Separate ions on basis
More informationMass spectrometry.
Mass spectrometry Mass spectrometry provides qualitative and quantitative information about the atomic and molecular composition of inorganic and organic materials. The mass spectrometer produces charged
More informationLecture 8: Mass Spectrometry
intensity Lecture 8: Mass Spectrometry Relative abundance m/z 1 Ethylbenzene CH 2 CH 3 + m/z = 106 CH 2 + m/z = 91 C 8 H 10 MW = 106 CH + m/z = 77 + 2 2 What information can be obtained from a MS spectrum?
More informationMass Spectrometry. Hyphenated Techniques GC-MS LC-MS and MS-MS
Mass Spectrometry Hyphenated Techniques GC-MS LC-MS and MS-MS Reasons for Using Chromatography with MS Mixture analysis by MS alone is difficult Fragmentation from ionization (EI or CI) Fragments from
More informationHarris: Quantitative Chemical Analysis, Eight Edition
Harris: Quantitative Chemical Analysis, Eight Edition CHAPTER 21: MASS SPECTROMETRY CHAPTER 21: Opener 21.0 Mass Spectrometry Mass Spectrometry provides information about 1) The elemental composition of
More informationMass Spectrometry (MS)
Mass Spectrometry (MS) Alternative names: Mass spectrometric (selective) detector (MSD) Spectrometry - methods based on interaction of matter and radiation Mass spectrometry - method based on formation
More informationSelecting an LC/MS Interface Becky Wittrig, Ph.D.
Selecting an LC/MS Interface Becky Wittrig, Ph.D. RESTEK CORPORATION LC/MS Interfaces I. Background of LC/MS I. Historical Perspective II. Reasons for use II. Interfaces I. Transport devices II. Particle
More informationLecture 8: Mass Spectrometry
intensity Lecture 8: Mass Spectrometry Relative abundance m/z 1 Ethylbenzene experiment CH 2 CH 3 + m/z = 106 CH 2 + m/z = 91 C 8 H 10 MW = 106 CH + m/z = 77 + 2 2 What information can we get from MS spectrum?
More informationIonization Techniques Part IV
Ionization Techniques Part IV CU- Boulder CHEM 5181 Mass Spectrometry & Chromatography Presented by Prof. Jose L. Jimenez High Vacuum MS Interpretation Lectures Sample Inlet Ion Source Mass Analyzer Detector
More informationMASS SPECTROMETRY. Topics
MASS SPECTROMETRY MALDI-TOF AND ESI-MS Topics Principle of Mass Spectrometry MALDI-TOF Determination of Mw of Proteins Structural Information by MS: Primary Sequence of a Protein 1 A. Principles Ionization:
More informationInstrumental Analysis. Mass Spectrometry. Lecturer:! Somsak Sirichai
303351 Instrumental Analysis Mass Spectrometry Lecturer:! Somsak Sirichai Mass Spectrometry What is Mass spectrometry (MS)? An analytic method that employs ionization and mass analysis of compounds in
More informationMass spectrometry and elemental analysis
Mass spectrometry and elemental analysis A schematic representation of a single-focusing mass spectrometer with an electron-impact (EI) ionization source. M: + e _ M +. + 2e _ Ionization and fragmentation
More informationMass Spectrometry Course
Mass Spectrometry Course Árpád Somogyi Mass Spectrometry Laboratory, Department of Chemistry and Biochemistry University of Arizona, Tucson, AZ Eötvös University, Budapest April 11-20, 2012 1 2 UA Chemistry
More informationMass spectrometry of proteins, peptides and other analytes: principles and principal methods. Matt Renfrow January 11, 2008
Mass spectrometry of proteins, peptides and other analytes: principles and principal methods Matt Renfrow January 11, 2008 Objectives of the Lecture 1. Make ions 2. Separate/Analyze/Detect ions 3. What
More informationAuxiliary Techniques Soft ionization methods
Auxiliary Techniques The limitations of the structural information in the normal mass spectrum can be partly offset by special mass-spectral techniques. Although a complete description of these is beyond
More informationMS Goals and Applications. MS Goals and Applications
MS Goals and Applications 1 Several variations on a theme, three common steps Form gas-phase ions choice of ionization method depends on sample identity and information required Separate ions on basis
More informationAnalysis of Polar Metabolites using Mass Spectrometry
Analysis of Polar Metabolites using Mass Spectrometry TransMed Course: Basics in Clinical Proteomics and Metabolomics. Oct 10-19, 2012 dd.mm.yyyy Vidya Velagapudi, Ph.D, Adjunct Professor Head of the Metabolomics
More informationIonization Methods in Mass Spectrometry at the SCS Mass Spectrometry Laboratory
Ionization Methods in Mass Spectrometry at the SCS Mass Spectrometry Laboratory Steven L. Mullen, Ph.D. Associate Director SCS Mass Spectrometry Laboratory Contact Information 31 oyes Laboratory (8:00-5:00
More information(Refer Slide Time 00:09) (Refer Slide Time 00:13)
(Refer Slide Time 00:09) Mass Spectrometry Based Proteomics Professor Sanjeeva Srivastava Department of Biosciences and Bioengineering Indian Institute of Technology, Bombay Mod 02 Lecture Number 09 (Refer
More informationQualitative Organic Analysis CH 351 Mass Spectrometry
Qualitative Organic Analysis CH 351 Mass Spectrometry Bela Torok Department of Chemistry University of Massachusetts Boston Boston, MA General Aspects Theoretical basis of mass spectrometry Basic Instrumentation
More informationfor the Novice Mass Spectrometry (^>, John Greaves and John Roboz yc**' CRC Press J Taylor & Francis Group Boca Raton London New York
Mass Spectrometry for the Novice John Greaves and John Roboz (^>, yc**' CRC Press J Taylor & Francis Group Boca Raton London New York CRC Press is an imprint of the Taylor & Francis Croup, an informa business
More informationIntroduction to GC/MS
Why Mass Spectrometry? Introduction to GC/MS A powerful analytical technique used to: 1.Identify unknown compounds 2. Quantify known materials down to trace levels 3. Elucidate the structure of molecules
More informationCHAPTER A2 LASER DESORPTION IONIZATION AND MALDI
Back to Basics Section A: Ionization Processes CHAPTER A2 LASER DESORPTION IONIZATION AND MALDI TABLE OF CONTENTS Quick Guide...27 Summary...29 The Ionization Process...31 Other Considerations on Laser
More informationMass Spectrometry: Introduction
Mass Spectrometry: Introduction Chem 8361/4361: Interpretation of Organic Spectra 2009 Andrew Harned & Regents of the University of Minnesota Varying More Mass Spectrometry NOT part of electromagnetic
More informationProudly serving laboratories worldwide since 1979 CALL for Refurbished & Certified Lab Equipment
www.ietltd.com Proudly serving laboratories worldwide since 1979 CALL +1.847.913.0777 for Refurbished & Certified Lab Equipment Applied Biosystems QStar Pulsar i Features of the API QSTAR Pulsar i The
More informationGRADUATE COURSE IN MASS SPECTROMETRY: LECTURE 2
DEPARTMENTS OF CHEMISTRY AND BIOCHEMISTRY GRADUATE COURSE IN MASS SPECTROMETRY: LECTURE 2 Mass Analysers Shabaz Mohammed October 20, 2015 High Vacuum System Turbo pumps Diffusion pumps Rough pumps Rotary
More informationCEE 772 Lecture #27 12/10/2014. CEE 772: Instrumental Methods in Environmental Analysis
Updated: 10 December 2014 Print version CEE 772: Instrumental Methods in Environmental Analysis Lecture #21 Mass Spectrometry: Mass Filters & Spectrometers (Skoog, Chapt. 20, pp.511 524) (Harris, Chapt.
More informationIon sources. Ionization and desorption methods
Ion sources Ionization and desorption methods 1 2 Processes in ion sources 3 Ionization/ desorption Ionization Desorption methods Electron impact ionization Chemical ionization Electro-spray ionisation
More informationMacromolecular Chemistry
Macromolecular Chemistry Lecture 8 Measuring Molecular Weight Membrane Osmometry Alfredo Vapor Phase Osmometry Linda Viscometry GW Gel Permeation Chromatography Size exclusion Chromatography Light Scattering
More informationCEE 772: Instrumental Methods in Environmental Analysis
Updated: 10 December 2014 Print version CEE 772: Instrumental Methods in Environmental Analysis Lecture #21 Mass Spectrometry: Mass Filters & Spectrometers (Skoog, Chapt. 20, pp.511-524) (Harris, Chapt.
More informationMass Spectrometry in MCAL
Mass Spectrometry in MCAL Two systems: GC-MS, LC-MS GC seperates small, volatile, non-polar material MS is detection devise (Agilent 320-MS TQ Mass Spectrometer) Full scan monitoring SIM single ion monitoring
More informationMass Spectrometry. A truly interdisciplinary and versatile analytical method
Mass Spectrometry A truly interdisciplinary and versatile analytical method MS is used for the characterization of molecules ranging from small inorganic and organic molecules to polymers and proteins.
More informationChoosing the metabolomics platform
GBS 748 Choosing the metabolomics platform Stephen Barnes, PhD 4 7117; sbarnes@uab.edu So, I have my samples what s next? You ve collected your samples and you may have extracted them Protein precipitation
More informationMS/MS .LQGVRI0606([SHULPHQWV
0DVV6SHFWURPHWHUV Tandem Mass Spectrometry (MS/MS) :KDWLV0606" Mass spectrometers are commonly combined with separation devices such as gas chromatographs (GC) and liquid chromatographs (LC). The GC or
More informationMass Analyzers. mass measurement accuracy/reproducibility. % of ions allowed through the analyzer. Highest m/z that can be analyzed
Mass Analyzers Double Focusing Magnetic Sector Quadrupole Mass Filter Quadrupole Ion Trap Linear Time-of-Flight (TOF) Reflectron TOF Fourier Transform Ion Cyclotron Resonance (FT-ICR-MS) Mass Analyzers
More information1. The range of frequencies that a measurement is sensitive to is called the frequency
CHEM 3 Name Exam 1 Fall 014 Complete these problems on separate paper and staple it to this sheet when you are finished. Please initial each sheet as well. Clearly mark your answers. YOU MUST SHOW YOUR
More informationLIQUID CHROMATOGRAPHY-MASS SPECTROMETRY (LC/MS) Presented by: Dr. T. Nageswara Rao M.Pharm PhD KTPC
LIQUID CHROMATOGRAPHY-MASS SPECTROMETRY (LC/MS) Presented by: Dr. T. Nageswara Rao M.Pharm PhD KTPC INTRODUCTION Principle: LC/MS is a technique that combines physical separation capabilities of liquid
More informationMass spectrometry: forming ions, to identifying proteins and their modifications Stephen Barnes, PhD
Mass spectrometry: forming ions, to identifying proteins and their modifications Stephen Barnes, PhD 4-7117 sbarnes@uab.edu Introduction to mass spectrometry Class 1 - Biology and mass spectrometry Why
More informationMass Spectrometry and Proteomics - Lecture 2 - Matthias Trost Newcastle University
Mass Spectrometry and Proteomics - Lecture 2 - Matthias Trost Newcastle University matthias.trost@ncl.ac.uk Previously: Resolution and other basics MALDI Electrospray 40 Lecture 2 Mass analysers Detectors
More informationsample was a solution that was evaporated in the spectrometer (such as with ESI-MS) ions such as H +, Na +, K +, or NH 4
Introduction to Spectroscopy V: Mass Spectrometry Basic Theory: Unlike other forms of spectroscopy used in structure elucidation of organic molecules mass spectrometry does not involve absorption/emission
More informationMass Spectrometry. Introduction EI-MS and CI-MS Molecular mass & formulas Principles of fragmentation Fragmentation patterns Isotopic effects
Mass Spectrometry Introduction EI-MS and CI-MS Molecular mass & formulas Principles of fragmentation Fragmentation patterns Isotopic effects 1 Introduction to MS Mass spectrometry is the method of analysis
More informationOther Methods for Generating Ions 1. MALDI matrix assisted laser desorption ionization MS 2. Spray ionization techniques 3. Fast atom bombardment 4.
Other Methods for Generating Ions 1. MALDI matrix assisted laser desorption ionization MS 2. Spray ionization techniques 3. Fast atom bombardment 4. Field Desorption 5. MS MS techniques Matrix assisted
More informationMass Spectrometry. What is Mass Spectrometry?
Mass Spectrometry What is Mass Spectrometry? Mass Spectrometry (MS): The generation of gaseous ions from a sample, separation of these ions by mass-to-charge ratio, and measurement of relative abundance
More informationHistory of Mass spectroscopy. Mass Spectroscopy. Introduction... Uses of Mass Spec. Where are Mass Spectrometers Used? Mass Spectroscopy Units
History of Mass spectroscopy Mass Spectroscopy CHEM 466 Upali Siriwardane Marilyn Cox Jim Plamer http://www.chemistry.ohiostate.edu/~allen/587%20w04/587%20w0 4%20130-136%20std.pdf http://www.cem.msu.edu/~cem333/week1
More informationVoyager-DE STR Biospectrometry Workstation Manufactured by PerSeptive Biosystems
Voyager-DE STR Biospectrometry Workstation Manufactured by PerSeptive Biosystems General Description The Voyager-DE STR Biospectrometry Workstation includes upgraded electronics, a 3-meter flight path,
More informationAnalytical Technologies and Compound Identification. Daniel L. Norwood, MSPH, PhD SCĪO Analytical Consulting, LLC.
Analytical Technologies and Compound Identification Daniel L. Norwood, MSPH, PhD SCĪ Analytical Consulting, LLC. Extractables/Leachables Characterization (USP) Characterization is the discovery,
More informationMolecular weight of polymers. Molecular weight of polymers. Molecular weight of polymers. Molecular weight of polymers. H i
Gel Permeation Chromatography (GPC) : Size Exclusion Chromatography GPC : 1. Chromatogram (V R vs H) H i Detector response Baseline N i M i 130 135 140 145 150 155 160 165 Elution volume (V R ) (counts)
More informationMASS ANALYSER. Mass analysers - separate the ions according to their mass-to-charge ratio. sample. Vacuum pumps
ION ANALYZERS MASS ANALYSER sample Vacuum pumps Mass analysers - separate the ions according to their mass-to-charge ratio MASS ANALYSER Separate the ions according to their mass-to-charge ratio in space
More informationMass Spectrometry. Anders Malmendal. 1. Physical principles. Mass Spectrometry
1. Physical principles Mass spectrometry is based on the laws determining the motions of charged particles. In a mass spectrometer, the motions of these particles are determined by the particle mass and
More informationLECTURE-13. Peptide Mass Fingerprinting HANDOUT. Mass spectrometry is an indispensable tool for qualitative and quantitative analysis of
LECTURE-13 Peptide Mass Fingerprinting HANDOUT PREAMBLE Mass spectrometry is an indispensable tool for qualitative and quantitative analysis of proteins, drugs and many biological moieties to elucidate
More informationFinnigan LCQ Advantage MAX
www.ietltd.com Proudly serving laboratories worldwide since 1979 CALL +847.913.0777 for Refurbished & Certified Lab Equipment Finnigan LCQ Advantage MAX The Finnigan LCQ Advantage MAX ion trap mass spectrometer
More informationMass spectrometry: forming ions, to identifying proteins and their modifications Stephen Barnes, PhD
Mass spectrometry: forming ions, to identifying proteins and their modifications Stephen Barnes, PhD 4-7117 sbarnes@uab.edu Introduction to mass spectrometry Class 1 - Biology and mass spectrometry Why
More informationMASS SPECTRA measure a compound s Mol. Wt. This ionization type is called: electron impact MS
MASS SPECTRA measure a compound s Mol. Wt. p. 213 M + Molecule e - Molecule + 2 e - + + Mole cule + + Mol ecule IONIZATION CHAMBER repellor plate accelerating plates variable field magnet + Mo + lecule
More informationChapter 5 Basic Mass Spectrometry
Chapter 5 Basic Mass Spectrometry 5.1 Introduction and History The earliest forms of mass spectrometry go back to the observation of canal rays by Goldstein in 1886 and again by Wien in 1899. Thompson
More informationAnalytical Technologies in Biotechnology Prof. Dr. Ashwani K. Sharma Department of Biotechnology Indian Institute of Technology, Roorkee
Analytical Technologies in Biotechnology Prof. Dr. Ashwani K. Sharma Department of Biotechnology Indian Institute of Technology, Roorkee Module - 6 Spectroscopic Techniques Lecture - 6 Atomic Spectroscopy
More informationPropose a structure for an alcohol, C4H10O, that has the following
Propose a structure for an alcohol, C4H10O, that has the following 13CNMR spectral data: Broadband _ decoupled 13CNMR: 19.0, 31.7, 69.5 б DEPT _90: 31.7 б DEPT _ 135: positive peak at 19.0 & 31.7 б, negative
More informationIDENTIFICATION OF ORGANOMETALLIC COMPOUNDS USING FIELD DESORPTION IONIZATION ON THE GCT
IDETIFICATIO OF ORGAOMETALLIC COMPOUDS USIG FIELD DESORPTIO IOIZATIO O THE GCT David Douce 1, Michael Jackson 1, Robert Lewis 1, Peter Hancock 1, Martin Green 1 and Stuart Warriner 2 1 Waters Corporation,
More information4. How can fragmentation be useful in identifying compounds? Permits identification of branching not observed in soft ionization.
Homework 9: Chapters 20-21 Assigned 12 April; Due 17 April 2006; Quiz on 19 April 2006 Chap. 20 (Molecular Mass Spectroscopy) Chap. 21 (Surface Analysis) 1. What are the types of ion sources in molecular
More informationStudy of Non-Covalent Complexes by ESI-MS. By Quinn Tays
Study of Non-Covalent Complexes by ESI-MS By Quinn Tays History Overview Background Electrospray Ionization How it is used in study of noncovalent interactions Uses of the Technique Types of molecules
More informationChem 550, Spring, 2012 Part I: OVERVIEW OF MASS SPECTROMETRY:
Chem 550, Spring, 2012 Part I: OVERVIEW OF MASS SPECTROMETRY: I. BASIC ELEMENTS OF A MASS SPECTROMETER Inlet System or Chromatograph Ion Source Mass Analyzer Detector Computer II. ION SOURCES A. Electron
More information2. Separate the ions based on their mass to charge (m/e) ratio. 3. Measure the relative abundance of the ions that are produced
I. Mass spectrometry: capable of providing both quantitative and qualitative information about samples as small as 100 pg (!) and with molar masses in the 10 4-10 5 kdalton range A. The mass spectrometer
More informationSecondary Ion Mass Spectroscopy (SIMS)
Secondary Ion Mass Spectroscopy (SIMS) Analyzing Inorganic Solids * = under special conditions ** = semiconductors only + = limited number of elements or groups Analyzing Organic Solids * = under special
More informationChemical Aspects of Mass Spectrometry
Chemical Aspects of Mass Spectrometry Abraham Badu Chemistry and Biochemistry, OSU July 12, 217 Spread of MS by Discipline https://masspec.scripps.edu/ mass spectrometry 2 1 Current Challenges in Mass
More information15.04.jpg. Mass spectrometry. Electron impact Mass spectrometry
Mass spectrometry Electron impact Mass spectrometry 70 ev = 1614 kcal/mol - contrast with energy from IR (1-10 kcal/mol) or NMR (0.2 cal/mol) - typical C-C bond = 100 kcal/mol Point: lots of energy in
More informationKJ3022 MS compendium gives a deeper explanation of what is mentioned in the slides
1 MS program 20.08.2013 MS: Ionization methods 22.08.2013 MS: Ionization methods + Analytical Information 27.08.2013 MS: Analytical Information + Analyzers 29.08.2013 MS: Analyzers + Questions 03.09.2013
More informationChapter 5. Complexation of Tholins by 18-crown-6:
5-1 Chapter 5. Complexation of Tholins by 18-crown-6: Identification of Primary Amines 5.1. Introduction Electrospray ionization (ESI) is an excellent technique for the ionization of complex mixtures,
More informationParticle Position Relative Mass Relative Charge Proton Nucleus 1 +1 Neutron Nucleus 1 0 Electron Orbitals 1/ Atomic Symbol
Atomic Structure Details of the three Sub-atomic (fundamental) Particles Particle Position Relative Mass Relative Charge Proton Nucleus 1 +1 Neutron Nucleus 1 0 Electron Orbitals 1/1840-1 Behaviour of
More informationFast Atom Bombardment (FAB)-MS
Fast Atom Bombardment (FAB)-MS FAB-MS was developed by Barber and coworkers in the early 1980s and soon became a very powerful technique for desorption ionization of thermally labile molecules. In FAB
More informationMALDI-TOF: a powerful tool for the analysis of biomolecules and large organic molecules
III Workshop 2013-2014 Corso del Dottorato in Ingegneria dei Materiali del Politecnico di Milano Methods of Characterization of Materials MALDI-TOF: a powerful tool for the analysis of biomolecules and
More informationDe Novo Metabolite Chemical Structure Determination. Paul R. West Ph.D. Stemina Biomarker Discovery, Inc.
De Novo Metabolite Chemical Structure Determination Paul R. West Ph.D. Stemina Biomarker Discovery, Inc. As a part of non targeted metabolomic analysis, when peaks in the mass spectra are thought to be
More informationCEE 772: Instrumental Methods in Environmental Analysis
Updated: 10 December 2014 Print version CEE 772: Instrumental Methods in Environmental Analysis Lecture #22 Mass Spectrometry: Chemical Ionization (Skoog,) (Harris, Chapt.) Mercer/Goodwill CEE 772 #22
More information( 1+ A) 2 cos2 θ Incident Ion Techniques for Surface Composition Analysis Ion Scattering Spectroscopy (ISS)
5.16 Incident Ion Techniques for Surface Composition Analysis 5.16.1 Ion Scattering Spectroscopy (ISS) At moderate kinetic energies (few hundred ev to few kev) ion scattered from a surface in simple kinematic
More informationAn ion source performs the following two functions:
Ionization The Ion Source An ion source performs the following two functions: 1) converts sample atoms or molecules to ionized particles (ions) in the gas phase (sometimes the task of introducing the atoms
More informationOlumide Adebolu. Chromatographic Fidelity and Matrix /Analyte Solubility in Complex Polymer Systems using HPLC-MALD/I TOF MS
Chromatographic Fidelity and Matrix /Analyte Solubility in Complex Polymer Systems using HPLC-MALD/I TOF MS Olumide Adebolu CHEM 395 March 1 st, 2007 Instructor : Prof J.Rusling Overview 2 Introduction
More informationMass spectrometry as analytical tool in catalysis research
Mass spectrometry as analytical tool in catalysis research Katrin Pelzer Functional Characterization AC, FHI-MPG Berlin 17/11/2006 Mass Spectrometry Modern Methods in Heterogeneous Catalysis Research K.
More informationIntroduction to LC-MS
Wednesday April 5, 2017 10am Introduction to LC-MS Amy Patton, MS Laboratory Manager, Pinpoint Testing, LLC Little Rock, AR DESCRIPTION: Amy Patton, laboratory manager for Pinpoint Testing, will begin
More informationIntroduction to the Q Trap LC/MS/MS System
www.ietltd.com Proudly serving laboratories worldwide since 1979 CALL +1.847.913.0777 for Refurbished & Certified Lab Equipment ABI Q Trap LC/MS/MS Introduction to the Q Trap LC/MS/MS System The Q Trap
More informationINTRODUCTION TO MASS SPECTROMETRY Instrumentation, Applications and Strategies for Data Interpretation
INTRODUCTION TO MASS SPECTROMETRY Instrumentation, Applications and Strategies for Data Interpretation FOURTH EDITION J. THROCK WATSON 0. DAVID SPARKMAN 2007 John Wiley & Sons Ltd, Chichester, 978-0-470-51634-8
More informationPresentation Basic Introduction to Instrumentation Matrix Effects Challenges
Keys to Implementing Mass Spectrometry in the Clinical Laboratory Paul J. Taylor Chromatography Mass Spectrometry Satellite Meeting, AACB 20th September, 2013 Dept of Clinical Pharmacology, Princess Alexandra
More informationMass Spectrometry (MS)
Mass Spectrometry (MS) MW Molecular formula Structural information GC-MS LC-MS To Do s Read Chapter 7, and complete the endof-chapter problem 7-4. Answer Keys are available in CHB204H MS Principles Molecule
More informationDissociation of Even-Electron Ions
Dissociation of Even-Electron Ions Andrea Raffaelli CNR Istituto di Fisiologia Clinica Via Moruzzi, 1, 56124 Pisa. E-Mail: andrea.raffaelli@cnr.it Web: http://raffaelli.ifc.cnr.it A Simple? ESI Spectrum
More informationMass Spectrometry. Quantitative Mass Spectrometry Chiral Mass Spectrometry
Mass Spectrometry Quantitative Mass Spectrometry Chiral Mass Spectrometry Quantitation by MS Goal is to develop methodology to sensitively, specifically, accurately and rapidly measure one or more compounds
More informationThe AccuTOF -DART 4G: The Ambient Ionization Toolbox
The AccuTOF -DART 4G: The Ambient Ionization Toolbox Introduction JEOL introduced the AccuTOF-DART in 2005 as the first commercially available ambient ionization mass spectrometer system. The atmospheric
More information