M M e M M H M M H. Ion Sources

Save this PDF as:
 WORD  PNG  TXT  JPG

Size: px
Start display at page:

Download "M M e M M H M M H. Ion Sources"

Transcription

1 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 be molecular or monatomic in the case of organic or inorganic mass spectrometry respectively. Examples of molecular and monatomic ions are shown below: Cu 63 e 63 Cu Atomic mass 63 Exact mass Figure 1: General representation of ion formation in ions sources. Ions are needed because their speed and direction of travel can be manipulated by using electric and/or magnetic fields. This manipulation is crucial to the separation and detection of the chemical species. Ions can be formed in a variety of ways. A few examples are presented below (In these examples, M represents a neutral molecule while the radical or ionic forms of M are indicated with the dot or charge sign respectively (M, M + and M - ).): 1. ejection of electrons from neutral molecules e M M e 2. electron capture M e M 3. protonation H M M H 4. Deprotonation H M M H

2 5. addition of other cations Na M M Na 6. addition of anions CH3COO M M CH3COO Devices that are used for the conversion of neutral molecules to molecular ions are called ion sources. Many types of Ion sources have been developed. Some examples are presented in the list below: Table 1. Common ion sources and their acronyms Ion Source Electron ionization source Chemical Ionization source Matrix Assisted Laser Desorption ionization source Electrospray Ionization sources Atmospheric Pressure Chemical Ionization source Acronym EI CI MALDI ESI APCI Electron ionization Source (EI) Electron source Repeller e - Ion Extraction Lens To MS Trap Sample in Figure 2: principle of operation of electron ionization ion source In EI, the sample to be analyzed is vaporized into the ionization chamber by heating. Pressure in the chamber is typically about torr. The neutral molecules (represented by the black circles) are bombarded by energetic electrons ( ) produced by the electron source which is made from

3 Relative Abundance tungsten or rhenium filament. Typically, an electron is removed from the neutral molecule to form a radical ion. M e M 2e m/z Figure 3: The EI mass spectrum of decanol (CH 3 (CH 2 ) 9 OH). Notice the absence of a signal at m/z 158 which is the molecular ion (M + ). The base (or tallest peak) is at m/z 42. This is the most stable ion. This indicates that the initially formed molecular ion fragmented significantly. For ions to form, the energy of electrons from the filament of the EI must be higher than the ionization energy of the analyte molecule. Ionization energies of organic molecules are about 10eV while that of the bombarding electrons is typically 70eV. As a result, the ion that is formed has a lot of excess energy which causes it to fragment further. The signals observed in the mass spectrum above (Figure 3) indicate the fragmentation pattern of the molecule. This pattern is often referred to as the fingerprint of the molecule. The expected molecular ion at m/z 158 is absent because of its relative instability. It fragmented into other ions whose signals are seen. The most stable fragment is the one at m/z 42 and this is called the base peak. Due to the extensive fragmentation that occurs in EI it is classified as a hard ionization source. Advantages and disadvantages of EI are presented in Table 2. Table 2. Advantages and disadvantages of electron ionization sources. Advantages Results in reproducible, instrument transferable, extensive fragmentation Information from the mass spectrum produced with EI can be used to elucidate the structure of a molecule. This is done by comparing the spectrum to several spectra in a Disadvantages Analytes must be in gas phase prior to introduction into the ion source This makes it unsuitable for thermally unstable and non-volatile compounds The non-volatility problem can be overcome by derivatization of the analyte to a volatile form (e.g.

4 large database containing spectra of known compounds.. Easily interfaced with a gas chromatograph RCOOH can be derivatized to RCOOR ) Some compounds fragment so extensively that the molecular ion peak is absent from their mass spectrum. This makes interpretation more challenging. Chemical Ionization Chemical ionization utilizes the same apparatus as EI but it is operated at higher pressure (~ Pa in the ion box). Also, the electron energy is increased to ev so that the electron beam can penetrate further into the ion box. Chemical ionization is an indirect process. The first step involves ionization of a reagent gas (such as methane, CH 4 ) with the energetic electrons from the filament CH e CH 2 e ( CH other ions) In the second step, reagents ions are formed CH CH CH CH CH CH C H H In the third step, the analyte molecule is ionized by reacting with the reagent ions through one or more of the following reactions: 5 4 M CH M H CH (Proton transfer) 5 5 M CH M CH (Adduct formation) M C H M C H (Adduct formation) M C H M H C H (Hydride Abstraction) Besides methane other reagents that are utilized include isobutyl chloride, water, ethanol, acetone, and methylamine.

5 Relative Abundance m/z Figure 4: The CI mass spectrum of decanol (CH 3 (CH 2 ) 9 OH). The peak at m/z 141 is the base peak and it is due to loss of OH - [M-OH] +. The peak at m/z 157 is the molecular ion peak due to hydride abstraction [M-H] +. As noted in the mass spectrum representation in Figure 4, chemical ionization produces less fragmentation of the molecular ion. As such, the mass spectrum Is simpler and cleaner compared to that obtained with EI. Additionally, the molecular ion is observed (at [M+H] +, [M-H] +, and/or [M + adduct] + ). However, CI does not produce sufficient fragmentation to facilitate structural information. Additionally, like EI, it is not suitable for thermally unstable compounds. Electrospray Ionization Source (ESI) With ESI, ions are generated under atmospheric pressure. Hence this approach is classified as atmospheric pressure ionization (API) technique. The ESI device is comprised of a needle (~ 0.2mm outer diameter, ~0.1mm inner diameter) that is encased in a sleeve through which a sheath gas flows. This gas (typically N 2 ) is used to nebulize the sample solution that is pumped through the needle. Sample flow rate is typically about L /min. In operation a high voltage (2-6kV relative to the ion extraction cone) is applied to the needle. Ions are typically formed in solution prior to desorption into the gas phase. To facilitate this, sample solutions are made in polar solvents such as aqueous methanol or aqueous acetonitrile. The solvent is typically modified with volatile weak acids such as formic, acetic acids, or trifluoroacetic acid, or salts of weak bases such as ammonium acetates. This facilitates abundance of charged species ( such as H + ) which are necessary for ion formation. Upon nebulization, the droplets are surrounded with charged species such as H +. As the droplets evaporate, the charge density increases. At a certain size, the charge density becomes high enough that the droplet explodes due to columbic repulsion between the charges. Charges are then transferred to the analytes (see Figure 5). The ions are typically adducts of H, ([M+H] + ), adducts of salt ions such as M+Na +, adducts of counter ions of the modifier e.g. M+NH 4 + and M+CH 3 COO -. These ions don t undergo significant fragmentations. Therefore, the mass spectrum obtained with ESI is generally clean and simple. Protonated or deprotonated molecular ions are typically observed.

6 ESI needle Sheath or nebulizing gas Analyte solution Analyte ion Charged aerosol Figure 5: Schematic diagram of an electrospray ionization device and ion formation process. Molecules such as proteins that have multiple sites through which they can be protonated or deprotonated can be multiply charged. The significance of this is that a large molecule can be observed at a lower m/z. One advantage of ESI over EI or CI is that it is readily interfaced with liquid-based separation techniques such as HPLC and capillary electrophoresis. Matrix Assisted Laser Desorption Ionization (MALDI) The MALDI process is split into two steps: sample preparation and ion formation. During sample preparation, the analyte to be transformed into ions is mixed with solution of a substance that is referred to as the matrix. The solvent is evaporated and the solid residue that is produced is placed under vacuum in the mass spectrometer, where it is irradiated with pulses of photons from a laser source (Figure 6). Radiation from Laser hv Desorption Desolvation and protonation Matrix Neutral Analyte

7 Figure 6: Schematic diagram of a Matrix assisted laser desorption ionization (MALDI) device and ion formation process. Energy from the photons causes a rapid heating of the crystals. This results in a localized ablation and sublimation of the matrix crystals. Intact analytes are entrained in the plume that is formed. Ionization can occur during this process via any of the following: proton transfer, ion molecule reactions, desorption of preformed ions. MALDI is commonly used for studying non-volatile and thermally labile compounds such as proteins, oligonucleotides, synthetic polymers and large inorganic compounds. Commonly used matrices ar cyano-4-hydrocinnamic acid for peptides; 3,5-dimethyoxy-4-hydroxycinnamic acid for proteins and polymers; 2,5-dihydroxybenzoic acid for peptides, proteins, lipids, and nucleic acids. 3 hydroxypicolinic acid is used for nucleic acid and DNA analysis. Laser sources that have been used include: nitrogen (337nm), Nd:YAG (355 and 266nm) Er:YAG (2.94 m) and CO 2 (10.6 m). Some advantages of this method include: simple sample preparation and tolerance to contamination from salts, buffers and detergents commonly used in sample preparation for biochemical analysis. Atmospheric Pressure Chemical Ionization (APCI) Atmospheric pressure chemical ionization (APCI) as the name indicates belongs to the group of ion sources that are operated under ambient atmospheric pressures. The principle of operation of APCI is similar to that of chemical ionization (CI) with the major difference that CI is operated under vacuum. APCI is comprised of a heated nebulizing probe, a corona discharge electrode (typically a needle) and a system of ion extraction lenses to transmit ions into a mass analyzer (see figure 1). Figure 1: Schematic diagram of a typical atmospheric pressure chemical ionization (APCI) source

8 In operation, the analyte solution (typically delivered with a syringe or Liquid chromatograph) is directed through a capillary tube (made of stainless steel or fused silica with ~120m internal diameter) at about 0.2-2ml/min into the APCI probe. A nebulizing gas at about 80psi is used to convert the solution into fine droplets. A heated ( o C) coaxial sheath gas flow helps to evaporate and convert the droplets into a stream of gaseous analyte and solvent molecules which are directed to the ionization region. The ionization region contains a discharge electrode that is held at a high potential (2 to 3 kv) with respect to the ion extraction lens. Assuming nitrogen is utilized as the nebulizer and sheath gas, ions such as the N 2 +., N 4 +, O 2 +. and NO + are formed in the corona discharge, These then interact with solvent molecules (e.g. water vapor from the atmosphere or sample) in a cascade of reactions that culminates in the production of secondary ions (e.g. water or solvent cluster ions). Reaction between the solvent ions and analyte molecules leads to the formation of analyte ion. For example: H O H O M M nh O 3 2 n 2 Application This ion sources is typically used in LC-MS for less polar (e.g. PAH, PCB, Fatty acids, Phthalates, triglycerides), thermally stable compounds. When compared to electrospray (ESI), APCI is more tolerant to contaminants that cause ion suppression. This makes it more useful for analysis of biological samples that contain high salt concentrations.

Chemistry Instrumental Analysis Lecture 37. Chem 4631

Chemistry 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 information

20.2 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. 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 information

Lecture 15: Introduction to mass spectrometry-i

Lecture 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 information

Chemistry Instrumental Analysis Lecture 34. Chem 4631

Chemistry 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 information

Mass Spectrometry. Electron Ionization and Chemical Ionization

Mass 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 information

Mass Spectrometry. General Principles

Mass 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 information

1) In what pressure range are mass spectrometers normally operated?

1) 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 information

Selecting an LC/MS Interface Becky Wittrig, Ph.D.

Selecting 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 information

Mass Spectrometry (MS)

Mass 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 information

Fundamentals of Mass Spectrometry. Fundamentals of Mass Spectrometry. Learning Objective. Proteomics

Fundamentals 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 information

Molecular Mass Spectrometry

Molecular 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 information

Mass spectrometry and elemental analysis

Mass 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 information

Harris: Quantitative Chemical Analysis, Eight Edition

Harris: 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 information

Chemistry 311: Topic 3 - Mass Spectrometry

Chemistry 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 information

TANDEM MASS SPECTROSCOPY

TANDEM 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 information

Mass Spectrometry in MCAL

Mass 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 information

Lecture 8: Mass Spectrometry

Lecture 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 information

Instrumental Analysis. Mass Spectrometry. Lecturer:! Somsak Sirichai

Instrumental 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 information

Mass spectrometry.

Mass 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 information

Lecture 8: Mass Spectrometry

Lecture 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 information

Ionization Techniques Part IV

Ionization 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 information

LC-MS Based Metabolomics

LC-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 information

Electrospray Ion Trap Mass Spectrometry. Introduction

Electrospray Ion Trap Mass Spectrometry. Introduction Electrospray Ion Source Electrospray Ion Trap Mass Spectrometry Introduction The key to using MS for solutions is the ability to transfer your analytes into the vacuum of the mass spectrometer as ionic

More information

Mass Spectrometry for Chemists and Biochemists

Mass 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 information

Ch 13. Basics of Mass Spectrometry (I) : Principles & Ionization Sources

Ch 13. Basics of Mass Spectrometry (I) : Principles & Ionization Sources 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

More information

Molecular Mass Spectrometry

Molecular 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 information

LIQUID 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 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 information

Analysis of Polar Metabolites using Mass Spectrometry

Analysis 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 information

HPLC solvents and mobile phase additives

HPLC solvents and mobile phase additives HPLC solvents and mobile phase additives The following is intended to be a guide for the choice of solvent and mobile phase additives. Of course the choice of solvents for LC will be dictated primarily

More information

CHAPTER A2 LASER DESORPTION IONIZATION AND MALDI

CHAPTER 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 information

Other 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. 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 information

Analytical 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 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 information

CEE 772: Instrumental Methods in Environmental Analysis

CEE 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

MS Goals and Applications. MS Goals and Applications

MS 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 information

1. The range of frequencies that a measurement is sensitive to is called the frequency

1. 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 information

IDENTIFICATION OF ORGANOMETALLIC COMPOUNDS USING FIELD DESORPTION IONIZATION ON THE GCT

IDENTIFICATION 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 information

Macromolecular Chemistry

Macromolecular 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 information

The AccuTOF -DART 4G: The Ambient Ionization Toolbox

The 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

Quattro Micro - How does it work?

Quattro Micro - How does it work? Quattro Micro - How does it work? 1 Introduction This document is designed to familiarise you with the principles behind how the Quattro Micro works. The level of this document is designed as Level One

More information

Mass 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 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 information

Mass spectrometry gas phase transfer and instrumentation

Mass 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 information

MS Goals and Applications. MS Goals and Applications

MS 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 information

Mass Spectrometry Course

Mass 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 information

Fast Atom Bombardment (FAB)-MS

Fast 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 information

Proudly serving laboratories worldwide since 1979 CALL for Refurbished & Certified Lab Equipment

Proudly 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 information

Direct Analysis in Real Time (DART) A New Ionization Technique

Direct Analysis in Real Time (DART) A New Ionization Technique Direct Analysis in Real Time (DART) A New Ionization Technique Introduction K. P. Madhusudanan Sophisticated Analytical Instrument Facility, Central Drug Research Institute, Lucknow, India - 226001 Direct

More information

Chapter 1. Introduction

Chapter 1. Introduction Chapter 1. Introduction 1-1 1.1. Overview In the past twenty years, charged droplets and strong electric fields have quietly revolutionized chemistry. In combination with an atmospheric-sampling mass spectrometer,

More information

sample was a solution that was evaporated in the spectrometer (such as with ESI-MS) ions such as H +, Na +, K +, or NH 4

sample 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 information

Utilizing ELSD and MS as Secondary Detectors for Prep HPLC and Flash Chromatography. Tips and Techniques to Optimize ELSD and MS based Purification

Utilizing ELSD and MS as Secondary Detectors for Prep HPLC and Flash Chromatography. Tips and Techniques to Optimize ELSD and MS based Purification Utilizing ELSD and MS as Secondary Detectors for Prep HPLC and Flash Chromatography Tips and Techniques to Optimize ELSD and MS based Purification Utilizing ELSD and MS as Secondary Detectors for Prep

More information

API Optimization, Source Design, and Other Considerations of LC/MS

API Optimization, Source Design, and Other Considerations of LC/MS API Optimization, Source Design, and Other Considerations of LC/MS Instrument Design Considerations: The Atmosphere-Vacuum Interface and Pumping System The hows and whys of the vacuum? We ve got to get

More information

Mass Spectrometry. A truly interdisciplinary and versatile analytical method

Mass 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 information

Mass Spectrometry. Hyphenated Techniques GC-MS LC-MS and MS-MS

Mass 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 information

KJ3022 MS compendium gives a deeper explanation of what is mentioned in the slides

KJ3022 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 information

15.04.jpg. Mass spectrometry. Electron impact Mass spectrometry

15.04.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 information

Ion sources. Ionization and desorption methods

Ion 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 information

4. How can fragmentation be useful in identifying compounds? Permits identification of branching not observed in soft ionization.

4. 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 information

Selecting Detectors for Compounds with No Optical Absorbance

Selecting Detectors for Compounds with No Optical Absorbance C146-E114 Selecting Detectors for Compounds with No Optical Absorbance Technical Report vol.15 1. Features of Absorbance Detectors In HPLC, the detector is selected in accordance with the analyte. Many

More information

BIOINF 4399B Computational Proteomics and Metabolomics

BIOINF 4399B Computational Proteomics and Metabolomics BIOINF 4399B Computational Proteomics and Metabolomics Sven Nahnsen WS 13/14 3. Chromatography and mass spectrometry Overview Recall last lecture Basics of liquid chromatography Algorithms to predict and

More information

Mass Spectrometry. Fundamental LC-MS. Electrospray Ionisation Instrumentation

Mass Spectrometry. Fundamental LC-MS. Electrospray Ionisation Instrumentation Mass Spectrometry Fundamental LC-MS Electrospray Ionisation Instrumentation i Wherever you see this symbol, it is important to access the on-line course as there is interactive material that cannot be

More information

Basics of Mass Spectrometry

Basics of Mass Spectrometry Handbook of instrumental techniques from CCiTUB Basics of Mass Spectrometry Lourdes Berdié 1, Isidre Casals 2, Irene Fernández 3, Olga Jáuregui 2, Rosa Maria Marimon 4, Joaquim Perona 4, and Pilar Teixidor

More information

Auxiliary Techniques Soft ionization methods

Auxiliary 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 information

TMT4320 Nanomaterials November 10 th, Thin films by physical/chemical methods (From chapter 24 and 25)

TMT4320 Nanomaterials November 10 th, Thin films by physical/chemical methods (From chapter 24 and 25) 1 TMT4320 Nanomaterials November 10 th, 2015 Thin films by physical/chemical methods (From chapter 24 and 25) 2 Thin films by physical/chemical methods Vapor-phase growth (compared to liquid-phase growth)

More information

Ionization Methods in Mass Spectrometry at the SCS Mass Spectrometry Laboratory

Ionization 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

Mass Spectroscopy. Base peak. Molecular Ion peak. The positively charged fragments produced are separated, based on their mass/charge (m/z) ratio. M+.

Mass 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 information

MS/MS .LQGVRI0606([SHULPHQWV

MS/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 information

Chapter 5 Basic Mass Spectrometry

Chapter 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 information

MASS SPECTROMETRY. Topics

MASS 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 information

Analytical Technologies and Compound Identification. Daniel L. Norwood, MSPH, PhD SCĪO Analytical Consulting, LLC.

Analytical 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 information

Agilent G3212 GC-APCI Source

Agilent G3212 GC-APCI Source Agilent G3212 GC-APCI Source Quick Start Guide Where to find information 2 Getting Started 3 Step 1. Start the Data Acquisition program for the GC and the Q-TOF 3 Step 2. Prepare the GC and Q-TOF for data

More information

MASS SPECTRA measure a compound s Mol. Wt. This ionization type is called: electron impact MS

MASS 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 information

Ch. 22 Mass Spectrometry (MS)

Ch. 22 Mass Spectrometry (MS) Ch. Mass Spectroetry (MS).1 MS easures ass of atos, olecules, or fragents of olecules -1. What is MS? Gaseous ato fro condensed phase ionized Accelerated & separated By ass to charge ratio /z M=00: 1 ion

More information

LECTURE-13. Peptide Mass Fingerprinting HANDOUT. Mass spectrometry is an indispensable tool for qualitative and quantitative analysis of

LECTURE-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 information

Finnigan LCQ Advantage MAX

Finnigan 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 information

Extrel Application Note

Extrel Application Note Extrel Application Note Real-Time Plasma Monitoring and Detection of Trace H 2 O and HF Species in an Argon Based Plasma Jian Wei, 575 Epsilon Drive, Pittsburgh, PA 15238. (Presented at the 191st Electrochemical

More information

CHROMATOGRAPHY AND MASS SPECTROMETER

CHROMATOGRAPHY AND MASS SPECTROMETER 22 CHROMATOGRAPHY AND MASS SPECTROMETER 22.1 INTRODUCTION We know that the biochemistry or biological chemistry deals with the study of molecules present in organisms. These molecules are called as biomolecules

More information

Qualitative Organic Analysis CH 351 Mass Spectrometry

Qualitative 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 information

Olumide Adebolu. Chromatographic Fidelity and Matrix /Analyte Solubility in Complex Polymer Systems using HPLC-MALD/I TOF MS

Olumide 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 information

Presentation Basic Introduction to Instrumentation Matrix Effects Challenges

Presentation 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 information

Welcome to Organic Chemistry II

Welcome to Organic Chemistry II Welcome to Organic Chemistry II Erika Bryant, Ph.D. erika.bryant@hccs.edu Class Syllabus 3 CHAPTER 12: STRUCTURE DETERMINATION 4 What is this solution Soda Tea Coffee??? 5 What is this solution Soda Tea

More information

LC MS analysis of metabolites. Basis of Chromatography

LC MS analysis of metabolites. Basis of Chromatography GBS 724 LC MS analysis of metabolites Stephen Barnes, PhD 4 7117; sbarnes@uab.edu Basis of Chromatography A moving (mobile) phase passes over an inert, stationary phase The compounds differentially interact

More information

CEE 772 Lecture #27 12/10/2014. CEE 772: Instrumental Methods in Environmental Analysis

CEE 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 information

INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRY

INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRY INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRY Edited by AKBAR MONTASER George Washington University Washington, D.C. 20052, USA WILEY-VCH New York Chichester Weinheim Brisbane Singapore Toronto CONTENTS

More information

Mass 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 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 information

MALDI-TOF: a powerful tool for the analysis of biomolecules and large organic molecules

MALDI-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 information

CEE 772: Instrumental Methods in Environmental Analysis

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 information

Supporting Information. Use of Mass Spectrometric Vapor Analysis to Improve Canine Explosive Detection Efficiency

Supporting Information. Use of Mass Spectrometric Vapor Analysis to Improve Canine Explosive Detection Efficiency Supporting Information Use of Mass Spectrometric Vapor Analysis to Improve Canine Explosive Detection Efficiency Ta-Hsuan Ong, Ted Mendum, Geoff Geurtsen, Jude Kelley, Alla Ostrinskaya, Roderick Kunz Chemical,

More information

Ch. 8 Introduction to Optical Atomic Spectroscopy

Ch. 8 Introduction to Optical Atomic Spectroscopy Ch. 8 Introduction to Optical Atomic Spectroscopy 8.1 3 major types of Spectrometry elemental Optical Spectrometry Ch 9, 10 Mass Spectrometry Ch 11 X-ray Spectrometry Ch 12 In this chapter theories on

More information

Ch.28 HPLC. Basic types of Liquid Chromatography Partition (LLC) Adsorption (LSC) Ion Exchange (IC) Size Exclusion (SEC or Gel Chromatography)

Ch.28 HPLC. Basic types of Liquid Chromatography Partition (LLC) Adsorption (LSC) Ion Exchange (IC) Size Exclusion (SEC or Gel Chromatography) Ch.28 HPLC 28.1 Basic types of Liquid Chromatography Partition (LLC) Adsorption (LSC) Ion Exchange (IC) Size Exclusion (SEC or Gel Chromatography) High Performance (Pressure) LC Glass column st.steel (high

More information

Mass Spectrometry: Introduction

Mass 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 information

Chapter 6. Neutral droplets in high electric fields as a. source of ions. Introduction to field-induced droplet

Chapter 6. Neutral droplets in high electric fields as a. source of ions. Introduction to field-induced droplet Chapter 6. Neutral droplets in high electric fields as a source of ions. Introduction to field-induced droplet ionization mass spectrometry 6-1 Adapted from Grimm, R. L. and Beauchamp, J. L. J. Phys. Chem.

More information

Chemical Aspects of Mass Spectrometry

Chemical 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 information

Assay Robustness Improvement for Drug Urinalysis Using FAIMS and H-SRM on a Triple- Quadrupole Mass Spectrometer

Assay Robustness Improvement for Drug Urinalysis Using FAIMS and H-SRM on a Triple- Quadrupole Mass Spectrometer 38 Current Trends in Mass Spectrometry November 6 Assay Robustness Improvement for Drug Urinalysis Using FAIMS and H-SRM on a Triple- Quadrupole Mass Spectrometer This article demonstrates the improved

More information

This document is a preview generated by EVS

This document is a preview generated by EVS TECHNICAL REPORT RAPPORT TECHNIQUE TECHNISCHER BERICHT CEN/TR 15641 August 2007 ICS 67.050 English Version Food analysis - Determination of pesticide residues by LC- MS/MS - Tandem mass spectrometric parameters

More information

Webinar: How to be More Successful with your ACQUITY QDa Detector Eric van Beelen

Webinar: How to be More Successful with your ACQUITY QDa Detector Eric van Beelen Webinar: How to be More Successful with your ACQUITY QDa Detector Eric van Beelen 2015 Waters Corporation 1 We are here to address any Questions you may have That s the benefit of participating to the

More information

AN INTRODUCTION TO ATOMIC SPECTROSCOPY

AN INTRODUCTION TO ATOMIC SPECTROSCOPY AN INTRODUCTION TO ATOMIC SPECTROSCOPY Atomic spectroscopy deals with the absorption, emission, or fluorescence by atom or elementary ions. Two regions of the spectrum yield atomic information- the UV-visible

More information

Introduction to Pharmaceutical Chemical Analysis

Introduction to Pharmaceutical Chemical Analysis Introduction to Pharmaceutical Chemical Analysis Hansen, Steen ISBN-13: 9780470661222 Table of Contents Preface xv 1 Introduction to Pharmaceutical Analysis 1 1.1 Applications and Definitions 1 1.2 The

More information

Propose a structure for an alcohol, C4H10O, that has the following

Propose 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 information

FAIMS Technology at a Glance

FAIMS Technology at a Glance FAIMS Technology at a Glance Field asymmetric ion mobility spectrometry (FAIMS), also known as differential mobility spectrometry (DMS), is a gas detection technology that separates and identifies chemical

More information

Welcome!! Chemistry 328N Organic Chemistry for Chemical Engineers. Professor: Grant Willson

Welcome!! Chemistry 328N Organic Chemistry for Chemical Engineers. Professor: Grant Willson Welcome!! - 50750 Organic Chemistry for Chemical Engineers Professor: Grant Willson Teaching Assistants: Ji yeon Kim, Jai Hyun Koh, Paul Meyer, Qingjun Zhu http://willson.cm.utexas.edu January 19,2016

More information

Introduction of Hitachi Chromaster 5610 MS Detector for High Performance Liquid Chromatograph

Introduction of Hitachi Chromaster 5610 MS Detector for High Performance Liquid Chromatograph SCIETIFIC ISTRUMET EWS 2016 Vol. 7 SEPTEMBER Technical magazine of Electron Microscope and Analytical Instruments. Technical Explanation Introduction of Hitachi Chromaster 5610 MS Detector for High Performance

More information