Mass Spectroscopy Quantitative Chemical Analysis Harris, 6th Edition

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Presentation transcript:

Mass Spectroscopy Quantitative Chemical Analysis Harris, 6th Edition Chapter 22 Mass Spectroscopy Quantitative Chemical Analysis Harris, 6th Edition

What is Mass Spec Generation and Separation of Charged Molecules based on a mass to charge ratio. Applications from Geochemistry to Biotechnology

Mass Definitions Atomic Mass – Mass from periodic table based isotope abundance Molecular Mass – Mass for the sums of the atomic masses (Water = 2*1.0079 + 15.9994 = 18.0152 Da) Nominal Mass - Sum of integer masses of most abundant isotopes. (Water = 18 Da)

Typical Mass Spectrometer Ion source - electron beam Ion separation - magnet Ion detection - Electron multiplier A high vacuum method (avoid collisions that will effect ions)

Ionization Process M + e- (70 eV) → M+. + e- (~55 eV) + e- ( 0.1 eV) Typical ionization energies are 9 to 10 eV

Chemical Ionization Add a gas such as methane in greater amount. The methane in ionized and then the energy is transferred to the analyte on collision. Much less energy passed to analyte

Resolution Most application require the ability to resolve integer difference in the working range. Some high resolution instruments are available and these can give exact molecular formula

Small portion of Methyl Stearate (CH3(CH2)16CO2CH3

Isotope patterns tell us much.

For interpretation

Quadrupole Ion Separators

Time of Flight

Quadrupole Ion Trap

Quadrupole Ion Trap

LC – MS Pneumatically Assisted Electrospray

Gas Phase Ion Formation

Outlet Photograph

CZE – MS Interface

Atmospheric Pressure Chemical Ionization APCI

Selected Ion Monitoring

Triple Quad Instruments

MALDI – Matrix Assisted Desorption / Ionization

MALDI Example

Electrospray of Proteins (Multiple Charges) Acidified bovine cytochrome c