Mass Spectroscopy

Introduction
 Mass spectrometry is an analytical technique used to quantify known
materials, to identify unknown compounds within a sample and to explain
the structure and chemical properties of different molecules.
 It is a micro-analytical technique in which the molecules are converted to
gaseous ions that are subsequently separated in a mass spectrometer
according to their mass-to-charge (m/z) ratio and detected.
 Mass spectrometry has both qualitative and quantitative uses.
 The mass spectrum of each compound is unique and can be used as a
“chemical fingerprint” to characterize the sample
 Mass spectrometry is used in many areas including pharmaceutical, clinical,
biotechnology and environmental.
Principle
 In mass spectrometry, molecules are bombarded with a beam of energetic electrons in gaseous using
tungsten or rhenium filament. Molecules are broken up into cations and many other fragments.
 These cations are formed due to loss of an electron
from a molecule and can be accelerated and
deflected by magnetic or electric fields.
 The deflection of ions depends on its mass, charge
and velocity.
 The deflection is recorded and the output is known
as mass spectrum.
 Each line upon the mass spectrum indicates the
presence of atoms or molecules of a particular mass.
 The most intense peak in the spectrum is taken as
the base peak. Its intensity is taken as 100 and other
peaks are compared with it.
Instrumentation
 The essential components of a mass spectrometer consist of:
A. A sample inlet

B. An ionization source

C. A mass analyzer

D. An ion detector

E. Vacuum system
A. Sample inlet
 Solid samples with lower vapor pressure: Directly inserted into ionization chamber &

volatilization is controlled by heating the probe

 Liquids are handled by hypodermic needle injection through a silicon rubber dam

 Gaseous samples are leaked into the ionization chamber directly by the help of mercury

manometer
B. Ionization methods
 Ionization method refers to the mechanism of ionization while the ionization source is the
mechanical device that allows ionization to occur.

 The different ionization methods are as follows:

 Protonation
 De-protonation
 Cationization
 Transfer of a Charged Molecule to the Gas Phase
 Electron Ejection
 Electron Capture
Ionization source
 Electrospray Ionization (ESI)

 Atmospheric Pressure Chemical Ionization (APCI)

 Atmospheric pressure photoionization (APPI)

 Matrix-assisted laser desorption/ionization (MALDI)

 Fast Atom Bombardment (FAB)

 Electron Ionization (EI)

 Chemical Ionization (CI)

C. Mass analyzer
 The mass analyzer separates different molecular ions, generate fragment ions and then measure mass of
the fragmented ions.
 The characteristics of mass analyzers are:
 Resolution
 Mass accuracy
 Sensitivity
 Scan speed
 With the advancement of ionization sources that can vaporize and ionize molecules, it has become
necessary to improve mass analyzer performance with respect to speed, accuracy, and resolution.
1. Quadrupoles
2. Magnetic sectors
3. Time-of-flight
1. Quadrupoles
2. Magnetic sectors
3. Time-of-flight
D. Ion detector
 Once the ions are separated by the mass analyzer, they reach the ion detector, which
generates a current signal from the incident ions.

 The most commonly used detectors in MS are as follows:

1. Faraday cup

2. Electron multiplier

3. Photomultiplier dynode

4. Charge (or Inductive) Detector

E. Vacuum system
 Mass analyzers require vacuum so that the analyte ions must be manageable and

sensitive to the electrostatic components of the instrument.

 This is used to remove the background (air) molecules, as the deflection of ions

takes place only by the influence of electric and magnetic fields, which would

otherwise result in deviation due to collision.

Applications
 Determination of molecular weight

 Determination of structure of compounds

 Determination of molecule abundance

 Differentiation between isomers

 Detection of impurity

 Identification of unknown compounds

Thank You