Documente Academic
Documente Profesional
Documente Cultură
GC/MS
Dr. Mufeed Batarseh
Training course 21-24 Jan 2007
Prince Faisal center for Dead sea, Environmental and Energy Research
Why GC/MS?
GC/MS Introduction 2
What is GC/MS ?
GC + MS GC/MS
• GC is superior in separating of multi-components.
• GC is not good at identifying peak components.
• MS allows identification from mass spectrum.
• SIM method of GC/MS allows accurate quantitation.
GC/MS Introduction 3
Capabilities of GC/MS
GC/MS Introduction 4
Sensitivity and Selectivity
z Full Scan
- Detection Limits of 1 - 10 picograms
- Identification of unknowns by reference library
- Confirmation by retention time and spectra
z Selected Ion Mode
- Detection Limits of 10 - 100 femtograms
- Identification by retention time
- Confirmation by Ion ratios
z Selectivity
- Compound (vs. functionality like ECD or NPD)
GC/MS Introduction 5
Universal and Specific
Interference-Free Quantification
Universal Specific
GC/MS Introduction 6
Universal and Specific
GC/MS Introduction 7
The GC/MS Interface
Vacuum Manifold
GC/MS Introduction 8
Jet Separator
From Vacuum To
GC MS
GC/MS Introduction 9
Direct Capillary Interface
z Advantages
- Simple
- Low cost
- Minimal
reactivity
dead volume
selectivity
z Disadvantages
- Limited flow rate
- Limits column ID range
GC/MS Introduction 10
Why is an Ion Source Needed?
GC/MS Introduction 11
Sample Ionization for GC
GC/MS Introduction 12
Sample Ionization
GC/MS Introduction 13
Electron Ionization Source
GC/MS Introduction 14
Electron Ionization Reactions
molecule + 2e-
molecule + e- .
+
Fragmentation
molecule mole cule
+ . +
+ .
ion radical
mole mo + le
+ +
neutral molecule
GC/MS Introduction 15
Advantages of Electron Ionization
z Simple construction
z High ionization efficiency (10-5)
z Highly characterized fragmentation patterns
“Fingerprints”
z Existing computer-searchable libraries of EI spectra
z Limited secondary reactions due to collisions
GC/MS Introduction 16
Disadvantages of Electron Ionization
GC/MS Introduction 17
Positive Chemical Ionization Reactions
R + e- R+ + 2e-
R+ + RH RH+ + R
RH+ + M MH+ + R
R = reagent
M = sample molecule
e- = electron
= radical electron
H = hydrogen
GC/MS Introduction 18
Reagent Gas Ions
H2 H2+. H3+
NO NO+. NO+
GC/MS Introduction 19
Advantages of Chemical Ionization
z Minimal fragmentation
z MW information, even when EI may not
z Reagent gases can be compound selective
- Selectivity by proton or electron affinity
- Isomer selectivity possible
- Double-bond location
- ECD selectivity possible
z ECD-like sensitivity possible
z Lower background spectra
GC/MS Introduction 20
Disadvantages of Chemical Ionization
GC/MS Introduction 22
Types Of Mass Analyzers
z Magnetic Sector
- High resolution
- High sensitivity
- High cost
z Time-of-Flight (TOF)
- High speed
100 - 1000 spectra/second
- High sensitivity
- Wide mass range
- High cost
GC/MS Introduction 23
Types of Mass Analyzers (continued)
z Ion Trap
- Complex Sample Matrix may cause problems
- Self Induced CI
- MS/MS
z Quadrupole
- Rapid Scanning
- Easily Interfaced
- High Sensitivity
- Best GC Detector EVER MADE
GC/MS Introduction 24
Advantages of Quadrupole Mass
Spectrometry
z High Sensitivity
z Simplicity of Operation
z Immunity to coeluting peaks
z Rapid Scanning
z Single and Multiple Ion Scanning
z Easily Interfaced
GC/MS Introduction 25
Quadrupole
Electron
Multiplier
Electron Reflector
Filament
Entrance Lens
Lens 2
Lens 1
Ionizer
GC Column
GC/MS Introduction 26
Quadrupole Mass Analyzer
+Vrf only
+ + + m2 m4
m1
m3
++ + m1 m2
m3
m4
GC/MS Introduction 27
The Detector
Vacuum Manifold
GC/MS Introduction 28
Detectors
z Electron Multiplier
- Continuous Dynode
- Discrete Dynode
- Electron Multiplier Disadvantages
Lifetime limited by ion dosage
Contamination
HV discharge
z Photomultiplier
- Long life (10 years)
- Immune to contamination
GC/MS Introduction 29
Continuous Dynode Electron Multiplier
ion
EM Gain with Time
107
0
106
EM voltage
Gain
105
104
103
-3000
2 6 10 14 18
Time (months)
GC/MS Introduction 30
Photomultiplier
Photocathode
Electron optics
Electron
multiplier
Anode
Mounting
Base
GC/MS Introduction 31
Photomultiplier Detection System
Conversions
Ions
Conversion Dynode
Electrons
Phosphor
Photons
Photomultiplier
Electron Current
GC/MS Introduction 32
Photomultiplier
Dynodes
Photoelectron
Secondary
Radiation electrons
hν
Photoemissive Anode
cathode
current-to-
voltage
High voltage (-)
amplifier
200 - 2000V
GC/MS Introduction 33
Vacuum System
Vacuum Manifold
GC/MS Introduction 34
Turbomolecular Pump
Rotating blade
Fixed blade
to
roughing
pump
Motor
GC/MS Introduction 35
GC/MS Summary
GC/MS Introduction 36
TurboMass Physical Components
Vacuum Manifold
GC/MS Introduction 37
Vacuum Pumps
z Backing Pump
- 3.0 m3/hr mechanical pump
GC/MS Introduction 38
250 L/sec Turbomolecular Pump
GC/MS Introduction 39
TurboMass Ion Optics
Magnet
Lens
Filament 2 Analytical
Quadrupole Phosphor
Repeller + Screen
Pre
Collector Lens Conversion
Quads Photo-
1 Dynode multiplier
Magnet
GC/MS Introduction 40
Ion Optics
Reference & CI RF Amplifier
Gas Inlets
Prefilter
Quadrupole
Outer PMT
Conversion
GC Ion Source Phosphor
Dynode
Column
GC/MS Introduction 41
Thank you
GC/MS Introduction 42