You are on page 1of 42

Introduction to TurboMass

GC/MS
Dr. Mufeed Batarseh
Training course 21-24 Jan 2007
Prince Faisal center for Dead sea, Environmental and Energy Research
Why GC/MS?

z Universal and specific


z Sensitive
z Positive identification with standard or library spectrum
z Interference-free quantitation
z Isotopically labeled internal standards

GC/MS Introduction 2
What is GC/MS ?

z Composite instrument made up of GC and 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

z Combines separation and identification techniques


z Provides both quantitative and qualitative information
about sample
z Offers the best solution to many analytical problems
z Interference-free quantitation

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

Inlet Transfer Ion Mass


System line Analyzer Detector
source
GC

High Vacuum Vacuum


Pump Gauges

Data System Backing MS


Pump Electronics

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?

z Charged particles (ions) can be easily manipulated


with electrical and magnetic fields
- focusing
- diverting
- filtering
- detecting
z Neutral particles (molecules) are much more difficult to
manipulate

GC/MS Introduction 11
Sample Ionization for GC

z Electron Ionization (EI)


- High energy - 70 eV
- Positive Ions
- Fragmentation - Structural information
z Chemical Ionization (CI)
- Low energy
- Positive and Negative Ions
- Ion-molecule reactions with Reagent Gas
- Methane, Isobutane, Ammonia typical

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

z Sample must be in gaseous state


z Can cause excessive fragmentation
z Some compounds do not yield molecular ion
z Spectra may not distinguish between isomers
z Some spectra are very complicated

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

Reagent Gas Molecular Ion Reagent Ion

CH4 CH4+. CH5+

H2 H2+. H3+

C4H10 C4H3+. C4H11+

NH3 NH3+. NH4+

CH3OH CH3OH+. CH3OH2+

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

z Less fragmentation than EI


z Spectrum not as informative
z Results depend on:
- reagent gas type, pressure
- temperature and reaction time
- analyte
z Spectrum may not be reproducible enough for library
search
z No commercially available computer-searchable
spectral libraries
z Requires more frequent ion source maintenance
GC/MS Introduction 21
The Mass Analyzer
Vacuum Manifold

Inlet Transfer Ion Mass


System line Analyzer Detector
source
GC

High Vacuum Vacuum


Pump Gauges

Data System Backing MS


Pump Electronics

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

Quadrupole Mass Filter

Entrance Lens
Lens 2
Lens 1

Ionizer
GC Column

GC/MS Introduction 26
Quadrupole Mass Analyzer

+Vrf only
+ + + m2 m4
m1
m3

( +Vdc + Vrf cos wt)

++ + m1 m2
m3
m4

GC/MS Introduction 27
The Detector
Vacuum Manifold

Inlet Transfer Ion Mass


System line Analyzer Detector
source
GC

High Vacuum Vacuum


Pump Gauges

Data System Backing MS


Pump Electronics

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

Focusing Electrode First dynode

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

Photoemissive Anode
cathode

current-to-
voltage
High voltage (-)
amplifier
200 - 2000V

GC/MS Introduction 33
Vacuum System
Vacuum Manifold

Inlet Transfer Ion Mass


System line Analyzer Detector
source
GC

High Vacuum Vacuum


Pump Gauges

Data System Backing MS


Pump Electronics

GC/MS Introduction 34
Turbomolecular Pump

Rotating blade

Fixed blade

to
roughing
pump
Motor

GC/MS Introduction 35
GC/MS Summary

z Universal and specific


z Sensitive
z Positive identification with standard or library spectrum
z Interference-free quantitation

GC/MS Introduction 36
TurboMass Physical Components
Vacuum Manifold

Inlet Transfer Ion Mass


System line Analyzer Detector
source
AutoSystem

High Vacuum Vacuum


Pump Gauges

Data System Backing MS


Pump Electronics

GC/MS Introduction 37
Vacuum Pumps

z High Vacuum Pump


- 250 L/sec Turbomolecular

z Backing Pump
- 3.0 m3/hr mechanical pump

GC/MS Introduction 38
250 L/sec Turbomolecular Pump

z Software controlled pump down


z Water cooling option
z Hardware controlled vent valve
- vents when pump slows to
50% full speed
z Maintenance free

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