Principles of Gas Chromatography and Its

Applications
Sathrugnan Karthikeyan
Analytical Solutions Leader

The world leader in serving science

 Analysis of Organics

Semi-
Volatile
Volatile

Non-
Elemental
Volatile

2
 Application of GC in Food Analysis

Comparison of GC and HPLC in food Analysis

3
 Snap shot about GC

GC is most widely used analytical technique in the world

–– Over 50 years in development
–– Fast Analysis
–– Small sample size

•GC is premier technique for separation and analysis of

volatile and semi-volatile compounds
–– Gases, liquids and solids
–– Organic and inorganic

4
 GC schematic/workflow

Key elements
7
4 6 • Gas
2 3 8
5 • Gas flow
1
• Injector
• Injection
• Oven temp
• Column
• Detector
• CDS

5
 Mobile phase – Gas

Most common mobile phase gases are N2, He or H2

• Carrier gas linear velocity determines the speed at solute molecules move
(function of column ID, length, pressure drop, column temp. & gas itself)

• Solute diffusion through the carrier gas

(limiting factor s are diffusion rate & linear velocity)

Van Deemter equation:

The van Deemter equation relates the resolving power (HETP, height equivalent to a theoretical plate) of a
chromatographic column to the various flow and kinetic parameters which cause peak broadening, as follows: Where

A = Eddy-diffusion parameter, related to channeling through a non-ideal packing [m]

B = diffusion coefficient of the eluting particles in the longitudinal direction, resulting in dispersion [m2 s−1] C =
Resistance to mass transfer coefficient of the analyte between mobile and stationary phase [s]
u = Linear Velocity [m s−1]

6
 Mobile phase – Gas flow

7
GC Injector
Split/ Splitless PTV

8
 Sample Injections
3 1. Liquid Injection
1
2. Dynamic Headspace

3. Online SPME

4. Purge and Trap

5. Thermal desorption

6. GC Pyrolysis

4 5 6
2

9
 GC Oven

Heater Shied; Fan; Temperature sensor;

Warm Air vent; Cold air intake; Inlet/outlet

The powerful and robust solution for superior oven performance

•Proprietary technology
• Perforated sheet metal walls and larger exhaust
•Large oven size
• Up to 2 capillary columns with standard cage
•Fast heating and cooling
• up to 125 °C/minute
•Both walls accessible
• Easy MS connections
• Additional devices

10
 GC Oven

Oven Temperature
• Set by the operator based on the type of analyte and column
• Should not be higher than the boiling point of analytes

Isothermal Temperature
• Simplest mixtures
• Temperature of the ovens remain constant

Programed Temperature (Gradient heating)

• Analysis of wide of range of volatiles
• Best separation in quickest time

11
 GC Columns

12
 GC Columns
GC Columns
Packed Column Capillary Column

13
 Column performance Evaluation

14
 Stationary Phases Summary

Name Phase Polarity

TG 1/ TG 1MS 100 % dimethyl polysiloxane Non polar

TG SimDist

TG 5/ TG5 MS (5% phenyl) methyl polysiloxane

TG V1 Cyanopropylphenyl polysiloxane

TG 1701 (14% cyanopropylphenyl) polysiloxane

35%
TG 35 MS (35% phenyl) polysilphenylene siloxane +
65%

TG 50 MS (50% phenyl) polysilphenylene siloxane

TG Wax/ Polyethylene glycol

TG Wax MS
TG FAME (70% cyanopropylphenyl) polysiloxane
Polar

15
 GC Detectors

• Thermal Conductivity Detector

• Flame Ionization Detector

• Electron Capture Detector

• Flame Photometric Detector

• Nitrogen Phosphorus Detector

• Mass Spectrometer Detector

16
 TRACE 1300 Series GC - A Completely New Platform

Versatility and Fast ROI: new

Savings: HeSaver module, Fully Hydrogen modular concept. Split/Splitless
compatible, Gas and power saving options, injector compatible with multi-
smart start-up, sleep functions vendor consumables and existing
GC methods for quick lab adoption

Performance:
Injectors with
integrated backflush Reliability/Up time:
Detectors with fast High quality materials,
response and auto- smart maintenance,
ranging capabilities routine grade reliability
New fast oven

Ease of Use: New touch Limited Bench-Space:

screen local user interface Smallest footprint,
Wide choice of CDS controls 2/3 of any other dual column GC

17
 Sample Injections

Liquid Injection

•Accurate volume

•Precise injection

•Proper rinsing

•Bubble free

•Inert/stable

18
Sample Injections

Liquid Injection - Automation

• Syringe Thermal Stability

• Cross-Contamination Free
• Injection Parameters
• Syringe Rinsing
• Standard Needle Depth
• High Accuracy
• High Precision

19
 Head Space GC
• Headspace' is the gas space above the sample in a
chromatography vial.

• Volatile sample components diffuse into the gas phase,

forming the headspace gas.

• Headspace gas chromatography is most suited to the

analysis of the very light volatiles in samples that can be
efficiently partitioned into the headspace gas volume
from the liquid or solid matrix sample.

• Higher boiling volatiles and semi-volatiles are not

detectable with this technique due to their low partition
in the gas headspace volume.

• Complex sample matrices, which may be difficult to

analyze directly or would otherwise require sample
extraction or preparation, are ideal candidates for
headspace

20
Sample Injections
Head Space gas injection - static

21
Sample Injections
Head Space gas injection - Dynamic

• Continuous gas extraction

• Trap volatiles on a sorbent

• Transfer to injector

• Thermally desorb

• Good for low concentration measurements

• Volatiles with unfavorable partition coefficients

22
 TriPlus 300 Headspace autosampler

High-throughput volatiles determinations

Reliable operations, unparalleled flexibility

Typical examples of headspace analyses

include:

•Volatile Organic Compounds (VOC) from

wastewater and contaminated land samples

•Residual solvents in packaging and

pharmaceuticals

•Blood alcohol and toxicology screening

•Aroma components from food and beverages

•Diagnostic gas analysis from oils

23
 Injection - SPME

• SPME is another type of sample introduction which

uses solvent free extraction

• It consists of coated fibers that are used to isolate

and concentrate analytes into a range of coating
materials.

• After extraction, the fibers are transferred to GC

injector for separation and quantification of the
target analytes.

• This is accomplished with the help of a syringe-like

handling device that protects your sample while
transferring from your sample to the instrument.

• This syringe-like device also protects your fiber

during storage

24
Injection - SPME

Head Space solid phase micro extraction: Extract the volatiles

from the gas phase to the fibers and concentrate

25
 Injection - SPME
• Different Phases available:
• Fiber coating available:
• Polydimethylsiloxane(PDMS)
• PDMS/Divinylbenzene (DVB)
• Polyacrylate
• Carboxen(CAR)/PDMS
• Carbowax(CW)/DVB
• CW/Templated Resin(TPR)
• StableFlex DVB/CAR/PDMS
26
– Non-bonded
• stable w/ some water-miscible
organic solvents
• slight swelling may occur
• NEVER use nonpolar organic
solvents
– Bonded
• stable with ALL organic solvents
• slight swelling possible w/ nonpolar
solvents
– Partially Crosslinked
• stable in most water-miscible
organic solvents
• May be stable in some nonpolar
solvents, but slight swelling possible
– Highly Crosslinked
• Equivalent to the partially
crosslinked, but some bonding to
core has occurred in the past
 Triplus-RSH - 3 in 1 auto sampler

• Integrated sampling system

• Liquid, Headspace & SPME

• Seamless operation

• Unmatched flexibility

• Ultimate productivity

27
 GC Detectors

• Thermal Conductivity Detector

• Flame Ionization Detector

• Electron Capture Detector

• Flame Photometric Detector

• Nitrogen Phosphorus Detector

• Mass Spectrometer Detector

28
Thermal Conductivity Detector

•This detector senses changes in

the thermal conductivity of the
column effluent and compares it
to a reference flow of carrier gas

• When column effluent pass

through the filament, the
temperature of filament
increases because of thermal
conductivity of compound is less
than that of carrier gas.

•The change in
filament
temperature affects resistance
29
 Thermal Conductivity Detector

Most applications are

 Petroleum Industry
 Chemical Industry
 Semi conductor Industry

Sensitivity
ppm to % range

30
 Flame Ionization Detector

• Combustion of organic compound in

hydrogen air flame led to form
ions which are collected & measured

• C=O do not generate signal while

halogen presence reduce the
sensitivity

• The current produced is proportional

to amount of the compound present.

31
 Flame Ionization detector

Most applications are

Petroleum Industry
Environmental
Pharmaceutical
Food and flavors

Sensitivity
ppm to % range

32
 Electron Capture Detector

• Measures the change in electrical

conductivity due to column effluent
compound, capturing electrons

• Very sensitive to electronegative

compounds

Working

Compounds from the column effluent

capture some of the electrons which
cause change in standing current.

33
 Electron Capture Detector

Most applications are Sensitivity

 Environment
ppb to ppm
 Chlorinated compounds (EPA 508.1)
 Trihalomethanes (EPA 501)
 Chlorinated acids (EPA 515.1)
 Acrylamide (EPA 8032)
 Chlorinated disinfected compound (EPA 551)
 Halogenated acid acids (EPA 552)
 Poly chlorophenols
 PCB, OCP, PBB, PDBE

34
 Electron Capture Detector - OCP

• Able to analyze 20 pesticides

• Fast separation and better detection limits

35
FPD

• Highly sensitive towards ‘S’

and ‘P’ containing compounds

• When compounds enters the

flame, light of different wavelength
are produced

• Wavelength are inside which will

only certain lights based on the
selection

• Organophosphorus pesticides

36
FPD
Most applications are
 Environment
 Organophosphorus
 Organic tin compounds
 Organosulfur compounds

 Food
 Organophosphorus
 Organosulfur compounds

Sensitivity
ppb to ppm
37
 Nitrogen Phosphorus Detector

In this thermal energy is used to ionize an analyte

which is produced from H2- cold plasma excitation.
The current flow between anode and cathode is
measured. It is very sensitive to N & P.

38
 Electron Capture Detector

Most applications are Sensitivity

 Environment & Food
ppb
 Analysis of nitrosamines
 Analysis of N & P pesticides

39
 Nitrogen Phosphorus Detector

Most applications are Sensitivity

 Environment
ppb to ppm
 Chlorinated compounds (EPA 508.1)
 Trihalomethanes (EPA 501)
 Chlorinated acids (EPA 515.1)
 Acrylamide (EPA 8032)
 Chlorinated disinfected compound (EPA 551)
 Halogenated acid acids (EPA 552)
 Poly chlorophenols
 PCB, OCP, PBB, PDBE

40
 Backflush Integration into Inlet Modules

• Instant connect split/splitless injector with backflush capabilities to shorten analysis

time and keep the analytical column and the detector cleaner
• Entire pneumatic circuit is integrated in the injector module
• No tubing nor fittings are used, minimizing risks of leaks and method complexity
No BKF Modified ASTM D3606
High boiling
Toluene hydrocarbons

Benzene

BKF
after 3 min

Toluene

Benzene

41
 Gas Supply to a Standard SSL

56 mL/min
Purge 5 mL/min • The same gas is used in the
He carrier path, septum purge
path, and split path.
Split
• Typically, only ~1/10…1/50 of
Helium
the total flow is used for the
50 mL/min
analytical column carrier flow.
SSL liner • Purge and split flows cannot
be reduced beyond a certain
limit without introducing
contamination into
column/detector (sample
matrix accumulated in liner
and lines, septa particles, air
Capillary diffusing from septa, seals off
column
1 mL/min gassing, …).

42
 HeSaver Inlet – How It Works (GC run)
5 mL/min
52 mL/min N2
N2
Purge • Inlet is supplied with
2 different gases:
Split Nitrogen and Helium
Nitrogen • Nitrogen purges the injector
50 mL/min while Helium only feeds the
(47 mL/min N2
SSL liner +3 mL/min He) analytical column
• During all “non-injection”
Anti-diffusion tubing. It
prevents N2 entering
periods, Helium is supplied
the column with a small with a flow that is just
4 mL/min countercurrent Helium
flow slightly higher than the
Helium
column flow (determined by
the column head pressure
Helium Capillary regulation)
column
Additional
• Helium consumption is
carrier gas line 1 mL/min drastically reduced
Helium

43
 A new Modular Approach to GC Instrumentation design

Pneumatic control Electronic boards Proportional solenoid valves

for gas control
Inlet/
detector
body Specific
electronic
control
boards
Pneumatic manifold

Inlet body heater and Insulation

Column connection (inside

the oven)

GC oven

• Instant connect modules incorporate:

• Injector (or detector) body
• Miniaturized IEC (Integrated Electronic gas Control)
• Gas manifolds and connections, restrictions and electronic valves are built-in
• Electronics for temperature and gas control, for signal amplifier and A/D conversion

44
 TRACE 1300 Series GC: Tailor Instrument Configuration

• Proprietary, patent-pending Thermo

Scientific “Instant Connect” modules

• Modules are user-installable in less

than two minutes
• Just remove three screws and put the
new module in place
• No special training, dedicated tools or
on-site service engineers required

• Every injector and detector is self-

sufficient
• Contains the Integrated Electronic
gas Control (IEC)
• Storing module calibration

45
 HeSaver Inlet – How It Works (Injection)
5 mL/min
56 mL/min
Purge N2 • During injection period,
N2 Helium is (almost) closed off
and nitrogen flows into the
Split column for sample
Nitrogen introduction.
50 mL/min N2
(or closed in • Helium is supplied at a bare
SSL liner
splitless) minimum flow of 0.1 mL/min
only to keep the connection
swept and avoid dead volume
negative effects during
0.1 mL/min injection.
He
• When GC is in stand-by (not
running samples) it can be left
Helium Capillary in this condition with almost
column
1.1 mL/min zero consumption of Helium
Additional
carrier gas line (1.0 N2 +
0.1 He)

46
 Quick recovery after module replacement

• iC-SSL inlet module replacement

Last run with old module First run after changing module

20
minutes

later

GC recovered normal operating conditions in less than 30’, including oven cooling
and column re-installation.

Modules store their calibration, so same performance were obtained. No need to

recalibrate method.

The same operation on any other GCs requires a Service Engineer and a full
working day, plus method re-calibration.

at least a 2000 $ savings (8 hrs x 250$/h=2000$)

47
Chromeleon CDS Simplifies Chromatography Process

Intelligent Functionality – it does everything you need

•AClhl romeleon 7 cmhraonmaagteosgrtahpehy

sestnatderstpsswwintithh
srebasemutwpltsleeesn

Workstation and Enterprise solution

48
 Mass Spectrometry Principle

• Find a way to “charge” an atom or molecule (ionization)

• Place charged atom or molecule in a magnetic field or subject it

to an electric field and measure its speed or radius of
curvature relative to its mass-to-charge ratio (mass analyzer)

• Detect ions using microchannel plate or electron multiplier tube

49
 Ionization Source

50
 Ionization and Fragmentation

51
 Quadrupole Mass Analyzer

52
 Detector (Electron Multiplier Tube)

• with off-axis dynode, discrete

dynode electron multiplier and
electrometer for broad analytical
dynamic range and excellent
sensitivity.
• The Linear-Log electrometer has
linear output up to 68 µA, which
provides electronic dynamic range
of greater than nine orders of
magnitude (> 109)

53
 Mass Spectrum

54
 ISQ Series – ISQ QD GC-MS

For budget-mindful laboratories seeking a reliable replacement

for stand-alone GCs, the ISQ QD from Thermo Scientific offers a
robust solution with Quality Design, MS Operational Simplicity,
and Proven Dependability.

Unlike other systems, ISQ

QD is a GC-MS that any
chromatographer can run,
afford, and rely upon.

55
 ISQ Series – ISQ LT GC-MS

For high-throughput, analytically-demanding laboratories,

requiring Utmost Sensitivity and Unstoppable Productivity,
the ISQ LT from Thermo Scientific offers the future-proof
investment into the Leading Technology, Simply Intelligent
GC-MS platform.

Unlike other systems,

ISQ LT does not need
to be vented to exchange
the source, while enjoying
industry-best sensitivity,
lowest detection limits,
and unlimited flexibility.

56
 ISQ Series – ISQ QD GC-MS Value Proposition

57
 ISQ Series GC-MS – Essential Product Features

• Two Models: ISQ QD and ISQ LT sharing:

• Performance
• Industry leading specifications
• Industry leading linear dynamic range – DynaMaxTM XR detection system
• Robustness
• ExtractaBriteTM Ion Source
• Inert, non-coated, high-temperature independently-heated ion source and ion
optics
• Reliability
• Dual filament design (with filament lens protection)
• Full Source RemovalTM on ISQ LT – unique amongst any other GC-MS system
• Versatility (ISQ LT only)
• Pulsed positive ion, negative ion, chemical ionization (PPINICI)
• Direct Probes capability
• Fast scanning plus low overhead = more data-to-disk for faster GC-MS

58
 A Tour of the ISQ Series Design

Follow an ion’s pathway through the ISQ Series system:

Inert Ion Volume and Repeller; Orthogonal Geometry Dual Filament;

ExtractaBrite Ion Source’s Lenses;
S-Shaped Flatapole Ion Guide;
Fast, Open-Architecture, Monolithic, Cleanable Quadrupole;
DynaMax XR Detection System;
Fast Data Processing Electronics Writing Data to File.

59
 A Tour of the ISQ Series Design
Ion Volume
Solid, highly inert material ensures
reliable performance in all ionization
modes, including EI and CI
…and Repeller
The repeller assists in maintaining
instrument performance over time. It
is composed of the same solid, inert
material as the other source
components.
60
Unique Dual Filament
Dual filament with improved low-
current regulation is protected by a
filament lens for improved lifetime.
Unique orthogonal design
provides same level of
performance – whether filament
#1 or filament #2 is selected.
 A Tour of the ISQ Series Design

ExtractaBrite Ion Source

Lenses 1, 2 and 3 plus the RF
lens, along with the repeller and
ion volume are contained in a
sleeve, all of which can be
removed from ISQ LT while the
system is under vacuum.

The ability to remove the entire

ion source from ISQ LT without
venting means you are never
down and always productive.

61
 A Tour of the ISQ Series Design

The S-Shaped Ion Guide

Reduces neutral noise
created by excited helium
atoms striking the detector.
Enables lower detection
limits (sensitivity) and better
selectivity.

Serves as an off-axis pre-

filter, removing the neutrals
right in the beginning – so
there is less interference
down the ion path.

62
 A Tour of the ISQ Series Design

Quadrupole Analyzer Assembly

Solid molybdenum, non-coated
quadrupole rods with 1.2 to 1100
a.m.u. mass range. Fast scanning
electronics, and fast acquisition
rates – up to 240 Hz of data written
to disk.
The analyzer rods are protected by
the S-shaped ion guide from
contamination. This design
requires no extensive heating of the
rods to keep them clean.

63
 A Tour of the ISQ Series Design

DynaMax XR Detection System

with off-axis dynode, discrete
dynode electron multiplier and
electrometer for broad analytical
dynamic range and excellent
sensitivity.
The Linear-Log electrometer has
linear output up to 68 µA, which
provides electronic dynamic range
of greater than nine orders of
magnitude (> 109).

64
 Designed for Sensitivity and Robustness

• ExtractaBrite Ion Source

• Repeller, ion volume, lenses and “RF lens”
• Contained in a keyed, easy-to-work-with
cartridge sleeve
• No tools required for assembly or
disassembly
• High efficiency ion focusing optics
• Repeller works with the RF Lens for a
‘push / pull’ approach to ion extraction

65
 Designed for Sensitivity and Robustness

• ExtractaBrite Ion Source

• Highly inert ion volume material
• High temperature ion optical path
• Open geometry flow pathway
• Independent heating of the ion source,
and ion optics/mass analyzer
• Select source temperature for method
performance; system will automatically run
ion optics/analyzer as hot as possible

66
 Designed for Sensitivity and Robustness

• ExtractaBrite Ion Source on ISQ LT

• Maintains performance at expected levels
for longer.
• No longer need to schedule “regular
maintenance” with instrument down.
• Simplifies sample preparation and clean-
up: can dedicate ion sources to particular
work and/or replace the ion source when it
becomes contaminated with a spare entire
source.

67
 Designed for Sensitivity and Robustness

• ExtractaBrite Ion Source: 180 batches and keeps going…

68
 ISQ Series – Intelligent, Sensitive, Robust

 Performance – A Legacy of Innovation

 DynaMAXTM XR detection system
 Fully Modular TRACE 1300 and 1310
 Robustness – Unstoppable Productivity
• ExtractaBriteTM Robust Source
 Reliability – Unstoppable Reliability
• Full Source RemovalTM
• Dual filament
 Productivity – The Best Business Decision
• High-speed data acquisition and write-to-disk
• Ease of Use – Power to the User
• Trace Finder 2.1 with Industry-Specific Workflow Solutions
of Trace Finder EFS and Clinical/Tox
 Flexibility – Ready for the Future Needs Today
• Fully upgradable on both GC and MS moieties
69
TSQ 8000 Evo GC-MS/MS

• For laboratories facing

•Changing regulatory
requirements
•Lower detection levels
•More compounds
•Less time
•Lower budgets
•Increased competition

Expect More
Productivity
70
Introducing EvoCell Technology

•EvoCell
• Rapid, innovative
collision cell technology

•Increased method capacity

• More compounds
• More SRM transitions
• More results

Expect More
Capacity

71
More Sensitivity; More Speed

•Enjoy higher sensitivity at

faster SRM speeds

•Up to 4 x more transitions

whilst maintaining method
sensitivity within the very
low concentration ranges

Expect More
Capacity
72
EvoCell - 666 compounds (5496 SRMs) in Rice

•Even under extreme

acquisition conditions
(>5000 SRMs)
•mean LODs 1.83 ppb
(of the 262 pesticides
quantified)

•Standard collision cell has

mean LOD 2.63 ppb when
running only 1300
transitions

Expect More
Capacity
73
Truly powerful methods use speed efficiently

Expect More
Capacity
74
Ultimate Sensitivity SRM - Pesticides

Expect More
Performance
•Difficult matrix –
green tea

•SRM as it should be
•High sensitivity
•High selectivity

•No need for “open”

or “wide "quadrupole
settings

75
Ultimate Sensitivity SRM - Dioxins and Furans

•Individual contribution of each

PCDD/F congener to fish sample
dioxin content (as TEQ pg/g)

•Comparison of TSQ 8000 EVO

GC-MS/MS
results with the GC- HRMS
values.

Expect More
Performance

76
ExtractaBrite Ion Source

•Patented RF lens
protects ion guide and Patented RF Lens
quads

•RF lens is removed

with source cartridge
without venting

•Repeller designed to
overcome ion burn once
it forms Repeller

Expect More
Robustness
77
Comprehensive source heating

Dual Independent
•TSQ 8000 Evo heats Heaters
all ion burn susceptible
areas
•Ion volume
•Lens stack
•Ion guide

•Drives routine grade

robustness in dirty matrix

Expect More
Robustness

78
Full ion source removal under vacuum

•Complete source cartridge

removal without venting the
system

•All maintenance can be

performed offline

•24/7 operation with a clean

spare source maintenance
routine

Expect More
Robustness

79
Screening Analysis with Orbitrap

80
 Exactive GC system: The Technology Inside

Orbitrap mass
analyzer Thermo
Scientific™
Incredible TRACE™ 1310 GC
HRAM System
performance
Unique modular
Highly regarded injector and
Q Exactive GC detector design
system
Rapid heat
platform
cycling Thermo

Scientific™

ExtractaBrite™

Ion Source

81
technology
 Orbitrap Mass Analyzer

k
  m/ z

• Ions injected into the Orbitrap are trapped

in
an electrostatic field
• Each ion oscillates axially with a
frequency that is proportional to its mass
• An image current of these oscillations is
measured using a split outer electrode
• This image is then converted to a mass
spectrum using Fourier transform
• The longer a signal (transient) is
measured,
the higher the resolution
82
 Exactive GC system Highlights

Resolving Power Mass Accuracy Sensitivity Dynamic Range

Up to
60,000 < 1ppm ppt >6 orders
at
m/z 200

• Maximum • Every scan • In full-scan • Excellent

selectivity coverage in
• All • High sample
• Fast enough concentrations selectivity profiling
for GC
• In complex • High spectral • “Triple quad
matrix fidelity grade”
quantitation in
• Across the mass
full-scan
range
• Everyday!

83
 Resolving Power: Sensitivity

• TIC signal
intensity vs.
scan number
• Increase the
resolving
15K 30K 60K power during
acquisition
• Negligible drop
in sensitivity

High selectivity analysis all of the time

84
 Resolving Power: Scan Rate @ 60K

XIC of dieldrin in baby food (m/z 262.85642) 100ppb

9 • Fast
8 10 acquisition
7 60,000 RP (m/z 200) • Important for
11 2.4 s peak
accurate
profiling of
6
12
17 scans narrow GC
peaks
5 13 • Full-scan with
4
resolving
14
3
power of 60
15
2 16 17 (FWHM
1
@ m/z 200)
generates 17
scans

Fast enough for GC!

*Acquired on the Q Exactive GC system – the Exactive GC system provides equivalent performance

85
 Resolving Power: Selectivity

Pyrimethanil in leek at 10 μg/Kg < 5 ppm ID criteria

False negative
Abundance
Relative

False negative
Abundance
Relative

Positive
Abundance

Detection
Relative

High Selectivity ∴ high sensitivity and confidence in identification

86
In depth example – O-Ring Extractables Study
Part 1: QEGC identification with NIST

87
 Pharmaceutical O-Rings extractables study

• 4 O-ring samples • Solvents

• A Red • Water
• 5M NaCl
• B Brown
• 50% Ethanol
• C White
• 100% Ethanol
• D Black • 1% PS-80
• Blank (control) • 0.5N NaOH
• 0.1M Phosphoric Acid
• 40 °C for 30 days

88
 GC-MS instrument conditions
TRACE 1310 GC Parameters

Injection Volume (mL): 1

Liner Single gooseneck
Inlet (°C): 280
Carrier Gas, (mL/min): He, 1.2
Oven Temperature Program:
Temperature 1 (oC): 40
Hold Time (min): 1
Temperature 2 (oC): 320
Rate (oC/min) 15
Hold Time (min): 10

Thermo Scientific™ Q Exactive™ GC Hybrid Q Exactive GC MS Parameters

Quadrupole-Orbitrap GC-MS/MS Transfer line (°C): 280
Thermo Scientific™ Trace™ 1310 GC Ionization type: EI
Ion source(°C): 230
Thermo Scientific™ TraceFinder™ Electron energy (eV): 70
Acquisition mode: Full scan
Mass range (Da): 50-650
Mass resolution (FWHM): 60k
Lockmass (m/z): 207.03235

89
 Scan speed and accurate mass error across a peak

Ethyl octanoate m/z 129.0910

90
 Compound Discovery and Identification

1. Peak detection
2. Spectral deconvolution
3. Library searching (e.g. NIST,
Wiley,
custom)
4. % TIC explained using elemental
composition and high resolution
filtering with accurate mass

91
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