Gamal A.

Hamid
To every one who has helped us
with support,
new books, hard/soft ware
And over the internet.
Special thanks to Thermo

Gamal A. Hamid
 Introduction

 Theory

 Hardware

 Analysis

 Applications

Gamal A. Hamid
 Declaration

Experience has shown that maximum value can be derived from a scientific instrument if
there is

one person who has a major responsibility for the instrument.

Thermo recommend that you designate a key operator to manage the operation and
maintenance of the TRACE system. also recommend that the key operator
receive training .

Gamal A. Hamid
 Gas Chromatography

 A separation technique in which the mobile

phase is a gas.

 Gas chromatography is always carried out in

a column.

 Separating mixtures of gases or volatile

materials based primarily on their physical

properties.

 It gives both: Quantitative, Qualitative

Gamal A. Hamid
 Theory

Chromatographic separation involves the use of:

Stati. Phase.

Mobile phase.

Carrier Gas.

Components of mixture carried in the mobile phase are differentially attracted to the
stationary phase and thus Move through the stationary phase at different rates.

Gamal A. Hamid
 Generally

 Boiling points is The number one factor to consider in

separation of compounds on the GCs.

 Differences in polarity of the compounds is only

important if you are separating a mixture of

compounds which have widely different polarities.

 Column temperature, the polarity of the column, flow

rate, and length of a column are constant .

Gamal A. Hamid
 Hardware

 Manual Injection.

 Automatic Injections.

 Injectors

 Columns

 Oven

 Detectors

 Carrier Gas

Gamal A. Hamid
 Sample Preinjection

Liquid introduction by syringe

 Most commonly used technique

 Different syringe types manual and automatic

Other techniques and devices

 Sampling valve (gas or liquids)

 Head-space (liquids or solids)

 Purge and trap (water)

 Thermal desorption (solids)

 SPME (vapours, liquids or solids)

 Pyrolizer (solids)

Gamal A. Hamid
 Manual Injection

Micro Syringes

Are used to introduce a known volume of

a liquid or gas samples.

Adaptor

Can be used to help control the volume

injected.

Gamal A. Hamid
Syringe injection

 Samples should be injected as a plug.

 Rapid and consistent injection is necessary

in order to obtain Acceptable precision

Injection Volume

 Liquids 0.1-10 µl is typical

 Gases 0.5- 5 ml is typical

Gamal A. Hamid
Hot Needle injection

1. Draw sample into syringe barrel.

2. Draw 2-3 ul air into barrel.

3. Inset needle into injection port and allow to heat for

a few seconds.

4. Rapidly inject sample and withdraw the needle.

5. This insure that all sample is injected and the hot needle

assists in solvent volatilization.

Gamal A. Hamid
Normal injection

1. Rinse the syringe with your sample at least twice .

2. Draw up the suggested amount of sample into the syringe.

3. Pull up about 1-2 ul of air. This will give a signal showing

the beginning of the elution.

4. Insert the needle through the injection port and septum

in one movement.

5. Quickly push the plunger.

Gamal A. Hamid
 Automatic Injection
Auto Injector AI 3000
Sample loading
Sample capacity: 8 Vials
Max. vial capacity: 2 ml
Injections/vial: 0-99
Syringes
Standard sampling: 10µl
Micro volume sampling: 5µl
Injection parameters
Max volume: 5µl
Min. Volume : 0.1µl
Increments: 0.1µl steps
Viscosity Delay: Yes/No

Gamal A. Hamid
 Automatic Injection
Auto Sampler AS 3000
Sample loading
Sample capacity: 105 Vials
Max. vial capacity: 2 ml
Injections/vial: 0-99
Syringes
Standard sampling: 10µl
Micro volume sampling: 5µl
Injection parameters
Max volume: 5µl
Min. Volume : 0.1µl
Increments: 0.1µl steps
Viscosity Delay: Yes/No

Gamal A. Hamid
 Auto Sampler TriPlus

Large sample vial capacity Max 2 trays installed

Simultaneously 1, 2 and 2.5 ml vials (up to 300 vials)
Syringe size: 5, 10, 100 and 250 µl.
Self recognized syringes and trays
Washing station: 4 x 10ml or 2 x 100ml; multiple
Solvent rinsing supported

 Rapid Mode: Allows to perform cleaning operations during GC

run or cooling time.
 Suitable for Ultra Fast GC requirements, eliminating dead
times between successive runs.

Gamal A. Hamid
 Head Space

Head-space gas analysis

 Volatiles reach equilibrium at STP

 An aliquot of headspace is total in liquid and gas phase

 Conc. in gas proportional Conc. In liquid phase With

headspace matrix left behind

 Clean and gentle chromatography

Representative of sample

Gamal A. Hamid
 Head-Space Applications

1. Determination of residual volatile solvents in pharmaceutical.

2. Blood alcohol analysis.

3. Determination of volatile hydrocarbons in waste water.

4. Determination of di-acetyl and dichetones in beers.

5. Monomers in polymers determination.

6. Determination of out-gassing solvents from packages.

7. Flavor profiles in drinking beverages or foods (cheese).

Gamal A. Hamid
 Cold and Trap

 Allows the analysis of trace of compounds in large volumes of

gaseous samples.
 The column can be cooled down to -150 °C by the action of
the liquid nitrogen,
 So to trap (i.e. to reconcentrate) the volatile compounds
contained in the sample.
 When the trapping is completed, the tube is heated with a fast
temperature programming rate (°C/s), reaching temperatures
up to 400 °C, so to transfer the trapped compounds into the
analytical column.

Gamal A. Hamid
 GC Basic Components

Injector

Carrier
Column
Gas

Detector Oven

Gamal A. Hamid
 1. Injector

The injection port Is a hollow, heated, glass-lined cylinder

 The injector is heated so that all components in the sample will be

vaporized.

 If the temperature is too low, separation is poor and broad spectral

peaks should result or no peak develops at all.

 If the injection temperature is too high, the specimen may

decompose or change its structure.

 The temperature of the sample port is usually about 50°C higher

than the boiling point of the least volatile component of the sample.

Gamal A. Hamid
 Injection Techniques

Vaporizing.
The liquid sample is evaporated prior to be transferred to the
separation column.

 Split Spliless: SSL (permanently hot)

 Programmed Temperature Vaporizer: PTV

 Direct: PKD, PPKD (permanently hot, low resolution columns)

Nonvaporizing.
The liquid sample evaporates into the separation column (or a
precolumn)

 Cold On Column: OC (permanently cool)

Gamal A. Hamid
 Septa

 Ensure optimal performance of your GC

instrument with bleed and temperature.

 Made of low-bleed silicone, have

excellent mechanical properties, are ideal
for demanding GC and GC-MS
applications, and may be used reliably up
to 400 °C.

 Septum must be replaced at least after

200 injections.

Gamal A. Hamid
Liner Types

Gamal A. Hamid
Liners Applications

Gamal A. Hamid
Quick Liner Selections

Gamal A. Hamid
 Injector Types

1. Split/ Splitless Injector

2. On-Column Injector

3. High Oven Temperature On-Column Injector

4. Large Volume On-Column Injector

5. Packed Column Injector

6. Purged Packed Injector

7. Programmable Temperature Vaporizing Injector

Gamal A. Hamid
 1. Split/Splitless Injector (vaporising injector)

Split mode

 The split vent is open, part of the sample go

into the column.

 When analyzing high concentration or neat

samples.

 Yields the sharpest peaks if the split gas is

properly mixed.

 Standard for capillary columns.

Gamal A. Hamid
Splitless mode

 The split vent is closed, most of the sample go

into the column.

 When analyzing low concentration or diluted

samples.

 Splitless times of ~ 1 minute are typical.

 Standard for capillary columns.

Gamal A. Hamid
 2. On-Column Injector

Non- vaporising injectors

 The sample is transferred as a liquid directly inside the

column under the oven temperature control.

 The sample evaporation takes place inside the column.

 Sample doesn’t come in contact with any “column-

external” device

 No vaporization step at a temperature above that of the

column

Gamal A. Hamid
Primary cooling
 Permanently active fan

 Keep the injector head at room temperature independently from oven temperature

Secondary cooling
 Temporary stream of compressed air

 Avoid evaporation from the needle even at oven T close or slightly higher than BP

 Reduces the length of the flooded zones

 Avoid liquid backflow reducing the vapor pressure at the plug front

 More eefficient and rapid cooling of the injector base after a temperature ramp
 Cooling Time, The amount of time the secondary cooling stays on after the start
the injection.

Gamal A. Hamid
 3. High Oven Temperature On-Column Injector

 The OCI is the same as the regular cold on column except

that a cooling jacket is installed in the GC oven around the
head of the column.
 This allows a cold on column injection with a high oven temp.

Temperature (°C).
 The temp. checkbox checked for this option to be used.

 This specifies cooling jacket temp. during injection.

 Duration (min) the duration of the jacket cooling from the

start of the run.

Gamal A. Hamid
 4. Large Volume on column injector

 LV-SL injection overcomes the limitation of the maximum sample

volume to 1-2 µL of classical splitless injection by exploiting the
Concurrent Solvent Recondensation technique (CSR).
 CSR technique allows injection of large volumes by combining a
restricted evaporation rate with an accelerated sample transfer
granted by the pressure surge generated by solvent evaporation
and by the quick solvent recondensation in a precolumn.
LV-SL has the following advantages:
 It is simpler because it allows injections of up to 50 µL in a
conventional split/splitless injector without any special tuning of
operating parameters;
 It is robust versus sample by-products or contaminants and
extremely suitable for food matrices.

Gamal A. Hamid
 5. Packed Column Injector

1. The PKD is used for injections with the sample vaporizing

directly in the column.

2. The PKD standard injector accepts metal or glass packed

columns.

3. The injector temperature may range from ambient to 400

°C. Injector temperature is regulated by a temperature
controller in the GC CPU board and monitored by a
platinum wire sensor.

Gamal A. Hamid
 6. Purged Packed Injector

The Purged Packed (PPKD) column injector is a packed column

injector with a septum purge.

The PPKD standard injector accepts wide-bore capillary columns.

The sample vaporizes in a liner and enters the wide-bore

capillary column.

The injector temperature is controllable from 50 °C to 400 °C.

You should use high temperature septa with a longer life

expectancy.

Gamal A. Hamid
 7. Programmable Temperature Vaporizing Injector

1. Can vary the temp. during injection in both split

and Splitless.
2. Can eliminate many of the unwanted effects ,
such as distillation of the sample within the
needle and large vapor clouds inside injector
chamber.
3. In Constant Temperature (CT) mode, the PTV
functions like a split/splitless injector.
4. Sample volumes are lower than when using S/SL
injector because of the smaller PTV liner volume .
5. Can analyze relatively dirty samples that can not
be analyzed using a traditional on-column.

Gamal A. Hamid
 Good injector

1. Capable to quantitative accept a broad volatility range.

2. Low discrimination.

3. To handle dirty and clean matrices.

4. With dirty matrices reduces sample clean-up and preserves the column.

5. With clean matrices boosts sensitivity with LVI techniques .

6. Extremely inert.

7. Able to handle polar/active compounds.

8. Provide optimum band shape.

Gamal A. Hamid
 GC Basic Components

Injector

Carrier
Column
Gas

Detector Oven

Gamal A. Hamid
 2. Column

The column

 Is where the chromatographic separation of the sample occurs.

 Several types of columns are available for different

chromatographic applications:

 The heart of the system.

 It is coated with a stationary phase which greatly influences the

separation of the compounds.

Gamal A. Hamid
Stationary phase
 Solid resin packed in a column , or

 Liquid supported by course paper or

 Inactive solid over which a mixture passes.

Each component of the mixture differs in the way

it adheres to this phase and therefore travels along

it at a unique rate.

Gamal A. Hamid
 The Adsorbents

There are two types of packing employed in GC, the adsorbents and the supports, on
which the stationary phase is coated.
There are both inorganic and organic types of adsorbents.

• Alumina, in an activated form, is used to separate the permanent gases and

hydrocarbons up to about pentane.
• Silica gel It is used for the separation of the lower molecular weight gases and some of
the smaller hydrocarbons sulfur gases, hydrogen sulfide, sulfur dioxide and carbon
disulfide.
• Synthetic zeolites used for the separation of hydrogen, oxygen, nitrogen, methane
and carbon monoxide and also rare gasses.

Gamal A. Hamid
 Types of Stationary Phase

POLYSILOXANES
 The most common stationary phases.

 They are available in the greatest variety and are the most stable, robust and
versatile.

 The most basic Poly Siloxane is the 100% methyl substituted

POLYETHYLENE GLYCOLS
 They are less stable, less robust and have lower temperature limits than most
Poly Siloxane.

 must be liquids under GC temperature conditions.

Gamal A. Hamid
 Inactive Solid Supports

 There have been a number of materials used as supports for

packed GC columns including,

 Celite (a proprietary form of a diatomaceous earth), fire-

brick (calcined Celite), fire-brick coated with metallic silver or

gold, glass beads, Teflon chips and polymer beads.

 Polystyrene beads

Gamal A. Hamid
 Column Types

Conventional
1/8-1/4 OD
6-8 feet in length
Stainless steel or glass tube
Preparative
>1/4 OD
> 10 feet in length
Capillary
0.1- 0.5 ID
10 – 100 meters in length

Gamal A. Hamid
 Factors Affecting Column Separations

Volatility of compound: Low boiling (volatile) components will

travel faster through the column than will high boiling components

Polarity of compounds: Polar compounds will move more slowly,

especially if the column is polar.

Column temperature: Raising the column temperature speeds up

All the compounds in a mixture.
Columns have lower and upper temperature limits.

Gamal A. Hamid
Column packing polarity: Usually, all compounds will move slower on
polar columns, but polar compounds will show a larger effect.

Flow rate of the gas through the column: Speeding up the carrier gas flow increases
the speed with which all compounds move through the column.

Length of the column: The longer the column, the longer it will take all compounds
to elute. Longer columns are employed to obtain better separation.

Gamal A. Hamid
 Loss of Separation or Resolution

 Contaminated column.

 Damaged stationary phase.

 Different column temperature, carrier flow rate

or column.

 Large changes in the sample concentration.

Improper injector operation.

Gamal A. Hamid
 Column Damage

 Column breakage

 Column bleed

 Thermal damage

 Oxygen damage

 Chemical damage

Gamal A. Hamid
 GC Basic Components

Injector

Carrier
Column
Gas

Detector Oven

Gamal A. Hamid
 3. Oven

 The use of a temperature programmed for the column oven

influences the separation process significantly and is used for

optimization of time and peak separation.

 The oven must not be opened when the oven temperature is

above room temperature.

 Never turn off the nitrogen flow unless the column and oven

are at room temperature.

Gamal A. Hamid
 The Oven Capabilities

 Temperature range 5 °C above ambient to 350 °C

 Temperature programming - up to six ramps

 Maximum run time - 999.99 minutes

 Temperature ramp rates - 0 to 120°C/min

 The oven accommodates one inlet, one detector,

and one column.

Gamal A. Hamid
 Multiple-ramp temperature programs

 A multiple-ramp temperature program changes the oven temperature from an initial value

to a final temperature, but with various rates, times , and temperatures in between.

 Multiple ramps can be programmed for temperature decreases as well as increases.

Gamal A. Hamid
 GC Basic Components

Injector

Carrier
Column
Gas

Detector Oven

Gamal A. Hamid
 4. Detector

The part of a gas chromatograph which signals the

change in composition of the mixture passing through it.

Gamal A. Hamid
 Detector types

1. Electron Capture Detector.

2. Flame ionization Detector.

3. Nitrogen Phosphors Detector.

4. Thermal Conductivity Detector.

5. Flame Photometric Detector.

6. Photo ionization Detector.

7. Electrolytic Conductivity Detector.

8. Mass Spectrometric Detector.

Gamal A. Hamid
 1. Electron Capture Detector
(ECD)
 Mechanism:

Electrons are supplied from a 63Ni foil lining the detector cell. A current is generated in
the cell. Electronegative compounds capture electrons resulting in a reduction in the
current. The amount of current loss is indirectly measured and a signal is generated.

Selectivity: Halogens, nitrates, conjugated carbonyls

Sensitivity: 0.1-10 pg (halogenated compounds);
1-100 pg (nitrates); 0.1-1 ng (carbonyls)
Linear range: 1000-10000
Gases: Nitrogen or argon/methane
Temperature: 300-400°C

Gamal A. Hamid
 2. Flame ionization Detector
(FID)
 Mechanism:

Compounds are burned in a hydrogen-air flame.

Carbon containing compounds produce ions that
are attracted to the collector.
The No. of ions hitting the collector is measured
and a signal is generated.

Selectivity: Compounds with C-H bonds.

Sensitivity: 0.1-10 ng
Linear range: 105-107
Gases: Combustion hydrogen and air; Makeup He or N2
Temperature: 250-300°C,and 400-450°C for high temp.

Gamal A. Hamid
 3. Nitrogen Phosphors Detector
(NPD)
 Mechanism:

Compounds are burned in a plasma surrounding

a rubidium bead supplied with hydrogen and air.
Nitrogen and phosphorous containing compounds
produce ions that are attracted to the collector.
The number of ions hitting the collector is measured
and a signal is generated.

Selectivity: Nitrogen and phosphorous

Sensitivity: 1-10 pg
Linear range: 104-10-6
Gases: Combustion - hydrogen and air; Makeup - Helium
Temperature: 250-300°C Gamal A. Hamid
 4.Thermal Conductivity Detector
 Mechanism:
(TCD)

A detector cell contains a heated filament with an applied current. As carrier

gas containing solutes passes through the cell, a change in the filament
current occurs.
The current change is compared against the current
in a reference cell.
The difference is measured and a signal is generated.

Selectivity: All compounds except for the carrier gas

Sensitivity: 5-20 ng
Linear range: 105-106
Gases: Makeup - same as the carrier gas
Temperature: 150-250°C
Gamal A. Hamid
 5. Flame Photometric Detector
(FPD)
 Mechanism:

Compounds are burned in a hydrogen-air flame. Sulfur and

phosphorous containing compounds produce light emitting species
(sulfur at 394 nm and phosphorous at 526 nm). A monochromatic filter
allows only one of the wavelengths to pass. A photomultiplier tube is
used to measure the amount of light and a signal is generated.
A different filter is required for each detection mode.

Selectivity: Sulfur or phosphorous containing compounds.

Only one at a time.
Sensitivity: 10-100 pg (sulfur); 1-10 pg (phosphorous)
Linear range: Non-linear (sulfur); 103-105 (phosphorous)
Gases: Combustion - hydrogen and air; Makeup - nitrogen
Temperature: 250-300°C

Gamal A. Hamid
 6. Photo ionization Detector
(PID)
 Mechanism:

Compounds eluting into a cell are bombarded with high energy photons emitted
from a lamp. Compounds with ionization potentials below the photon energy are
ionized. The resulting ions are attracted to an electrode, measured, and a signal is
generated.

Selectivity: Depends on lamp energy. Usually used for

aromatics and olefins (10 eV lamp).

Sensitivity: 25-50 pg (aromatics); 50-200 pg (olefins)

Linear range: 105-106
Gases: Makeup - same as the carrier gas
Temperature: 200°C

Gamal A. Hamid
 7. Electrolytic Conductivity Detector
(ELCD)
 Mechanism:

Compounds are mixed with a reaction gas and passed through a high temperature
reaction tube. Specific reaction products are created which mix with a solvent and
pass through an electrolytic conductivity cell. The change in the electrolytic
conductivity of the solvent is measured and a signal is generated. Reaction tube
temperature and solvent determine which types of compounds are detected.

Selectivity: Halogens, sulfur or nitrogen containing compounds.

Only one at a time.
Sensitivity: 5-10 pg (halogens); 10-20 pg (S); 10-20 pg (N)
Linear range: 105-106 (halogens); 104-105 (N); 103.5-104(S)
Gases: Hydrogen (halogens and nitrogen); air (sulfur)
Temperature: 800-1000°C (halogens), 850-925°C (N), 750-825°C (S)

Gamal A. Hamid
 8. Mass Detector

 Mechanism:
Compounds are bombarded with electrons (EI) or gas molecules (CI). then fragmented into
characteristic charged ions or fragments. The resulting ions are focused and accelerated into
a mass filter. mass filter selectively allows all ions of a specific mass to pass through to the
electron multiplier. All of the ions of the specific mass are detected. The mass filter then
allows the next mass to pass through while excluding all others. The mass filter scans
stepwise through the designated range of masses several times per second. The total
number of ions are counted for each scan. The abundance or number of ions per scan is
plotted versus time to obtain the chromatogram (called the TIC). A mass spectrum is
obtained for each scan which plots the various ion masses versus their abundance or
number.

Selectivity: compound gives fragments within mass range.

Sensitivity: 1-10 ng (full scan); 1-10 pg (SIM)
Linear range: 105-106
Gases: None
Temperature: 250-300°C (transfer line), 150-250°C (source)
Gamal A. Hamid
 Good Detector

Properties of a good detector.

1. High sensitivity.
2. Rapidly respond to concentration changes.
3. Large linear range.
4. Stable with respect to noise and drift.
5. Low sensitivity to variation in flow,
6. Pressure and temperature.
7. Possible selectivity.
8. Produces an easily handled signal.
9. A temperature range from room temperature to at least 400 C.

Gamal A. Hamid
 GC Basic Components

Injector

Carrier
Column
Gas

Detector Oven

Gamal A. Hamid
 5. Carrier gas

An inert gas, which is used to sweep a mixture to

be separated through a gas chromatograph ,

(helium, hydrogen, or nitrogen).

 Push the sample through the gas

chromatograph column.

 Clean out the gas chromatograph column after

sample analysis.

Gamal A. Hamid
 Carrier Gas Control

 The Flow mode has four options for the  The electronic control of the carrier gas
carrier gas control: allows also the following operations.

o Constant flow  Column Evaluation

o Constant pressure  Gas Saver Function

o Programmed flow  Leak Check

o Programmed pressure

o Split flow control (in ml/min)

o Septum purge flow control (in mL/min)

Gamal A. Hamid
 Gas Purity

 All pure gases are classified by grade, so you can be certain

of purity levels.

 The first digit of the classification indicates the number of

nines purity (for example, 5.0 = 99.999% purity).

 The second digit is the number following the last nine (for

example 4.7 helium has a guaranteed minimum purity of

99.997% and a corresponding maximum impurity level of

0.003% or 30ppm).

Gamal A. Hamid
The carrier gas
Ultra-pure and research-grade gases of up to 99.9999% (Grade 6.0) purity.

The carrier gas system often contains a molecular sieve to remove water or
other impurities.

Linear Velocity (u)

Is the speed at which the carrier gas or mobile phase travels through the
column.

The linear velocity is generally expressed in cm/s.

The linear velocity is independent of the column diameter while the flow rate
is dependent on the column diameter.

Gamal A. Hamid
 Required Gases Purities

Helium For carrier gas: 99.995%1 high purity, with less than 1.0 ppm each of
 water, oxygen, and total hydrocarbons after purification.
 Use water, oxygen, and hydrocarbon traps.
Hydrogen For carrier or detector fuel gas: 99.995%1 high purity, with <
 1.0 ppm of total hydrocarbons after purification.
 Use water, oxygen and hydrocarbon traps.
Air For detector fuel gas: 99.995%1 high purity.
 Air compressors are not acceptable because they do not
 meet pressure, water, and hydrocarbon requirements.
Nitrogen For carrier or make-up gas: 99.995% high purity, with less than 1.0
 ppm of total hydrocarbons after purification.
Argon 5% Methane For ECD make-up gas: 99.995%1 high purity.

Gamal A. Hamid
 Leak Detection
CAUTION

 Do not use liquid soap leak detectors to check for leaks. Liquid

soap leak detectors may contaminate you system.

 A mixture of 50% H2O/50% methanol or isopropyl

 Alcohol may be used as a liquid leak detector.

 WARNING! Never use liquid leak detectors on or around

electronic pneumatic circuits

Gamal A. Hamid
 Generators

Nitrogen Generator
The nitrogen generator can also operate directly from the laboratory compressed air supply.
General contaminants are first removed with appropriate filters and adsorbents and the
purified air passes over layers of polymeric hollow fiber membranes through which nitrogen
selectively permeates.

Hydrogen Generator
In the Packard Hydrogen Generator, hydrogen is generated electrolytically from pure
deionized water.

The electrolysis unit uses a solid polymer electrolyte and thus does not need to be supplied
with electrolytes, only the deionized water.

Gamal A. Hamid
 Hydrogen

 Hydrogen is a colorless, odorless, highly flammable gas with the

molecular formula H2 and an atomic weight of 1.00794, making
it the lightest element.

 Hydrogen is potentially explosive and must be used with

extreme care.

 Hydrogen is a dangerous gas that, when mixed with air, could

create an explosive mixture.

 Hydrogen is a dangerous gas, particularly in an enclosed area

when it reaches a concentration corresponding to its lower
explosion level (4% in volume).

Gamal A. Hamid
 Chromatogram

1. The data recorder plots the signal from the detector over time.

2. The retention time, is qualitatively indicative of the type of compound.

3. The area under the peaks or the height of the peak is indicative of the amount of

each component.

Gamal A. Hamid
 Retention Time (RT)

 RT, is the time it takes for a compound to travel

from the injection port to the detector.

 Thousands of chemicals may have the same

retention time, peak shape, and detector

response.

 For example, under certain conditions, DDT has the

same retention time as PCBs (polychlorinated

biphenyls).

Gamal A. Hamid
 Retention Time Shifts

1. Different column temperature.

2. Different carrier gas flow rate or linear velocity.

3. Leak in the injector, especially the septum.

4. Contaminated column.

5. Change in the sample solvent.

Gamal A. Hamid
 Simple Checks

1. Gases - pressures, carrier gas average linear velocity,

2. and flow rates (detector, split vent, septum purge).

3. Temperatures - column, injector, detector .

4. System parameters - purge activation times, detector attenuation, mass ranges, etc.

5. Gas lines and traps - cleanliness, leaks, expiration.

6. Injector consumables - septa, liners, O-rings and ferrules.

7. Sample integrity - concentration, degradation, solvent, storage.

8. Syringes - handling technique, leaks, needle sharpness, cleanliness.

9. Data system - settings and connections.

Gamal A. Hamid
 Troubleshooting categories
1. Baseline disturbances.

2. Irregular peak shapes or sizes.

3. Retention time shifts.

4. Loss of separation or resolution.

5. Quantitation difficulties.

6. Rapid column deteriorations.

7. Ghost peaks .

8. Broad solvent fronts.

Gamal A. Hamid
 Troubleshooting Tools
1. An electronic leak detector

2. A flow meter

3. An accurate thermometer

4. A reliable analytical column

5. New syringes

6. Spare septa and high temperature septa

7. Spare ferrules

8. Detector cleaning solutions

9. Spare recorder and electrometer cables

10. Instrument manuals

Gamal A. Hamid
Major Current GC Markets

Gamal A. Hamid
 Environmental

What is the environmental market?

1. Testing or commercial laboratories
2. Industrial laboratories
3. Government laboratories
4. Research institutes

Requirements of the applications

1. Drinking water
2. High sensitivity Waste
3. Sensitivity and selectivity Air
4. Sample introduction

Gamal A. Hamid
 Clean water analysis

Pollutants in water

 Halocarbons

 Acid priority pollutants: phenols,

chlorophenols, nitrophenols

 Pesticides and PCBs

 Base neutral priority pollutants

 Polynuclear aromatic hydrocarbons

Gamal A. Hamid
 Petrochemical and Gas

Large replacement business

 Refinery
 Oil Industry
 Gas suppliers

Requirements of the applications

 Multi-valves applications
 Fastest possible cycle time
 QC of gases: sensitivity
 Customized software
 Easy to use data handling and reporting

Gamal A. Hamid
 Food & Beverages

 Very extended market field

 No really regulated methods

 Ideal market to exploit the TRACE GC modularity

 Requirements of the applications

o QC of producers: Sensitivity and rapidity

o Multi detection capability

o Correct sample inlet (PTV-OC)

o Easy to use data handling and reporting

Gamal A. Hamid
 Pharmaceutical

 Highly regulated market (pharmacopeia)

 Requires Validation package

 Requirements of the applications

o Limited instrument requirements SSL/NPD/FID

o Highly Automated market

o High sensitivity detectors

o A unified chromatography software

Gamal A. Hamid
gamal_a_hamid@hotmail.com
Gamal A. Hamid