GC School

－ Basic Course －
 What is GC?
Liquid Components
Gas Components
Target ： Mixed
Components
（ Gas or Liquid ）

(Sample Injection Port)

GC By applying heat, each
component is vaporized.

Components are introduced into a column by carrier gas

Each component is separated with the column

(Detector)
The quantity of each component which came out from the
column is changed into electric signal.

What is component and

Data Processor how much of it is contained
 The Principle of Chromatography
Sample
Injection
A＋B
Injection
Port

A＋B

Colum
n
B

B
A

Detector A B

Peak B
Peak A

Time
 What does an analysis result show?

・ Time after injecting a sample until a component

reaches detector (Retention Time)

→ What? : Qualitative ？
？
Analysis ？ ？
？
・ Peak area or height of component

→ How much? : Quantitative

Analysis
 Qualitative Analysis
When analysis is carried out on the same analytical conditions, the
same component is eluted at the surely same time.
（ Retention time is equal ）

Unknown
Sample

Standard sample Component A Component B

(mixed solution of
components A and B)

Sample Injection

Since retention time is the only qualitative information,

standard sample is required for qualitative analysis in GC
(fundamentally).
 Quantitative Analysis
The peak area (height) of component is proportional to the quantity
of the component which reached the detector .

Conc.
Component A (ppm)
Unknown Sample
1uL 100

Peak Area ： 700 70

Standard Sample
1uL
(Component A 100ppm) Component A

700 1000
Peak Area
Peak Area ： 1000

Standard sample is required also

for a quantitative analysis.
Structure of GC
 Structure of GC

Flow Injection Port Detector

Controller

Data Processor
Electric
Signal
Column Oven
Gas Cylinder

Column
 Carrier Gas and Detector Gas

Carrier Gas
He and N2 are usually used.
(In the case of a capillary column, helium is desirable)
The gas of 99.999% or more of purity is used.

Detector Gas
TCD ... No need
FID ... H2, Air
ECD ... N2
Temperature of Injection Port and Detector
Temperature of injection port
The temperature of injection port is set that the components in a sample
can be vaporized enough.
(It does not need to be remarkably high temperature)
Although it is usually set as the same temperature as detector in many
cases.

Temperature of detector
The temperature of detector is always set higher than the temperature
of column.
(usually 20-30 ℃ higher than the programmed final temperature of
column.)
GC COLUMN
 GC Columns
Packed Column Capillary Column
Fused Silica
or Stainless Steel
Stainless Steel
or Glass

Stationary
Phase
Stationary
Phase

•I.D. 2-4mm
PLOT(Porous Polymer)
•Length 0.5-5m (most case is 2m
length) •I.D. 0.1 ， 0.25 ， 0.32 ， 0.53mm
•Length 5-100m （ most case is 30m length
）
DETECTOR
 Detectors
Detectable Minimum Detectable
Detector Compounds Quantities*
General detectors
Thermal Conductivity All compounds except 10ppm
Detector （TCD） carrier gas (10ng)
Flame Ionization 0.1ppm
Organic Compounds
Detector（FID） (0.1ng)
High sensitive and selective detectors
Electron Capture Organic halogen 0.1ppb
Detector （ECD） compounds (0.1pg)
Organic metal compounds
 TCD (Thermal Conductivity Detector)
• Detection of all compounds except carrier gas is possible
• Helium is mainly used as carrier gas

The main examples of application

Gas analysis
Analysis of compounds undetectable by FID, such as water,
formaldehyde, and formic acid
 FID (Flame Ionization Detector)
• Respond to almost of organic compounds ( containing carbon)
<exception>
There is no response to C of carbonyl group or carboxyl group (C=O).
(CO, CO2, HCHO, HCOOH, etc.)

• The main examples of application

Analysis of organic compounds
 FID (Flame Ionization Detector)

to Data processor
Organic compounds burn in hydrogen flame
and several ppm of those become the
Collector following ions.

Hydrogen
flame
High
voltage

Air
Quartz
nozzle Hydrogen （ +
Makeup gas ）

Column
outlet
Sample Injection Method
 Sampling Method of Liquid Sample

Sample does not

uL Sucks air into uL uL vaporize until a
3 the needle 3 3 plunger is pushed,
2 portion after 2 2 since there is no
measuring the sample in the needle
1 volume of 1 1
portion.
0 liquid sample. 0 0
Sample
solution
Injection Port
Air
(High temperature)
 Injection

Just after injection

uL uL
3 3
2 2
1 1
0 0 Since the needle portion is
Injection Port heated, the components with low
(High temperature) boiling point vaporize too much
and transfer into a column.
Headspace Mode
Troubleshooting
 Leak Problem
Problem Possible Causes
1. Gas cylinder, regulators, inlet tubing , clogged inlet filters.
2. Flow settings in Method file.
3. Bad septum.

Leak 4. Tight Nuts ,tubes, & column edges.

5. Bad O-ring.
6. Broken Glass insert \ Liner.

7. Bad column ferrules.

 Contamination
Problem Possible Causes
1. Gas puirty and expired inlet filter.
2. dirty Syringe.

Contamination in 2. Bad septum.

Injection Port 3. Dirty glass insert / Liner & silica wool inside, Dirty O-ring.
4. Dirty injection port inside path.
5. Dirty column edge.
 Contamination

Problem Possible Causes

1. Dirty column edge.

Contamination in Detector , 2. Dirty FID jet (Nozzle).

Baseline Problems, Flame can't 2. Dirty collector.
ignite 3. Make up gas puirty.
4. Column bleeding.
The Relation between Column Temperature
and Separation
C15 170 degree C Isothermal
Analysis
The separation of C12-C15 is
C12 C18 comparatively good.
Elution of components with high boiling
point is late and peak width spreads.

C15 230 degree C Isothermal

C18
C12 Analysis
Elution of components with high
C23 boiling point is comparatively early.
The separation of C12-C15 is poor.

100 degree C -10 degree C /min-280

C15 degree C
C18 Analysis with Programmed Temperature
n-Paraffin is eluted mostly at equal intervals.
Separation of components with low boiling point
C12 C23
is good, and also components with high boiling
point is eluted early.
Injection Port