Instrumentation for Gas Chromatography

3- Columns
1- Mobile Phase (Carrier Gas) 2- Sample Injection System
The heart of the GC system
Purpose: transport the sample through the column to • Purpose: transfer the analyte into the column. Packed Open tubular/capillary
the detector • Slow injection or oversized samples cause band broading and poor
• 2 to 4 mm I.D. WCOT SCOT PLOT
The carrier gas is generated from the gas cylinder and its resolution so sample should be introduced onto the column as a " of vapor
• 1 to 4 meters long
pressure and flow rate are regulated • 100 to 530 µm I.D.
• Glass or metal
• 10 m to 100 m long
• Packed with a suitable solid adsorbent or liquid coated
• Oxygen and hydrogen can't be used → active gas Sample injectors • Tubing fused silica, glass, copper, stainless steel
solid adsorbent
• Impurities (air or water) → sample decomposition, Split/ Splitless injection • Stationary phase is coated on the internal wall of
• Peak broadening due to zone (eddy) diffusion resulting
column and detector deterioration • Most common method of Injection into Capillary Columns. the column as a film 0.1 to 5 μm thick
from multitude of pathways a molecule can pass through
• Molecular sieve ( oxygen trap, and chemical filter → remove • Micro syringes inject the sample through a rubber septum into a flash • Sharper peaks → no eddy diffusion
column.
water and impurities vaporizer port at the head of the column either completely or partially. • Up to 500 000 theoretical plates excellent separations
• The temperature of the sample port is usually about 50°C higher than the • Most popular type
boiling point of the least volatile component of the sample.

A. Molecular Sieve Trap

B. Hydrocarbon Trap
C. Oxygen Trap

A carrier gas should have the following properties Split injection mode Splitless injection mode
1. High purity (99.9995 %) (use a trap in line)
Mechanism by which portion of the Most of the sample goes through
2. Inert so that no reaction with stationary phase or instrument.
injected sample is discarded the column
3. Compatible with the detector
 Nitrogen with a flame ionization detector (FID) is used, Advantages Advantages
 Helium when a mass spectrometer is used as the detector 1. Suitable for concentrated samples Suitable for quantitative and
 An additional gas may be required as fuel for the detector for 2. Narrow analyte band on column trace analysis
example, hydrogen and air for a flame ionization detector)
4. Cheap and available Disadvantages Disadvantages
In most cases, a selection between helium and nitrogen. Not suitable for trace analysis Risk of back flash

4- Oven 5- GC detectors
• The oven houses the column. • Monitor the carrier gas as it emerges from the column Classification of Detectors
• The oven is always equipped with a ventilator to guarantee a • Generate a signal in response to variation in its  Concentration vs. Mass sensitive
strong air circulation. composition due to eluted components Concentration sensitive Mass sensitive
• The oven must be thermally insulated from both the injection responds to the conc. of the responds to the number of
port and the detector. Types of GC detectors: analyte in the mobile phase ions that contact the
• The oven is an air thermostat that provide a constant (isothermal) • Thermal conductivity detector (TCD) (MP involved in the signal detector (MP not involved
or defined (programmed) increase of the column temperature. • Electron capture detector (ECD) formation). in the signal formation).
• The “simplest” way to alter the separation in GC is to alter the • Flame ionization detector (FID) • non destructive • Destructive
temperature program of the oven. • Nitrogen phosphorous detectors (NPD)
• Flame Photometric Detector (FPD)  Selective vs. Universal
Isothermal temperature Temperature programming
• Photo Ionization Detector (PID) Selective Universal
• The column temperature is • The column temperature • Mass detector Responds to particular types Detecting all solutes
constant throughout the analysis. increases as a function of time. Three temperature zones can be identified: of compounds
• Isothermal GC is not a good • Suitable to separate mixtures 1. Injector temperature (TI): should allow flash vaporization of all sample Ideal Detector • trace analysis • qualitative screening
choice for samples containing with various boiling points and components. 1. Sensitive 2. Reproducible
analytes with varying boiling still have good 2. Column temperature (TC) which is adjusted as the average boiling points 3. Linear response to analytes 4. Rapid response.  Destructive vs. Nondestructive
points. chromatography. of sample components. 5. Nondestructive to sample 6. Low background noise.
• Compounds may appear as • Shorter analysis time 3. Detector Temperature (TD) which should exclude any possible 7. Wide temperature range from room temperature to at
overlapping peaks condensation inside the detector. least 400oC

Generally, an intuitive equation can be used to adjust all three zones

depending on the average boiling point of the sample components This
equation is formulated as:
TI = TD = TC + 50oC

Mass Spectrometry
• The most important detector for GC
• By comparing a generated mass spectrum for the unknown compound with a database (on the PC) or by generating a
mass spectrum from a known standard of the suspected compound

Data Acquisition
• The output from a GC MS system can be visualized as a chromatogram (a plot of signal intensity versus time)
superimposed with a mass spectrum for each compound separated