GAS CHROMATOGRAPHY (GC)

Mobile Phase (N2)

Separation of individual components from a
sample mixture through the repeated
distribution of the components between the
stationary phase (column) and a gaseous
mobile phase (Nitrogen/Helium/Argon).
Stationary Phase
(column)

AA C
AC C C AA
C AABC B BB CCC
A A B BB C CC
B B AB B AA B C
BC
Sample separated components
 GAS CHROMATOGRAPHY-FLOW DIAGRAM
Flame Gases (H2 & Air)

Flame-
Carrier Gas (Ar/He/N2) Ionization
Detector
(FID)
Flame

Injector Column
(Sample Injection)

Oven

Columns Used :-
Packed
FFAP
AT-1000
OV-101
Capillary
DB-1
HP-5
 CRITERIA FOR GC
• Technique of choice for separating thermally stable and volatile compounds
• Basics --
• Distribution of sample between two phases,
• Stationary bed of large surface area (COLUMN)
• Second is mobile phase – a gas that percolates through the stationary
phase
• GLC: stationary phase is a liquid coated on a inert solid support
• GSC: solid adsorbent as a stationary phase
• Versatile and selective
• Large range of liquid phases with usable temp upto 450°C
• Can be used to analyze gaseous, liquid and solid samples
• Sample MUST be volatile at temperatures BELOW 350°C
 ADVANTAGES OF GC
 Speed – Very fast, run can be completed in minutes
 Resolution – High resolution of closely related
compounds
 Qualitative analysis – Identification of substance by
retention time
 Quantitative analysis – Quantification of identified
substance by area under peak
 Sensitivity – Highly sensitivity (can be quantified in
ppm range)
 Simplicity – Relatively simple to operate and
understand
 COLUMN TYPES
• Capillary (open tubular)
 Inner wall modified with thin (1 m) film of liquid
 0.3 - 0.5 mm ID; 10 - 50 m length
 Can load few g analyte only
 WCOT, SCOT, PLOT, FSOT

• Packed
 Solid particles either porous or non-porous coated with thin (1
m) film of liquid
 1 - 8 mm ID; 1 - 10 m length
 Can load upto few hundred g analyte
 IMPORTANCE OF TEMPERATURE IN GC ANALYSIS
Injection Port Temperature
Hot enough to vaporize the sample rapidly
Low enough to avoid thermal decomposition or rearrangement of
the sample
Column Temperature
High enough so that analysis is accomplished in reasonable time
Low enough that separation is achieved
Retention time approx. doubles for every 30°C decrease in
temperature
Lower the temperature, higher the ratio of partitioning
coefficients in stationary phase
Temperature programming for effective separation
Detector temperature
Type of detectors – Flame-ionization detectors (FID), Thermal
Conductivity Detector (TCD) etc.
Hot enough to prevent condensation of sample, peak broadening
and loss of component peaks
TCD is more sensitive to temperature than FID
 ANALYSIS DONE BY GC

Finished Goods – Actives

 Quantitative analysis of actives by capillary column DB-1

Raw Materials –
 Turpentine Oil – In Netel GC by using AT-1000 column
 Clove Oil – In Netel GC by using OV-101 column

Others –
 Related substances in Mentha Oil
 Analysis of actives in solids
 ADVANCEMENTS IN GC
 Headspace GC
 To detect volatile components in sample
 To analyze vapours above the sample (liquid)
 Multiple headspace extraction
 Gas Chromatography – Mass Spectrometry (GC-MS)
 Detection of residual solvents in pharmaceutical
 Study of constituents of essential oil
 Determination of fatty acids

GC-MS Process
ANY QUESTIONS