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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).
Stationary Phase
(column)

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

Flame-
Carrier Gas (N2) Ionization
Detector
(FID)
Flame

Injector Column
(Sample Injection)

Oven

Columns Used :- Specifications :-


NETEL GC
10%FFAD/CHROMWHP –S.S.
15%DLES/CHROMWHP –GLASS
NUCON GC As Per Reference
S.S. Column/PORAPAK-Q (support)
NETEL GC – MICHRO9100
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 (Nitrogen)
• 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
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

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