GAS CHROMATOGRAPHY

(GC)
Principle
Partition of molecules between gas (mobile
phase) and liquid (stationary phase).

Gas Chromatography
Filters/Traps

Data system
H

RESET

Regulators

Syringe/Sampler
Inlets
Detectors

Gas Carrier

Hydrogen

Air

Column

gas system
inlet
column
detector
data
system

Carrier gases move analytes through the column.

Helium, hydrogen and nitrogen most often used.
Nitrogen provides highest efficiency (only subtle
differences to the other gases), but run time is long.
Helium provides good efficiency and short analysis times,
but is expensive (and will become even more expensive).
Hydrogen provides shortest analysis times over a broad
range of linear velocities.
Purification of carrier gases essential for maintaining of
high quality in GC

GC Columns

Packed columns
Typically a glass or
stainless steel coil.
1-5 total length and 5 mm
inner diameter.
Filled with the st. ph. or a
packing coated with the
st.ph.

Capillary columns
Thin fused-silica.
Typically 10-100 m in length
and 250m inner diameter.
St. ph. coated on the inner
surface.
Provide much higher
separation eff.
But more easily overloaded
by too much sample.

GC Packed vs. Capillary Columns

DETECTORS

Ideal detector:
1. Adequate sensitivity: now 0.1 ng to fg solute/s
2. Good stability and reproducibility
3. Linear response to solute over several orders of
magnitudes
4. Temperature range from T room to at least 400C
5. Short response time that is independent of flow rate
6. High reliability and ease of use
7. Similarity in response toward all solutes or highly
selective and predictable response toward one or
more classes of solutes
8. Nondestructive of sample

Thermal Conductivity Detector (TCD)

Flame Ionization Detector (FID)

Electron Capture Detector

ECD detects ions in the exiting from the gas chromatographic column by the
anode electrode.
3

H or 63Ni which emits particles.

Ionization : N2 (Nitrogen carrier gas) + (e) = N2+ + 2e

These N2+ establish a base line
X (F, Cl and Br) containing sample + (e) XIon recombination : X- + N2+ = X + N2

The nitrogen phosphorous detector (NPD)

The photoionisation detector (PID)

Flame Photometric GC Detector

The reason to use more than one kind of detector for gas chromatography is to
achieve selective and/or highly sensitive detection of specific compounds
encountered in particular chromatographic analyses. The determination of
sulfur or phosphorus containing compounds is the job of the flame
photometric detector (FPD). This device uses the chemiluminescent reactions
of these compounds in a hydrogen/air flame as a source of analytical
information that is relatively specific for substances containing these two
kinds of atoms. The emitting species for sulfur compounds is excited S2. The
lambda max for emission of excited S2 is approximately 394 nm. The emitter
for phosphorus compounds in the flame is excited HPO (lambda max =
doublet 510-526 nm). In order to selectively detect one or the other family of
compounds as it elutes from the GC column, an interference filter is used
between the flame and the photomultiplier tube (PMT) to isolate the
appropriate emission band. The drawback here being that the filter must be
exchanged between chromatographic runs if the other family of compounds is
to be detected.

Flame Ionization Detectors

Chromatograms

Chromatograms

Supelco PTE-5

Supelco SPB-50

Chimiti la pensie!
The responsibility for
change
lies within us. We must
begin with ourselves,
teaching ourselves not to
close
our
minds
prematurely to the novel,
the surprising, the
seemingly radical.
Alvin Toeffler