Академический Документы
Профессиональный Документы
Культура Документы
prof. aza
Department of Pharmacy,
Andalas University
STIFI Perintis, Padang
STIFAR, Pekan Baru
STIFI Bhakti Pertiwi, Palembang
prof. aza
Definition
The basis for gas chromatographic separation is
the distribution of a sample between two phases.
One of these phases is stationary bed of large
surface area, and the other phase is gas which
percolates through the stationary bed.
If the stationary phase is a solid, we speak of GasSolid Chromatography. This depends up on the
adsorptive properties of the column packing to
separate samples, primarily gases.
If the stationary phase is a liquid, we speak of Gas
liquid Chromatography (GLC). The liquid is spread
as a thin film over an inert solid and the basis for
separation is the partitioning of the sample in and
out of this liquid film.
prof. aza
GC/MS
Gas Chromatography/Mass
Spectrometry (GC/MS) is a
combination of two
instrumental techniques,
gas chromatography and
mass spectrometry. The
gas chromatograph is used
to separate a mixture into
component parts and
deliver them to the mass
spectrometer. The mass
spectrometer breaks the
molecules into ions and
records the resulting
spectrum. This spectrum
conclusively identifies the
compound.
prof. aza
prof. aza
prof. aza
Chromatogram,
A Typical gasliquid
chromatography
displays each
component as
peak
prof. aza
Resolution
The resolution of chromatographic peaks is
related to two factors: column efficiency, and
solvent efficiency.
Column efficiency is concerned with the peak
broadening of initially compact band as it passes
through the column.
The broadening results from the column design
and operating conditions, and can be quantitatively
described by the height equivalent to a
theoretical plate.
The HETP is that length of column necessary for
the attainment of solute equilibrium between the
moving gas phase and stationary liquid phase.
prof. aza
Hypothetical representation of
Chromatographic separation
prof. aza
Advantages of Gas
Chromatography
Speed, the entire analysis is completed within 23
minutes.
High Resolution. By using selective solvents, GC
can provide resolution impossible by distillation or
other techniques.
Qualitative analysis. The retention time is that
time from injection to the peak maxima. This
property is characteristic of the sample and the
liquid phase at a given temperature. Each
compound has only one retention time. This
retention time is not influenced by the presence
of other component.
prof. aza
Temperature
Injection-port temperature should be hot enough
to vaporize the sample so rapidly that no loss in
efficiency results from the injection technique
and must be low enough so that thermal
decomposition or rearrangement is avoided.
Column temperature should be high enough so that
the analysis is accomplished in a reasonable length
of time. The retention time doubles for every 300
C decrease in column temperature. For the most
samples the lower the column operating
temperature, the higher the ratio of partition
coefficient in the stationary phase and the better
the resultant separation.
Detector temperature should be high enough so
that condensation of the sample and or liquid
phase does not occur.
prof. aza
Detector
Sensitivity
TCD
All
compound
10 ppm
FID
Organic
substances
0.1 ppm
ECD
0.1 ppb
prof. aza
Carrier gas
Commonly used gases are hydrogen,
helium, und nitrogen. The carrier gas
should be :
Inert to avoid interaction with sample
or solvent.
Able to minimize gaseous diffusion.
Inexpensive.
Suitable for detector used.
prof. aza
Solid support
The purpose of the solid support is to
provide a large uniform, inert surface area
for distributing the liquid phase. Some
desirable support properties are :
Inert (avoid adsorption).
High crushing strength.
Large surface area.
Regulator shape, uniform size.
prof. aza
Stationary phase
Ideally the solvent should have the
following characteristic:
Samples must exhibit different
distribution coefficients.
Sample should have a reasonable
solubility in the solvent.
Solvent should have a negligible vapor
pressure at operating temperature.
prof. aza
Resolution
The resolution of chromatographic peaks is
related to two factors: column efficiency, and
solvent efficiency.
Column efficiency is concerned with the peak
broadening of initially compact band as it passes
through the column.
The broadening results from the column design
and operating conditions, and can be quantitatively
described by the height equivalent to a
theoretical plate.
The HETP is that length of column necessary for
the attainment of solute equilibrium between the
moving gas phase and stationary liquid phase.
prof. aza
Resolution, continued
Solvent efficiency result from the solutesolvent interaction and determines the
relative position of solute bands on a
chromatogram.
Solvent efficiency is expressed as the
ratio of peak maxima (adjusted retention
times).
Column efficiency is measured by the
number of the theoretical plates.
prof. aza
Resolution, continued
The true separation of two
consecutive peaks is
measured by the resolution.
Resolution is a measure of
both the column and solvent
efficiency.
If R = 1, the resolution of
two equal-area peaks is
approximately 98% complex.
If R = 1,5, base line
separation (99,7% resolution)
ia achieved.
prof. aza
Separation of
two bands as
a function of
resolution
(Rs) and
relative band
size (I/1, ,
1/16).
prof. aza
prof. aza
Normal
Effects of a
change in k,
N, or a on the
resolution of
two bands
prof. aza
HETP = L/N
prof. aza
Band asymmetry,
(a) Definition of
asymmetry factor,
As; (b-e) examples
of band asymmetry
prof. aza
prof. aza
prof. aza
prof. aza
prof. aza
HETP = 2 dp + 2 Dgas
+ 8
k
df 2 x
(1+k)2 Dliq
prof. aza
2 Dgas
= a constant which is a
measures of packing
irregularities.
dp = average particle
diameter of the solid
support.
prof. aza
df2
(1+k)2 Dliq
k = capacity factor =
k ( Fliq / Fgas )
k = partition coefficient of
the solute, expressed as
the amount of solute per
unit volume of liquid
phase divided by the
amount of solute per unit
volume of gas phase
Illustration of Multipaths
Basic measurement
prof. aza
Science for a
better future