Temperature

programming in GC
Training course on GC/MS
Nha Trang 13-18/10 2008
Charlotta Rylander

Separation of compounds by
GC

In GC, analytes are separated according to boiling

point and polarity and other properties.
The boiling point affect how easily the analytes
evaporate. Molecules with low boiling point will elute
early from the GC column, hence, compounds with
high boiling point will elute late.
Analytes interact with the GC column. If the column
is non-polar, analytes with high polarity will travel
fast through the column while more non-polar
compounds will be retained.

Temperature effects

Temperature

Vapour pressure of analytes

Retention time

Partitioning
coefficient

Isothermal column
temperature

If the GC is run isothermally, the

column temperature is constant
throughout the analysis.
Fast eluting compounds may then
appear as overlapping peaks and
late eluting compounds will have
long retention time and broad
peak shape.
Isothermal GC is not a good
choice for samples containing
analytes with varying boiling
points.

http://ull.chemistry.uakron.edu/chemsep/slide.php?
Chapter=/chemsep/GC/&Last=100&Slide=56

Temperature programming
By

increasing the
temperature as a function
of time, it is possible to
separate mixtures with
various boiling point and
still have good
chromatography.
In addition, the total
analysis time will be
shorter.
http://ull.chemistry.uakron.edu/chemsep/slide.php?
Chapter=/chemsep/GC/&Last=100&Slide=56

Isothermal GC temperature/
Temperature programming
Isotherm column
temperature

Temperature
programming

www.chem.agilent.com

Setting up a temperature
program
Trial and error technique!

Setting up a temperature
program

Try to find publications about analysis of the

analytes of interest. Usually, the temperature
program is reported.
Useful internet sites:
http://chromatographyonline.findpharma.com/lcgc/

http://spectroscopymag.findpharma.com/spectrosco
py

Setting up a temperature
program

Always use standard solutions when

setting up a temperature program.
The injector temperature must be
optimized before start. If the injector
temperature is too low, the analytes
will not be vaporized. If it is too high,
we may loose analytes. Check boiling
point of analytes before start. Ramp
temperature on column when
optimizing injector temperature.
Take care when using on column
detector. Check the boiling point of
solvents and solvent mixtures.

http://www.cartage.org.lb/en/themes/Sciences/Chemist
ry/Analyticalchemistry/MethodsInstrumentation/Chrom
atography/Gaschromatography/splitinj.gif

Setting up a temperature
program

Start with ramping the temperature (50C-300C, 510C/min, depending on analytes) to make sure you
elute all compounds. From that run it is possible to
determine the final temperature of the GC
programme.
Identify possible coelutions.
In areas with coelutions, add isothermal periods.
Initial temperature should be determined based on
best possible separation of the the first few peaks.
Experiment with various ramps between initial and
final temperature to get the best separation and
shortest method.