Start-Up And Testing Column And Chromatograph - MACHEREY-NAGEL OPTIMA Gebrauchsanleitung

Installation and operating instructions
II. Start-up and testing column and chromatograph
1. Conditioning
Each column has been conditioned prior to its quality control. Con-
ditioning is used to elute volatile components of sample molecules
and stationary phase and to remove active sites of the inner column
surface.
Conditioning should always be performed after a longer stor-
age of the column and performed until the baseline is stable
(usually approx. 4 h).
The two numerical temperature values mentioned in the cer-
tificate indicate the (lower) isothermal long-term temperature
(= conditioning temperature) and the (higher) short-term tempera-
ture (= maximum in temperature gradients during 5–15 min).
During conditioning never exceed the long-term temperature, and
make sure that the gas supply is never interrupted.
2. Column test
Each column from MACHEREY-NAGEL is tested in a gas chromato-
graph, and the individual chromatogram with conditions (the test cer-
tificate) is supplied with the column. It should be retained for future
reference.
If possible you should reproduce the included test chromatogram
before using the column for your analytical tasks. The respective test
mixture can be separately purchased (see www.mn-net.com).
This will indicate whether
„ column installation is correct
„ samples are properly injected
„ the overall chromatographic system including evaluation works
accurately.
By reproducing the column test you document the performance of
the column, and thus you can at any time compare the state of the
column with the initial quality.
Using the column test, you can identify a number of typical failures;
this is the reason why reproduction of this test should always be the
first step in troubleshooting.
If the test result is satisfactory, the planned application can be op-
erated.
10
www.mn-net.com
3. Checking column installation
What should you do when your own test does not show the same
result as the test certificate?
a) Check the correct installation of the column and test again.
b) Compare the faulty chromatogram with the examples in our trou-
bleshooting and try to correct the problem.
c) Contact your nearest MACHEREY-NAGEL office or your local
distributor and ask for help.
4. Troubleshooting
If you cannot reproduce the test chromatogram of your capillary col-
umn, this may be due to one of the following reasons (see page 11
and 12).
For example, a dead volume in the injector produces tailing. This is
especially strong for early eluting components in a temperature pro-
gram. Dead volume in the detector also results in tailing, however, in
this case all components are affected.