Kelley Smith
2/3/2013
CHM 335.502
Ion Chromatography
Background:
This refers to modern, efficient, methods for separating and determining ions on columns with relatively
low ion exchange capacity. Although ion exchange separations have been around since ion-exchange
resins were developed in the mid-1930s. Ion chromatography as it is practiced today was first developed
in the mid-1970s when it was shown that anion or cation mixtures can be resolved on HPLC columns
packed with anion-exchange or cation-exchange resins. At that time, detection was generally performed
with conductivity measurements, which were not ideal because of high electrolyte concentrations in the
mobile phase. The development of low-exchange capacity columns allowed the use of low-ionicstrength mobile phases that could be further deionized to allow high sensitivity conductivity detection.
Currently several other deter types are available for ion chromatography, including spectrophotometric
and electrochemical. Ion chromatography was an outgrowth of ion exchange chromatography, which
during the Manhattan Project was developed for the separation of closely related rare earth cations
with cation-exchange resins. This monumental work, which laid the theoretical ground work for ion
exchange separations, was extended after World War II to many other types of materials, ultimately, it
led to automated methods for the separation and detection of amino acids and other ionic species in
complex mixtures. The development of modern HPLC began in the late 1960s but its application to
separation of ionic of ionic species was delayed by the lack of a sensitive general method of detecting
such eluted ionic species as alkali and alkaline earth cations and halide, acetate, and nitrate anions. This
situation was remedied in 1975 by the development by workers at the DOW chemical company of an
eluent suppressor technique, which made possible the conductometric detection of eluted ions
Procedure:
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Check helium.
Check bottles.
Open Chromeleon
Click File> Open> My Panels> Control Panel> Object Type
Select ICS -90 system
Turn small black knob to purge the system. (NOT the knob with red tape on it)
Turn the pump on
Equilibrate for 20 minutes
Create new sequence
A. Click File> New Sequence (using Wizard)
B. Leave time base intact
C. Select number of samples
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 The 7 anion standard should not be counted
 Injection/vial= 1
 Start position= 2
 Injection volume= 10 microliters
 Click Apply> Next
D. Set up the & anion standard
 Number of vials= 1
 Inject/vial= 1
 Start= 1
 Injection volume= 10 microliters
 Click Apply> Next
E. Make no changes on Methods and Reporting
F. Name the sequence and leave location
G. Hit Done
Click Batch> Edit
Make sure the sequence listed is the one you created if not click Remove
Click Add and add sequence
Click Start. Prompt will tell you to inject. Inject standard and click Ok
Let sample run
Open your sequence when 7 anion standard is done running.
Click File> Open> Sequence> Click your sequence
This should bring you to a dialog box that lists. Select 7 anion standard
Got to the peak analysis. Double click first peak
This should bring up a dialog box where you can type the peak name. Do that for each peak.
Make sure the Batch has finished running or is stopped.
To stop select batch drop menu> stop>check immediately and leave program running.
Make sure the eluent is filled to the top.
If waste container is full move the tubing to a new container.