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: 1. 2. 3. 4. 5. 6. 7. 8. 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 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 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.