DO NOT REMOVE
Ion Chromatograph (IC)
Standard Operating Procedure
INSTRUMENT:
Dionex ICS-90
INSTRUMENT START-UP:

If the instrument was off, follow the alternate start-up procedure on page 9
A. Check helium in gas storage room (if less than 80 psi, notify assistant)
B. Turn on the helium valve at bench top
C. Instrument helium pressure: 9 psi
1. Let the system equilibrate before you adjust the pressure
2. Helium pressure should NOT be above 10 psi
1
DO NOT REMOVE
D. Make sure the eluent level is above the half way mark
E. Open Chromeleon software
(The program should be open unless the instrument was off)
F. Open the control panel in Chromeleon
1. Go to File
2. Select Open
3. Select Look in
4. Select DBV2NT21_local
5. Select My Panels
2
DO NOT REMOVE
6. Select Object of Type drop down menu
7. Select Control Panel
8. Select ICS-90_system
G. Make Sure instrument is connected
------------------------------------------------------------------------------------------------------------------------------PRIMING THE PUMP:
A. Turn off the pump
3
DO NOT REMOVE
B. Turn the small black knob 1 turn to left to purge the system for 30 seconds
1. Make sure eluent is flowing into the waste jar
2. DO NOT keep turning the knob
C. Turn on the pump
1. Leave the system open for an additional 30-45 seconds while eluent is still
flowing into the waste jar
D. Close the system by turning the black knob to the right
E. Leave pump on and let the system equilibrate for 20 minutes
F. Make sure the flow rate is 1 mL/min
(Check the flow coming from the black tube in the waste container)
G. DO NOT TOUCH the black knob located in the center labeled DO NOT TOUCH!
(This knob will increase the pressure and cause seals to break as well as blow the pump)
---------------------------------------------------------------------------------------------------------------------
4
DO NOT REMOVE
RUNNING AN EXPERIMENT:
A. From the file menu, select new then sequence using wizard. The sequence
dialogue box will appear.
B. DO NOT change anything in the Timebase screen
C. Select number of Samples
1. Name your samples
2. Enter the number of samples
(The 7 anion standard should not be counted in this number)
3. Injections per vial=1
4. Start Position=2
(The 7 Anion Standard is first and you will set this on the next screen)
5. Injection Volume=10L (because it is a 10L loop)
6. Click Apply
(You should see the box on the right change to accommodate your changes)
7. Click Next
5
DO NOT REMOVE
D. 7 Anion Standard
1. Number of Vials=1
2. Injections per Vial=1
3. Start Position=1
(Since this is done you can manually name the peaks in the standard and it
will automatically name the peaks in any spectra you run after this)
4. Injection Volume=10L
5. Click Apply if any changes were made
6. Click Next
E. DO NOT change anything in the Methods and Reporting screen
F. Name your sequence
(DO NOT change the location)
6
DO NOT REMOVE
G. Finish the sequence wizard
H. From the batch menu, select edit and make sure the sequence you created is
listed. If you batch does not appear, select remove and add your file.
I. Click Start - this should give you a prompt to manually inject 7 anion standard
J. Inject the standard and Click Ok on the prompt box
K. The program will prompt you to inject each sample
(Samples take approximately 16 minutes to complete)
L. If there are no peaks after several injections and the conductivity extremely high
the regenerate needs to be replaced
(see procedure on page 11 for regenerate calculation)
--------------------------------------------------------------------------------------------------------------------------
ANALYZING SPECTRA:
A. Open your Sequence after the 7 anion standard is running
1. Select File
2. Select Open
3. Select Sequence
4. Click the sequence that you are currently running
B. This should bring up a dialog box that has your sequence listed, select the seven
anion standard
7
DO NOT REMOVE
C. In the peak analysis tab, double click on the first peak and type in the name of
the peak in the dialogue box.
D. To name each peak, use the standard spectra on page 12
1. NOTE: there is no acetate present in the 7 anion standard
E. To name individual peaks
1. Click on the peak in the graph to select the peak.
2. Right click and select Peak Properties.
3. Manually type in the name and push enter after each one to move to the
next peak
------------------------------------------------------------------------------------------------------------------------INSTRUMENT SHUT-DOWN:
A. Make sure the Batch has finished running or has been stopped
1. To stop the batch, select the Batch menu, click stop, and select the
immediately option
B. Leave the Chromeleon Program running
(The system will go into low flow method after 6 hours of inactivity)
C. Make sure the eluent is filled to the top
D. Turn off the helium valve on the bench top
E. Check waste (notify assistant if full)
------------------------------------------------------------------------------------------------------------------------------WASTE CONSIDERATIONS FOR INSTRUMENTAL CHEMISTRY COURSE:
A. Samples and Standards may be disposed of in the sink
-------------------------------------------------------------------------------------------------------------------------------
8
DO NOT REMOVE
ALTERNATE START-UP PROCEDURE:
1.
Turn the Instrument On
1. The button is located in the middle on the back of the instrument
2. If the instrument has been off for a substantial time, change the regenerate and
the eluent
2. Check helium in gas storage room (if less than 80 psi, notify assistant)
3. Turn on the helium valve at bench top
D. Instrument helium pressure: 9 psi
1. Let the system equilibrate before you adjust the pressure
2. Helium pressure should NOT be above 10 psi
9
DO NOT REMOVE
F. Make sure the eluent level is above the half way mark
G. Open Chromeleon software
(The program should be open unless the instrument was off)
H. Open the control panel in Chromeleon
1. Go to File
2. Select Open
3. Select Look in
4. Select DBV2NT21_local
2. Select My Panels
10
DO NOT REMOVE
3. Select Object of Type drop down menu
4. Select Control Panel
5. Select ICS-90_system
I. Make Sure instrument is connected
Follow the PRIMING THE PUMP SECTION
------------------------------------------------------------------------------------------------------------------------------IC Eluent:
To prepare the eluent for the IC, use a 2000 mL volumetric flask and dilute 20 mL of Eluent in
distilled water
IC Regenerate:
To prepare the eluent for the IC, us a 2000 mL volumetric flask and dilute 5 mL of 6 M sulfuric
acid in distilled water
11