Docstoc

IC_SOP

Document Sample
IC_SOP Powered By Docstoc
					                                 Ion Chromatography SOP
Instrument: Dionex ICS-90

Program: Chromeleon
General Procedure:

      Before operating the instrument check the helium in the gas room
           o If the tank’s pressure is below 80 psi let the lab assistants and/or instructor know
                     If the pressure is below 40 psi replace the tank
      There is a pressure gauge on the instrument
           o Make sure the helium is flowing to the instrument
           o The pressure gauge should read 9 psi
                     If not turn the black knob next to the gauge in the direction the needle needs to
                       move
      Check the Regenerant and Eluent bottles on the instrument
           o If either bottle is less than half full refill using the containers near the instrument or make
               more
                     To make more eluent take 10 mL of the concentrated eluent from the drawer and
                       dilute to 1 L with distilled water
                     To make new regenerant add 1.7 mL of concentrated sulfuric acid to a 2 L
                       volumetric flask with distilled water
                             Before refilling the regenerant or eluent turn off the gas to the instrument



      Open the Chromeleon program from the icon on the desktop.
      Equilibrate the instrument:
          o In the program: File, Open
          o Change the file type to control panel and in the MyPannels folder click to open the ICS-90
                system.
          o Turn the pump off in the program
          o Turn the small black knob on the pump to the left
                     Do NOT touch the knob that says “Do Not Touch”
                     Let the system purge the system for 30 seconds
                              Check if eluent is flowing into the waste jug under the counter
          o Turn on the pump in the program
                     Let the system purge for another 30-45 seconds.
                              Check if eluent is flowing
          o Turn the knob on the pump back to the right
                     Be careful to not over tighten the knob
        o Let the system equilibrate for 20-30 minutes.
        o Check the flow of the eluent by taking a graduated cylinder in the waste bucket and
            collecting the waste
                  After one minute check if the waste amounts to about 1 mL
                          If there is not 1 mL the case wait another 10-15 minutes and check again.
                             (If there is still no flow find the experts, lab assistant, or Dr. Foy).
   Set up Software:
        o Create a new sequence by opening the file menu then new then sequence
        o Click next in the box that comes up
        o Set injection parameters
                  Select the number of different vials being used
                  Set the number of injections per vial desired
                  The start poisition should be 2
                  The injection volume should be 10µL
                  Click apply
                  Click next
        o Don’t change the Methods and Reporting
        o Name the sequence with your initials
        o Click done
   Running the sequence
        o Go to the batch menu click edit
        o Find the sequence you created by clicking add and finding your sequence
        o Click start
                  A prompt will tell you to inject your sample
        o Inject the standard with a sterilized syringe into the injector port until a small amount
            comes out into the waste beaker located next to the instrument.
        o Click OK on the prompt
        o The run will take 16 minutes
                  If there are no peaks try injecting the sample again
                          If there are no peaks after several injections and the conductivity is
                             extremely high replace the regenerate
   Name Peaks:
        o Open your sequence:
                  Click file then open then select sequence then click your sequence name
        o Double click the 7 anion standard in the dialogue box that has a list of the names of your
            injections
        o Find the peak analysis tab
                  Double click on the first positive peak
        o A dialogue box will appear
                  Name each peak according to the blue sheet in the drawer following the order
                        Press enter after naming each peak
                              there is no peak for the acetate ion
       Shutting Down:
           o Make sure the batch is stopped by going to the Batch menu>Stop
           o Leave the Chromeleon program RUNNING (the system will go into low flow method after 6
                hours of inactivity)
           o Fill the eluent to the top
           o If the waste container is full move the tube to a new container
                    Put a cap on the full waster container
                    Bring the full container to the prep room using the elevator
                    Neutralize the waste in a large beaker on a stir plate and magnetic stir bar, using
                        20 mule team borax (located in storage area, ASK IF YOU NEED HELP)
                    Use universal indicator to check pH (the color should change from pink to green)
                    Flush down the drain with plenty of water

Lab Procedure:

       You will run four different water samples
       Run two samples each day
       Run two trials of each sample
       Follow the general procedure
            o Day1
                      Set the sample to 2 vials and 2 injections per vial
                                This indicates that the first injection is the standard, followed by 2
                                   injections of each sample
                      Use the same standard both days
            o Day 2
                      Same procedure as Day 1
                      Make a calibration curve of your samples
                                plot ppm vs height and area

Ask the experts, assistants, or instructor if you have any questions

				
DOCUMENT INFO
Shared By:
Categories:
Tags:
Stats:
views:1
posted:3/31/2012
language:
pages:3