Pickering Laboratories Pinnacle PCX - Page 148

7.12
Section 7
TroubleshooTing
Pinnacle Operators Manual
Pickering Laboratories Inc.
1. Remove the column and flush HPLC system with water. Put column Regenerant on.
2. Connect the column in reversed direction and flush with Regenerant. Use a very slow flow rate so that the
back pressure does not exceed 2000 psi.
3. Keep flushing until pressure drops. Keep raising the flow rate until pressure is normal at standard operating
conditions. Normal pressure for guard column is < 500 psi. Normal column pressure without a guard <2000
psi.
4. Reinstall guard and analytical columns in normal direction.
5. Run a chromatogram to check for resolution.
IF NaOH IS ON COLUMN
1) Do not restart the system. Dissolved silica or C18 phase will reprecipitate in the post-column reactors, or
flowcell. These additional complications then require replacement of both reactor coils as well as your column.
2) Immediately depressurize the post-column system by loosening the “To Detector” fitting.
3) Disconnect the outlet of the column.
4) Restart the HPLC pump to flush the column with 100% MeOH for 20 minutes. Complete steps 2–4 as quickly
as possible because the longer the hydroxide stays inside the column, the less chance that the column will
survive.
5) Catch the effluent from the column with paper towels. Alternatively, connect the outlet of the column to a
piece of spare tubing directing the effluent to waste.
6) Turn off the HPLC pump and reconnect the outlet of the column and the “To Detector” fitting.
7) Turn on the HPLC and post-column system and run a calibration standard. Pay special attention to the first
four peaks. If these four peaks are not resolved, the column needs to be replaced.
TO REMOVE IRON CONTAMINATION FROM COLUMN
Flush guard and column with the Glyphosate Restore solution.
TO PUMP RESTORE THROUGH THE GLYPHOSATE COLUMNS
Usually only the guard column is contaminated. We suggest you buy a spare guard column to minimize
down-time.
1) Remove the analytical column after ensuring no residual post-column pressure.
2) Reverse the guard column and pump RESTORE through the guard at 0.4 mL/min for a minimum of 30 min,
directing the effluent to waste.
3) Pump K200 eluant through the guard long enough to displace RESTORE — about 30 min
4) Reconnect the column and guard in the normal directions and restart the HPLC and post-column systems.
If analytical column is also contaminated, reverse the column and flush with Restore for 2 hrs. Equilibrate with
K200 for 1 hour before use.