Refilling the CI Calibrant Vial for the Agilent 5975 and 5977 Series GC/MSD

Answer

This Information Applies To: Agilent 5975 and 5977 series GC/MSD

 Issue: 

If the PFDTD signal is absent or low, but the reagent ions are normal, you may have run out of CI Calibrant. 

Inspect the calibration vial on the back of the flow controller. If necessary, fill the vial with PFDTD according to the instructions in this article.

Steps to Follow:

Materials needed

• Wrench, open-end, 1/4-inch × 5/16-inch (p/n 8710–0510)
• PFDTD calibrant, for GC/MS – 1 mL (p/n 8500–8510)
• Syringe or pipette

 CI calibrant refilling process

1. Set the reagent gad flow to Gas Off.

2. Vent the MSD.

3. Turn off the GC.

4. Remove the capillary column from the GC/MSD interface.

5. Place a column nut with a blank ferrule on the end of the interface. This action will help keep contamination out of the MSD.

6. The foreline pump may be located either on the floor, on the lab bench next to the MSD, or under the analyzer chamber at the back of the MSD. Move it as needed to provide slack in the tubing and cables.

7. Move the MSD away from the GC until you have access to the GC/MSD interface cable. (See Figure 1)

   Caution: Disconnecting the interface, or LVDS cable with the GC on, can cause a fault condition.

    

8. Disconnect the GC/MSD interface cable and the LVDS cable (if applicable). LVDS cable position will vary on different models of GC (See Figure 1)

   
   Figure 1. Separating the MSD and GC
   1.Interface Cable, 2. LVDS cable (if present)
   
   

9. Continue to move the MSD until you have access to the CI Calibration Valve.

10. Loosen the calibration vial collar by turning it counterclockwise. Do not remove the collar.

11. Remove the calibration vial. (See Figure 2)
    

    
    Figure 2. Removing the CI Calibration Vial
    
    

    Caution: Do not rinse the vial with any solvents. Never expose the inside of the vial to chlorinated solvents, isopropyl alcohol, or water. Exposition to the mentioned solvents will result in severe loss of CI sensitivity.

    
    

12. Fill the vial no higher than the bottom of the internal tube with fresh PFDTD calibrant (8500–8510).

13. Replace the vial and tighten the collar. (See Figure 3)

    
    Figure 3. Filling and installing the CI Calibration Vial
    
    

14. Reconnect the Interface cable, and the LVDS cable.

15. Reposition the MSD next to the GC.

16. Reinstall the capillary column.

17. Pump down the MSD.

Caution: After removing the calibrant vial, you must purge the calibration valve. Failure to do so will result in severe contamination of the ion source and damage to the filament and electron multiplier.

To Purge the Calibration Valve

After adding new PFDTD to the CI calibration vial, you must purge the air out of the vial and valve.

1. If the vacuum gauge controller is on, turn it off.
2. Verify that PCICH4.U file is loaded.
3. In the Tune and Vacuum Control view, under the Vacuum menu, click Purge Calibrant Valve. This action will open the CI calibration valve for several minutes with all analyzer voltages turned off

Learn how to effectively maintain your Agilent 5977B GC/MSD: Agilent 5977 GC/MSD with MassHunter Workstation e-learning path available from Agilent education.