Refilling the EI Calibration Vial for the Agilent 5975 and 5977 Series GC/MSD

Answer

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

Issue:

Tuning the Agilent GC/MSD with EI sources, requires the use of perfluorotributylamine (PFTBA). The calibration vial will be depleted eventually due to regular use. This article explains how to refill the calibration vial.

Steps to follow:

Materials required

• GC/MS Tuning Standard - PFTBA (p/n 05971-60571)
• Syringe or pipette

To Refill the Calibrant vial

1. Stop any tuning or data acquisition.

2. Turn off the analyzer and the vacuum gauge controller (if installed). (See Figure 1).

   1. In the Tune and Vacuum Control view, under the Execute menu, click MS OFF.

   2. Under the Vacuum menu, click Tune Vacuum Gauge on/off...

   3. Select the off radio button, and click OK.

      
      Figure 1. Turning off vacuum gauge and analyzer
      
      

3. After removing the front analyzer window cover, loosen the calibration vial collar

4. Without removing the collar, remove the calibration vial. (See Figure 2)

   
   
   Figure 2. Removing the EI Calibration Vial
   
   

5. Using a syringe or pipette, fill about 70 µL of PFTBA into the vial (Figure 3). With the vial vertical, the liquid should be just below the end of the internal tube. In the horizontal position, the liquid should not touch the internal tube (Figure 4).

   
   Figure 3. Filling the Calibration vial
   
   
   Figure 4. PFTBA level in the calibration vial.
   
   

6. Push the calibration vial into the vial, as far as possible, and then withdraw the vial 1 mm.

7. Turn the collar clockwise to tighten it. The collar should be snug but not overly tight.

8. Reinstall the analyzer window cover (Figure 5).

   
   Figure 5. Reinstalling the EI Calibration Vial

Caution: After removing a calibration vial, you must purge the calibration valve. Failure to do so may result in damage to the filaments and the electron multiplier.

To purge the calibration valve

1. If the vacuum gauge controller is on, turn it off.

2. In Tune and Vacuum Control view, under the Vacuum menu, select Purge Calibrant Valve (Figure 6).

   
   Figure 6. Purging the Calibrant Valve
   

The EI Calibration will open 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.