This Information Applies To: 5977A and 5977B
Content:
This procedure is to guide the installation of a capillary column on 5977A/B GC/MS with a standard column nut or self tightening nut.
Steps to follow:
The GC and MS operates at high temperatures. In order to avoid burns, do not touch any parts of GC and MS until you are sure they are cool.
Always wear safety glasses when handling capillary columns. Use care to avoid puncturing your skin with the end of the column.
Always wear clean gloves while handling any parts that go inside the GC or the analyzer chambers.
Prerequisites
- Vent the MS, refer to How To Vent (Shut Down) the GC/MSD - EI - MassHunter. Open the vent valve by turning the knob counterclockwise (see Figure 1).
Figure 1 Vent valve - Install a capillary column in the inlet, refer to Capillary column installation quick reference guide. Alternatively, you could use a self-tightening column nut to install the column(see Figure 2, the nut part number is G3440-81011) with short ferrules (the part number refers to Figure 3) to install the column.
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Column ID Ferrule PN 0.1-0.25 mm 5181-3323 0.32 mm 5062-3514 0.45-0.53 mm 5062-3512 |
| Figure 2 Self-tightening column nut for inlet/detector | Figure 3 Short graphite/vespel (15%/85%) ferrules |
- Condition the column.
- Open the front cover and could see the type of ion source for SST, Inert, and Xtr EI, but for high efficiency sources, you just only see the type on the front cover ( see Figure 2)
5977A/B SST EI, Inert EI, Xtr EI, CI 5977B High Efficiency Source (HES) Figure 2 How to identify GCMS ion source type
Steps:
1. Open the analyzer chamber. Be sure you can see the end of the GC/MS interface. You could directly observe the end of the column inside the analyzer chamber for SST and inert EI, but for Xtr, HES EI, and CI source, you need to remove the tip seal assembly (including ceramic tip seal, spring, and tip cap) (see Figure 3).
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| 5977A/B SST and inert EI |
5977A Xtr EI 1- Tip seal 2- Tip cap |
5977B Xtr and HES EI 1- Tip seal 2- Tip cap |
5977A/B CI 1- Tip seal and spring |
| Figure 3 Ion source transfer line |
3. Slide the column into the GC/MS interface. The tapered end of the ferrule must point towards the nut (see Figure 4). Alternatively use a self tightening nut for MS interface (see Figure 5).
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Figure 4 1- GCMS interface 2- Ferrule 3- Nut |
Figure 5 1-Self tightening nut for inlet, PN G3440-81011 2-Self tightening nut for MS, PN G3440-81013 |
4. Adjust the column so it extends this specified distance from the end of the transfer line (best to push the column the whole way through, cut the column, then pull back until it’s at a specified length).
For an SST/Inert/Xtr EI source installation, the column extends 1 to 2 mm.
For a high efficiency source installation, the column extends 4 to 5 mm.
For a CI Source Installation, the column extends about 1 mm.
note: Use the flashlight and magnifying loupe if necessary to see the end of the column inside the analyzer chamber. Do not use your finger to feel for the column end.
5. Hand-tighten the nut. Ensure the position of the column does not change as you tighten the nut, and be sure to not over tighten the nut. if you use a self tightening nut, tighten the nut in the clockwise direction, continue to tighten until you feel the ferrule grip the column. and then jump to step 9 to continue the operation (steps 7 and 8 are not needed for self tightening nut).
6. Check the GC oven to be sure that the column does not touch the oven walls.
7. Tighten the nut 1/4 to 1/2 turn.
8. Check the nut’s tightness after one or two heat cycles; tighten additionally as appropriate.
9. Install the tip seal assembly at the end of the GC/MS interface (don't need for 5977A/B with SST and inert EI source). For the CI GC/MS interface and the EI GCMS interface with an Xtr and HES source install the tip seal spring, then align and gently slide the ceramic tip seal, next step for 5977A with Xtr source, slide the tip cap and tighten two screws onto the tip cap. for 5977B with Xtr and HES source, screw the knurled nut onto the end of the interface (see Figure 6).
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5977A with Xtr source 1-Spring 2-Tip seal 3-Tip cap |
GC/MS CI source 1-Tip seal and spring |
5977B with Xtr and HES source 1-Knurled nut 2-Spring |
| Figure 6 GCMS Tip seal assembly |
10. Gently check the alignment of the ion source and the interface tip seal for CI GC/MS and EI GC/MS with an Xtr and HES source. When the ion source is aligned correctly, the front analyzer chamber can be closed all the way with no resistance except the spring tension from the interface tip seal.
11. Close the analyzer chamber door.
Learn more on how to effectively operate your GCMS, please refer to the following link:
Agilent 5977 GC/MSD with MassHunter Workstation e-Learning course on Agilent University
Keywords: Column installation, 5977A, 5977B, HES, XTR, ion source, self tightening nut
