Leak Checking Sources Service Note V002
Leak Checking Sources Service Note V002
Leak Checking Sources Service Note V002
3
1 10
2
2.5
0.8 8
1.5
2
0.6 6
1.5
1
0.4 4
1
0.5
0.2 2
0.5
0 0 0 0
H20 N2 H20 N2 H20 N2 H20 N2
Compound Com pound Com pound Com pound
3.5 3.5 6 12
3 3
5 10
2.5 2.5
4 8
2 2
3 6
1.5 1.5
2 4
1 1
1 2
0.5 0.5
0 0 0 0
39 40 41 39 40 41 39 40 41 39 40 41
It should be noted that depending upon the instrument under investigation and the resolution
at which it is operating the actual appearance would vary. If the resolution in a sector field
instrument is greater than about 2000 Resolving Power then at mass 40, two distinct peaks
will be observed, that of Argon at lower mass and a higher mass "background" peak. At lower
resolutions a single poorly shaped peak will be observed. Similarly at mass 28 Da, with
increasing resolving power more substances may be separated out from the Nitrogen peak.
At 10,000 resolution one typically may distinguish 4 to 5 separate peaks depending upon
instrument usage.
Leak finding:
If a leak in the source is suspected by monitoring either, or both, of the tests described above
it must be localised and corrected. Should a GC column be fitted then there will be a large
flow of generally Helium present in the source preventing it’s use when leak checking unless
the column is removed. To find very small leaks however this must be done but to check the
complete system including the GC we should arrange a controllable supply of Argon. This is
often present in the lab but if not, a small bottle, regulator and a length of preferably plastic
tubing terminated in an “Eppendorf” pipette tip will be required. A small gas flow is best for
accurate location: by dipping the tip/tube end into a small solvent (Ethanol) beaker of a good
idea of the flow will be gained. Select mass 40, 39·9624 Da, on the mass spectrometer at
any standard operating resolution and set the peak display such that normalise is off, a span
such that the peak nearly fills the scope and is about ¾ of the height of the display. It is
always a good idea to check that you really are monitoring the peak of interest, the easiest
way to do this is to inject a few microlitres of Argon into the reference inlet and ensure that the
peak you are monitoring increases accordingly. This should be done initially with a somewhat
larger span and then reducing it such that the Argon peak is clearly visible. Naturally, before
testing the Argon must be fully pumped away. To check: spray around each vacuum
connection/seal with Argon for a second or two, withdraw, wait and monitor the peak intensity
on the display. On large surfaces, view-ports, lids etc. the tip should be moved all around the
sealing surfaces. If a leak is present then at a certain point an increase in the Argon signal
will be observed. An idea of the size of the leak is made with two observations: 1. by how
Valve Description
1 CI Pump-out
2 Flow regulator
3 CI Gas On/Off
Analyser Source
Reactant Gas
Bottle/Regulator
CI Line to 1 2 3
Instrument
Inlets Pump
Basic checks should, and must, be carried out each time a bottle is changed or CI is to be
operated again after a long time interval.
Setting up:
• Ensure the gas bottle is valved off at the bottle itself.
• Select CI mode on the instrument and pump out the CI line. If necessary, open the
CI regulating valve/mass flow controller “fully” too allow its evacuation.
• Monitor the Inlets line pressure. On a leak tight line the Inlets pressure should
recover to approximately that before pumping out the CI line.
• Open the output of the bottle’s regulator valve, NOT the valve on the Bottle itself to
evacuate the regulator valve. Again the Inlets pressure should return to it’s initial
pressure. Note: Some regulator valves are not capable of holding a vacuum and will
leak through the valve when evacuated. In this case close off the regulator’s output
valve.
• Close the CI Pump-out Valve and monitor the Inlets pressure. No large improvement
should be seen for a leak tight system. On systems with a mass flow controller fitted
one can monitor the flow read-back with the line closed off, evacuated and with the
flow controller set to fully open. Should a leak be present a flow read-back will be
seen.
• Again open the CI Pump-out Valve and open the CI valve to connect the CI line
through into the source. When the Inlets line recovers, close the CI Pump-out valve.
• Monitor the source high vacuum reading. It should remain at the same pressure as
when the CI Pump-out valve was open. If not, a leak is to be suspected.
The complete CI line from the bottle/regulator connection to the ion source can be leak
checked when the system is in operate mode, set to monitor Argon or Helium, masses
40 Da or 4 Da respectively. Even though the instrument is in CI mode, possibly with a
dedicated CI source fitted, Argon or Helium may be monitored under EI conditions: until
we actually fill the CI source with reactant gas the ionisation processes present in fact EI.
Tuning is as normal, either start tuning on mass 28, 40, 2 or 4 Da depending upon signal
levels, set an emission current at 70eV Electron Energy of about 1000uA to ensure that a
reasonable electron beam passes through the inner source and then tune as normal. For
2.5 3.5
2.5
1.5
1
1.5
0.5 1
0.5
0
H20 N2
Compound 0
39 40 41
The following two displays show the same substances but when a major leak is present:
12
12
10 10
8 8
6
6
4
4
0
H20 N2
0
Com pound 39 40 41
Quick Tests.
Are the intensities of “air” peaks affected by the state of the GC’s injector purge valves:
Yes Leak in or before the injector including the column connection to the injector.
No Leak not associated with the Injector system /column connection.
Do the air levels/ratios improve when the Reference Gas is valved off:
Trapped air/Leaking Septum/Leak in the Reference gas system. Pump out try
again/investigate further
None of the above:
Leak associated with the remaining system requiring further investigation.
How strong a response / quickly does it return to initial conditions is observed:
Large signal quick to return to the initial level. Big Leak
Weak signal slow to return to the initial level. Small Leak
Useful Substances / Masses.
Hydrogen H2 2 Da 2·0157 Da
Helium He 4 Da 4·0026 Da
Water H2O 18 Da 18·0106 Da
Nitrogen N2 28 Da 28·0061 Da
Argon Ar 40 Da 39·9624 Da