Troubleshooting Contamination Problems; Ensure Clean Gas Supplies; Isolate Problem To Carrier Or Makeup Gas Supplies - Agilent Technologies 6890 Series Service Manual

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Electron Capture Detector (ECD)

Troubleshooting contamination problems

Troubleshooting contamination problems
Persistent problems with high background or ghost peaks with temperature
programming are almost always due to contamination from dirty samples,
consumables, or the carrier/makeup gas systems.
Begin with the procedure in chapter 5, Volume 3, of the Operating Manual. If
this procedure, which can be performed by the user, does not solve the
problem, perform the following steps.

Ensure clean gas supplies

Before continuing, verify that the supply gases are of adequate purity.
1.
Carrier and makeup purity must be >99.999%.
2.
After confirming purity, verify that the tank regulators have stainless
steel diaphragms (equivalent to Agilent part no. 8507-0407).
3.
Install new 1/8-inch copper supply tubing—part no. 5180-4196. Many
times "clean" tubing from other sources has caused high ECD background.
At the same time, install new traps in both the carrier and makeup
supplies. Place the moisture trap (part no. 5060-9084) closest to the tank
and the indicating oxygen trap (part no. 3150-0528) closest to the GC.
Leak test the entire plumbing setup very carefully.

Isolate problem to carrier or makeup gas supplies

Determine what components of the apparent contamination are from the
carrier vs. makeup systems in the GC. Sharp, well-resolved peaks that elute
during a temperature program with no injection are from the carrier/inlet
system. Broader "humps" in the baseline are usually from the makeup system.
Overall high background (>500 Hz) can be contaminated gas from either the
carrier or makeup supply or a contaminated detector cell.
Remove the column from the detector and inspect the installation of the
makeup gas adapter. It is quite common for the adapter to be installed too
low. To check this, measure from the bottom of the 1/4-inch Swagelok nut to
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Detectors
Agilent 6890 Gas Chromatograph Service Manual
Jun 2001

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