17 Chromatographic Checkout
252 Operation Manual
To Check ECD Performance
1 Gather the following:
• Evaluation column, HP-5 30 m × 0.32 mm × 0.25 µm (19091J-413)
• ECD performance evaluation (checkout) sample (18713–60040, Japan: 5183-0379)
• 4-mL solvent and waste bottles or equivalent for autoinjector.
• Chromatographic-grade isooctane
• 2-mL sample vials or equivalent for sample.
• Inlet and injector hardware See “To Prepare for Chromatographic Checkout.”
2 Verify the following:
• Clean fused silica indented mixing liner installed. If not, install it.
• Chromatographic-grade gases plumbed and configured: helium for carrier gas, nitrogen
for makeup.
• Empty waste vials loaded in sample turret.
• 4-mL vial with diffusion cap filled with hexane and inserted in Solvent A injector position.
3 Replace consumable parts (liner, septum, traps, syringe, and so forth) as needed for the
checkout. See “To Prepare for Chromatographic Checkout.”
4 Install the evaluation column.
• Bake out the evaluation column for at least 30 minutes at 180 °C.
• Be sure to configure the column.
5 Display the signal output to determine baseline output. A stable baseline output at any
value between 0.5 and 1000 Hz (OpenLAB CDS ChemStation Edition display units)
(inclusive) is acceptable.
• If the baseline output is < 0.5 Hz, verify that the electrometer is on. If the offset is still
< 0.5 Hz, your detector requires service.
• If the baseline output is > 1000 Hz, there may be chemical contamination contributing to
the signal. Bakeout the ECD. If repeated cleanings do not give an acceptable signal,
check gas purity. Use higher purity gases and/or install traps.
6 Create or load a method with the parameter values listed in Table 45.
Table 45 ECD Checkout Conditions
Column and sample
Type HP-5, 30 m × 0.32 mm × 0.25 µm
(19091J-413)
Sample ECD checkout (18713-60040 or Japan:
5183-0379)
Column mode Constant flow
Column flow 6.5 mL/min (helium)
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