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Chromatographic Checkout : To Verify FPD Performance (Sample 5188-5245
To Verify FPD Performance (Sample 5188-5245
To verify FPD performance, first check the phosphorus performance, then the sulfur performance.
Preparation
Phosphorus performance
1 Gather the following:
? Evaluation column, DB5 15 m × 0.32 mm × 1.0 μm (123-5513
? FPD performance evaluation (checkout sample (5188-5245
? Phosphorus filter
? Sulfur filter and filter spacer
? 4-mL solvent and waste bottles or equivalent for autoinjector.
? 2-mL sample vials or equivalent for sample.
? Chromatographic-grade isooctane for syringe wash solvent.
2 Verify the following:
? Capillary column adapter installed. If not, it.
? Chromatographic-grade gases plumbed and configured: helium as carrier gas,
nitrogen, hydrogen, and air.
? Empty waste vials loaded in sample turret.
? 4-mL vial with diffusion cap filled with isooctane and inserted in Solvent A injector
position.
3 Verify the lit offset is set appropriately. Typically, it should be about 2.0 pA for the
checkout method.
4 Install the evaluation column. (See the procedure for the , , , or in the Maintenance manual.
? Set the oven, inlet, and detector to 250 °C and bake out for at least 15 minutes.
(See the procedure for the , , , or in the Maintenance manual.
? Configure the column.
5 If it is not already installed, install the.
6 Create or load a method with the parameter values listed in Table 15.
Table 15 FPD Phosphorus Checkout Conditions
Column and sample
Type DB-5MS, 15 m × 0.32 mm × 1.0 μm (123-
5513
Sample FPD checkout (5188-5245
Column mode Constant flow
Column flow 7.5 mL/min
Split/splitless inlet
Temperature 250 °C
Mode
Splitless Total purge flow
69.5 mL/min Purge flow 60 mL/min
页码,1/5To Verify FPD Performance (Sample 5188-5245
Purge time 0.75 min
Septum purge 3 mL/min
Packed column inlet
Temperature 250 °C
Septum purge 3 mL/min
Cool on-column inlet
Temperature Oven track
Septum purge 15 mL/min
PTV inlet
Mode Splitless
Inlet temperature 80 °C
Initial
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