17 Chromatographic Checkout
262 Operation Manual
To Check FPD+ Performance (Sample 5188-5245,
Japan)
To verify FPD+ performance, first check the phosphorus performance, then the sulfur
performance.
Preparation
1 Gather the following:
• Evaluation column, DB5 15 m × 0.32 mm × 1.0 µm (123-5513)
• FPD performance evaluation (checkout) sample (5188-5245, Japan), composition:
n-Dodecane 7499 mg/L ( 5%), Dodecanethiol 2.0 mg/L ( 5%), Tributyl Phosphate
2.0 mg/L ( 5%), tert-Butyldisulfide 1.0 mg/L ( 5%), in isooctane as solvent
• 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.
• Inlet and injector hardware See “To Prepare for Chromatographic Checkout.”
2 Verify the following:
• 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 Replace consumable parts (liner, septum, traps, syringe, and so forth) as needed for the
checkout. See “To Prepare for Chromatographic Checkout.”
4 Verify the lit offset is set appropriately. Typically, it should be about 2.0 pA for the checkout
method.
5 Install the evaluation column.
• Set the oven, inlet, and detector to 250 °C and bake out for at least 15 minutes.
6 Configure the column.
Phosphorus performance
1 If it is not already installed, install the phosphorus filter.
2 Create or load a method with the parameter values listed in Table 47.
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