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, install 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 SS , PP , COC , or PTV 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 SS , PP , COC , or PTV in the Maintenance manual.)
• Configure the column.
5 If it is not already installed, install the phosphorus filter .
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
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
track Temperature Oven
Septum purge 15 mL/min
PTV inlet
Mode Splitless Inlet temperature 80 °C
Initial time 0.1 min
Rate 1 720 °C/min
Final temp 1 350 °C
Final time 1 2 min
Rate 2 100 °C/min
Final temp 2 250 °C
Final time 2 0 min
Purge time 0.75 min
Purge flow 60 mL/min
Septum purge 3 mL/min
Detector Temperature 200
°C (On)
Hydrogen flow 75.0 mL/min (On)
Air (oxidizer) flow 100.0 mL/min (On)
Mode Constant makeup flow Off Makeup flow 60.0 mL/min (On)
Makeup gas type Nitrogen
Flame On
Lit offset Typically 2 pA
Electrometer On
Oven
Initial temp 70 °C
Initial time 0 min
Rate 1 10 °C/min
Final temp 105 °C
Final time 0 min
Rate 2 20 °C/min
Final temp 2 190 °C
Final time 2 7.25 min for sulfur
12.25 min for phosphorus
ALS settings (if installed)
Sample washes 2
Sample pumps 6
Injection volume 1 µL
Syringe size 10 µL
PreInj Solvent A Washes 2
PreInj Solvent B Washes 0
PostInj Solvent A Washes 2
PostInj Solvent B Washes 0
Viscosity delay 0
Plunger speed Fast
PreInjection dwell 0
PostInjection dwell 0
Manual injection
