Chromatographic Checkout : To Verify FPD Performance (Sample 5188-5245To Verify FPD Performance (Sample 5188-5245To verify FPD performance, first check the phosphorus performance, then the sulfur performance.PreparationPhosphorus performance1 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 injectorposition.3 Verify the lit offset is set appropriately. Typically, it should be about 2.0 pA for thecheckout 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 ConditionsColumn and sampleType DB-5MS, 15 m × 0.32 mm × 1.0 µm (123-5513Sample FPD checkout (5188-5245Column mode Constant flowColumn flow 7.5 mL/minSplit/splitless inletTemperature 250 °CModeSplitless Total purge flow69.5 mL/min Purge flow 60 mL/min页码，1/5To Verify FPD Performance (Sample 5188-5245 Purge time 0.75 minSeptum purge 3 mL/minPacked column inletTemperature 250 °CSeptum purge 3 mL/minCool on-column inletTemperature Oven trackSeptum purge 15 mL/minPTV inletMode SplitlessInlet temperature 80 °CInitial time 0.1 minRate 1 720 °C/minFinal temp 1 350 °CFinal time 1 2 minRate 2 100 °C/minFinal temp 2 250 °CFinal time 2 0 minPurge time 0.75 minPurge flow 60 mL/minSeptum purge 3 mL/minDetectorTemperature 200 °C (On Hydrogen flow 75.0 mL/min (OnAir (oxidizer flow 100.0 mL/min (On Mode Constant makeup flow Off Makeup flow 60.0 mL/min (On Makeup gas type NitrogenFlame OnLit offset Typically 2 pA Electrometer OnOvenInitial temp 70 °CInitial time 0 minRate 1 10 °C/minFinal temp 105 °CFinal time 0 minRate 2 20 °C/minFinal temp 2 190 °CFinal time 2 7.25 min for sulfur 12.25 min for phosphorus ALS settings (if installed Sample washes 2Sample pumps 6Injection volume 1 µL Syringe size 10 µLPreInj Solvent A Washes 2 PreInj Solvent B Washes 0 PostInj Solvent A Washes 2 PostInj Solvent B Washes 0 Viscosity delay 0Plunger speed FastPreInjection dwell 0PostInjection dwell 0Manual injection页码，2/5To Verify FPD Performance (Sample 5188-5245If the baseline output is too high:If the baseline output is zero, verify the electrometer is on and the flame is lit.If performing an injection using an autosampler, start the run using the data systemor press [Start] on the GC.If performing a manual injection (with or without a data system:Sulfur performanceInjection volume1 µL Data SystemData rate 5 Hz7 Ignite the FPD flame, if not lit.8 Display the signal output and monitor. This output typically runs between 40 and 55 but can be as high as 70. Wait for the output to level off. This takes approximately 1 hour.• Check column installation. If instal led high, the stationery phase burns out and increases measured output.• Check for leaks.• Bake out the detector and column at 250 °C.• Wrong flows set for installed filter9 If using a data system, prepare the data system to perform one run using the loaded checkout method. Make sure that the data system will output a chromatogram.10 Start the run.a Press [Prep Run] to prepare the inlet for splitless injection.b When the GC becomes ready, inject 1 µL of the checkout sample and press[Start] on the GC.11The following chromatogram shows typical results for a new detector with new consumable parts installed.12 Install the.13 Make the following method parameter changes.If the baseline output is too high:If the baseline output is zero, verify the electrometer is on and the flame is lit.If performing an injection using an autosampler, start the run using the data system or press [Start] on the GC.If performing a manual injection (with or without a data system:Table 16 Sulfur method parameters ParameterValue ( mL/min H 2flow50 Air flow 6014 Ignite the FPD flame, if not lit.15 Display the signal output and monitor. This output typically runs between 50 and 60 but can be as high as 70. Wait for the output to level off. This takes approximately 2 hours.• Check column installation. If installed high, the stationery phase burns out and increases measured output.• Check for leaks.• Bake out the detector and column at 250 °C.• Wrong flows set for installed filter16 If using a data system, prepare the data system to perform one run using the loaded checkout method. Make sure the data system will output a chromatogram.17 Start the run.a Press [Prep Run] to prepare the inlet for splitless injection.b When the GC becomes ready, inject 1 µL of the checkout sample and press[Start] on the GC.18 The following chromatogram shows typical results for a new detector with newconsumable parts installed.© 2007 Agilent Technologies, Inc. 04.11.2007页码，5/5To Verify FPD Performance (Sample 5188-5245。