Agilent7890A气相色谱仪FPD检测器性能测试(精)

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 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