AOAC-RI ERP Book - FAOM METHOD.pdf

7DEOH * *& FRQGLWLRQV XVHG E\ FROODERUDWLYH VWXG\ SDUWLFLSDQWV Laboratory No. 1 2 3 4 5 GC Instrument Thermo Trace GC Ultra Agilent 6890N Agilent 6890N Agilent 6890 Agilent 7890A Inlet type PTV (Thermo 816, RP - 2004) PTV (Gerstel CIS 4) S/SL (Agilent) PTV (Gerstel CIS 4) Multi-mode (Agilent) Column type Thermo TR-50MS Restek Rxi-17Sil MS Agilent J&W DB-17MS Restek Rxi-17Sil MS Restek Rxi-17Sil MS

Column dimension 30 m × 0.25 mm id, 0.25 μm 30 m × 0.25 mm id, 0.25 μm 30 m × 0.25 mm id, 0.25 μm 30 m × 0.25 mm id, 0.25 μm 30 m × 0.25 mm id, 0.25 μm Retention gap dimension NA NA NA 2 m × 0.25 mm id, 0.25 μm NA Run time, min 40 49.97 47.17 46 39.33 Oven temperature program 60°C (1 min), 12°C/min to 210°C, 8°C/min to 340°C (10 min) 50°C (4.3 min), 30°C/min to 220°C, 2°C/min to 240°C, 5°C/min to 360°C (6 min) 80°C (1 min), 30°C/min to 220°C, 2°C/min to 270°C (1.5 min), 5°C/min to 320°C 65°C (4 min), 30°C/min to 220°C (0.5 min), 3°C/min to 320°C (5 min) 65°C (0.5 min), 15°C/min to 220°C, 4°C/min to 330°C (1 min) +H ÀRZ SUHVVXUH SURJUDP P/ PLQ FRQVWDQW ÀRZ P/ PLQ FRQVWDQW ÀRZ P/ PLQ FRQVWDQW ÀRZ 1.3 mL/min (15 min), 50 mL/min 2 to 2 mL/min P/ PLQ FRQVWDQW ÀRZ Injection mode PTV solvent split PTV solvent vent Pulsed splitless 379 VROYHQW YHQW VWRS ÀRZ PTV solvent vent Injection volume, μL 8 8 1 8 5 Inlet temperature (program) 50°C (2.3 min), 6.7°C/s to 300°C (1 min), 10°C/s to 350°C (10 min) 50°C (2.3 min), 12°C/s to 340°C 320°C 15°C (0.5 min), 12°C/min to 275°C 70°C (0.15 min), 600°C/min to 325°C (5 min) Liner Thermo, LVI Silcosteel, 2 mm id *HUVWHO &,6 GHDFWLYDWHG EDIÀHG liner, 2 mm id Restek, single-gooseneck splitless, 4 mm id Gerstel, CIS4 deactivated EDIÀHG OLQHU PP LG Agilent, dimpled deactivated, 2 mm id PTV solvent vent time 0.1 min 138 s NA 0.5 min 0.1 min 379 VROYHQW YHQW ÀRZ P/ PLQ 50 50 NA 100 50 PTV solvent vent pressure, psi NA 50 NA 1.80 5 Pressure pulse and duration NA NA 50 psi for 0.2 min NA NA 6SOLW YHQW SXUJH ÀRZ DQG VWDUW 50 mL/min, 1 min 20 mL/min 50 mL/min, 1 min 50 mL/min, 2.5 min 60 mL/min, 2.6 min *DV VDYHU ÀRZ DQG VWDUW WLPH 15 mL/min, 3 min NA 15 mL/min, 6 min 30 mL/min, 3 min NA MS transfer line temperature, °C 250 280 280 280 300 6 7 8 9 10 GC instrument Agilent 7890 Agilent 7890 Agilent 6890N Agilent 6890N Agilent 6890N Inlet type S/SL (Agilent) S/SL (Agilent) S/SL (Agilent) PTV (Apex, ProSep 800 Plus) PTV (Gerstel CIS 4) Column type Restek Rxi-17Sil MS Restek Rxi-17Sil MS Agilent J&W DB-EUPAH Phenomenex ZB-50 Agilent J&W DB-EUPAH

Column dimension 30 m × 0.25 mm id, 0.25 μm 30 m × 0.25 mm id, 0.25 μm 20 m × 0.18 mm id, 0.14 μm 30 m × 0.25 mm id, 0.25 μm 20 m × 0.18 mm id, 0.14 μm Retention gap dimension 1 m × 0.25 mm NA NA NA NA GC run time, min 46.33 41.63 31.83 48.27 36.17 Oven temperature program 65°C (0.5 min), 15°C/min to 220°C, 4°C/min to 330°C (8 min) 80 ° C (4.3 min), 30 ° C/min to 220 ° C, 2 ° C/min to 240 ° C, 5 ° C/min to 300 ° C (1 min), 30 ° C/min to 350 ° C (8 min) 80°C (1 min), 30°C/min to 130°C, 12°C/min to 240°C, 3.5°C/min to 310°C 80°C (4.6 min), 30°C/min to 130°C (5 min), 10°C/min to 260°C (15 min), 10°C/min to 320°C (3 min); Post run: 80°C (1 min) 55°C (3 min), 30°C/min to 220°C, 2°C/min to 240°C, 3°C/min to 285°C; 15°C/min to 310°C (1 min); Post run: 330°C (2 min)

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