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M

astovska

et al

.:

J

ournal of

AOAC I

nternational

V

ol

.

98, N

o

. 2, 2015 

489

Table 2014.08G. GC conditions used by collaborative study participants

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)

He flow/pressure program

1.2 mL/min (constant flow)

1.3 mL/min (constant flow)

1.3 mL/min (constant flow)

1.3 mL/min (15 min),

50 mL/min

2

to 2 mL/min

2 mL/min (constant flow)

Injection mode

PTV solvent split

PTV solvent vent

Pulsed splitless

PTV solvent vent (stop flow)

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 Gerstel, CIS4 deactivated baffled

liner, 2 mm id

Restek, single-gooseneck splitless,

4 mm id

Gerstel, CIS4 deactivated

baffled liner, 2 mm id

Agilent, dimpled deactivated,

2 mm id

PTV solvent vent time

0.1 min

138 s

NA

0.5 min

0.1 min

PTV solvent vent flow, mL/min

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

Split vent purge flow and start

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

Gas saver flow and start time

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)