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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)
Candidates for 2016 Method of the Year
244