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9
blesome compounds at 0.5 ng on column relative
to the method minimum, the average RF for the
calibration range (0.5-120 ng on-column), and lin-
earity evaluated by RRF RSD and linear regression.
Calibrations were also assessed for the full list
of compounds. For the initial calibration (ICAL)
as a whole to meet acceptance criteria, less
than 10% of the individual compounds may
have failing RSDs (or correlations, if alterna-
tive fit methods are used). When the peak
response RSDs were evaluated over the entire
calibration range for the full list of compounds,
the average RSD was 8.7% and only 10 of the
compounds tested had RSDs greater than
20%. Linearity results for both indicator and
non-indicator compounds demonstrate that
detection limits can be lowered for semivola-
tiles analysis by using a highly inert system that
allows the lower end of the calibration range to
be extended.
Figure 1: Extend the calibration range for difficult semivolatiles down to 0.5 ng on-column by using a highly inert analytical system.
(total ion chromatogram of EPA Method 8270 and Appendix IX compounds)
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Restek Recommends
For ultimate sample path inertness:
EZ Twist Top® Injection Port
Sky™ Inlet Liners
Flip Seal™ Inlet Seals
Rxi®-5Sil MS Columns
Figure 2: Response differential for
2,4-dinitrophenol and 4-nitrophenol.
1. 2,4-Dinitrophenol (m/z 184)
2. 4-Nitrophenol (m/z 139)
See Figure 1 for analytical conditions.
45,46
4.60 4.80 5.00 5.20 5.40 5.60 5.80 6.00 6.20 6.40 6.60 6.80 7.00 7.20 7.40 7.60 7.80 8.00 8.20 8.40 8.60 8.80 9.00 9.20 9.40
12
13,14
15
16,17
18
19
20,21
22 2324
25
26,27,28
29,30,31
32
33
34,35
36
37
38
39
40
41
42,43
44 47,48
49
50
51
52,53 5455
56
57
58,59
60
61 62
63
64
65
66
67
69
70
71
72
73
74
75
76
77
78,79
80
81
82 83,8485,86
87
8889
90,91
92,93
94
95
96
97
98
99,100
101
102103
104
105
106
107
108,109
110
111
68
4.40
1,2
3
4 5
6
7 8
9
10 11
112
113
114
115
116
117
118,119 121
120 122
123
124
125,126
127,128
129
131
131,132,133
134
135
136,137
138
139
140
141
142
143144 145
2.50 3.00 3.50 4.00 4.50 5.00 5.50 6.00 6.50 7.50 8.00 8.50 9.00 9.50 10.00 10.50 11.00 11.50 12.00 12.50 13.00 13.50 14.00 14.50 15.00 15.50 16.00 16.50 17.00 7.00
EIC:
12 = m/z 106
15,16 = m/z 93
EIC: m/z 162 EIC: m/z 232
EIC:m/z 106
EIC:
143 = m/z 276
144 = m/z 278
Time (min)
4.60 4.40 4.80
12
15
16
14.00
137 138
16.50
143 144
7.20
66
67
7.25
8.05 8.10
87
86
GC_EV1269
Column: Rxi®-5Sil MS, 30 m, 0.25 mm ID, 0.25 µm (cat.# 13623); Sample: 8270 MegaMix® (cat.# 31850), 8270 Benzidines mix (cat.# 31852), Benzoic acid (cat.# 31879), Revised B/N surrogate mix (cat.# 31888), Acid sur-
rogate mix (4/89 SOW) (cat.# 31063), Revised SV internal standard mix (cat.# 31886), Appendix IX mix #1 (cat.# 31625), Appendix IX mix #2 (cat.# 31806); Diluent: Dichloromethane; Conc.: 0.5 µg/mL (IS/SS 20 μg/mL);
Injection:1 µL pulsed splitless (hold 0.59 min); Liner: Sky™4 mm single taper w/wool (cat.# 23303); Inj. Temp.: 270 °C; Pulse Pressure: 30 psi (206.8kPa); Pulse Time: 0.64 min; Purge Flow: 100 mL/min;Oven: 40 °C (hold 1
min) to 280 °C at 25 °C/min to 320 °C at 5 °C/min (hold 1 min); CarrierGas: He, constant flow; Flow Rate: 1.2 mL/min;Detector: MS; Mode: Scan; Transfer Line Temp.: 280 °C; Analyzer Type: Quadrupole; Source Temp.: 276 °C;
Quad Temp.: 150 °C; Electron Energy: 70 eV; Solvent Delay Time: 2.19 min; Tune Type: DFTPP; Ionization Mode: EI; Scan Range: 35-550 amu; Scan Rate: 5.36 scans/sec;Instrument: Agilent 7890A GC & 5975C MSD; Notes:
7890 Siltek®-treated EZ Twist Top® split/splitless injection port (cat.# 22178), Flip Seal™ dual Vespel® ring inlet seal (cat.# 23411); For peak identifications, visit and enter GC_EV1269 in the search.
• Quantify down to 0.5 ng on-column
• Separate key PAHs.
• Analyze 145 semivolatiles in 17 minute analysis.
For more environmental applications, visit
3
4
5
6
7
8
9
10
7.30 7.40 7.50 7.60 7.70 7.80 7.90 8.00 8.10 8.20 8.30 8.40 8.50
1
2
Time
1
2
1
2
0.5 ng
On-Column
10 ng
On-Column
2,4-DNP
RF=0.055
2,4-DNP
RF=0.19