203 / 413
Results
These run conditions produced excellent resolution and response for all of the target analytes in a run time of less than 16 minutes.
Figure 1 shows the SIM trace at 0.005µg/mL (5pg on column). The system was calibrated at eight levels, from 0.005 to 10µg/mL in
single ion monitoring mode. The SIM acquisition program used for this analysis is shown in Figure 1. Each calibration standard con-
tained eighteen target PAHs, two internal standards (
p
-terphenyl-d14 and perylene-d12), and the surrogate (2-fluorobiphenyl). At
each level, the relative response factor (RRF) was calculated for all compounds and linearity was determined by calculating the percent
relative standard deviation (%RSD) for all response factors, as shown in Table II. The %RSDs for all compounds are in the low single
digits with an average for all compounds of 4.7%.
The Rxi®-5Sil MS column allows for a very broad calibration range, in this case 2000-fold from 5pg to 10ng while maintaining exceptional
linearity. Using the Rxi®-5Sil MS column and an optimized temperature program is an excellent solution to the challenges posed by
SIM PAH analyses.
•
5
•
2008 vol. 1
Environmental
Rxi®-5Sil MS Columns (fused silica)
(Crossbond
®
, selectivity close to 5% diphenyl/95% dimethyl
polysiloxane)
ID df (µm)
temp. limits
length cat. #
price
0.25mm 0.25 -60 to 330/350°C 30-Meter 13623
acenaphthene
acenaphthylene
anthracene
benzo(a)anthracene
benzo(a)pyrene
benzo(b)fluoranthene
benzo(k)fluoranthene
benzo(ghi)perylene
chrysene
dibenzo(a,h)anthracene
fluoranthene
fluorene
indeno(1,2,3-cd)pyrene
naphthalene
phenanthrene
pyrene
SV Calibration Mix #5 / 610 PAH Mix
(16 components)
2,000µg/mL each in methylene chloride, 1mL/ampul
cat. # 31011
1-Methylnaphthalene
1,000µg/mL in methanol, 1mL/ampul
cat. # 31283
2-Methylnaphthalene
1,000µg/mL in methylene chloride, 1mL/ampul
cat. # 31285
2-Fluorobiphenyl
2,000µg/mL in methylene chloride, 1mL/ampul
cat. # 31091
(ea.)
Relative Response Factor
Compound
0.005
0.01
0.05
0.1
0.5
1
5
10
Avg
%RSD
p
-Terphenyl-d14 (IS)
-
-
-
-
-
-
-
-
-
-
Naphthalene
0.825
0.778
0.822
0.785
0.760
0.774
0.771
0.721
0.779
4.28
2-Methylnaphthalene
0.539
0.518
0.556
0.525
0.512
0.524
0.521
0.495
0.524
3.42
1-Methylnaphthalene
0.503
0.478
0.518
0.483
0.470
0.481
0.476
0.455
0.483
4.05
2-Fluorobiphenyl (SS)
0.689
0.664
0.691
0.680
0.664
0.679
0.669
0.608
0.668
3.93
Acenaphthylene
0.879
0.838
0.917
0.887
0.868
0.899
0.904
0.856
0.881
3.00
Acenaphthene
0.541
0.508
0.544
0.522
0.508
0.522
0.514
0.482
0.518
3.80
Fluorene
0.700
0.662
0.709
0.677
0.659
0.679
0.668
0.627
0.673
3.80
Phenanthrene
1.108
1.049
1.119
1.068
1.028
1.050
1.022
0.953
1.050
4.97
Anthracene
1.052
0.962
1.043
1.003
0.981
1.013
0.993
0.921
0.996
4.27
Fluoranthene
1.239
1.161
1.254
1.206
1.166
1.195
1.171
1.093
1.185
4.25
Pyrene
1.364
1.254
1.355
1.295
1.256
1.284
1.247
1.155
1.276
5.20
Perylene-d12 (IS)
-
-
-
-
-
-
-
-
-
-
Benzo(a)anthracene
1.111
0.980
1.086
1.054
1.048
1.087
1.090
1.017
1.059
4.12
Chrysene
1.153
1.041
1.116
1.073
1.057
1.078
1.043
0.951
1.064
5.59
Benzo(b)fluoranthene
1.282
1.039
1.183
1.146
1.139
1.185
1.204
1.144
1.165
5.92
Benzo(k)fluoranthene
1.327
1.119
1.223
1.189
1.183
1.229
1.225
1.136
1.204
5.35
Benzo(a)pyrene
1.037
0.967
1.146
1.083
1.038
1.089
1.134
1.080
1.072
5.36
Indeno(1,2,3-cd)pyrene
1.457
1.224
1.379
1.366
1.333
1.387
1.471
1.424
1.380
5.69
Dibenzo(a,h)anthracene 1.195
1.027
1.150
1.180
1.094
1.164
1.233
1.173
1.152
5.56
Benzo(ghi)perylene
1.331
1.118
1.238
1.263
1.140
1.192
1.244
1.190
1.215
5.68
Table I
Relative response factors and %RSD for calibration standards (0.005-10μg/mL).
Direct Injection Liners for Agilent GCs
(For 0.25/0.32/0.53mm ID Columns)
ID* x OD & Length (mm)
qty.
cat.#
price
Drilled Uniliner
®
(hole near top)
4.0 ID x 6.3 OD x 78.5
ea.
21054
4.0 ID x 6.3 OD x 78.5
5-pk.
21055
4.0 ID x 6.3 OD x 78.5
25-pk.
20998
Drilled Uniliner
®
(hole near top) w/ Wool
4.0 ID x 6.3 OD x 78.5
ea.
21054-200.1
4.0 ID x 6.3 OD x 78.5
5-pk.
21055-200.5
4.0 ID x 6.3 OD x 78.5
25-pk.
20998-214.25
*Nominal ID at syringe needle expulsion point.