restekadv07 - page 77

Figure 1
The Rtx
®
-200 column provides unique
separation of the VOCs listed in
USEPAMethod 8260.
• 4 •
Xylenes are aromatic hydrocarbons that naturally
occur in petroleum and coal tar; they also can be
commercially derived from these substrates. The US
Environmental Protection Agency (EPA) does not
require separation of the three xylene isomers(
m-
,
p-
,
o-
xylene), but rather requests their calculation
as totals or sums.
1
Some states, such as New York,
have action limits based on
m
- and
p
-xylene sepa-
rately. However, the isomers of
m
- and
p
-xylene are
difficult to resolve using gas chromatography (GC)
andmost capillary columns.
Separating
m-
and
p-
Xylene Isomers
Using anRtx
®
-200GCColumn
by Christopher English, Environmental Innovations Chemist
The commonway to perform a GC separation of
m
- and
p
-xylene is by using a polyethylene glycol
(PEG) stationary phase, such as the Restek
Stabilwax
®
column. Chromatographically, baseline
separation is possible with this column; however,
the highly polar phase does not separatemany of
the other volatile organic compounds (VOCs).
Themore ideal column choice for this separation is
the Rtx
®
-200 column. The Crossbond
®
trifluoro-
propylmethyl polysiloxane (TFP) stationary phase
features exceptionally low bleed at operating tem-
peratures up to 360°C.
The Rtx
®
-200 column provides unique separation
of VOCs listed in US EPAMethods 524 and 8260
(Figure 1), and is the best column to separate
xylene isomers for specific state requirements
(Figure 2). The only limitation of this column is the
resolution of the gases.
Trifluoropropyl stationary phases, like that of the
Rtx
®
-200 column, have a unique selectivity because
of the electrophilic nature of the fluorine-contain-
ing polymer. This creates interactions with electron-
richmolecules like ketones and halogenated com-
pounds. The unique selectivity results in different
elution orders and resolves compounds that phenyl,
cyano, andmethyl phases cannot. The Rtx
®
-200
column can be used to confirm tentatively identified
compounds and resolvemultiple coelutions, mak-
ing it ideal for requirements such as those dictated
by New York State.
1. Toxicologicological Profile for Total Xylenes. Prepared by
Clements Associates, Inc., under Contract No. 205-88-0608.
Prepared for Agency of Toxic Substances andDisease Registry,
US Public Health Services, Atlanta, GA. December 1990.
Reference not available fromRestek.
57
58
59
60
61
62
63,64
67
68
57. 1,3-dichloropropane
58. ethyl methacrylate
59. bromoform
60. 1,1,1,2-tetrachloroethane
61. ethylbenzene
62. 4-methyl-2-penanone
63. chlorobenzene
64. chlorobenzene-D5
65.
m
-xylene
66. 2-picoline (250ppb)
67.
p
-xylene
68.
n
-butyl acetate
69.
o-
xylene
Conditions for Figures 1& 2
60m, 0.25mm ID, 1.0µmRtx
®
-200 (cat.# 15056)
10ppb each component in 5mL of ROwater;
Concentrator:
Tekmar LSC-3100 Purge and Trap;
Trap:
Vocarb
®
3000 (type K);
Purge:
11min. @
40mL/min. @ ambient temperature;
Dry purge:
1min. @ 40mL/min.;
Desorb preheat:
245°C;
Desorb:
250°C for 2min., flow 10mL/min.;
Bake:
260°C for 8min.;
Interface:
transfer line
0.53mm IDSilcosteel
®
MXT
®
tubing;
Oven program:
40°C (hold 10min.) to 100°C@ 6°C/min. (hold 1
min.) to 210°C@ 30°C/min. (hold 7min.);
Carrier
gas:
helium@ ~1.3mL/min. constant flow (adjust
dichlorodifluoromethane to a retention time of 4.1
min. @ 40°C);
Detector:
Agilent 5973MS, scan
range 35 to 300 AMU
65,66
m-
xylene
p-
xylene
Ions 91 and 106
(peaks 65, 67, 69, Figure 1)
Ion 91
Ion 106
o-
xylene
Figure 2
An extracted ion chromatogram shows the Rtx
®
-200 column separates
m/p
-xylene isomers.
Innovations atWork
Separatem/p-xylene isomers!
Rtx
®
-200Columns
(Crossbond
®
trifluoropropylmethyl polysiloxane) Stable to 360°C
For the complete Rtx
®
-200 column offering, refer toRestek’s
Annual Chromatography Products Guide
(lit. cat.# 59960).
Rtx
®
-200 (Fused Silica Tubing)
ID df (µm)
temp. limits
15-Meter
30-Meter
60-Meter
105-Meter
0.25mm 1.00 -20 to 290/310°C 15050
15053
15056
15059
MXT
®
-200 (MXT
®
Tubing)
ID df (µm)
temp. limits
15-Meter
30-Meter
0.25mm 1.00
-20 to 310°C
75050
75053
for
more
info
Request Applications Note #59190.
69
22
20
min.
GC_EV00381
GC_EV00380
Unique separation of VOCs
satisfy state requirements
Low bleed at high operating
temperatures (stable to 360°C)
An extensive selection of
analytical referencematerials
for USEPA
Method 8260B is available fromRestek. Please see page 16 of this
newsletter or visit our web site at
for ordering
information.
22.00
21.80
22.40
22.20
22.80
22.60
23.00
min.
1...,67,68,69,70,71,72,73,74,75,76 78,79,80,81,82,83,84,85,86,87,...297
Powered by FlippingBook