environmental
Applications
note
Restek Corporation • (800) 356-1688 • (814) 353-1300 •
#59343
environmental
Fast Analysis of Dioxin andRelatedCompoundsUsing anRtx
®
-5MS Column
Dioxin and furan testing can be very time consuming and cost-
ly. Total analyses times can easily exceed one hour per sample,
and instrument time on high-resolutionmass spectrometers
(MS) is quite valuable. In addition, many samples analyzed for
dioxins and furans require analysis for polychlorinated
biphenyls (PCBs) aswell. Researchers at theOntarioMinistry
of the Environment (MOE) andRestek have recently developed
amethod formore rapid dioxin, furan, and PCB analysis.
Historically, chlorinated dioxins and furans have been analyzed
by gas chromatography (GC) separately fromPCBs. In 1998,
theWorldHealthOrganization (WHO) reported toxic equiva-
lent factors (TEFs) for the 12 dioxin-like PCB congeners.
1
This
enabled concentrations of PCBs to be expressed in terms of
2,3,7,8-TCDD, themost toxic form of dioxin. Using similar
methods to analyze dioxins and PCBs allows detection limits
up to three orders ofmagnitude lower than that of conventional
PCB congenermethods. The toxicity of a single sample now
can be reported in toxic equivalents of 2,3,7,8,-TCDD (i.e.,
toxic equivalent quantities [TEQ]) by summing the toxic equiv-
alents of each of the 17 toxic dioxin congeners and 12 dioxin-
like PCB congeners.
Extractswere prepared according toCanada’sMOEMethod
3418, which is similar to the combination of USEnvironmental
ProtectionAgency (EPA)Methods 1613 and 1668. The extracts
are further cleaned using activated carbon.
2
This allows for the
collection of two sample extract fractions: one containing the
dioxins, furans, and coplanar PCBs; and the other containing the
remaining PCBs, chlorinated and brominated diphenyl ethers,
and other non-planar organic compounds. The chlorinated
diphenyl ethers interferewith the furans and, therefore, they
need to be analyzed separately. Normally, dioxins and furans,
and PCBs (congeners) are analyzed separately on a 60m analyti-
cal column usingGC/high resolutionmass spectrometry
(GC/HRMS) with analysis times of 50 to 90minutes each.
Figure 1
The Rtx
fi
-5MS column and a combined system can separate dioxin-like PCBs and dioxins/furans within 30minutes.
Inj. temp.:
280°C;
Carrier gas:
helium;
Det.:
Agilent
6890GC coupled to aMicromass Ultima HRMS
@10,000RP.
20m, 0.1mm ID, 0.1µmRtx
®
-5MS (custom cat.#
58136).
Column head pressure:
100psi;
Oven
program:
100°C (hold 1min.) to 200°C@ 100°C/min,
to 235°C@ 13°C/min., to 300°C@ 27°C/min. (hold 4
min.);
Inj. volume:
0.2mL
40m, 0.18mm ID, 0.18µmRtx
®
-5MS (custom cat.#
550590).
Column head pressure:
61psi;
Oven
program:
100°C (hold 0.62min.) to 200°C@
64.5°C/min, to 235°C@ 4.8°C/min. (hold 6.2min.),
to 300°C@ 9.7°C/min.( hold 5.6min.);
Inj. volume:
1.0mL
GC_EV00392
