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• 10 •

800-356-1688 •

www.restek.com

2005 vol. 1

High Resolution GC/MS Separations of

Dioxin or Furan Congeners

Using an Rtx

®

-Dioxin2 Column

by Gary Stidsen, GC Columns Marketing Manager

•Resolves all 2,3,7,8-substituted dioxinsfrom each other and from non-toxic congeners.

•Resolves furan congeners from chlorodiphenyl ethers.

• Eliminates need for a second column.

• Low bleed stationary phase, stable to 320ºC.

An analysis for dioxins or furans typically

includes extensive sample extract cleanup, fol-

lowed by high-resolution mass spectrometry,

and a primary requirement of the analytical col-

umn is complete separation of the toxic dioxin or

furan congeners (substitutions in the 2, 3, 7, and

8 positions). Unfortunately, separation of the

toxic congeners from the non-toxic congeners

proves difficult on almost all stationary phases.

Quantification for some target congeners is

inaccurately high, due to coelution with non-

toxic congeners. The coelution issue has result-

ed in the use of confirmation columns, most

commonly high cyanopropyl stationary phases,

in order to more accurately quantify the toxic

congeners. Unfortunately, cyanopropyl columns

exhibit poor thermal stability, and therefore

offer poor lifetime in this application.

With these problems in mind, Restek chemists

developed the Rtx

®

-Dioxin2 capillary GC column.

This column effectively resolves the 2,3,7,8-sub-

stituted congeners from each other and from

non-toxic congeners. Figure 1 shows the sepa-

ration of the tetrachlorodibenzodioxins on a 60-

meter Rtx

®

-Dioxin2 column. 2,3,7,8-TCDD is well

resolved from the other congeners in this group

and can be quantified accurately.

Coelutions of toxic and non-toxic congeners also

can make quantification of the hexachlorodiben-

zofurans difficult, but an Rtx

®

-Dioxin2 column

resolves furan congeners as effectively as diox-

ins. Figure 2, a chromatogram for the HCDF con-

gener group in reference material WMS-01,

shows the congeners are very well resolved.

Values for 1,2,3,4,7,8-hexachlorodibenzofuran,

or for other congeners, compare favorably with

values from the other columns typically used for

this analysis.

We can provide elution orders for all of the

commonly analyzed congeners, and chro-

matograms for each congener group in the WMS-

01 reference material. If you would like this

detailed information, or additional information

about Rtx

®

-Dioxin2 columns, please contact us.

Rtx

®

-Dioxin2 Columns (fused silica)

ID

df (µm)

temp. limits

40-Meter

60-Meter

0.18mm

0.18

20°C to 320°C

10759

$650

0.25mm

0.25

20°C to 320°C

10758

$750

Figure 1

2,3,7,8-Tetrachlorodibenzodioxin resolved from other TCDD congeners,

using an Rtx®-Dioxin2 column.

Column and Conditions for

Figures 1 and 2:

Column: 60m, 0.25mm ID, 0.25µm

Rtx

®

-Dioxin2 (cat.# 10758)

Oven temp.: 130°C (hold 1 min.) to

205°C @ 45°C/min. to 305°C @

6°C/min. (hold 30 min.);

Dead time: 2.89 min.; Carrier gas:

helium at 1.5mL/min., constant flow

NativeTCDDs

321.8936 m/z

1,2,3,4-TCDD-C13

2,3,7,8-TCDD-C13

C13 labels

331.9386 m/z

GC_EV00702

2,3,7,8-TCDD

Chromatograms courtesy of

Karen MacPherson and Eric

Reiner, Ontario Ministry of the

Environment, Etobicoke,

Ontario, Canada.

WMS-01 and HCDF reference

material courtesy of

Wellington Laboratories,

Guelph, Ontario, Canada.

Figure 2

Hexachlorodibenzofuran congeners resolved by an Rtx®-Dioxin2 column.

Native HCDFs

373.8207 m/z

WMS-01

C13 labels

331.9386 m/z

1,2,3,4,7,8-HCDF-C13

1,2,3,6,7,8-HCDF-C13

2,3,4,6,7,8-HCDF-C13

1,2,3,7,8,9-HCDF-C13

GC_EV00703

1,2,3,4,7,8-HCDF

1,2,3,6,7,8-HCDF

2,3,4,6,7,8-HCDF

1,2,3,7,8,9-HCDF

restek

innovation

!

Pittcon®

presentation

This information will be presented by Dr. Frank Dorman,

Oral Session 1000, Tuesday afternoon, March 1.

Plan to attend Dioxin 2005,

and visit Restek!