EPA-EAD: 1613: Dioxins and Furans by HRGC/HRMS

Summary
Analytes
Revision
Data and Sites

Official Method Name

Tetra- through Octa-Chlorinated Dioxins and Furans by Isotope Dilution HRGC/HRMS

Current Revision

October 1994

Media

VARIOUS

Instrumentation

Gas Chromatography with Mass Spectrometry Detection

Method Subcategory

Organic

Method Source

EPA-EAD

Citation

EPA Method Guidance CD-ROM (includes MCAWW Methods, and most current EPA Methods)

Brief Method Summary

Samples are extracted, cleaned, and concentrated. Extracts are analyzed using high resolution gas chromatography/high resolution mass spectrometry (HRGC/HRMS). An individual CDD/CDF is identified by comparing the GC retention time and ion abundance ratio of two exact m/z's with the corresponding retention time of an authentic standard and the theoretical or acquired ion-abundance ratio of the two exact m/z's. Quantitative analysis is performed using selected ion current profile (SICP) areas.

Scope and Application

This method determines tetra- through octa-chlorinated dibenzo-p-dioxins (CDDs) and dibenzofurans (CDFs) in water, soil, sediment, sludge, tissue, and other sample matrices.

Applicable Concentration Range

Not Available.

Interferences

(A) Glassware contamination: Thoroughly clean glassware as soon as possible after use with solvent, sonication, and multiple rinses. Do not bake reusable glassware as part of routine cleaning.
(B) Reagent contamination: Use high purity reagents.
(C) Matrix interferences: Demonstrate matrix is free from interferences by running reference matrix method blanks. The natural lipid content of tissue can interfere in the analysis of tissue samples. Remove by lipid removal process.
(D) Extracted interferences: Interference from extracted non-target compounds, with retention times similar to target compounds, can be reduced by cleaning the extract.

Quality Control Requirements

The minimum requirements consist of an initial demonstration of laboratory capability, analysis of samples spiked with labeled compounds to evaluate and document data quality, and analysis of standards and blanks as tests of continued performance.

Sample Handling

Collect samples in amber glass containers. Maintain aqueous samples in the dark at 0-4^oC. If residual chlorine is present, add 80 mg sodium thiosulfate per liter of water. If sample pH is greater than 9, adjust to pH 7-9 with sulfuric acid. Maintain solid, semi-solid, oily, and mixed phase samples in the dark at <4^oC; after receipt at the laboratory, store in the dark at <-10^oC.

Maximum Holding Time

1 year (prior to extraction).

Relative Cost

$201 to $400

Sample Preparation Methods

None.

This method has 25 analytes associated with it.

Analyte	Detection Level	Bias	Precision
1,2,3,4,6,7,8-Heptachlorodibenzo-p-dioxin(35822-46-9) 1,2,3,4,6,7,8-HEPTACHLORODIBENZODIOXIN 1,2,3,4,6,7,8-Heptachlorodibenzo-p-dioxin 1,2,3,4,6,7,8-HpCDD Dibenzo[b,e][1,4]dioxin, 1,2,3,4,6,7,8-heptachloro-	50.000 pg/L	N/A	N/A
1,2,3,4,6,7,8-Heptachlorodibenzofuran(67562-39-4) 1,2,3,4,6,7,8-Heptachlorodibenzofuran 1,2,3,4,6,7,8-HpCDF	50.000 pg/L	N/A	N/A
1,2,3,4,7,8,9-Heptachlorodibenzofuran(55673-89-7) 1,2,3,4,7,8,9-Heptachlorodibenzofuran 1,2,3,4,7,8,9-HpCDF	50.000 pg/L	N/A	N/A
1,2,3,4,7,8-Hexachlorodibenzo-p-dioxin(39227-28-6) 1,2,3,4,7,8-Hexachlorodibenzo-p-dioxin 1,2,3,4,7,8-Hexachlorodibenzo[1,4]dioxin 1,2,3,4,7,8-HxCDD Dibenzo[b,e][1,4]dioxin, 1,2,3,4,7,8-hexachloro- Hexachlorodibenzo(b,e)(1,4)dioxin,1,2,3,4,7,8-	50.000 pg/L	N/A	N/A
1,2,3,4,7,8-Hexachlorodibenzofuran(70648-26-9) 1,2,3,4,7,8-Hexachlorodibenzofuran 1,2,3,4,7,8-HxCDF Dibenzofuran, 1,2,3,4,7,8-hexachloro-	50.000 pg/L	N/A	N/A
1,2,3,6,7,8-Hexachlorodibenzo-p-dioxin(57653-85-7) 1,2,3,6,7,8-Hexachlorodibenzo-p-dioxin 1,2,3,6,7,8-HxCDD	50.000 pg/L	N/A	N/A
1,2,3,6,7,8-Hexachlorodibenzofuran(57117-44-9) 1,2,3,6,7,8-Hexachlorodibenzofuran 1,2,3,6,7,8-HxCDF	50.000 pg/L	N/A	N/A
1,2,3,7,8,9-Hexachlorodibenzo-p-dioxin(19408-74-3) 1,2,3,7,8,9-Hexachlorodibenzo-p-dioxin 1,2,3,7,8,9-HxCDD Hexachlorodibenzo-p-dioxin, mixture Hexachlorodibenzo-p-dioxin,123789	50.000 pg/L	N/A	N/A
1,2,3,7,8,9-Hexachlorodibenzofuran(72918-21-9) 1,2,3,7,8,9-Hexachlorodibenzofuran 1,2,3,7,8,9-HxCDF	50.000 pg/L	N/A	N/A
1,2,3,7,8-Pentachlorodibenzo-p-dioxin(40321-76-4) 1,2,3,7,8-PeCDD 1,2,3,7,8-PeDD 1,2,3,7,8-Pentachlorodibenzo-p-dioxin 1,2,3,7,8-Pentachlorodibenzodioxin	50.000 pg/L	N/A	N/A
1,2,3,7,8-Pentachlorodibenzofuran(57117-41-6) 1,2,3,7,8-PeCDF 1,2,3,7,8-Pentachlorodibenzofuran	50.000 pg/L	N/A	N/A
2,3,4,6,7,8-Hexachlorodibenzofuran(60851-34-5) 2,3,4,6,7,8-Hexachlorodibenzofuran 2,3,4,6,7,8-HxCDF	50.000 pg/L	N/A	N/A
2,3,4,7,8-Pentachlorodibenzofuran(57117-31-4) 2,3,4,7,8-PeCDF 2,3,4,7,8-Pentachlorodibenzofuran Pentachlorodibenzofurans	50.000 pg/L	N/A	N/A
2,3,7,8-Tetrachlorodibenzo-p-dioxin(1746-01-6) 2,3,7,8-TCDD 2,3,7,8-Tetrachlorodibenzo-p-dioxin Dibenzo-p-dioxin, 2,3,7,8-tetrachloro- Dibenzo[b,e][1,4]dioxin, 2,3,7,8-tetrachloro- Dioxin Tetrachlorodibenzo-1,4-dioxin,2,3,7,8-	10.000 pg/L	N/A	N/A
2,3,7,8-Tetrachlorodibenzofuran(51207-31-9) 2,3,7,8-TCDF 2,3,7,8-Tetrachlorodibenzofuran Dibenzofuran, 2,3,7,8-tetrachloro-	10.000 pg/L	N/A	N/A
Octachlorodibenzo-p-dioxin(3268-87-9) 1,2,3,4,6,7,8,9-Octachlorodibenzo-p-dioxin Dibenzo-p-dioxin, octachloro- Dibenzo[b,e][1,4]dioxin, octachloro- OCDD Octachlorodibenzo-p-dioxin Octachlorodibenzo-p-dioxins	100.000 pg/L	N/A	N/A
Octachlorodibenzofuran(39001-02-0) Dibenzofuran, octachloro- OCDF Octachlorodibenzofuran Perchlorodibenzofuran	100.000 pg/L	N/A	N/A
Total HpCDD(37871-00-4) Total HpCDD	N/A	N/A	N/A
Total HpCDF(38998-75-3) Total HpCDF	N/A	N/A	N/A
Total HxCDD(34465-46-8) Total HxCDD	N/A	N/A	N/A
Total HxCDF(55684-94-1) Total HxCDF	N/A	N/A	N/A
Total PeCDD(36088-22-9) Total PeCDD	N/A	N/A	N/A
Total PeCDF(30402-15-4) Total PeCDF	N/A	N/A	N/A
Total TCDD(41903-57-5) Total TCDD	N/A	N/A	N/A
Total TCDF(55722-27-5) Total TCDF	N/A	N/A	N/A

Precision Descriptor Notes:
Detection Level Note:	The Minimum Level (ML) for each analyte is defined as the level at which the entire analytical system must give a recognizable signal and acceptable calibration point. It is equivalent to the concentration of the lowest calibration standard, assuming that all method-specified sample weights, volumes, and cleanup procedures have been employed. MLs are shown for water. ML range for solids is 1 - 10 ng/kg.

Precision Descriptor Notes:

Detection Level Note:

The Minimum Level (ML) for each analyte is defined as the level at which the entire analytical system must give a recognizable signal and acceptable calibration point. It is equivalent to the concentration of the lowest calibration standard, assuming that all method-specified sample weights, volumes, and cleanup procedures have been employed. MLs are shown for water. ML range for solids is 1 - 10 ng/kg.

Revision	PDF/Link
October 1994

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EPA-EAD: 1613: Dioxins and Furans by HRGC/HRMS

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