Method 8280B Water

Polychlorinated Dibenzodioxins (PCDDs) and Polychlorinated Dibenzofurans (PCDFs) by High Resolution Gas Chromatography/Low Resolution Mass Spectrometry (HRGC/LRMS)


This method is for the determination of 2,3,7,8-tetrachlorinated dibenzo-p-dioxin (2,3,7,8-TCDD), 2,3,7,8-tetrachlorinated dibenzofuran (2,3,7,8-TCDF), and the 2,3,7,8-substituted penta-, hexa-, hepta-, and octachlorinated dibenzo-p-dioxins (PCDDs) and dibenzofurans (PCDFs) in water at part-per-trillion (ppt) concentrations.  The sample is filtered prior to extraction to remove particulates. The filtrate is extracted with methylene chloride using a separatory funnel, liquid-liquid extractor or solid phase extraction (SPE).  The particulates are extracted separately with toluene using a Soxhlet extractor.  After extraction C13-labeled standards are spiked into the sample to monitor clean-up efficiency.  Clean-up options for the extracts are an acid-base wash, gel permeation, alumina, silica gel and Florisil column clean-ups.  After clean-up the extract is concentrated and analyzed by high  resolution gas chromatography/low resolution mass spectrometry (HRGC/LRMS).

This is an isotope dilution method.

A calculation of the TEQ (toxicity equivalent concentration) is done for each sample using international toxicity equivalency factors (TEFs).  A high TEQ, greater than 7 ppt, will require analysis on a second GC column unless 2,3,7,8-TCDF is separated from its closest eluting isomers from analysis on the primary column.

This method replaces Methods 8280 and 8280A.

 


(EPA SW-846)

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Method Data

Hold Times, Preservatives, Preps, Collection, Analytical & Documentation
Holding Time:   30 days from collection to extraction and 45 days from extraction to analysis.
Preservatives:   Cool to ≤ 6°C. If residual chlorine is present, add 80 mg sodium thiosulfate per liter of sample. If pH > 9, adjust to pH 7-9 with sulfuric acid.
Required Preps:   1L amber glass bottle
Collection Method:   Grab sampling, SW-846 Chapter 4
Analytical Methodology:   HRGC/LRMS
Documentation:   8280B

Analyte List*

Analyte Formula CAS Number Detection Limit
2,3,7,8-Tetrachloro-dibenzo-p-dioxin
1746-01-6
10
 ppt
1,2,3,7,8,9-Hexachlorodibenzo-p-dioxin
19408-74-3
50
 ppt
PCDF, Totals
30402-15-4
 
Octachlorodibenzo-p-dioxin
C12Cl8O2
3268-87-9
100
 ppt
HxCDD, Totals
34465-46-8
 
1,2,3,4,6,7,8-Heptachlorodibenzo-p-dioxin
35822-46-9
50
 ppt
PCDD, Totals
36088-22-9
 
HpCDD, Totals
37871-00-4
 
HpCDF, Totals
38998-75-3
 
Octachlorodibenzofuran
39001-02-0
100
 ppt
1,2,3,4,7,8-Hexachlorodibenzo-p-Dioxin
39227-28-6
50
 ppt
1,2,3,7,8-Pentachlorodibenzo-p-Dioxin
40321-76-4
50
 ppt
TCDD, Totals
41903-57-5
 
2,3,7,8-Tetrachlorodibenzofuran
C12H4Cl4O
51207-31-9
10
 ppt
1,2,3,4,7,8,9-Heptachlorodibenzofuran
55673-89-7
50
 ppt
HxCDF, Totals
55684-94-1
 
TCDF, Totals
55722-27-5
 
2,3,4,7,8-Pentachlorodibenzofuran
57117-31-4
50
 ppt
1,2,3,7,8-Pentachlorodibenzofuran
57117-41-6
50
 ppt
1,2,3,6,7,8-Hexachlorodibenzofuran
57117-44-9
50
 ppt
1,2,3,6,7,8-Hexachlorodibenzo-p-dioxin
57653-85-7
50
 ppt
2,3,4,6,7,8-Hexachlorodibenzofuran
60851-34-5
50
 ppt
1,2,3,4,6,7,8-Heptachlorodibenzofuran
67562-39-4
50
 ppt
1,2,3,4,7,8-Hexachlorodibenzofuran
70648-26-9
50
 ppt
1,2,3,7,8,9-Hexachlorodibenzofuran
72918-21-9
50
 ppt

* The analytes and detection limits listed for each method represent the typical detection limits and analytes reported for that particular method. Keep in mind that analyte lists may vary from laboratory to laboratory. Detection limits may also vary from lab to lab and are dependent upon the sample size, matrix, and any interferences that may be present in the sample.