EPA: 8280B: Polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs) in water, soil, fly ash, and chemical wastes and sludge by high resolution gas chromatography/ low resolution mass spectrometry (HRGC/LRMS)

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Official Method Name

METHOD 8280B: POLYCHLORINATED DIBENZO-p-DIOXINS (PCDDs) AND POLYCHLORINATED DIBENZOFURANS (PCDFs) BY HIGH-RESOLUTION GAS CHROMATOGRAPHY/LOW-RESOLUTION MASS SPECTROMETRY (HRGC/LRMS)

Current Revision

Revision 2, February 2007

Media

VARIOUS

Instrumentation

High Resolution Gas Chromatography/Low Resolution Mass Spectrometry

Method Subcategory

Organic

Method Source

EPA

Citation

Method 8280B: Polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs) by high resolution gas chromatography/low resolution mass spectrometry ((HRGC/LRMS)

Brief Method Summary

A designated amount of water, soil, fly ash, or chemical waste samples is spiked with internal standards and extracted according to a matrix-specific extraction procedure. Aqueous samples are filtered, and solid samples that show an aqueous phase are centrifuged before extraction. Soil, fly ash, or chemical waste samples are extracted with the combination of a Dean-Stark water trap and a Soxhlet extractor using toluene or using pressurized fluid extraction (PFE) or microwave extraction. Water samples are extracted with a separatory funnel or liquid-liquid extractor using methylene chloride, and the particulate fraction that results from filtering the water samples is extracted separately in a Soxhlet extractor using toluene or by solid-phase extraction (SPE). After extraction and the initial concentration, Cl₄-labeled 2,3,7,8-TCDD is added to each extract to measure the efficiency of the cleanup process. Sample extract cleanup may include acid-base washing treatment, and gel permeation, alumina, silica gel, Florisil® and activated carbon on Celite 545® chromatography. After cleanup, the extract is concentrated to near dryness. Immediately prior to injection, internal standards are added to each extract, and an aliquot of the extract is injected into an HRGC/LRMS system capable of performing the selected ion monitoring.

Scope and Application

This method is appropriate for the detection and quantitative measurement of 2,3,7,8-tetrachlorodibenzo-p-dioxin (2,3,7,8-TCDD), 2,3,7,8-tetrachlorodibenzofuran (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 concentrations), soil, fly ash, and chemical waste samples, including stillbottom, fuel oil, and sludge matrices (at part-per-billion concentrations).

Applicable Concentration Range

water (10 - 50 ng/L), fly soil and chemical ash (1.0 - 5.0 ug/kg), waste (10 - 50 ug/kg)

Interferences

(A) Solvents, reagents, glassware contamination: Selection of reagents and purification of solvents by distillation in all-glass systems may be necessary. Analysts should avoid using PVC gloves. Use of high-purity reagents and pesticide-grade solvents helps to minimize interference problems. Purification of solvents by distillation, in all glass systems, may be required. (B) Interferants coextracted from the sample: Retention times of target analytes must be verified using reference standards. These values must correspond to the retention time windows established in Sec. 9.3.1.3. While cleanup techniques are provided as part of this method, unique samples may require additional cleanup steps to achieve the sensitivity described in this method. (C) No single column is known to resolve all 210 isomers. The 60-m DB-5 GC column is capable of 2,3,7,8-TCDD isomer specificity (Sec. 6.2.1). In order to determine the concentration of the 2,3,7,8-TCDF (if detected on the DB-5 column), the sample extract must be reanalyzed on a column capable of 2,3,7,8-TCDF isomer specificity (e.g., DB-225, SP-2330, SP-2331, or equivalent).

Quality Control Requirements

Calibration solutions, Internal standard solution, Recovery standard solution, Calibration verification solution, Cleanup standard, Matrix spiking standard, Window defining mix, Column performance solutions, Method blanks,

Sample Handling

Grab and composite samples should be homogenized in the field and collected in glass containers not pre-rinsed with sample. Fish tissue should be ground in a stainless steel grinder. Sampling equipment must be free of potential sources of contamination. If residual chlorine is present in aqueous samples, add 80 mg of sodium thiosulfate per liter of sample. If the sample pH is greater than 9, adjust it to a pH of 7 to 9 with sulfuric acid.

Maximum Holding Time

Extracted within 30 days (≤ 6 deg C, <-10 deg C for fish tissue, dark); analyzed within 45 days

Relative Cost

Sample Preparation Methods

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-	N/A	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	N/A	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	N/A	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-	N/A	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-	N/A	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	N/A	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	N/A	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	N/A	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	N/A	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	N/A	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	N/A	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	N/A	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	N/A	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-	N/A	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-	N/A	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	N/A	N/A	N/A
Octachlorodibenzofuran(39001-02-0) Dibenzofuran, octachloro- OCDF Octachlorodibenzofuran Perchlorodibenzofuran	N/A	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:	QC samples should include a method blank, a matrix spike, a duplicate, and a laboratory control sample (LCS) in each analytical batch and the addition of surrogates to each field sample and QC sample when surrogates are used. Any method blanks, matrix spike samples, and replicate samples should be subjected to the same analytical procedures as those used on actual samples. Documenting the effect of the matrix should include the analysis of at least one matrix spike and one duplicate unspiked sample or one matrix spike/matrix spike duplicate pair. A laboratory control sample (LCS) should be included with each analytical batch. The LCS consists of an aliquot of a clean (control) matrix similar to the sample matrix and of the same weight or volume. The LCS is spiked with the same analytes at the same concentrations as the matrix spike, when appropriate. When the results of the matrix spike analysis indicate a potential problem due to the sample matrix itself, the LCS results are used to verify that the laboratory can perform the analysis in a clean matrix.
Detection Level Note:	The sample specific estimated quantitation limit (EQL) is the estimate made by the laboratory of the concentration of a given analyte required to produce a signal with a peak height of at least 2.5 times the background signal level. The estimate is specific to a particular analysis of the sample, and will be affected by sample size, dilution, etc. An EQL is calculated for each 2,3,7,8-substituted isomer that is not identified, regardless of whether or not non-2,3,7,8-substituted isomers in that homologue are present. The EQL is also calculated for 2,3,7,8-substituted isomers giving responses for both the quantitation ions that are less than 2.5 times the background level. Use the formulae on p. 39 to calculate an EQL for each absent 2,3,7,8-substituted PCDD/PCDF. The background level (H_n) is determined by measuring the height of the noise at the expected retention times of both the quantitation ions of the particular 2,3,7,8-substituted isomer. If none of the isomers within a homologue are detected, then the EQL for the "total" homologue concentration is the lowest EQL for any of the 2,3,7,8-substituted isomers that were not detected. Do not add together the EQLs for the various isomers. If a 2,3,7,8-substituted isomer is reported in the homologue, then no EQL for the "total" is calculated. An estimated maximum possible concentration (EMPC) is calculated for 2,3,7,8-substituted isomers that are characterized by a response with an S/N of at least 2.5 for both the quantitation ions, and meet all of the identification criteria except the ion abundance ratio criteria or when a peak representing a PCDPE has been detected. An EMPC is a worst-case estimate of the concentration. Calculate the EMPC according to the formulae on p.40.

Precision Descriptor Notes:

QC samples should include a method blank, a matrix spike, a duplicate, and a laboratory control sample (LCS) in each analytical batch and the addition of surrogates to each field sample and QC sample when surrogates are used. Any method blanks, matrix spike samples, and replicate samples should be subjected to the same analytical procedures as those used on actual samples. Documenting the effect of the matrix should include the analysis of at least one matrix spike and one duplicate unspiked sample or one matrix spike/matrix spike duplicate pair. A laboratory control sample (LCS) should be included with each analytical batch. The LCS consists of an aliquot of a clean (control) matrix similar to the sample matrix and of the same weight or volume. The LCS is spiked with the same analytes at the same concentrations as the matrix spike, when appropriate. When the results of the matrix spike analysis indicate a potential problem due to the sample matrix itself, the LCS results are used to verify that the laboratory can perform the analysis in a clean matrix.

Detection Level Note:

The sample specific estimated quantitation limit (EQL) is the estimate made by the laboratory of the concentration of a given analyte required to produce a signal with a peak height of at least 2.5 times the background signal level. The estimate is specific to a particular analysis of the sample, and will be affected by sample size, dilution, etc. An EQL is calculated for each 2,3,7,8-substituted isomer that is not identified, regardless of whether or not non-2,3,7,8-substituted isomers in that homologue are present. The EQL is also calculated for 2,3,7,8-substituted isomers giving responses for both the quantitation ions that are less than 2.5 times the background level. Use the formulae on p. 39 to calculate an EQL for each absent 2,3,7,8-substituted PCDD/PCDF. The background level (H_n) is determined by measuring the height of the noise at the expected retention times of both the quantitation ions of the particular 2,3,7,8-substituted isomer. If none of the isomers within a homologue are detected, then the EQL for the "total" homologue concentration is the lowest EQL for any of the 2,3,7,8-substituted isomers that were not detected. Do not add together the EQLs for the various isomers. If a 2,3,7,8-substituted isomer is reported in the homologue, then no EQL for the "total" is calculated. An estimated maximum possible concentration (EMPC) is calculated for 2,3,7,8-substituted isomers that are characterized by a response with an S/N of at least 2.5 for both the quantitation ions, and meet all of the identification criteria except the ion abundance ratio criteria or when a peak representing a PCDPE has been detected. An EMPC is a worst-case estimate of the concentration. Calculate the EMPC according to the formulae on p.40.

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EPA: 8280B: Polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs) in water, soil, fly ash, and chemical wastes and sludge by high resolution gas chromatography/ low resolution mass spectrometry (HRGC/LRMS)

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