EPA: 8290A: POLYCHLORINATED DIBENZO-p-DIOXINS (PCDDs) AND POLYCHLORINATED DIBENZOFURANS (PCDFs) BY HIGH-RESOLUTION GAS CHROMATOGRAPHY/HIGH-RESOLUTION MASS SPECTROMETRY (HRGC/HRMS)

Summary
Analytes
Revision
Data and Sites

Official Method Name

POLYCHLORINATED DIBENZO-p-DIOXINS (PCDDs) AND POLYCHLORINATED DIBENZOFURANS (PCDFs) BY HIGH-RESOLUTION GAS CHROMATOGRAPHY/HIGH-RESOLUTION MASS SPECTROMETRY (HRGC/HRMS)

Current Revision

EPA 8290A, Revision 1, February 2007

Media

VARIOUS

Instrumentation

High Resolution Gas Chromatography/High Resolution Mass Spectrometry

Method Subcategory

Organic

Method Source

EPA

Citation

Method 8290A: Polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs) by high-resolution gas chromatography/high-resolution mass spectrometry (HRGC/HRMS)

Brief Method Summary

A designated amount of soil, sediment, fly ash, water, sludge (including paper pulp), still bottom, fuel oil, chemical reactor residue, fish tissue, or human adipose tissue is spiked with a solution containing specified amounts of each of the nine isotopically (¹³C₁₂) labeled PCDDs/PCDFs. The sample is then extracted according to a matrix-specific extraction procedure. The extracts are then submitted to an acid-base washing treatment and dried. Following a solvent exchange step, the extracts are cleaned up by column chromatography on alumina, silica gel, and activated carbon. The preparation of the final extract for HRGC/HRMS analysis is accomplished by adding 10 to 50 µL (depending on the matrix) of a nonane solution containing 50 pg/µL of the recovery standards ¹³C₁₂-1,2,3,4-TCDD and ¹³C₁₂-1,2,3,7,8,9-HxCDD. The former is used to determine the percent recoveries of tetra- and pentachlorinated PCDD/PCDF congeners, while the latter is used to determine the percent recoveries of the hexa-, hepta- and octachlorinated PCDD/PCDF congeners. An aliquot of the concentrated extract is injected into an HRGC/HRMS system capable of performing selected ion monitoring at resolving power of at least 10,000 (10 percent. valley definition).

Scope and Application

This method provides procedures for the detection and quantitative measurement of polychlorinated dibenzo-p-dioxins (tetra- through octachlorinated homologues; PCDDs), and polychlorinated dibenzofurans (tetra- through octachlorinated homologues; PCDFs) in soil, sediment, fly ash, water, sludge (including paper pulp), still bottom, fuel oil, chemical reactor residue, fish tissue, or human adipose tissue and at part-per-trillion (ppt) to part-per-quadrillion (ppq) concentrations.

Applicable Concentration Range

Water (0.01 - 2 pg/g), soil/sediment, fish tissue, fly ash, human adipose tissue (1.0 - 200 pg/g).

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

High-resolution concentration calibration (HRCC) solutions, GC column performance check (evaluation) solution, Sample fortification solution, Recovery standard solution, Performance evaluation samples, Field blanks, Fortified field blank (optional), Rinsate sample (optional), duplicate analyses (optional).

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.

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:	Calculate the percent recovery of the nine internal standards measured in the sample extract.
Detection Level Note:	Two methods of calculation can be used, as follows, depending on the type of response produced during the analysis of a particular sample. For samples giving a response for both quantitation ions (Tables 6 and 9) that is less than 2.5 times the background level, use the first expression on p. 41 to calculate an EDL for each 2,3,7,8-substituted PCDD/PCDF that does not have a response with S/N ≥ 2.5. 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 in Sec. 11.8.4 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 first expression on p. 40.

Precision Descriptor Notes:

Calculate the percent recovery of the nine internal standards measured in the sample extract.

Detection Level Note:

Two methods of calculation can be used, as follows, depending on the type of response produced during the analysis of a particular sample. For samples giving a response for both quantitation ions (Tables 6 and 9) that is less than 2.5 times the background level, use the first expression on p. 41 to calculate an EDL for each 2,3,7,8-substituted PCDD/PCDF that does not have a response with S/N ≥ 2.5. 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 in Sec. 11.8.4 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 first expression on p. 40.

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EPA 8290A, Revision 1, February 2007

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EPA: 8290A: POLYCHLORINATED DIBENZO-p-DIOXINS (PCDDs) AND POLYCHLORINATED DIBENZOFURANS (PCDFs) BY HIGH-RESOLUTION GAS CHROMATOGRAPHY/HIGH-RESOLUTION MASS SPECTROMETRY (HRGC/HRMS)

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