Method 1614

Brominated Diphenyl Ethers in Water, Soil, Sediment and Tissue by HRGC/HRMS


This method is for the determination of polybrominated diphenyl ethers (PBDEs) from aqueous, solid, tissue, and multi-phase matrices by high resolution gas chromatography/high resolution mass spectrometry (HRGC/HRMS).

Aqueous samples are extracted using solid-phase extraction (SPE), separatory funnel extraction (SFE), or continuous
liquid/liquid extraction (CLLE).  Solid, semi-solid, and multi-phase samples (excluding tissue) are extracted using a Soxhlet/Dean-Stark extractor.  Fish and other tissue is dried with anhydrous sodium sulfate and extracted for 18-24 hours using methylene chloride in a Soxhlet extractor.  Lipid content should also be determined for tissue samples.  Tissue sample extracts are cleaned up using an anthroopogenic isolation column.  All sample extracts are cleaned up using and acid/base column and gel permeation, silica gel, and/or Florisil or alumina chromatography, as required.


(EPA: Office of Water)

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Method Data

Hold Times, Preservatives, Preps, Collection, Analytical & Documentation
Holding Time:   Aqueous samples are good for up to one year if properly preserved and stored in the dark at <6°C. Solid, semi-solid, tissue and other matrices may be stored for up to one year if stored in the dark at <-10°C.
Preservatives:   If residual chlorine is present, add 80mg of sodium thiosulfate per L of aqeuous sample. Ship all samples at <6°C. Store aqueous samples at <6°C and solid, semi-solid, tissue and other matrices at <-10°C.
Required Preps:   1L Amber glass bottle with Teflon-lined lid
Collection Method:   Grab sampling
Analytical Methodology:   HRGC/HRMS
Documentation:   1614

Analyte List*

Analyte Formula CAS Number Detection Limit
4-Bromodiphenyl ether (4-MoBDE, IUPAC 3)
C12H9BrO
101-55-3
315
 pg/L
Decabromodiphenyl ether (DeBDE, IUPAC 209)
C12Br10O
1163-19-5
4900
 pg/L
3-Bromodiphenyl ether (3-MoBDE, IUPAC 2)
C12H9BrO
6876-00-2
200
 pg/L
2,4’-Dibromodiphenyl ether (2,4'-BDE, IUPAC 8)
C12H8Br2O
BDE-8
13
 pg/L
3,3’-Dibromodiphenyl ether (3,3'-DiBDE, IUPAC 11)
C12H8Br2O
BDE-11
13
 pg/L
2,6-Dibromodiphenyl ether (2,6-DiBDE, IUPAC 10)
C12H8Br2O
BDE-10
18
 pg/L
3,4-Dibromodiphenyl ether (3,4-DiBDE, IUPAC 12)
C12H8Br2O
BDE-12
7
 pg/L
2,4-Dibromodiphenyl ether (2,4-DiBDE, IUPAC 7)
C12H8Br2O
BDE-7
13
 pg/L
2-Bromodiphenyl ether (2-MoBDE, IUPAC 1)
C12H9BrO
BDE-1
360
 pg/L
4,4’-Dibromodiphenyl ether (4,4'-BDE, IUPAC 15)
C12H8Br2O
BDE-15
9
 pg/L
2,2',4-Tribromodiphenyl ether (2,2',4-TrBDE, IUPAC 17)
C12H7Br3O
147217-75-2
12
 pg/L
2,3’,4-Tribromodiphenyl ether (2,3'4-TrBDE, IUPAC 25)
C12H7Br3O
147217-77-4
16
 pg/L
2,4,4’-Tribromodiphenyl ether (2,4,4'-TrBDE, IUPAC 28)
C12H7Br3O
41318-75-6
27
 pg/L
2',3,4-Tribromodiphenyl ether (2',3,4-TrBDE, IUPAC 33)
C12H7Br3O
BDE-33
27
 pg/L
2,4,6-Tribromodiphenyl ether (2,4,6-BDE, IUPAC 30)
C12H7Br3O
BDE-30
16
 pg/L
2,4',6-Tribromodiphenyl ether (2,4'6-TrBDE, IUPAC 32)
C12H7Br3O
BDE-32
11
 pg/L
3,3',4-Tribromodiphenyl ether (3,3',4-TrBDE, IUPAC 35)
C12H7Br3O
147217-80-9
12
 pg/L
3,4,4’-Tribromodiphenyl ether (3,4,4'-TrBDE, IUPAC 37)
C12H7Br3O
147217-81-0
12
 pg/L
2,2’,4,4’-Tetrabromodiphenyl ether (2,2',4,4'-TeBDE, IUPAC 47)
C12H6Br4O
5436-43-1
27
 pg/L
2,2’,4,5’-Tetrabromodiphenyl ether (2,2',4,5'-TeBDE, IUPAC 49)
C12H6Br4O
243982-82-3
28
 pg/L
2,2’,4,6'-Tetrabromodiphenyl ether (2,2',4,6'-TeBDE, IUPAC 51)
C12H6Br4O
BDE-51
10
 pg/L
2,3’,4,4’-Tetrabromodiphenyl ether (2,3',4,4'-TeBDE, IUPAC 66)
C12H6Br4O
189084-61-5
14
 pg/L
2,3’,4’,6-Tetrabromodiphenyl ether (2,3',4',6-TeBDE, IUPAC 71)
C12H6Br4O
189084-62-6
19
 pg/L
2,4,4’,6-Tetrabromodiphenyl ether (2,4,4',6-TeBDE, IUPAC 75)
C12H6Br4O
189084-63-7
15
 pg/L
3,3’,4,4'-Tetrabromodiphenyl ether (3,3',4,4'-TeBDE, IUPAC 77)
C12H6Br4O
93703-48-1
10
 pg/L
3,3’,4,5'-Tetrabromodiphenyl ether (3,3',4,5'-TeBDE, IUPAC 79)
C12H6Br4O
BDE-79
13
 pg/L
2,2’,3,4,4’-Pentabromodiphenyl ether (2,2',3,4,4'-PeBDE, IUPAC 85)
C12H5Br5O
182346-21-0
37
 pg/L
2,2’,4,4’,5-Pentabromodiphenyl ether (2,2',4,4'5-PeBDE, IUPAC 99)
C12H5Br5O
60348-60-9
27
 pg/L
2,2’,4,4’,6-Pentabromodiphenyl ether (2,2',4,4',6-PeBDE, IUPAC 100)
C12H5Br5O
189084-64-8
27
 pg/L
2,3,3',4,4'-Pentabromodiphenyl ether (2,3,3',4,4'-PeBDE, IUPAC 105)
C12H5Br5O
BDE-105
72
 pg/L
2,3,4,5,6-Pentabromodiphenyl ether (2,3,4,5,6-PeBDE, IUPAC-116)
C12H5Br5O
BDE-116
54
 pg/L
2,3’,4,4’,5-Pentabromodiphenyl ether (2,3',4,4',5-PeBDE, IUPAC 118)
C12H5Br5O
BDE-118
35
 pg/L
2,3’,4,4’,6-Pentabromodiphenyl ether (2,3',4,4',6-PeBDE, IUPAC 119)
C12H5Br5O
189084-66-0
35
 pg/L
2,3',4,5,5'-Pentabromodiphenyl ether (2,3',4,5,5'-PeBDE, IUPAC 120)
C12H5Br5O
BDE-120
35
 pg/L
3,3’,4,4’,5-Pentabromodiphenyl ether (3,3',4,4'-5-PeBDE, IUPAC 126)
C12H5Br5O
25
 pg/L
2,2',3,3',4,4'-Hexabromodiphenyl ether (2,2',3,3',4,4'-HxBDE, IUPAC 128)
C12H4Br6O
172
 pg/L
2,2’,3,4,4’,5’-Hexabromodiphenyl ether (2,2',3,4,4',5'-HxBDE, IUPAC 138)
C12H4Br6O
182677-30-1
59
 pg/L
2,2’,3,4,4’,6’-Hexabromodiphenyl ether (2,2',3,4,4',6'-HxBDE, IUPAC 140)
C12H4Br6O
BDE-140
64
 pg/L
2,2’,4,4’,5,5’-Hexabromodiphenyl ether (2,2',4,4',5,5'-HxBDE, IUPAC 153)
C12H4Br6O
68631-49-2
47
 pg/L
2,2’,4,4’,5',6-Hexabromodiphenyl ether (2,2',4,4',5',6-HxBDE, IUPAC 154)
C12H4Br6O
BDE-154
30
 pg/L
2,2’,4,4’,6,6’-Hexabromodiphenyl ether (2,2',4,4',6,6'-HxBDE, IUPAC 155)
C12H4Br6O
35854-94-5
23
 pg/L
2,3,4,4’,5,6-Hexabromodiphenyl ether (2,3,4,4',5,6-HxBDE, IUPAC 166)
C12H4Br6O
189084-58-0
109
 pg/L
2,2’,3,4,4’,5,6-Heptabromodiphenyl ether (2,2',3,4,4',5,6-HpBDE, IUPAC 181)
C12H3Br7O
189084-67-1
91
 pg/L
2,2',3,4,4',5',6-Heptabromodiphenyl ether (2,2',3,4,4',5',6-HpBDE, IUPAC 183)
C12H3Br7O
207122-16-5
137
 pg/L
2,3,3’,4,4’,5,6-Heptabromodiphenyl ether (2,3,3',4,4',5,6-HpBDE, IUPAC 190)
C12H3Br7O
189084-68-2
118
 pg/L
2,2',3,4,4',5,5',6-Octabromodiphenyl ether (2,2',3,4,4',5,5',6-OcBDE, IUPAC 203)
C12H2Br8O
BDE-203
593
 pg/L
2,2',3,3',4,4',5,5',6-Nonabromodiphenyl ether (2,2',3,3',4,4',5,5',6-NoBDE, IUPAC 206)
C12HBr9O
BDE-206
366
 pg/L
2,2',3,3',4,4',5,6,6'-Nonabromodiphenyl ether (2,2',3,3',4,4',5,6,6'-NoBDE, IUPAC 207)
C12HBr9O
BDE-207
227
 pg/L
2,2',3,3',4,5,5',6,6'-Nonabromodiphenyl ether (2,2',3,3',4,5,5',6,6'-NoBDE, IUPAC 208)
C12HBr9O
BDE-208
220
 pg/L

* 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.