Method 1668C Tissue

Polychlorinated Biphenyls (PCBs) in Tissue Samples


This method is used for the determination of polychlorinated biphenyls (PCBs) at low levels from soil, sediment, and biosolid samples using isotope dilution HRMS (high resolution mass spectrometry).  All 209 individual PCBs are determined as well as the Totals for each congener group (e.g. Total Mono-PCB, Total Di-PCB).  Special interest is paid to the twelve PCBs designated by the World Health Organization (WHO) as the most toxic.  This subset of PCBs may also be called the co-planar or dioxin-like PCBs.  It is not currently possible to separate each of the 209 PCBs and some are reported as co-eluting compounds.

 

Wrap the samples in foil since the method requires the samples be protected from light.  Ideally, tissue samples should be frozen and shipped on dry ice.  Samples should be stored at <-10°C.

 

Samples are typically extracted with methylene chloride using a 10 gram wet weight equivalent sample size adjusted for lipids.  A lipid determination is required.  Keep in mind that this is a performance based method so lab procedures may vary.  Because of the variances in tissue, it's important that the samples are thoroughly homogenized prior to extraction.  If possible, it's best to homogenize them while frozen.

 

The sample extracts undergo an extensive cleanup prior to analysis in order to remove interferences (dioxins, pesticides, PAH, etc.) in order to achieve the low limits of detection. 

 

NOTE:  This method is an update of and replaces Methods 1668, 1668A and 1668B.


(EPA 821/R-97-001)

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Method Data

Hold Times, Preservatives, Preps, Collection, Analytical & Documentation
Holding Time:   The method states that samples are good for up to one year if kept in the dark and at less than -10°C.
Preservatives:   None specified in method although it's recommended to ship the samples frozen and on dry ice.
Required Preps:   4oz Amber glass bottle with Teflon-lined lid
Collection Method:   Various techniques
Analytical Methodology:   HR GC/MS
Documentation:   1668C

Analyte List*

Analyte Formula CAS Number Detection Limit
2,3',4,4',5-Pentachlorobiphenyl (118)
C12H5Cl5
31508-00-6
0.8
 pg/g
3,3',4,4'-Tetrachlorobiphenyl (77)
C12H6Cl4
32598-13-3
0.8
 pg/g
2,3,3',4,4'-Pentachlorobiphenyl (105)
C12H5Cl5
32598-14-4
0.8
 pg/g
3,3',4,4',5,5'-Hexachlorobiphenyl (169)
C12H4Cl6
32774-16-6
0.8
 pg/g
2,3,3',4,4',5-Hexachlorobiphenyl (156)
C12H4Cl6
38380-08-4
0.8
 pg/g
2,3,3',4,4',5,5'-Heptachlorobiphenyl (189)
C12H3Cl7
39635-31-9
0.8
 pg/g
2,3',4,4',5,5'-Hexachlorobiphenyl (167)
C12H4Cl6
52663-72-6
0.8
 pg/g
3,3',4,4',5-Pentachlorobiphenyl (126)
C12H5Cl5
57465-28-8
0.8
 pg/g
2',3,4,4',5-Pentachlorobiphenyl (123)
C12H5Cl5
65510-44-3
0.8
 pg/g
2,3,3',4,4',5'-Hexachlorobiphenyl (157)
C12H4Cl6
69782-90-7
0.8
 pg/g
3,4,4',5-Tetrachlorobiphenyl (81)
C12H6Cl4
70362-50-4
0.8
 pg/g
2,3,4,4',5-Pentachlorobiphenyl (114)
C12H5Cl5
74472-37-0
0.8
 pg/g
Di-CB, Total
C12H8Cl2
DiPCB
 
Hepta-CB, Total
C12H7Cl3
HeptaPCB
 
Hexa-CB, Total
C12H6Cl4
HexaPCB
 
Mono-CB, Total
C12H9Cl1
MonoPCB
 
Nona-CB, Total
C12H1Cl9
NonaPCB
 
Octa-CB, Total
C12H2Cl8
OctaPCB
 
Penta-CB, Total
C12H5Cl5
PentaPCB
 
Tetra-CB, Total
C12H6Cl4
TetraPCB
 
Tri-CB, Total
C12H7Cl3
TriPCB
 

* 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.