Method 1668C Air

Polychlorinated Biphenyls (PCBs) in Stationary Source Emissions


This method is used for the determination of polychlorinated biphenyls (PCBs) at low levels from stationary source emissions 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.

 

Samples are collected isokinetically using a modified Method 5 train which consists of a glass fiber filter containing no organic binders, XAD-2 resin trap, and a series of water impingers. The sampling train is rinsed with acetone and/or methylene chloride.  The rinses and impinger water are collected and sent to the laboratory for extraction and analysis.  

 

Typically all components of the train, including the rinses, are extracted and combined to produce one extract for analysis which represents the entire sampling train.  This extract is then split and 50% of the extract is archived in case there are problems and re-analysis is necessary.  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.  If there are problems with the cleanup, the archived portion of the sample extract can be processed avoiding the need to resample. 

 

Note that Method 1668A was developed by EPA's office of Science and Technology for the analysis of water, soil, sediment, biosolids, tissues and other matrices.  It does not specifically reference air matrices but it is a performance based method.  This is the method chosen for compliance projects because of it's specificity and 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:   None specified in method, however, some laboratories extract the samples within 14 days and analyze within 40 days from extraction per SW-846 requirements for soil/water matrices.
Preservatives:   Keep samples in the dark. Liquid samples (rinses and impinger water) stored on ice for transport to laboratory (4°C± 2).
Required Preps:   None specified in method.
Collection Method:   Modified Method 5 train following modified Method 23/0010 procedures.
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
40
 pg
3,3',4,4'-Tetrachlorobiphenyl (77)
C12H6Cl4
32598-13-3
40
 pg
2,3,3',4,4'-Pentachlorobiphenyl (105)
C12H5Cl5
32598-14-4
40
 pg
3,3',4,4',5,5'-Hexachlorobiphenyl (169)
C12H4Cl6
32774-16-6
40
 pg
2,3,3',4,4',5-Hexachlorobiphenyl (156)
C12H4Cl6
38380-08-4
40
 pg
2,3,3',4,4',5,5'-Heptachlorobiphenyl (189)
C12H3Cl7
39635-31-9
40
 pg
2,3',4,4',5,5'-Hexachlorobiphenyl (167)
C12H4Cl6
52663-72-6
40
 pg
3,3',4,4',5-Pentachlorobiphenyl (126)
C12H5Cl5
57465-28-8
40
 pg
2',3,4,4',5-Pentachlorobiphenyl (123)
C12H5Cl5
65510-44-3
40
 pg
2,3,3',4,4',5'-Hexachlorobiphenyl (157)
C12H4Cl6
69782-90-7
40
 pg
3,4,4',5-Tetrachlorobiphenyl (81)
C12H6Cl4
70362-50-4
40
 pg
2,3,4,4',5-Pentachlorobiphenyl (114)
C12H5Cl5
74472-37-0
40
 pg
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.