Analytical Assessment Technology Advancements ...
Analytical Assessment Technology Advancements & Common Analytical Pitfalls
Mike Ericson Laboratory Director Con-Test Analytical Laboratory
Analytical Assessment Technology Advancements and Common Analytical Pitfalls Michael Erickson
PCB Structure
PCB 18
Aroclor 1242 • Aroclors are comprised of varying ratios of the 209 PCB congeners • Aroclor mixtures are characterized by the amount of chlorine they contain (i.e. 1242 contains 42% chlorine)
PCB Homologues IUPAC # Compounds 1 2-Chlorobiphenyl 2 3-Chlorobiphenyl 3 4-Chlorobiphenyl 4 2,2'-Dichlorobiphenyl 5 2,3-Dichlorobiphenyl 6 2,3'-Dichlorobiphenyl 7 2,4-Dichlorobiphenyl 8 2,4'-Dichlorobiphenyl 9 2,5-Dichlorobiphenyl 10 2,6-Dichlorobiphenyl 11 3,3'-Dichlorobiphenyl 12 3,4-Dichlorobiphenyl 13 3,4'-Dichlorobiphenyl 14 3,5-Dichlorobiphenyl 15 4,4'-Dichlorobiphenyl 16 2,2',3-Trichlorobiphenyl . . . . . . 206 2,2',3,3',4,4',5,5',6-Nonachlorobiphenyl 207 2,2',3,3',4,4',5,6,6'-Nonachlorobiphenyl 208 2,2',3,3',4,5,5',6,6'-Nonachlorobiphenyl 209 2,2',3,3',4,4',5,5',6,6'-Decachlorobiphenyl
Isomer Class 1 Cl 1 Cl 1 Cl 2 Cl 2 Cl 2 Cl 2 Cl 2 Cl 2 Cl 2 Cl 2 Cl 2 Cl 2 Cl 2 Cl 2 Cl 3 Cl . . . 9 Cl 9 Cl 9 Cl 10 Cl
Homologues Monochlorobiphenyl
Dichlorobiphenyl
Trichlorobiphenyl . . .
Nonachlorobiphenyl Decachlorobiphenyl
Dioxin-like Compounds
Tetrachlorodioxin
PCB 77
PCB 54
Similar geometry (planar) and chlorine substitution pattern Of the 209 congeners 12 are dioxin-like Three most toxic congeners include PCB 77, 126 & 169 (non-
ortho substitution)
PCB Extraction Methods Solids SW-846 3540C Soxhlet Extraction (TSCA, Region 1) SW-846 3550C Ultrasonic Extraction SW-846 3545A Pressurized Fluid Extraction (PFE) SW-846 3546 Microwave Extraction Liquids SW-846 3510C Liquid-Liquid Extraction SW-846 3535 Solid Phase Extraction
SW-846 3540C Soxhlet Extraction
Analytical Methods SW-846 8000C SW-846 8082 Water, Soil, Sediment Wipes, Paint, Caulking TO-10A, TO-4 Air – PUF EPA 680 Homologues SW-846 8270 Modified Congeners
Extract Clean-up Methods SW-846 3665A Sulfuric Acid Clean-up Elevated baselines Complex chromatograms
SW-846 3660B Sulfur Clean-up Elemental Sulfur in many sediments Solubility is similar to PCBs
SW-846 3620C Florisil Cartridge Clean-up Polar hydrocarbons Other polar material
Enhanced column Clean-up Primarily for troublesome caulking
Aroclor 1242 “under” sulfur peak
Aroclor 1242 with Sulfur Interference Removed
Enhanced Clean-up with Interference Removed
PCB’s in Air Sampling
HIGH VOLUME
LOW VOLUME
Polychlorinated biphenyls are sampled on a PUF (polyurethane foam) cartridge. High volume samples are taken on large high volume PUF’s by EPA Method TO-4A. Low volume samples can be taken by EPA Method TO-10A.
PCB’s in Caulking, Air, Wipes… Typical Reporting Limits PCB Aroclors in Air* TO-4A (High Volume) TO-10A (Low Volume)
0.062-0.62 ng/m3 0.0028-0.83 ug/m3
Optional NIOSH 5503* 0.069-2.0 ug/m3 * RL calculated from sample volume
PCB 8082 in caulking/paint
Mike Ericson Laboratory Director Con-Test Analytical Laboratory
Analytical Assessment Technology Advancements and Common Analytical Pitfalls Michael Erickson
PCB Structure
PCB 18
Aroclor 1242 • Aroclors are comprised of varying ratios of the 209 PCB congeners • Aroclor mixtures are characterized by the amount of chlorine they contain (i.e. 1242 contains 42% chlorine)
PCB Homologues IUPAC # Compounds 1 2-Chlorobiphenyl 2 3-Chlorobiphenyl 3 4-Chlorobiphenyl 4 2,2'-Dichlorobiphenyl 5 2,3-Dichlorobiphenyl 6 2,3'-Dichlorobiphenyl 7 2,4-Dichlorobiphenyl 8 2,4'-Dichlorobiphenyl 9 2,5-Dichlorobiphenyl 10 2,6-Dichlorobiphenyl 11 3,3'-Dichlorobiphenyl 12 3,4-Dichlorobiphenyl 13 3,4'-Dichlorobiphenyl 14 3,5-Dichlorobiphenyl 15 4,4'-Dichlorobiphenyl 16 2,2',3-Trichlorobiphenyl . . . . . . 206 2,2',3,3',4,4',5,5',6-Nonachlorobiphenyl 207 2,2',3,3',4,4',5,6,6'-Nonachlorobiphenyl 208 2,2',3,3',4,5,5',6,6'-Nonachlorobiphenyl 209 2,2',3,3',4,4',5,5',6,6'-Decachlorobiphenyl
Isomer Class 1 Cl 1 Cl 1 Cl 2 Cl 2 Cl 2 Cl 2 Cl 2 Cl 2 Cl 2 Cl 2 Cl 2 Cl 2 Cl 2 Cl 2 Cl 3 Cl . . . 9 Cl 9 Cl 9 Cl 10 Cl
Homologues Monochlorobiphenyl
Dichlorobiphenyl
Trichlorobiphenyl . . .
Nonachlorobiphenyl Decachlorobiphenyl
Dioxin-like Compounds
Tetrachlorodioxin
PCB 77
PCB 54
Similar geometry (planar) and chlorine substitution pattern Of the 209 congeners 12 are dioxin-like Three most toxic congeners include PCB 77, 126 & 169 (non-
ortho substitution)
PCB Extraction Methods Solids SW-846 3540C Soxhlet Extraction (TSCA, Region 1) SW-846 3550C Ultrasonic Extraction SW-846 3545A Pressurized Fluid Extraction (PFE) SW-846 3546 Microwave Extraction Liquids SW-846 3510C Liquid-Liquid Extraction SW-846 3535 Solid Phase Extraction
SW-846 3540C Soxhlet Extraction
Analytical Methods SW-846 8000C SW-846 8082 Water, Soil, Sediment Wipes, Paint, Caulking TO-10A, TO-4 Air – PUF EPA 680 Homologues SW-846 8270 Modified Congeners
Extract Clean-up Methods SW-846 3665A Sulfuric Acid Clean-up Elevated baselines Complex chromatograms
SW-846 3660B Sulfur Clean-up Elemental Sulfur in many sediments Solubility is similar to PCBs
SW-846 3620C Florisil Cartridge Clean-up Polar hydrocarbons Other polar material
Enhanced column Clean-up Primarily for troublesome caulking
Aroclor 1242 “under” sulfur peak
Aroclor 1242 with Sulfur Interference Removed
Enhanced Clean-up with Interference Removed
PCB’s in Air Sampling
HIGH VOLUME
LOW VOLUME
Polychlorinated biphenyls are sampled on a PUF (polyurethane foam) cartridge. High volume samples are taken on large high volume PUF’s by EPA Method TO-4A. Low volume samples can be taken by EPA Method TO-10A.
PCB’s in Caulking, Air, Wipes… Typical Reporting Limits PCB Aroclors in Air* TO-4A (High Volume) TO-10A (Low Volume)
0.062-0.62 ng/m3 0.0028-0.83 ug/m3
Optional NIOSH 5503* 0.069-2.0 ug/m3 * RL calculated from sample volume
PCB 8082 in caulking/paint
