pcb analysis methods

The internal standard is added to the clean extract, and the sample is analyzed by HRGC-ECD. 1996. 1997. Toxicol. 1992; Corsolini et al. Below is an overview of the available methods and their utility for use in risk assessment and monitoring efforts. TABLE F-7 Methods Appropriate for the Cleanup of Environmental Extracts for PCB Analysis. 1997). This cell bioassay has been utilized for the screening and monitoring of Ah-active components in environmental extracts of sediment, water, air, and tissue (invertebrates, fish, birds, and mammals). Fundam. PCBs can be quantified by immunoassay methods, such as enzyme-linked immunosorbent assay (ELISA). The extracts are cleaned up using back extraction with sulfuric acid, followed by gel permeation, silica gel, Florisil, and activated carbon chromatography. New York District./U.S. Excellent correlation has been observed between the TODD-equivalent concentrations determined from this bioassay and instrumental analysis when these methods have been applied to the same sample (Tillitt et al. PCB is extracted into acetone/ hexane or acetone/methylene chloride using soxhlet extraction technique. Silver Spring, MD: U.S. Department of Commerce. For a sample size of 20 g of tissue or soil and a final extract volume of 0.25 mL, the H4IIE-luc assay will detect 1 part per trillion (ppt; pg/g of wet weight) TODD-equivalents. EPA 530/SW-846. 68-C3–309. Slice analysis is the process of obtaining the cross-section structure of the PCB through a series of methods and steps such as sampling, inlaying, slicing, polishing, corrosion, and observation. 40(1):33–54. Solvent is exchanged to hexane or other solvent for cleanup and analysis. Toxicol. Changes in methodology include the use of PCB-specific congeners for internal standards and surrogate materials and use of extraction and cleanup methods developed for the NOAA NS&T program. 2.2 Extracts for PCB analysis may be subjected to a sequential sulfuric acid/potassium permanganate cleanup (Method 3665) designed specifically for these analytes. For that reason, many standard EPA methods have been rewritten to allow the use of capillary GC columns for the analysis of environmental samples. Environ. Examples include USAGE New York District, EPA Region 2 testing procedures to fulfill Green Book testing requirement for the testing of dredged material for ocean dumping (USAGE 1992), EPA Region 9 San Francisco Bay, St. Johns (Florida) Water Management District, Puget Sound Dredge Disposal Activity (PSDDA), and EPA EMAP marine assessment program (Heitmuller and Valente. 1994b. All of the GC analytical methods below are appropriate for the analysis of PCBs in sediments, soils, water, or biological tissue, provided appropriate extraction and cleanup methods are used. 9. This section is intended to provide a brief overview of the available approaches to sample extraction and extract cleanup and compares several of the methods. ...or use these buttons to go back to the previous chapter or skip to the next one. Williams, L.L., J.P.Giesy, N.DeGalan, D.A.Verbrugge, D.E.Tillitt, G.T.Ankley, and R.A.Welch. Second, the Aroclor mixture has a distinct congener percent composition; therefore, the assumption that 1016:1260 congener co-elution domain response factors represent the response factors for individual Aroclors is fundamentally unsound (Newman et al. The failure mechanism is then analyzed by using various physical and chemical methods to analyze the mechanism that causes PCB failure or defect generation, such as virtual welding, contamination, mechanical damage, moisture stress, dielectric corrosion, fatigue damage, CAF or ion migration, stress overload and so on. Tetrachloro-m-xylene is used as a surrogate to monitor recovery. Environ. Toxicol. [Online]. In general, many more methods exist for the extraction of PCBs from soils and sediments than for extraction from biological tissue. J. Chromatogr. Kannan, K., K.A.Maruya, and S.Tanabe. Available: http://www.epa.gov/epaoswer/hazwaste/test/sw846.htm. For sediments and soils, sample extracts are cleaned with copper and silica gel. Some circuit design solutions need to be considered for waterproofing, especially when they are produced in large quantities, generation costs, environmental protection issues, process capabilities, etc. In addition, the NOAA NS&T method is presented. 1998. 1992. 1997. Through slice analysis, you can get rich information about the microstructure of the PCB (through-holes, plating, etc. 1–51 in Sampling and Analytical Methods of the National Status and Trends Program, National Benthic Surveillance and Mussel Watch Projects 1984–1992, Vol. overestimated the concentrations determined by summing the concentrations of individual congeners. and no ortho positions, are clearly the most toxic congeners of PCBs (Giesy and Kannan 1998). This method determines and quantifies PCB Aroclors as outlined in the following methods: EPA method 508, 608, EPA SW-846 Method 8082, Webb-McCall, and AOAC 970.52, 983.21. Sci. Environmental Monitoring and Assessment Program EMAP-Estuaries Lousianian Province 1993 Quality Assurance Project Plan. Additional cleanup and instrumental analysis of non-ortho coplanar PCB congeners provide an MDL of 1–10 pg/g for sediment (dry weight) and biological tissue (wet weight). Not a MyNAP member yet? U.S. Army Corps of Engineers. Tillitt, D.E., J.P.Giesy, and G.T.Ankley. The bioassay integrates potential nonadditive interactions among AhR agonists and other compounds by measuring a final receptor-mediated response (Giesy et al. One of the primary purposes of this bioassay is to prioritize samples for more extensive quantification by instrumental analysis. Instrumentation: High-resolution gas chromatography with low-resolution mass spectrometry (HRGC-MS). Environ. Similarly, several other computer programs incorporating multivariate analysis have been developed to normalize PCB concentrations in samples to those in Aroclor standards (Stalling et al. Jinghongyi Pcb (Hk) Co., Limited have been specialized in Pcb Prototype manufacture for many years. Alumina, a porous and granular form of aluminum oxide, is adsorptive and is used to separate classes of organic compounds based on their chemical polarity. These cells express firefly luciferase in response to AhR agonists. Sensitivity can be optimized to detect samples in the low (0.5–1.5 ppm) range. For this reason, the method cannot be used if non-PCB analytes are to be measured in the same extract. For example, microbially mediated anaerobic reductive dechlorination is common in sediments in which chlorines are removed from the PCB biphenyl rings (Bedard and Quensen 1995). Water layer, if any, is discarded. Bedard, D.L., and J.F.Quensen, 3rd. Several studies have confirmed a correlation between the structure-activity relationships for PCBs. Instrumentation: High-resolution gas chromatography with electron capture detection (HRGC-ECD). Adding congeners to the calibration standards and demonstrating acceptable MDLs for those standards might expand the list of 19 PCB analytes. PCB Testing and Inspection Methods 1) PCB Section Analysis- The Most Important Analysis Method in the PCB Industry. Evaluation of these profiles might indicate whether mixed Aroclors were present and the degree of weathering. The method separates classes of compounds based on molecular size. This method is similar to the NOAA National Status and Trends (NS&T) method but is less rigorous than the NOAA method in several ways. Durell, G., and J.Seavey Fredriksson. In most studies, the PCDF and PCN contents were not quantified, and their contribution to technical PCBs-induced toxicity is unknown. 25(1):87–92. The basic method has been used in the NOAA NS&T program since 1984 for the routine analysis of PCB congeners in sediments and biological tissue samples. Method: Extraction and Analysis of PCB and Non-ortho-Coplanar PCBs in Biological Matrices (Cannan and Giesy 1998). The methods below identify between 18 and 78 congeners, which are reported individually or as two or three co-eluting congeners. EPA 821/R-97–001. 1994a. Do you enjoy reading reports from the Academies online for free? [Online]. Heitmuller, P.T., and R.Valente. A sample extract is added to an alumina column, which is eluted with a series of solvents of increasing polarity to isolate PCB. As an example, determination of the concentrations of PCBs based on the COMSTAR algorithm, a statistical procedure to determine total PCBs based on marker congeners and peak ratios (Burkhard and Weininger 1987). Only in the past 10 years has the toxicity of individual congeners been studied. Sci. The method is, TABLE F-4 Immunoassay Method for PCB Screening, EPA method 4020, screening for PCBs by immunoassay, 5 g of soil or sediment, or nonaqueous waste liquids, Soil samples are extracted with methanol and test kit reagents. Table F-5 presents and compares several extraction procedures suitable for soils and sediments with a percent solids content of greater than 20%. 1996. Chem. Draft. Sci. Figure 1 shows the full-scan chromatogram of the standard mixture. Currently there are three general types of EPA methods available for analysis of PCBs in sediment. 1987. Quantification Method: Uses the internal standard method with a decachlorobiphenyl (PCB 209) as the single internal standard is used. Chem. Analytes Measured: PCBs are measured as Aroclor formulations or congener. The cost on a per sample basis ranges from $50 to $500, depending on the sample matrix, number of samples to be analyzed, and extent of quality-assurance-quality-control protocols. Test Methods for Evaluating Solid Waste: Physical/. Most of the early methods were direct adaptations of chlorinated pesticide procedures. ‹¬Ñ1t¶gªa‰òAÖUY 1Ôj'5ßÁ'Äø«õúQð‰Êòðúë‚UµþžyPí8ðÁˆ¾X“j¸z3Û'„ ;ä5";–U^¤®Ë}›5z{sɟÚł\ž+4+ø“I^ÉC)÷`¾ÝÉý¯• 'Á¿±ê!êRM0¹L€ð®~ͱRS¤™jP#^ï”fpǛ‘¿3ÚúmuõPúr¬YŽf€Äv/2›MgãR”þD4EUæOLD†ÜÌï?ß=Ã\«‡6×%èY32 Arch. Note that many PCB extraction and cleanup methods, as well as the analytical methods, are performance based. and principal component analysis (PCA) of PCB congeners may be used to evaluate the linkage between the samples and likely point or nonpoint sources—PCB “fingerprinting” analogous to techniques used to identify fugitive petroleum products (Stout et al 1998). Discussion: This PCB congener method by low-resolution mass spectrometry is a performance-based method based on EPA method 8270b (EPA. Symposium Series 284. However, the FDA has published methods for tissue, as well as NOAA NS&T. Res. View our suggested citation for this chapter. However, the method has several drawbacks that limit its application to screening. Environ. Environmental Protection Agency, Office of Solid Waste and Emergency Response, Washington, DC. Environ. The 12 WHO-Toxic congeners are calibrated over the range 20 - 40,000 pg/L (2.0-4,000 ng/kg). Comparison of ah receptor-mediated luciferase and ethoxyresorufin-o-deethylase induction in H4IIE cells: implications for their use as bioanalytical tools for the detection of polyhalogenated aromatic hydrocarbons. NTIS PB95–187332. Detection limits of individual congeners can be achieved in the lower parts per billion to parts per trillion. Copper plating: The copper foil on a PCB is laminated to the board to provide conductivity, but the quality of the cop Res. Instrumentation: High-resolution gas chromatography with electron capture detection (HRGC-ECD) or electrolytic conductivity detection (ELCD). The above analytical methods must be used with appropriate extraction and extract cleanup techniques to be effective. Otherwise, method 8082 is acceptable for measuring the 19 PCB congeners in environmental samples. MacLeod, W.D., J.W.Brown, A.J.Friedman, D.G.Burrows, O.Maynes, R.W.Pearce, C.A.Wigren, and R.G.Bogar. Speciation and quantitation of aroclors in hazardous wastes based on PCB congener data. A collaborative study of 209 PCB congeners and 6 Aroclors on 20 different HRGC columns. First, the use of single-point extrapolations assumes linear-response factors throughout the range of PCB concentrations to be analyzed, when in fact that assumption, is rarely the case. However, mono-ortho congeners are relatively less toxic than non-ortho congeners. FeSO4 amendments stimulate extensive anaerobic PCB dechlorination. Many research applications, particularly those investigating ecological effects require comprehensive, quantitative, congener-specific analysis of PCBs (Frame 1997). This method is an improvement of earlier iterations of the procedure and provides greater laboratory flexibility. Rev. Analytes Measured: The PCB congeners tested by the method include 78 individual PCB congeners and 28 co-eluting groups of two to three congeners as listed: PCB 1, PCB 3, PCBs 4/10, PCB 6, PCBs 7/9, PCBs 8/5, PCBs 12/13, PCBs 16/32, PCBs 17/15, PCBs 18, PCBs 19, PCBs 21, PCB 22, PCBs 24/27, PCB 25, PCB 26, PCB 28, PCB 29, PCB 31, PCBs 33/20, PCB 40, PCBs 41/64/71, PCBs 42/37, PCB 43, PCB 44, PCB 45, PCB 46, PCBs 47/75, PCB 48, PCB 49, PCB 51, PCB 52, PCB 53, PCBs 56/60, PCB 59 PCB 63, PCB 66, PCBs 70/76, PCB 74, PCB 82, PCB 83, PCB 84, PCB 85, PCBs 87/115/81, PCB 89, PCB 91, PCB 92, PCB 95, PCB 97, PCB 99, PCB 100, PCBs 101/90, PCB 105, PCBs 107/147, PCBs 110/77, PCB 114, PCB 118, PCB 119, PCB 124, PCB 128, PCBs 129/126, PCB 130, PCB 131, PCB 132, PCB 134, PCBs 135/144, PCB 136, PCB 137, PCBs 138/160/163, PCBs 141/1709, PCB 146, PCBs 149/123, PCB 151, PCB 153, PCB 156, PCB 158, PCB 167, PCB 169, PCBs 170/190, PCBs 171/202, PCB 172, PCB 173, PCB 174, PCB 175, PCB 176, PCB 177, PCB 178, PCB 180, PCB 183, PCB 184, PCB 185, PCBs 187/182, PCB 189, PCB 191, PCB 193, PCB 194, PCBs 195/208, PCB 197, PCB 198, PCB 199, PCB 200, PCBs 201/157, PCBs 203/196, PCB 205, PCB 206, PCB 207, PCB 209 (PCB congeners presented as PCB/PCB represent co-eluting PCB peaks under most analytical conditions. 1993). Typically for tissue samples, sample extracts are cleaned with alumina and size-exclusion high-pressure liquid chromatography (HPLC). The discrepancies in the congener composition between the commercial mixture and real-world environmental exposures imply that the predictive value of studies based on commercial mixtures might be limited with respect to estimating risks from environmental exposure. The utility of the two GC-based methods of PCB analysis (Aroclor and congener-specific), based on costs and benefits, is summarized in Table F-1. The use of decachlorobiphenyl (PCB 209) as an internal standard will result in negative bias if Aroclor 1268 is present in environmental samples (Aroclor 1268 contains 4.8% of PCB 209) (Kannan et al. The method for the analysis of chlorinated biphenyl congeners (CBC) in water, soil, sludge, tissue (non-human), biosolid, ash, oil, and oily matrix samples is based on EPA method 1668C (using HRSM01.2 SOW). Typically for tissue samples, sample extracts are cleaned with alumina and size-exclusion HPLC. Solvent is exchanged to hexane or other solvent for cleanup and analysis. October. Environmental Protection Agency Region 2, New York, NY. Typical approaches for handling PCB congener data include. In contrast, certain aquatic animals selectively enrich arylhydrocarbon receptor (AhR)-active congeners, an enrichment that can result in greater relative proportion of these toxic congeners in tissues than in technical mixtures (Williams et al. The steps involved may leverage technologies and tools to zoom in on factors that lead to the problems and provide input for PCB designers for remedial actions. Discussion: The surrogate compound is spiked into the sample, the sample is then extracted by an appropriate method, and the extract is concentrated. However, because of the ease of use and rapidity, the method is often used for field screening of PCBs. Decachlorobiphenyl (PCB209) is used as a surrogate to determine recovery. Thus, this method might not be suitable for calculating TODD-equivalent concentrations. Method: EPA SW 846 Method 8082/PCBs by Gas Chromatography for Congener (EPA 1996a), Analytes Measured: The 19 PCB congeners tested by the method include PCB 1, PCB 5, PCB 18, PCB 31, PCB 44, PCB 52, PCB 66, PCB 87*, PCB 101*, PCB 110, PCB 138*, PCB 141, PCB 151, PCB 153, PCB 170*, PCB 180, PCB 183, PCB 187*, PCB 206.

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