Summary Analytes Revision Data and Sites. Official Method Name. The software includes a robust text search engine to allow searches by method number, anlayte name, and key words. This method has 25 analytes associated with it. Octachlorodibenzo-p-dioxin 1,2,3,4,6,7,8,9-Octachlorodibenzo-p-dioxin Dibenzo-p-dioxin, octachloro- Dibenzo[b,e][1,4]dioxin, octachloro- OCDD Octachlorodibenzo-p-dioxin Octachlorodibenzo-p-dioxins. The Water Quality Portal contains sample results from sites that use this method.

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Environmental Protection Agency, and approved for publication. Mention of trade names or commercial products does not constitute endorsement or recommendation for use. Specifications are also provided for separate determination of 2,3,7,8-tetrachloro- dibenzo-p-dioxin 2,3,7,8-TCDD and 2,3,7,8-tetrachloro-dibenzofuran 2,3,7,8-TCDF.

Each laboratory that uses this method must demonstrate the ability to generate acceptable results using the procedure in Section 9. The analyst is permitted to modify the method to overcome interferences or lower the cost of measurements, provided that all performance criteria in this method are met. The requirements for establishing method equivalency are given in Section 9. The extract is concentrated for cleanup. The methylene chloride extract is concentrated and combined with the SDS extract prior to cleanup.

The filter and disk are extracted in an SDS extractor, and the extract is concentrated for cleanup. Samples containing multiple phases are pressure filtered and any aqueous liquid is discarded. Coarse solids are ground or homogenized. Any non-aqueous liquid from multi-phase samples is combined with the solids and extracted in an SDS extractor. The sample is mixed with sodium sulfate, allowed to dry for 12 - 24 hours, and extracted for hours using methylene chloride:hexane in a Soxhlet extractor.

The extract is evaporated to dry ness, and the lipid content is determined. After equilibration, mL of hydrochloric acid and mL of methylene chloride:hexane are added, and the bottle is agitated for hours. The extract is evaporated to dryness, and the lipid content is determined.

After extraction, 37Q4-labeled 2,3,7,8-TCDD is added to each extract to measure the efficiency of the cleanup process. High-performance liquid chromatography HPLC can be used for further isolation of the 2,3,7,8- isomers or other specific isomers or congeners. Prior to the cleanup procedures cited above, tissue extracts are cleaned up using an anthropogenic isolation column, a batch silica gel adsorption, or sulfuric acid and base back-extraction, depending on the tissue extraction procedure used.

After cleanup, the extract is concentrated to near dryness. The non-2,3,7,8 substituted isomers and congeners are identified when retention times and ion-abundance ratios agree within predefined limits. Specific selection of reagents and purification of solvents by distillation in all-glass systems may be required. Where possible, reagents are cleaned by extraction or solvent rinse. Sonication of glassware containing a detergent solution for approximately 30 seconds may aid in cleaning.

Glassware with removable parts, particularly separatory funnels with fluoropolymer stopcocks, must be disassembled prior to detergent washing.

The tap water rinse is followed by. All materials used in the analysis shall be demonstrated to be free from interferences by running reference matrix method blanks initially and with each sample batch samples started through the extraction process on a given hour shift, to a maximum of 20 samples.

For example, a reference sample of human adipose tissue containing pentachloronaphthalene can be used to exercise the cleanup systems when samples containing pentachloronaphthalene are expected. Interferences coextracted from samples will vary considerably from source to source, depending on the diversity of the site being sampled. The most frequently encountered interferences are chlorinated biphenyls, methoxy biphenyls, hydroxydiphenyl ethers benzylphenyl ethers, polynuclear aromatics, and pesticides.

Each piece of reusable glassware should be numbered to associate that glassware with the processing of a particular sample. This will assist the laboratory in tracking possible sources of contamination for individual samples, identifying glassware associated with highly contaminated samples that may require extra cleaning, and determining when glassware should be discarded.

The lipid contents of different species and portions of tissue can vary widely. Lipids must be removed by the lipid removal procedures in Section Exposure to these compounds should be reduced to the lowest possible level. It is soluble in water to approximately ppt and in organic solvents to 0. A reference file of material safety data sheets MSDSs should also be made available to all personnel involved in these analyses.

It is also suggested that the laboratory perform personal hygiene monitoring of each analyst who uses this method and that the results of this monitoring be made available to the analyst. Additional information on laboratory safety can be found in References The references and bibliography at the end of Reference 13 are particularly comprehensive in dealing with the general subject of laboratory safety.

Well- ventilated, controlled access laboratories are required. Assistance in evaluating the health hazards of particular laboratory conditions may be obtained from certain consulting laboratories and from State Departments of Health or Labor, many of which have an industrial health service.

Each laboratory must develop a strict safety program for handling these compounds. The practices in References 2 and 14 are highly recommended. Gross losses to the laboratory ventilation system must not be allowed. During analytical operations that may give rise to aerosols or dusts, personnel should wear respirators equipped with activated carbon filters.

Eye protection equipment preferably full face shields must be worn while working with exposed samples or pure analytical standards.

Latex gloves are commonly used to reduce exposure of the hands. Plastic bag liners should be used in waste cans. Janitors and other personnel must be trained in the safe handling of waste. Satisfactory cleaning may be accomplished by rinsing with. Chlorothene, then washing with any detergent and water. If glassware is first rinsed with solvent, then the dish water may be disposed of in the sewer. Given the cost of disposal, it is prudent to minimize solvent wastes. Persons who convey the bags and launder the clothing should be advised of the hazard and trained in proper handling.

The clothing may be put into a washer without contact if the launderer knows of the potential problem. The washer should be run through a cycle before being used again for other clothing. Extraction and analysis by GC with an electron capture detector BCD can achieve a limit of detection of 0. Less than 0. A secondary containment system around the shaker is suggested to prevent the spread of acid and solvents in the event of such a breakage.

The speed and intensity of shaking action should also be adjusted to minimize the possibility of breakage. Equivalent performance may be achieved using apparatus and materials other than those specified here. Meeting the performance requirements of this method is the responsibility of the laboratory. Caps shall be lined with fluoropolymer. Only glass or fluoropolymer tub- ing shall be used. If the sampler uses a peristaltic pump, a minimum length of compressible silicone rubber tubing may be used in the pump only.

Before use, the tubing shall be thoroughly rinsed with methanol, followed by repeated rinsing with reagent water to minimize sample contamination. An integrating flow meter is used to collect proportional composite samples. Store in a bottle with a fluoropolymer-lined screw-cap. Break up aggregates with a stirring rod until a uniform mixture is obtained.

The same type of alumina must be used for all samples, including those used to demonstrate initial precision and recovery Section 9. Use within five days of baking. Store in a dessicator. Soxhlet extract in g portions for 24 hours. Pack with 1. Use within 90 minutes of cooling.

Cut paper to simulate the surface area of the paper sample being tested. May be prepared by extraction with methylene chloride. When not being used, standards are stored in the dark at room temperature in screw-capped vials with fluoropolymer-lined caps. A mark is placed on the vial at the level of the solution so that solvent loss by evaporation can be detected. If solvent loss has occurred, the solution should be replaced.

Stock solutions. Observe the safety precautions in Section 5, and the recommendation in Section 5. For example, weigh 1 to 2 mg of 2,3,7,8-TCDD to three significant figures in a mL ground-glass- stoppered volumetric flask and fill to the mark with nonane.

After the TCDD is completely dissolved, transfer the solution to a clean mL vial with fluoropolymer- lined cap. Reference standards that can be ' used to determine the accuracy of calibration standards are available from CIL and may be available from other vendors.

When diluted, the solution will become the PAR Section 7. This solution is diluted with acetone prior to use Section 7. Each sample requires 1. The cleanup standard is added to all extracts prior to cleanup to measure the efficiency of the cleanup process.

Dilute 10 uL of the precision and recovery I standard Section 7. One mL each are required for the blank and OPR with each matrix in each batch. GC retention time window defining solution and isomer specificity test standard Used to define i the beginning and ending retention times for the dioxin and furan isorners and to demonstrate isomer specificity of the GC columns employed for determination of 2,3,7,8-TCDD and 2,3,7,8- I TCDF.

In this case, an isomer-specificity I test standard containing the most closely eluted isomers listed in Table 5 CIL EDF, or j equivalent may be used.

Aqueous samples that flow freely are collected in refrigerated bottles using automatic I sampling equipment. Solid samples are collected as grab samples using wide-mouth jars. If residual chlorine is present in aqueous samples, add 80 mg sodium thiosulfate per i liter of water. EPA Methods If sample pH is greater than 9, adjust to pH with sulfuric acid.


EPA Method 1613B

Reiner 3 , Peter Gorst-Allman 4 1. National Metrology Institute of South Africa, 2. Restek Corporation, 3. Ontario Ministry of the Environment, 4. LECO Africa. Link: www.



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