quality control measures described in each of these methods should be followed. Sample quality control guidance is provided in Chapter One of EPA (1986) where applicable. In particular, each run should include: (i) blank sample to evaluate potential contamination of the extract; (ii) spiked samples to determine & recovery; (iii) calibration checks at the beginning and end of each run to monitor instrument drift (additional checks may be required by the analytical method); (iv) sample replication to assess precision (in the case of animal tissues for the bioaccumulation testing, 3 sub-samples of the homogenate from one of the five replicates in the test treatments for each of the 3 species must also be analyzed for the chemical constituents of concern); and (v) analyses of sediment and/or tissue standard such as those available from the National Institute of Standards and Technology (Formerly the National Bureau of Standards) or the National Research Council of Canada. Information on acquiring these materials is provided in Appendix I of this document. This provide a check on extracation efficiencies and general analytical accuracy. All data required in i through iv should be reported on the appropriate Forms provided in Chapter One of SW 846 (EPA 1986). The laboratory may also be required to analyze a "blind" sample on an annual basis to assess the lab's general performance. Failure to adequately perform these analyses or the above stated quality control measures will lead to rejection of the data by the COE. 3. Bioassay/Bioaccumulation Testing All bioassay/bioaccumulation testing procedures must follow the methods outlined in EPA/COE (1978) with the modifications described in Sections D and E. A11 bioassays must be performed at 20° C (±2°) in either natural seawater or a synthetic seawater adjusted to 30 ppt salinity. If a synthetic seawater is used, the mixture must be allowed to age sufficiently prior to use. If natural seawater is used, the influent water must be checked at the start and finish of each test for all compounds that will be analyzed as part of the bioaccumulation testing. Reference and control sediments must be collected from the locality specified in Section A. Bulk testing must be 25 performed for each new batch of sediment. Control bioassays must maintain an average of 90% survival rate among the the replicates for each species tested. Failure to maintain the survival rates will invalidate the testing procedures and require retesting of the control, reference, and test samples. Standard toxicant tests must be performed on on species used in the suspended particulate phases when this test this test is required. The procedures required for for this test are described in Appendix II. 4. Internal Laboratory Quality Assurance 5. Before performing the tests, the laboratory must submit their current Quality Assurance Manual (QAM) for review by the regional COE/NED office. Once the QAM manual is accepted annually, only documentation of that approval is necessary. The manual should include the following: (a) (b) A list of all analytical equipment (make, model and year) and devices used in the biological and chemical work, laboratory calibration methods, precision and accuracy standards, number of times standards are checked, maintenance schedules, record keeping methods, personnel responsibilities, and source of test animals. Labeling system employed to ensure proper tracking of samples from collection through analysis to within the chain of custody procedure documented in the final report. Laboratory Inspections The laboratory facilities are subject to periodic inspection by COE/NED and EPA personnel. Original copies of data, records, and quality control concerning sediment testing for a client for a Department of the Army permit must be maintained for a period of at least five (5) years and must be available during laboratory inspections. Such The COE/NED may require analysis of quality control samples by any laboratory for the purpose of determining compliance with its analytical requirements. samples shall be performed at least once per calendar year or as requested by the COE. The laboratory shall provide the COE/NED with the analytical results from such quality control samples upon request. The COE/NED will periodically inspect laboratories for the purpose of evaluating their capabilities in performing the requirements specified in the Guidance Manual. 26 REFERENCES APHA/AWWA/WPCF. 1985. Standard Methods for Examination of Water and Wastewater. 16th Ed. American Public Health Assoc., Washington, D.C. 1268 pp. Battelle. 1985. Method for Semivolatile Organic Priority Pollutants in Fish, Final Report. EPA Contract No. 68-03-1760 EPA, Washington, D.C. Environmental Protection Agency (EPA)/Corps of Engineers (COE). 1978. Ecological evaluation of proposed discharge of dredged material into ocean waters, April 1978. U.S. Army Engineer Waterways Experiment Station, Vicksburg, MS. Environmental Protection Agency (EPA). 1986. SW-846 Test methods for evaluating solid waste. U.S. EPA, Office of Solid Waste and Emergency Response, Washington, D.C. Folk, R. 1974. Petrology of Sedimentary Rocks. Publishing Co., Austin, TX. Hemphill Guy, H.P. 1969. Laboratory Theory & Methods for Sediment Analysis. Book 5; U.S. Geological Survey, 55 pp. Palermo, M.R. 1986. Development of a Modified Elutriate Test for Estimating the Quality of Effluent for Confined Dredged Material Disposal Areas. Technical Report D-86-4. U.S. Army Corps of Engineers Waterways Experiment Station, Vicksburg, MS. Palermo, M.R. M.R. and E.L. Thackston. 1988. Refinement of Column Settling Test Procedures for Estimating the Quality of Effluent from Confined Dredged Material Disposal Areas. Technical Report D-88-9. U.S. Army Corps of Engineers Waterways Experiment Station, Vicksburg, MS. Swartz, R.C., W.A. De Ben, J.K.P. Jones, J.O. Lamberson and F.A. Cole. 1985. Phoxocephelid Amphipod Bioassay for Marine Sediment Toxicity. In: Aquatic Toxicology and Hazard Assessment; Seventh Symposium, ASTM STP 854, R.D. Cardwell, R. Purdy & R.C. Bahner (eds.). American Society for Testing and Materials, Philadelphia, PA pp. 284-307. Tetra Tech, Inc. 1986 a. Analytical Methods for U.S. EPA Priority Pollutants and 301 (h) Pesticides in Estuarine and Marine Sediments. Final Report. EPA Contract No. 69-01-6938. Office of Marine & Estuarine Protection, EPA, Washington, D.C. Tetra Tech, Inc. 1986 b. Bioaccumulation Monitoring Guidance: 4. Analytical Methods for U.S. EPA Priority Pollutants and 301 (h) Pesticides from Estuarine and Marine Organisms. EPA Contract No. 68-01-6938. Office of Marine and Estuarine Protection, EPA, Washington, D.C. U.S. Army Corps of Engineers (COE). 1985. USACOE Permit Program, A Guide for Applicants. Pamphlet EP1145-2-1. May, 1985. COE/NED, Waltham, MA. 28 Harbor Marine Sediments (4) HS-3, HS-4, HS-5, HS-6 PAH NRCC1 Send requests and price list to the following addresses: National Research Council of Canada Marine Analytical Chemistry Standards Program Division of Chemistry Montreal Road Ottawa, Ontario, Canada K1AOR9 Telephone (613) 933-2359 National Institute of Standards & Technology (NBS Standard Reference Material Catalog) Office of Standard Reference Materials Gaithersburg, MD 20899 Telephone (301) 975-6776 U.S. Environmental Protection Agency Quality Assurance & Research Division Rm. 525 EMSL-Cincinatti Cincinatti, Ohio 45268 Telephone (513) 569-7325 Available free on limited basis (2 per quarter year) |