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Pacific Northwest Pretreatment Conference September 2005

Pacific Northwest Pretreatment Conference September 2005. William A. Telliard Director, Analytical Methods Engineering and Analytical Support Branch Office of Science and Technology. NPDES Program. 5 Priority Areas for 2005. Improve Monitoring, Reporting, and Information

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Pacific Northwest Pretreatment Conference September 2005

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  1. Pacific Northwest Pretreatment Conference September 2005 William A. Telliard Director, Analytical Methods Engineering and Analytical Support Branch Office of Science and Technology

  2. NPDES Program

  3. 5 Priority Areas for 2005 • Improve Monitoring, Reporting, and Information • Achieve Overall Gain in Wetlands Quality and Quantity • Restore Impaired Watersheds, Coastal Waters • Advance Sustainable, Affordable Infrastructure • Increase Drinking Water Safeguards Against Pathogens and Other Contaminants

  4. Improve Monitoring, Reporting, and Information • Permitting for Environmental Results • Office of the Inspector General • Effluent Guidelines/Pretreatment Standards • Tools: • PCS → ICIS-NPDES • CROMERRR • e-NOI

  5. Permitting for Environmental Results Mehan August 15, 2003 Memorandum: • Integrity • Efficiency – Tools, Watershed-Permitting • Results – Data, Characterization, Prioritization

  6. Permitting for Environmental Results (cont.) As of April 13, 2005: • 51 Profiles Received to Date • 38 States/Territories Profiles on Web • All Region 3 Profiles Posted

  7. OIG Pretreatment Program Evaluation “EPA Needs to Reinforce Its National Pretreatment Program” Report No. 2004-P-00030, (September 28, 2004) • 3 Objectives • 8 Recommendations • 2 Strategies

  8. OIG Pretreatment Program Evaluation (cont.) • Guidance for EPA & States on IUs (CIUs) in POTWs without Pretreatment Programs • Results-based Measure(s) • Training • TBLL, Streamlining, etc. • Evaluate Resources

  9. Many OIG Evaluations . . . . • Results-based Measure(s) • Pretreatment Program (specifically) • Effluent Guidelines Program • “New” 50-POTW Study? • NPDES Program • “Priority” Permits [Tools: ICIS-NPDES, CROMERRR, e-NOI, etc.]

  10. CWA §304(m) and 304(g) Strategy • 2004 Effluent Guidelines Program Plan September 2, 2004 (69 FR 53705) • Investigate • Drinking Water Supply and Treatment • Airports Deicing Operations • Revise Current Regulations: • Vinyl Chloride Manufacturing (OCPSF) • Chlor-Alkali Manufacturing (Inorganic Chem.) • 2006 Plan to be proposed in August 2005

  11. Methods Update Proposal

  12. Methods Update Proposal • EPA proposed revisions and updates to wastewater and drinking water methods and monitoring regulations on April 6, 2004 (69 FR 18166) • The proposal addressed: • Wastewater Methods • Other Updates to Wastewater Regulations • Drinking Water Methods • Request for Comments on Guidance Document • A final rule is anticipated in late-2005

  13. EPA Office of Water’s Methods Update Rule Starring: Brad Pitt and Zazou Pitts Coming to a theater near you this September!

  14. Coming Attractions • More choices of methods! • More flexible methods! • Easier to modify methods without prior approval!

  15. Updating Water and Wastewater Methods in Part 136

  16. Wastewater Methods • EPA proposed: • Three chemical ATPs for general use in NPDES monitoring: • Waters Corporation Method D6508 for determination of anions by capillary ion electrophoresis • Lachat QuikChem Method 10-204-00-1-X for determination of total cyanide using MICRODIST • Kelada-01 method for determination of total and available cyanide using UV-digestion, flash distillation and colorimetry • One chemical ATP for use in the pulp and paper industry • NCASI Method CP–86.07 for determination of chlorinated phenolics by In situ Acetylation and GC/MS

  17. EPA Method 245.7 for Mercury • EPA proposed EPA Method 245.7, “Mercury in Water by Cold Vapor Atomic Fluorescence Spectrometry.” • The Association of Metropolitan Sewerage Agencies (AMSA) petitioned the Agency to approve Method 245.7 as an alternative to EPA Method 1631. • Both methods use CVAFS and allow for trace analysis of mercury. However, EPA 245.7 uses a lower cost analyte isolation procedure. • In response, EPA conducted a multi-laboratory validation of this method in 2001 to assess the method’s performance. • A detection limit of 5 ng/L was achieved. • In reagent water, average recoveries ranged between 85% to 105%, and relative standard deviations (RSDs) were below 15%. • Recoveries in industrial and municipal effluents ranged from 64% to 120%.

  18. Previously Proposed Methods • EPA reproposed methods from a 10-18-95 proposal. • The methods have been used through interim approvals since that time, so reproposal allowed EPA to receive comments on their use. • Approval of the methods would harmonize approved revisions of drinking water and wastewater versions of inorganic methods, and would formalize approval of new technologies in wastewater monitoring, including: • Inductively Coupled Plasma-Mass Spectrometry (e.g., EPA 200.8) • Stabilized Temperature Graphite Furnace Atomic Absorption Spectroscopy (i.e., EPA 200.9) • Ion Chromatography (e.g., EPA 300.0, EPA 218.6)

  19. VCSB Methods for Wastewater • EPA proposed updated revisions of methods approved from voluntary consensus standards bodies (VCSBs). • Eighty-five (85) revised Standard Methods • Seventy (70) revised ASTM International methods • EPA proposed two new ASTM International methods. • D6888-03: Standard Test Method for Available Cyanide with Ligand Displacement and Flow Injection Analysis (FIA) Utilizing Gas Diffusion Separation and Amperometric Detection • D6919-03: Determination of Dissolved Alkali and Alkaline Earth Cations and Ammonium in Water and Wastewater by Ion Chromatography

  20. Method Flexibility for Wastewater • EPA proposed and requested comment on increased flexibility in methods used for wastewater monitoring. • Under the proposal, analysts would be allowed to modify a method provided that: • The analyte measured is not “method-defined” • The chemistry of the method or the determinative technique are not changed • The performance meets specified performance requirements and is documented

  21. Method Flexibility for Wastewater (cont.) • Potentially allowable changes include: • Changes between automated and manual discrete instrumentation • Changes in the calibration range (provided that the modified range covers any relevant regulatory limit) • Changes in equipment, such as using similar equipment from a vendor other than that mentioned in the method • Changes in equipment operating parameters, such as changing the monitoring wavelength of a colorimeter • Increases in purge-and-trap sample volumes • Use of salts and inert surfactants to improve recovery in hard-to-analyze matrices

  22. Sampling Collection, Handling, and Preservation • EPA proposed updates to grab and composite sampling requirements at 40 CFR parts 122, 136, and 403. • Resolve inconsistencies that currently exist • Allow composite samples for oil and grease • The proposal revised sample collection, handling, and preservation requirements, including: • Raising the maximum holding temperature from 4oC to 6.00oC • Revising preservation procedures for Cr(VI) and extending the holding time from 24 hours to 28 days • Suggesting metals samples be preserved in the lab, not the field • Removing requirement for icing metals samples for shipment • Updating holding time requirements based on new studies

  23. Cyanide Update • EPA requested comment on revisions to the cyanide sample preservation requirements. • Based on comments, EPA is removing ascorbic acid preservation and adding footnotes to address interferences from: • Sulfur • Sulfide • Thiocyanate • Aldehydes • Carbonates • Chlorine and hypochlorite

  24. Withdrawal of MCAWW Methods • EPA proposed to withdraw approval at 40 CFR 136 for 109 MCAWW methods and retain 30 methods or replace them with newer versions of the same numbered method. • The majority are single-analyte 200-Series methods for metals. • Older methods for metals are largely supplanted by multi-analyte methods such as 200.7, 200.8, and 200.9, or newer VCSB methods that utilize the same analytical techniques as the methods to be withdrawn. • MCAAW methods contain minimal QC requirements compared to VCSB and newer EPA methods.

  25. Withdrawal of MCAWW Methods (cont.) • EPA proposed the withdrawal of Method 413.1, the Freon-based oil and grease method • Effective date of withdrawal would coincide with the end of the laboratory-use exemption, proposed to occur on December 31, 2005. • Hexane-based methods would serve as the sole standard for oil and grease measurements.

  26. Comments • EPA received over 100 comments on the proposal from: • Wastewater and drinking water utilities • Academics • Industry or trade groups • Method developers • VCSBs • State regulatory agencies • Citizens

  27. Comments (cont.) • Significant areas of concern were: • Cyanide distillation methods, particulate cyanides, and interferences • “Total recoverable” digestion for metals • Withdrawal of older MCAWW methods • Proposed use of Microtox • EPA’s approach to approving modified methods • Default QC and reporting requirements for new or revised methods • In addition, collectively, the comments brought to light over 100 typographical errors introduced into the tables in Parts 136 and 141 by the Office of the Federal Register during typesetting.

  28. For Further Information • The Methods Update Rule • Marion Kelly, kelly.marion@epa.gov • 202-566-1045 • Water and Wastewater Methods • William A. Telliard, telliard.william@epa.gov • 202-566-1061 • Don’t call after January 5, 2006 … • Drinking Water Methods • Herb Brass, brass.herb@epa.gov • 513-569-7936

  29. Methods Activities and Studies

  30. Methods Activities and Studies • Methods Development • Detection and Quantitation Efforts • National Studies • Contacts

  31. Methods Development

  32. Development and Validation of EPA Method 1614 • Method 1614: GC/high resolution MS method for determination of polybrominated diphenyl ethers (PBDEs) - brominated flame retardants • Developed at Axys Analytical • 8 PBDEs of primary concern – measured by isotope dilution • 36 other PBDE congeners – measured by internal standard • Draft method has been available since September 2003 • Single-laboratory validation underway • Two laboratories analyzing two samples of each matrix • 3 matrices (POTW effluent, industrial effluent, and fish tissue) • Data to be evaluated this winter, report in Spring 2005

  33. EPA/ASTM Study of Deuterated Solvents for Determination of Oil and Grease by I-R • In collaboration with ASTM D 19 • U.S. Navy preliminary studies • Deuterated methylene chloride shows some promise; deuterated n-hexane and deuterated toluene do not

  34. EPA/ASTM Method for Oil and Grease, and TPH, by Infra-red Spectrometry • Background • Existing I-R method for determination of total petroleum hydrocarbons (TPH) in wastewater is EPA Method 418.1 • EPA Method 418.1 is not approved at 40 CFR part 136 • EPA Method 418.1 uses CFC-113 (Freon-113) as the extraction solvent • Use of CFC-113 produced or imported after December 31, 2001, is banned for wastewater testing – only “old” Freon may be used • EPA has withdrawn Method 413.1 (gravimetric) from 40 CFR part 136 • Status of EPA/ASTM method • ASTM method written by Wilks Instruments • ASTM method approved through ballot in 2004 (designated D7066-04) • Method uses Flon S-316 (dimer/trimer of chlorotrifluoroethylene) as extraction solvent • EPA plans to propose ASTM method with next update to part 136. We expect to approve it as an ATP for use in the mean time.

  35. EPA/ASTM Method for NP and APEs • Nonylphenol (NP) and alkylphenol ethoxylates (APEs) are surfactants • EPA is working collaboratively with ASTM to develop and validate method • Status of EPA/ASTM method • Draft method written by Schenectady International, Inc. • Draft method balloted and revised • Interlaboratory validation study planned for late 2005 • Holding time study has been performed by EPA Region V • Standards and samples to be provided by EPA • Laboratories would be nearly all volunteers (any takers?) • Expect final ballot in 2006 • EPA would propose after ASTM approval

  36. GC/HRMS Method for Pesticides • Greater specificity • Lower detection limits • Focus on biosolids • Supports recommendations of the National Research Council • Begin multiple single-lab validation studies in late 2005 • To be tested in POTW influents and effluents, as well as a number of drinking water facilities

  37. GC/HRMS Method for Pesticides (cont.) • Target analytes will include: • 34 organochlorine pesticides • 21 organophosphorus pesticides • 7 triazine herbicides • 3 pyrethroid pesticides

  38. Assessment of Detection and Quantitation Concepts • EPA is assessing existing and alternative procedures for determining the sensitivity of analytical test methods. • The results of EPA’s initial assessment were released to the public through a Federal Register notice published in March 2003. • Based on this assessment, EPA proposed revisions to the Minimum Detection Limit (MDL) procedure at 40 CFR part 136, Appendix B. Also published in March 2003. • EPA held a public meeting on the results of its detection and quantitation limits assessment on May 1, 2003, in Chicago, IL.

  39. Assessment of Detection and Quantitation Concepts (cont.) • EPA received 136 comment packages on the Agency’s assessment and proposed revisions. • Final notice regarding EPA’s assessment was signed November 1, 2004. • On September 15, 2004 EPA published a Federal Register Notice (69 FR 55547) announcing the Agency’s intent to work with stakeholders towards development of detection and quantitation limits and use of the limits under the Clean Water Act

  40. Federal Advisory Committee (FAC) • EPA conducted a half-day public meeting on January 26, 2005, to present the findings and recommendations in the Situation Assessment Report on Detection and Quantitation Approaches and Uses in Clean Water Act Programs. • The first meeting of the FAC was held June 21 – 22, 2005 in Washington, DC. • Meeting introduced committee members, and developed a technical work group. • First task is identifying definitions of detection and quantitation concepts • Subsequent FAC meetings will be held September 29 - 30 and December 8 - 9, 2005 in Arlington, VA

  41. National Sewage Sludge Survey • EPA conducted its first National Sewage Sludge Survey (NSSS) in 1989 • 180 POTWs, 239 samples, and determination of 412 individual pollutants • EPA conducted a follow-up survey of dioxins and furans in treated sewage sludge in Spring 2001 to support Round Two Sewage Sludge Regulation • 94 POTWs, 113 samples, and determination of 167 individual compounds/congeners • EPA is undertaking a new NSSS in 2005 to determine whether levels of pollutants in treated sewage sludge are lower than in 1989 as a result of improved treatment technologies

  42. National Sewage Sludge Survey • Survey will fulfill a primary recommendation of the NRC Committee on Toxicants and Pathogens in Biosolids Applied to Land • 100 POTWs to be selected from the universe of 16,000+ POTWs nationwide • Analytes include: • Metals - Antimony, Arsenic, Barium, Beryllium, Cadmium, Chromium, Cobalt, Copper, Iron (total), Lead, Manganese, Mercury, Molybdenum, Nickel, Selenium, Silver, Thallium, Zinc • PAHs - Benzo(a)pyrene, Fluoranthene, 2-Methylnaphthalene, Pyrene • Other Organics - bis (2-Ethylhexyl) phthalate, 4-Chloroaniline • Inorganics - Fluoride, Nitrate/Nitrite, Total Phosphorus • Microbiologicals - Fecal Coliform, Salmonella

  43. Upcoming Industries to be Sampled • The Engineering and Analysis Division (EAD) will be sampling the following industries in 2005, in response to EPA’s 304(m) plan: • Airport deicing operations • Tobacco manufacturing • POTWs (sewage) • Vinyl chloride/chlor-alkali plants • Drinking water treatment facilities • Uniform National Discharge Standards (UNDS) for naval vessels • EAD is also sampling Alaskan cruise ship discharges

  44. Contacts SASB Branch Chief Richard Reding (202) 566-2237 Chemical Methods William Telliard (202) 566-1061 Remember - don’t call after January 5, 2006 Biological Methods Robin Oshiro (202) 566-1075

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