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Status of Methods and Method Regulations in EPA’s Water Programs. ASTM D19 Meeting Cocoa Beach, Florida January, 2006 Dale Rushneck, Interface, Inc. Methods Update Proposal.

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Status of methods and method regulations in epa s water programs l.jpg

Status of Methods and Method Regulationsin EPA’s Water Programs

ASTM D19 Meeting

Cocoa Beach, Florida

January, 2006

Dale Rushneck, Interface, Inc.


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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 Spring 2006


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Wastewater Methods

  • EPA proposed:

    • Three chemical ATPs for general use in NPDES monitoring:

      • ASTM International 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


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EPA Method 245.7 – Mercury by CVAFS

  • 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.

    • However, EPA 245.7 omits the gold traps.

  • EPA conducted a inter-laboratory study of Method 245.7 in 2001.

    • Method detection limit = 5 ng/L.

    • Average recovery = 85 – 105% in reagent water.

    • Relative standard deviation (RSD) in reagent water <15%.

    • Average recovery in industrial and municipal effluent = 64 – 120%


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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 for 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)


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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


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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


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Sampling Collection, Handling, and Preservation

  • 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


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Cyanide Preservation

  • Based on comments and on ASTM D19 discussions, EPA is revising cyanide preservation to:

    • Remove ascorbic acid as a preservative

    • Add sodium borohydride and sodium arsenite as preservatives

  • EPA is revising preservation requirements to address interferences from:

    • Sulfur

    • Sulfide

    • Thiocyanate

    • Aldehydes

    • Carbonates

    • Chlorine and hypochlorite


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Turbidity Update

  • EPA reproposed use of an alternative primary turbidity calibration standard (AMCO-AEPA-1 or AMCO-Clear)


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Withdrawal of MCAWW Methods

  • EPA proposed to withdraw 109 Methods for Chemical Analysis of Water and Wastes (MCAWW) from 40 CFR part 136, 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.


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Withdrawal of MCAWW Methods (cont.)

  • EPA proposed to withdraw Method 413.1, and other Freon-based oil and grease methods

    • Freon is presently banned for testing oil and grease, and total petroleum hydrocarbons (TPH), in wastewater.

    • EPA has been accepting data from tests using “old” Freon (made or imported prior to 2002) until Freon-base methods are withdrawn.

    • After withdrawal, hexane-based methods would serve as the sole standard for oil and grease measurements.

    • EPA may propose ASTM S-316-based method in future.


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New Drinking Water Methods

  • EPA proposed four new chemical ATPs for drinking water monitoring:

    • ASTM Method D6508 for the determination of anions by capillary ion electrophoresis

    • Industrial Test Systems (ITS) free chlorine test strip method

    • OI Analytical Method 1677-DW for determination of available cyanide by ligand exchange and amperometry

    • Georgia Institute of Technology’s method for “The Determination of Radium-226 and Radium-228 in Drinking Water by Gamma-ray Spectrometry Using HPGE or Ge(Li) Detectors”


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New Drinking Water Methods (cont.)

  • EPA proposed the addition of EPA Method 327.0 to 40 CFR 141.74 for the measurement of chlorine dioxide residuals.

  • EPA proposed updated revisions of methods approved from voluntary consensus standards bodies (VCSBs).

    • Fifty-two (52) revised Standard Methods

    • Twenty-four (24) 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


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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


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Notice of Data Availability – 2/16/05 (70 FR 7909)

  • The NODA announced the availability of new information on methods for wastewater analyses (40 CFR 136):

    • A microdistillation procedure for cyanide and its ability to recover particulate forms of cyanide

    • Total Kjeldahl nitrogen (TKN) analyses

    • Mercury analyses

    • Total suspended solids analyses

    • Microtox

    • Method 624 for volatiles

    • Waters Method D6508


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NODA (cont.)

  • The NODA also provides new information on drinking water analyses (40 CFR 141) regarding:

    • Interferences affecting Syngenta Method AG-625

  • Revised versions of VCSB methods proposed in 2004:

    • ASTM D6888-04 for available cyanide

    • ASTM D5673-03 for metals by ICP/MS

    • ASTM D4658-03 for sulfide

  • Revisions to Georgia Institute of Technology’s method for Radium-226 and Radium-228 in Drinking Water by Gamma-ray Spectrometry


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Wastewater Methods Under Development

  • Method 1668A - PCB congeners by GC/HRMS

    • Awaiting method detection limit data from EPA Regional labs

  • Method 1614 - PBDE congeners by GC/HRMS

    • Method being revised to incorporate 15-m column and temperature-programmed injector to improve precision and recovery of BDE 209

  • Nonylphenol and alkylphenol ethoxylates by GC/MS

    • Development in collaboration with ASTM International

    • Development by EPA Region V laboratory


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Wastewater Methods Under Development (cont)

  • Methods to support studies of pollutants discharged from Publicly Owned Treatment Works (POTWs)

    • Based on study by USGS

      • Organo-chlorine and organo-phosphate pesticides by GC/HRMS

      • Herbicides by GC/HRMS

      • Antibiotics by LC/MS/MS

      • Drugs by LC/MS/MS

      • Steroids and hormones by GC/HRMS

  • Kinetic test procedure for prediction of coal mine drainage


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Detection/quantitation FACA Committee

  • EPA created a Federal Advisory Committee Act (FACA) committee to attempt to resolve issues surrounding detection and quantitation in EPA’s wastewater programs

    • Main FACA committee has held three meetings

    • Main FACA committee has established several workgroups

      • Policy workgroup

      • Technical workgroup

        • Workgroup for single-laboratory studies

        • Workgroup for inter-laboratory studies

  • Details at EPA’s FACA Committee web site:

    http://www.epa.gov/waterscience/methods/det/


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