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New and Revised Clean Water Act Methods Proposed

September 23rd, 2010

New and Revised Clean Water Act Methods ProposedIn August 2010 the EPA issued a notice proposing new and revised analytical methods to be used under the Clean Water Act (CWA).

The proposed rule, entitled “Guidelines Establishing Test Procedures for the Analysis of Pollutants Under the Clean Water Act; Analysis and Sampling Procedures”, will affect numerous EPA Methods, ASTM Methods, Standard Methods, and alternative test methods.

EPA methods:

  • Method 1664B – N-Hexane Extractable Material (HEM; Oil and Grease) and Silica Gel Treated N-Hexane Extractable Material (SGTHEM; Non-polar Material) by Extraction
  • Method 200.5 – Determination of Trace Elements in Drinking Water by Axially Viewed Inductively Coupled Plasma – Atomic Emission Spectrometry
  • Method 525.2 – Test Methods for Pesticide Active Ingredients
  • Method1614A – Brominated Diphenyl Ethers in Water, Soil, Sediment, and Tissue by HRGC/HRMS
  • EPA Method 1668C – Chlorinated Biphenyl Congeners in Water, Soil, Sediment, Biosolids, and Tissue by HRGC/HRMS
  • Method 1622 – “Cryptosporidium in Water by Filtration/IMS/FA” and Method 1623, “Cryptosporidium and Giardia in Water by Filtration/IMS/FA
  • Methods 1103.1, 1106.1, 1600, 1603, and 1680
  • Method 1627 – Kinetic Test Method for the Prediction of Mine Drainage Quality
  • Method 624 – Purgeables

ASTM methods:

  • D2036-09 – Standard Test Methods for Cyanides in Water
  • D6888-09 – Standard Test Method for Available Cyanide with Ligand Displacement and Flow Injection Analysis Utilizing Gas Diffusion Separation and Amperometric Detection
  • D7284-08 – Standard Test Method for Total Cyanide in Water by Micro Distillation followed by Flow Injection Analysis with Gas Diffusion Separation and Amperometric Detection
  • D75 11-09e2 – Standard Test Method for Total Cyanide by Segmented Flow Injection Analysis, In-Line Ultraviolet Digestion and Amperometric Detection
  • D7237-10 – Standard Test Method for Free Cyanide with Flow Injection Analysis Utilizing Gas Diffusion Separation and Amperometric Detection; This method determines free cyanide with the same instrumentation and technology as currently approved methods ASTM D6888-09 and OIA 1677-09
  • D888-09 – Standard Test Method for Dissolved Oxygen in Water; This method may be used for biological oxygen demand and carbonaceous oxygen demand
  • D7573-09 – Standard Test Method for Total Carbon and Organic Carbon in Water by High Temperature Catalytic Combustion and Infrared Detection
  • D7065-06 – Standard Test Method for Determination of Nonylphenol, Bisphenol A, p-tert-Octylphenol, Nonylphenol Monoethoxylate, and Nonylphenol Diethoxylate in Environmental Waters by Gas Chromatography Mass Spectrometry
  • D7574-09 – Standard Test Method for Determination of BPA in Environmental Waters by Liquid Chromatography/Tandem Mass Spectrometry
  • D7485-09 – Standard Test Method for Determination of NP, OP, NP1EO, and NP2EO in Environmental Waters by Liquid Chromatography/Tandem Mass Spectrometry

In addition, the EPA has proposed adding eight alternate test procedures:

  • Hach Company’s Method 10360 – Luminescence Measurement of Dissolved Oxygen in Water
  • In-Situ Incorporated’s Method 1002-8-2009 – Dissolved Oxygen Measurement by Optical Probe
  • In-Situ Incorporated’s Method 1003-8-2009 – Biochemical Oxygen Demand (BOD) Measurement by Optical Probe
  • In-Situ Incorporated’s Method 1004-8-2009 – Carbonaceous Biochemical Oxygen Demand (CBOD) Measurement by Optical Probe
  • Mitchell Method M5271 and M5331 – uses laser based nephelometry to measure turbidity in drinking water and wastewater
  • Thermo Scientific’s Orion Method AQ4500 – uses LED based nephelometry to measure turbidity
  • Systea Scientific, LLC’s Systea Easy (1-Reagent) Nitrate Method – uses automated discrete analysis and spectrophotometry to determine concentrations of nitrate and nitrite combined or singly

The Standard Methods to be impacted, include those for oil and grease, ammonia, boron, inorganic ions, arsenic, selenium, aluminum, beryllium, chemical oxygen demand, phosphorous, oxygen, potassium, silica, sulfate and sulfide.

In addition, EPA is proposing minimum quality control requirements to improve consistency across method versions; corrections to previously approved methods; and various changes to sample collection, preservation, and holding time requirements.

For complete information on these methods read the proposed rule by visiting

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3 Responses to “New and Revised Clean Water Act Methods Proposed”

  1. curtis p chun Says:

    the intention of upgrading monitoring compliance standards is to accurately depict pollutants discharge as it relates to sustaining an appropriate environment.

    timeliness of this depiction has been benefited by technological advances and applications.

    careful review and incorporation of the upgrade into operational procedures of commercial industrial municipal entities generating and discharging pollutants need to theme this same intent.

    otherwise benefit is unachieved even with the announced upgrade.

  2. Bahi Says:

    Regarding method OIA-1677 for Available Cyanide. The method requires a field pretreatment sample if sulfide is found in the sample. This pretreatment must take 15 minutes after collecting the sample. I heard that there is no need for such pretreatment in the field as long as the concentration of sulfide is less than 50 mg/l and the sample will be treated at the laboratory for removing sulfide using acid reagents. I want to know if such information is correct and if yeas where I can find this alternative to field pretreatment of Av,CN in the field for removing sulfide. Thanks and have a pleasant evening.

  3. Tom Kissinger Says:

    Bahi, Here’s what I found in the method:

    7.10 Sample Preservation Reagents
    7.10.1 The presence of sulfide may result in the conversion of cyanide to thiocyanate. While lead acetate test paper has been recommended for determining the presence of sulfide in samples, the test is generally unreliable and is typically not usable for sulfide concentrations below approximately 1ppm. The use of lead carbonate (Aldrich Chemical Co. Catalog No. 336378, or equivalent), followed by immediate filtration of the sample is required whenever sulfide ion is present. If the presence of sulfide is suspected but not verifiable from the use of lead acetate test paper, two samples may be collected, one without lead carbonate addition and another with lead carbonate addition followed by immediate filtration. Analyze both samples. If sulfide is present, the preserved sample should contain higher levels of cyanide than the unpreserved sample. Lead acetate test paper may be used, but should be tested for minimum level of sulfide detection by spiking reagent water aliquots with decreasing levels of sulfide and determining the lowest level of sulfide detection attainable. The spiked samples are tested with lead acetate test paper moistened with acetate buffer solution. The buffer solution is prepared by dissolving 146 g anhydrous sodium acetate, or 243 g sodium acetate trihydrate in 400 mL of reagent water, followed by addtion of 480 g concentrated acetic acid. Dilute the solution to 1L with reagent water. Each new batch of test paper and/or acetate buffer should be tested to determine the lowest level of sulfide ion detection prior to use.
    8.2 Preservation techniques
    8.2.1 Samples containing sulfide ion
    Test the sample with lead acetate test paper (Section 7.10.1) to determine the presence or absence of sulfide ion. If sulfide ion is present, the sample must be treated immediately (within 15 minutes of collection) with sufficient solid lead carbonate (Section 7.10.1) to remove sulfide (as evidenced by the lead acetate test paper), and immediately filtered into another sample bottle to remove precipitated lead sulfide.
    If sulfide ion is suspected to be present, but its presence is not detected by the lead acetate paper test, two samples should be collected. One is treated for the presence of sulfide and immediately filtered, while the second is not treated for sulfide. Both samples must be analyzed. (Tests conducted prior to the interlaboratory validation of this method showed significant and rapid losses of cyanides when lead sulfide was allowed to remain in contact with the sample during holding times of three days or less. As a result, the immediate filtration of samples preserved with lead carbonate is essential (Reference 15.6)).

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