Tenn. Comp. R. & Regs. 0400-45-01-.14 - LABORATORY CERTIFICATION

(1) General
(a) For the purpose of determining compliance with physical, chemical, biological and radiological constituents and maximum contaminant levels set forth in this rule chapter, analyses of samples may be considered only if they have been analyzed by a laboratory certified by the Department. Laboratories which are certified by the Department are designated "state-certified laboratories." Analysis for turbidity, free chlorine residual, temperature, pH, alkalinity, calcium, conductivity, orthophosphate, daily chlorite, and silica may be performed by persons approved by the Department. Approved methodology must be used.
(b) The Tennessee Laboratory Certification Program is established for the purpose of evaluating laboratories to determine technical capability to analyze for one or more groups of the contaminants, disinfectant residuals, disinfection byproducts and disinfectant precursors listed in Rules 0400-45-01-.06 through 0400-45-01-.10, 0400-45-01-.12, 0400-45-01-.21, 0400-45-01-.24 through 0400-45-01-.26, and 0400-45-01-.36 through 0400-45-01-.40. Department laboratory certification officer(s) shall be experienced professional staff members of the Department of Environment and Conservation, Division of Water Resources and certified by the U.S. Environmental Protection Agency. Certification officer(s) shall supervise the certification program.
(c) A laboratory desiring certification in microbiological and/or chemical analysis shall make written application to the Department of Environment and Conservation, Division of Water Resources. The applicant shall indicate those group(s) of contaminants for which it seeks certification:

Chemistry

1. General (wet)
2. Inorganic
3. Organic Chemicals
4. Disinfection Byproducts
5. Polychlorinated Biphenyls (PCBs)
6. Radiochemistry
7. Microbiology
(i) Enzyme Substrate Coliforms
(ii) Membrane Filter Coliforms
(iii) Heterotrophic Plate Count
(iv) Enterococci
(d) The laboratory shall upon request supply to the Department all information requested concerning its equipment, facilities, data, and the qualifications of its laboratory staff. Certified laboratories must have an on-site audit conducted every three years by the certification officer or his/her designee.
(e) A laboratory desiring certification will arrange for an American Association for Laboratory Accreditation (A2LA) approved vendor to send performance evaluation samples to the laboratory for testing pursuant to its proficiency testing program. A2LA approved Performance Evaluation venders can be viewed at: http://www.a2la.org/dirsearchnew/nelacptproviders.cfm. The laboratory's performance in correctly evaluating such sample(s) will be sent to both the laboratory and to the certification officer. All direct costs for the performance evaluation samples will be borne by the laboratory requesting certification.
(f) The certification officer shall review the written report of the laboratory performance evaluation and together with his review of requirements set forth in this rule shall determine the certification ranking.
(g) Certified laboratories must maintain all records and correspondence used to determine compliance with the requirements of these Rules for a period of not less than six (6) years. Adequate information must be available to reconstruct results for compliance and performance evaluation (PE) samples. This includes all raw data, calculations, and quality control data. Electronic data must be backed up by protected tape, hard disk, or other method approved by the Department. Water system clients should be notified before disposing of any records so that they may request copies if needed. Performance evaluation samples shall be analyzed annually.
(h) Certified Laboratories shall comply with all requirements set forth in the latest edition of EPA Manual for the Certification of Laboratories Analyzing Drinking Water except where those requirements differ from the requirements set forth in this chapter.
(2) In order for a laboratory to be certified by the Department:
(a) It must have a written quality assurance (QA) plan which addresses the following parts:
1. Laboratory organization and responsibility.
2. Process used to identify clients' Data Quality Objectives.
3. Standard Operating Procedures with dates of last revision.
4. Field sampling procedures.
5. Laboratory sample receipt and handling procedures.
6. Instrument calibration procedures.
7. Analytical procedures.
8. Data reduction, validation, reporting and verification.
9. Type of quality control (QC) checks and the frequency of their use.
10. List schedules of internal and external system and data quality audits and inter-laboratory comparisons.
11. Preventive maintenance procedures and schedules.
12. Corrective action contingencies.
13. Record keeping procedures.
(i) If a particular part is not relevant, the QA plan should state this and provide a brief explanation.
(ii) All laboratories analyzing drinking water compliance samples must adhere to any required QC procedures specified in the approved method. Documentation for many of the listed QA plan parts may be made by reference to appropriate sections of the latest edition of EPA Manual for the Certification of Laboratories Analyzing Drinking Water, the laboratory's standard operating procedures (SOPs), or other literature (e.g., promulgated methods, Standard Methods for the Examination of Water and Wastewater, etc.). The QA Plan should be updated at least annually.
(b) It must complete the performance evaluation samples as described in paragraph (9) of this rule.
(c) On an annual basis and with each application for certification or recertification, all laboratories except Tennessee public water systems shall convey to the Department, Division of Water Resources, payment for the activities necessary for each group of contaminants for which it desires certification or recertification. All laboratories except Tennessee public water systems shall pay annually an administrative certification fee as listed in the fee schedule. The fee schedule is as follows:

Fee Type

Fee in Dollars

1. Administrative In-State

$1000

2. Administrative Out-of-State

$750

3. General Chemistry-Turbidity, Corrosivity, pH

$500

4. Inorganics - Trace Metals, Sodium, Nitrite, Nitrate, Fluoride, Sulfate, Cyanide, Asbestos, Chlorite, and Bromate

$500

5. Organics

$500

6. Disinfection Byproducts - Trihalomethanes and Haloacetic acids

$500

7. Polychlorinated Biphenyls (PCB)

$500

8. Radiochemistry

$500

9. Enzyme Substrate - Total Coliform and E.-Coli

$500

10. Membrane Filter - Total Coliform, Fecal Coliform, E.-Coli

$500

11. Heterotrophic Plate Count

$500

12. Enterococci

$500
(i) Certification fees shall be retained by the Department even if the laboratory applying for certification does not qualify for certification.
(ii) If the certification fee is not paid within 30 days after the receipt of the invoice, certification of the laboratory is automatically revoked.
(iii) The reinstatement fee for a laboratory that fails to pay its certification fee by the invoice due date shall be $500 in addition to the fees specified in this subparagraph.
(3) Ranking Scheme of Laboratories - Based upon a review of the written application, the facts determined from any inspection, and the results of a laboratory performance evaluation, a certification officer may classify a laboratory as follows for the particular group(s) of contaminants for which it seeks certification:
(a) Certified - A laboratory that meets the minimum requirements as set forth in these rules.
(b) Provisionally Certified - A laboratory which has deficiencies but can still produce valid analytical data.
(c) Not Certified - A laboratory which possesses major deficiencies such that it cannot consistently produce valid analytical data in order to determine compliance with the maximum contaminant level. Analytical data will not be accepted from a laboratory with this ranking.
(d) Interim Certification - Interim certification may be granted in certain circumstances when it is impossible or unnecessary to perform an on-site audit. Interim certification status may be granted if, for example, the Certification Officer determines that the laboratory has the appropriate instrumentation, is using the approved methods, has adequately trained personnel to perform the analyses, and has satisfactorily analyzed PE samples, if available, for the contaminants in question. The Certification Officer should perform an on-site audit as soon as possible but no later than three years. An example of a situation where this type of certification is warranted would be a laboratory that has requested certification for the analysis of additional analytes that involve a method for which it already has certification.
(4) Downgrading Certification Status - A laboratory certified to perform analyses may be downgraded to a Provisionally Certified status for a particular parameter, or for one or more groups of contaminants for which it has been certified for any one of the following reasons:
(a) Failure to analyze a set of performance evaluation samples within established acceptance limits described in paragraph (9) of this rule. If more than one concentration of a particular contaminant was provided for analysis, the laboratory must analyze all concentrations provided except where otherwise stated.
(b) Failure to notify the Department within 30 days of any changes either in personnel, equipment, or laboratory location which may impair analytical capability.
(c) Failure to maintain the minimum required standard of quality as contained in the most recent version of the EPA Manual for the Certification of Laboratory Analyzing Drinking Water as determined by an on-site evaluation by a Department representative.
(d) During a provisional status period, which may last for up to one year plus any extension period pending proceedings for revocation of its certification, the laboratory may continue to analyze samples for compliance purposes, but it must notify its clients of its downgraded status in writing on all reports.
(e) Failure to report compliance data to the public water system or the Department in a timely manner. Data that may cause the system to exceed a MCL shall be reported as soon as possible to the system and to the Department.
(5) Revoking Certification Status - A laboratory certified to perform analyses may be downgraded from a Certified or a Provisionally Certified status to a Not Certified status for a particular parameter, or for one or more groups of contaminants for which it has been certified, including but not limited to any of the reasons listed in subparagraphs below. Commercial laboratories must notify their public water system customers of the change in certification status by mail within 45 days of a downgrade in status by the Department and retain copies of such notice for six years.
(a) Failure to analyze an initial and a follow-up or cross check performance evaluation sample within established acceptance limits.
(b) Failure to correct identified deviations (including continued use of unapproved methods and equipment) within the time specified by the Department.
(c) Reporting as data derived from its own laboratory analysis, that data obtained from analyses of the sample(s) performed by another laboratory.
(d) Falsification or inaccurate reporting of analytical data.
(e) Failure to report to the Department analytical results as specified by Rule 0400-45-01-.18. Analytical results must be submitted on forms furnished by the Department. Forms may be obtained from the Division of Water Resources. A certified laboratory shall submit results of its analyses to both the appropriate Department's field office and the Department's central office.
(f) Failure to perform the analysis within the time period prescribed by the analytical procedure. However, the time period shall not be more than thirty (30) days from the sample collection date, except for lead and copper tap samples collected pursuant to Rule 0400-45-01-.33.
(g) Failure to notify its drinking water customers of any downgrade or revocation of its certification status and to keep records of the notice to customers.
(h) Failure of the laboratory to reject any sample taken for compliance purposes that does not meet acceptable criteria for the type container and preservative, maximum holding time, chain of custody, proper sample collection and transport, and sample report form that contains the location, date, time of collection, collector's name, preservative added, and other special remarks concerning the sample. Indelible ink shall be used for completing the sample report form.
(i) Failure of the Laboratory Director to give timely notice to the party responsible for collecting the sample that improper sampling technique, container, transport, holding time, method preservative or documentation was used.
(j) Failure to provide written sampling procedures with sample containers sent to customers for collecting drinking water samples.
(k) Failure to meet the method detection limits.
(l) Failure to maintain all data necessary to reconstruct analytical results reported for compliance samples.
(m) Failure to pay certification fees as listed in subparagraph (2)(c) of this rule.
(6) Procedure for Revocation
(a) The Department or the certification officer shall notify the laboratory by certified mail of its intent to revoke certification.
(b) If the local laboratory objects to the determination to revoke certification, the laboratory shall submit a written notice of appeal to the Department within thirty (30) days after issuance of the notice of intent to revoke certification. The notice of appeal will be referred to the Tennessee Water Quality Control Board. The Board will set a hearing date and conduct proceedings in accordance with the Uniform Administrative Procedures Act, Chapter 5 of Title 4. If no notice of appeal is so filed, certification will be revoked.
(c) The notice of appeal shall set forth the grounds and reasons for objection and shall ask for a hearing before the Tennessee Water Quality Control Board. It shall be signed by a duly authorized representative of the laboratory such as the president/owner of a commercial laboratory, or the mayor, utility manager, president, or laboratory supervisor in the case of a municipal or utility district laboratory.
(d) If the Water Quality Control Board modifies or sets aside the determination of the Department, the Department will reevaluate the local laboratory within sixty (60) days of issuance of the decision by the Board.
(7) Reinstatement of Certification - Certification of a laboratory will be reinstated when it demonstrates to the Department that the deficiencies which resulted in provisional certification or revocation have been corrected. Such demonstration may result from an on-site evaluation and/or a successful analysis of samples on the next regularly scheduled performance evaluation.
(8) Reciprocity of Certified Laboratories - The Department may authorize acceptance of analyses from laboratories certified by other states or by the U.S. Environmental Protection Agency. Authorization will be granted on a reciprocal basis for laboratories from those states which accept Tennessee laboratory certification. Laboratories desiring Department approval of their certification from the U.S. E.P.A. or from another state must submit to the Department copies of all correspondence pertaining to the grant of certification, including the results of any performance evaluation sample analyses.
(9) Proficiency Evaluation (PE) Samples or Performance Test (PT) Samples
(a) In order to receive and maintain full certification for an analyte, the following are required for each analyte for which a laboratory is certified:
1. The laboratory must analyze PE samples (if available) acceptable to the Department at least once a year for each analyte and by each method used to analyze compliance samples. PE samples are also referred to as Performance Test (PT) samples.
2. Results from analysis of the PE samples must be within the acceptable limits set forth in this chapter.
3. The laboratory must document the corrective actions taken when a PE sample is analyzed unsuccessfully. A copy of this documentation must be available for review by the certification officer.
4. A make up PE sample must be successfully analyzed within three months of being notified that a PE sample was not acceptable.
(b) Excluding vinyl chloride, the laboratory may be certified for all VOCs if they successfully analyze at least 80% of the regulated VOCs. The 80% Rule does not apply to the regulated trihalomethanes (THM) or haloacetic acids (HAAs). Laboratories are certified for total THMs and HAA5 but each regulated THM and HAA concentration must be reported, evaluated and passed individually to pass the PE sample. If a laboratory fails one of the regulated THMs or HAAs, it cannot be certified for total THMs or HAA5, but must analyze another PE sample and pass all of the regulated THMs or HAAs in a PE sample to be certified to analyze compliance monitoring samples for total trihalomethanes or total haloacetic acids.

The following table summarizes the 80% Rule.

Analyte(s)

PE Success Requirement

Vinyl Chloride

100%

20 VOCs

80% *

4 Regulated THMs

100%

5 Regulated HAA5s

100%

*A lab will not maintain certification for analyte(s) which it repeatedly fails.

(c) Acceptable studies for the determination of total coliforms and E. coli shall be part of a drinking water study. Each study shall contain a set of ten samples in various combinations of total coliforms, E. coli, non-coliforms, and at least one blank. To be certified, laboratories must successfully analyze nine of the ten samples with no false negatives.
(10) Analytical Requirements
(a) Microbiology
1. Suppliers of water for community water systems and non-community water systems shall analyze for coliform bacteria for the purpose of determining compliance with paragraph (4) of Rule 0400-45-01-.06. The standard sample volume required for total coliform analysis, regardless of the analytical method used is 100 milliliters. Analyses shall be conducted in accordance with one of the analytical methods in following table:

TABLE 0400-45-01-.14(10)(a) 1.

Organism

Methodology

Citation1

Total Coliforms2

Total Coliform Fermentation Technique3,4,5

9221 A, B

Total Coliform Membrane Filter Technique6

9222 A, B, C

Presence-Absence (P-A) Coliform Test5,7

9221

ONPG-MUG Test8

Colisure Test9

E*Colite®Test10

m-ColiBlue24®Test11

Readycult®Coliforms 100 Presence/Absence Test12

Membrane Filter Technique using Chromocult®Coliform Agar13

Colitag®Test14

9223

Footnotes

1 Methods 9221 A, B; 9222 A, B, C; 9221 D and 9223 are contained in Standard Methods for the Examination of Water and Wastewater, 18th edition (1992) and 19th edition (1995) American Public Health Association, 1015 Fifteenth Street NW, Washington, D.C. 20005; either edition may be used. In addition, the following online versions may also be used: 9221 A, B, D-99, 9222 A, B, C-97 and 9223 B-97. Standard Methods Online are available at http://www.standardmethods.org. The year in which each method was approved by the Standard Methods Committee is designated by the last two digits in the method number. The methods listed are the only online versions that may be used.

2 The time from sample collection to initiation of analysis may not exceed 30 hours. Systems are encouraged but not required to hold samples below 10°C during transit.

3 Lactose broth, as commercially available, may be used in lieu of lauryl tryptose broth, if the system conducts at least 25 parallel tests between this medium and lauryl tryptose broth using the water normally tested, and this comparison demonstrates that the false-positive rate and false-negative rate for total coliform, using lactose broth, is less than 10 percent.

4 If inverted tubes are used to detect gas production, the media should cover these tubes at least one-half to two-thirds after the sample is added.

5 No requirement exists to run the completed phase on 10 percent of all total coliform-positive confirmed tubes.

6 MI agar also may be used. Preparation and use of MI agar is set forth in the article, "New medium for the simultaneous detection of total coliform and Escherichia coli in water'' by Brenner, K.P., et al., 1993, Appl. Environ. Microbiol. 59:3534-3544. Also available from the Office of Water Resource Center (RC-4100), 401 M. Street SW, Washington, DC 20460, EPA/600/J-99/225.

7 Six-times formulation strength may be used if the medium is filter-sterilized rather than autoclaved.

8 The ONPG-MUG Test is also known as the Autoanalysis Colilert System.

9 A description of the Colisure Test, Feb 28, 1994, may be obtained from IDEXX Laboratories, Inc., One IDEXX Drive, Westbrook, Maine 04092. The Colisure Test may be read after an incubation time of 24 hours.

10 A description of the E*Colite® Test, "Presence/Absence for Coliforms and E. Coli in Water,'' Dec 21, 1997, is available from Charm Sciences, Inc., 36 Franklin Street, Malden, MA 02148-4120.

11 A description of the m-ColiBlue24® Test, Aug 17, 1999, is available from the Hach Company, 100 Dayton Avenue, Ames, IA 50010.

12 The Readycult® Coliforms 100 Presence/Absence Test is described in the document, "Readycult® Coliforms 100 Presence/Absence Test for the Detection and Identification of Coliform Bacteria and Escherichla coli in finished water", November 2000, Version 1.0, available from EM Science (an affiliate of Merck KggA, Darmstadt Germany), 480 S. Democrat Road, Gibbstown, NJ 08027-1297. Telephone number is (800) 222-0342, e-mail address is: adellenbusch@emscience.com.

13 Membrane Filter Technique using Chromocult® Coliform Agar is described in the document, "Chromocult® Coliform Presence/Absence Membrane Filter Test Method for Detection and Identification of Coliform Bacteria and Escherichla coli in finished water", November 2000, Version 1.0, available from EM Science (an affiliate of Merck KggA, Darmstadt Germany), 480 S. Democrat Road, Gibbstown, NJ 08027-1297. Telephone number is (800) 222-0342, e-mail address is: adellenbusch@emscience.com.

14 Colitag® product for the determination of the presence/absence of total coliforms and E. coli is described in "Colitag® Product as a Test for Detection and Identification of Coliforms and E. coli Bacteria in Drinking Water and Source Water as required in National Primary Drinking Water Regulations," August 2001, available from CPI International, Inc., 5580 Skylane Blvd., Santa Rosa, CA, 95403 telephone (800) 878-7654, Fax (707) 545-7901, Internet address http://www.cpiinternational.com.

(i) The following table gives the alternative testing methods for total coliforms to those in table 0400-45-01-.14(10)(a) 1.:

TABLE 0400-45-01-.14(10)(a) 1.(i)

Organism

Methodology

SM 21st Edition1

Other

Total Coliforms

Total Coliform Fermentation Technique

9221 A, B

Total Coliform Membrane Filter Technique

9222 A, B, C

Presence-Absence (PA) Coliform Test

9221 D

ONPG-MUG Test

9223

ColitagTM

Modified

ColitagTM2

Footnotes

1 Standard Methods for the Examination of Water and Wastewater, 21st edition (2005). Available from American Public Health Association, 800 I Street NW, Washington, DC 20001- 3710

2 Modified ColitagTM Method. "Modified ColitagTM Test Method for the Simultaneous Detection of E. Coli and other Total Coliforms in Water (ATP D05-0035)," August 28, 2009. Available at http://www.nemi.gov or from CPI International, 5580 Skylane Boulevard, Santa Rosa, CA 95403.

2. Where a determination of fecal coliform density is not required, public water systems must conduct fecal coliform analysis in accordance with the following procedure:
(i) When the MTF Technique or Presence-Absence (P-A) Coliform Test is used to test for total coliforms, shake the lactose-positive presumptive tube or P-A bottle vigorously and transfer the growth with a sterile 3-mm loop or sterile applicator stick into brilliant green lactose bile broth and EC medium to determine the presence of total and fecal coliforms, respectively.
(ii) For EPA-approved analytical methods which use a membrane filter, remove the membrane containing the total coliform colonies from the substrate with a sterile forceps and carefully curl and insert the membrane into a tube of EC medium (The laboratory may first remove a small portion of selected colonies for verification), swab the entire surface with a sterile cotton swab and transfer the inoculum to EC medium (do not leave the cotton swab in the EC medium), or inoculate individual total coliform-positive colonies into EC Medium. Gently shake the inoculated EC tubes to insure adequate mixing and incubate in a waterbath at 44.5 + 0.2°C for 24 + 2 hours. Gas production of any amount in the inner fermentation tube of the EC medium indicates a positive fecal coliform test. The preparation of EC medium is described in Method 9221E in Standard Methods for the Examination of Water and Wastewater, 18th Edition (1992), 19th Edition (1995), and 20th Edition (1998); the cited method in any one of these three editions may be used.
3. Public Water Systems choosing to test for E. coli in lieu of fecal coliform must use the following methods:
(i) EC medium supplemented with 50 ug/ml of 4-methylumbelliferyl-beta-D-glucuronide (MUG) (final concentration), as described in Method 9222 G in Standard Methods for the Examination of Water and Wastewater, 19th edition (1995) and 20th edition (1998). Either edition may be used. Alternatively, the 18th edition (1992) may be used if at least 10 ml of EC medium, as described in part 2 of this subparagraph, is supplemented with 50 ug/ml of MUG before autoclaving. The inner inverted fermentation tube may be omitted. If the 18th edition is used, apply the procedure in part 2 of this subparagraph for transferring a total coliform-positive culture to EC medium supplemented with MUG, incubate the tube at 44.5 + 0.2°C for 24 + 2 hours, and then observe fluorescence with an ultraviolet light (366nm) in the dark. If fluorescence is visible, E. coli are present.
(ii) Nutrient agar supplemented with 100 µg/ml of 4methylumbelliferyl-beta-D-glucuronide (MUG) (final concentration), as described in Method 9222G in Standard Methods for the Examination of Water and Wastewater, 19th edition (1995) and 20th edition (1998). Either edition may be used for determining if a total coliform-positive sample, as determined by a membrane filter technique, contains E. coli Alternatively, the 18th edition (1992) may be used if the membrane filter containing a total coliform-positive colony(ies) is transferred to nutrient agar, as described in Method 9221B (paragraph 3) of Standard Methods (18th edition), supplemented with 100 ug/ml of MUG. If the 18th edition is used, incubate the agar plate at 35°C for 4 hours and then observe the colony(ies) under ultraviolet light (366 nm) in the dark for fluorescence. If fluorescence is visible, E. coli are present.
(iii) Minimal Medium ONPG-MUG (MMO-MUG) Test, as set forth in the article "National Field Evaluation of Defined Substrate Method for the Simultaneous Detection of Total Coliforms and Escherichia coli from Drinking Water; Comparison with Presence-Absence Techniques" (Edberg et al.), Applied and Environmental Microbiology, Volume 55, pp. 1003-1008, April 1989. (Note: The Autoanalysis Colilert System is an MMO-MUG test). If the MMO-MUG test is total coliform-positive after a 24-hour incubation, test the medium for fluorescence with a 366-nm ultraviolet light (preferably with a 6-watt lamp) in the dark. If fluorescence is observed, the sample is E. coli-positive. If fluorescence is questionable (cannot be definitively read) after 24 hours incubation, incubate the culture for an additional four hours (but not to exceed 28 hours total) and again test the medium for fluorescence. The MMO-MUG Test with hepes buffer in lieu of phosphate buffer is the only approved formulation for the detection of E. coli.
(iv) The Colisure Test. A description of the Colisure Test may be obtained from the Millipore Corporation, Technical Services Department, 80 Ashby Road, Bedford, MA 01730.
(v) The membrane filter method with MI agar, a description of which is cited in footnote 6 to table 0400-45-01-.14(10)(a) 1.
(vi) E*Colite® Test, a description of which is cited in footnote 10 to table 0400-45-01-.14(10)(a) 1.
(vii) m-ColiBlue24® Test, a description of which is cited in footnote 11 to table 0400-45-01-.14(10)(a) 1.
(viii) Readycult® Coliforms 100 Presence/Absence Test, a description of which is cited in footnote 12 to the table 0400-45-01-.14(10)(a) 1.
(ix) Membrane Filter Technique using Chromocult® Coliform Agar, a description of which is cited in footnote 13 to table 0400-45-01-.14(10)(a) 1.
(x) Colitag®, a description of which is cited in footnote 14 to table 0400-45-01-.14(10)(a) 1.
(xi) As an option to subpart (iii) of this part, a system with a total coliform-positive, MUG-negative, MMO-MUG test may further analyze the culture for the presence of E. coli by transferring a 0.1 ml. 28-hour MMO-MUG culture to EC Medium + MUG with a pipet. The formulation and incubation conditions of EC Medium + MUG, and observation of the results are described in subpart (i) of this part. Alternative methods are given in the following table:

TABLE 0400-45-01-.14(10)(a) 3.(xi)

Alternative Testing Methods for E. coli

Organism

Methodology

SM 20thEdition1

SM 21stEdition2

SM Online3

Other

E. coli

ONPG-MUG Test

9223 B

Modified

ColitagTM4

Footnotes

1 Standard Methods for the Examination of Water and Wastewater, 20th Edition (1998). Available from American Public Health Association, 800 I Street NW, Washington, DC 20001-3710.

2 Standard Methods for the Examination of Water and Wastewater, 21st edition (2005). Available from American Public Health Association, 800 I Street, NW, Washington, DC 20001- 3710

3 Standard Methods Online are available at http://www.standardmethods.org. The year in which each method was approved by the Standard Methods Committee is designated by the last two digits in the method number. The methods listed are the only online versions that may be used.

4 Modified ColitagTM Method. "Modified ColitagTM Test Method for the Simultaneous Detection of E. Coli and other Total Coliforms in Water (ATP D05-0035)," August 28, 2009. Available at http://www.nemi.gov or from CPI International, 5580 Skylane Boulevard, Santa Rosa, CA 95403.

4. Public Water systems required to monitor under parts (2)(a)1. and (5)(b)2. of Rule 0400-45-01-.31 for total coliforms, fecal coliforms, or heterotrophic bacteria must use one of the methods listed in the following table.

TABLE 0400-45-01-.14(10)(a) 4.

Organism

Methodology

Citation1

Total Coliform2

Total Coliform Fermentation Technique3,4,5

Total Coliform Membrane Filter Technique6

ONPG-MUG Test7

9221 A, B, C

9222 A, B, C

9223

Fecal Coliforms2

Fecal Coliform Procedure8

Fecal Coliform Filter Procedure

9221 E 9222 D

Heterotrophic bacteria2

Pour Plate MethodSimPlate9

9215 B

Footnotes

1. Except where noted, all methods refer to Standard Methods for the Examination of Water and Wastewater, 18th edition (1992), 19th edition (1995), or 20th edition (1998), American Public Health Association, 1015 Fifteenth Street NW., Washington, DC 20005. The cited methods published in any of these three editions may be used. In addition, the following online versions may also be used: 2130 B-01, 9215 B-00, 9221 A, B, C, E-99, 9222 A, B, C, D-97, and 9223 B-97. Standard Methods Online are available http://www.standardmethods.org. The year in which each method was approved by the Standard Methods Committee is designated by the last two digits in the method number. The methods listed are the only Online versions that may be used.

2. The time from sample collection to initiation of analysis may not exceed 8 hours. Systems must hold samples below 10 deg. C during transit. {8 hour holding time only applies to parts (2)(a)1. and (5)(b)2. of Rule 0400-45-01-.31 }

3. Lactose broth, as commercially available, may be used in lieu of lauryl tryptose broth, if the system conducts at least 25 parallel tests between this medium and lauryl tryptose broth using the water normally tested, and this comparison demonstrates that the false-positive rate and false-negative rate for total coliform, using lactose broth, is less than 10 percent.

4. Media should cover inverted tubes at least one-half to two-thirds after the sample is added.

5. No requirement exists to run the completed phase on 10 percent of all total coliform-positive confirmed tubes.

6. MI agar also may be used. Preparation and use of MI agar is set forth in the article, "New medium for the simultaneous detection of total coliform and Escherichia coli in water'' by Brenner, K.P., et. al., 1993, Appl. Environ. Microbiol. 59:3534-3544. Also available from the Office of Water Resource Center (RC-4100T), 1200 Pennsylvania Avenue, NW., Washington DC 20460, EPA/600/J-99/225. Verification of colonies is not required.

7. The ONPG-MUG Test is also known as the Autoanalysis Colilert System.

8. A-1 Broth may be held up to seven days in a tightly closed screw cap tube at 4 deg. C.

9. A description of the SimPlate method, "IDEXX SimPlate TM HPC Test Method for Heterotrophs in Water'', November 2000, can be obtained from IDEXX Laboratories, Inc., One IDEXX Drive, Westbrook, Maine 04092, telephone (800) 321-0207.

(i) Alternative testing methods for those contaminants found in table 0400-45-01-.14(10)(a) 4. are given in the following table:

Organism

Methodology

SM 21st Edition1

Total Coliform

Total Coliform Fermentation Technique

9221 A, B, C

Total Coliform Membrane Filter Technique

9222 A, B, C

ONPG-MUG Test

9223

Fecal Coliforms

Fecal Coliform Procedure

9221 E

Fecal Coliform Filter Procedure

9222 D

Heterotrophic Bacteria

Pour Plate Method

9215 B

Footnotes

1 Standard Methods for the Examination of Water and Wastewater, 21st edition (2005). Available from American Public Health Association, 800 I Street, NW, Washington, DC 20001-3710.

5. Public water systems required to enumerate E. coli in source water as required by Rule 0400-45-01-.39 must use one of the approved methods in the following table:

TABLE 0400-45-01-.14(10)(a) 5.

Parameter and units

Method1

EPA

Standard methods 18th,19th, 20th

Ed.

Standard methods online

AOAC, ASTM, USGS

Other

E. coli , number per 100 ml16

MPN2,3,4multiple tube,

9221B / 9221F6,8

9221B-99 / 9221F6,8

multiple tube/multiple well

9223B7

9223B-977

991.155

Colilert®7,10 Colilert-18®7,9,10

MF two step

1103.113

9222B/9222G12, 9213D

9222B-97 / 9222G12

D5392-934

MF single step

160314 , 160415

mColiBlue-24®11

Footnotes

1. The method must be specified when results are reported.

2. Tests must be conducted to provide organism enumeration (density). Select the appropriate configuration of tubes/filtrations and dilutions/volumes to account for the quality, character, consistency, and anticipated organism density of the water sample.

3. To assess the comparability of results obtained with individual methods, it is suggested that side-by-side tests be conducted across seasons of the year with the water samples routinely tested in accordance with the most current Standard Methods for the Examination of Water and Wastewater or EPA alternate test procedure (ATP) guidelines.

4. ASTM. 2000, 1999, 1996. Annual Book of ASTM Standards-Water and Environmental Technology. Section 11.02. ASTM International. 100 Barr Harbor Drive, West Conshohocken, PA 19428.

5. AOAC. 1995. Official Methods of Analysis of AOAC International, 16th Edition, Volume I, Chapter 17. Association of Official Analytical Chemists International. 481 North Frederick Avenue, Suite 500, Gaithersburg, MD 20877-2417.

6. The multiple-tube fermentation test is used in 9221B.1. Lactose broth may be used in lieu of lauryl tryptose broth (LTB), if at least 25 parallel tests are conducted between this broth and LTB using the water samples normally tested, and this comparison demonstrates that the false-positive rate and false-negative rate for total coliform using lactose broth is less than 10 percent. No requirement exists to run the completed phase on 10 percent of all total coliform-positive tubes on a seasonal basis.

7. These tests are collectively known as defined enzyme substrate tests, where, for example, a substrate is used to detect the enzyme b-glucuronidase produced by E. coli.

8. After prior enrichment in a presumptive medium for total coliform using 9221B.1, all presumptive tubes or bottles showing any amount of gas, growth or acidity within 48 h ± 3 h of incubation shall be submitted to 9221 F. Commercially available EC-MUG media or EC media supplemented in the laboratory with 50 ±g/mL of MUG may be used.

9. Descriptions of the Colilert®, Colilert-18®, Quanti-Tray®, and Quanti-Tray®/2000 may be obtained from IDEXX Laboratories, Inc., 1 IDEXX Drive, Westbrook, ME 04092.

10. Descriptions of the Colilertn, Colilert-18®, Quanti-Tray®, and Quanti-Tray®/2000 may be obtained from IDEXX Laboratories, Inc., 1 IDEXX Drive, Westbrook, ME 04092.

11. A description of the mColiBlue24® test, Total Coliforms and E. coli, is available from Hach Company, 100 Dayton Ave., Ames, IA 50010.

12. Subject total coliform positive samples determined by 9222B or other membrane filter procedure to 9222G using NA MUG media.

13. USEPA. 2002. Method 1103.1: Escherichia coli (E. coli) In Water By Membrane Filtration Using membrane-Thermotolerant Escherichia coli Agar (mTEC). U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA-821-R-02-020.

14. USEPA. 2002. Method 1603: Escherichia coli (E. coli) In Water By Membrane Filtration Using Modified membrane-Thermotolerant Escherichia coli Agar ( modified mTEC). U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA-821-R-02-023.

15. Preparation and use of MI agar with a standard membrane filter procedure is set forth in the article, Brenner et al. 1993. "New Medium for the Simultaneous Detection of Total Coliform and Escherichia coli in Water.'' Appl. Environ. Microbiol. 59:3534-3544 and in USEPA. 2002. Method 1604: Total Coliforms and Escherichia coli (E. coli) in Water by Membrane Filtration by Using a Simultaneous Detection Technique (MI Medium).U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA 821-R-02-024.

16. Recommended for enumeration of target organism in ambient water only.

(i) The time from sample collection to initiation of analysis may not exceed 30 hours unless the system meets the condition of subpart (ii) of this part.
(ii) The Department may approve on a case-by-case basis the holding of an E. coli sample for up to 48 hours between sample collection and initiation of analysis if the Department determines that analyzing an E. coli sample within 30 hours is not feasible. E. coli samples held between 30 to 48 hours must be analyzed by the Colilert reagent version of Standard Method 9223B as listed in table 0400-45-01-.14(10)(a) 5.
(iii) Systems must maintain samples between 0°C and 10°C during storage and transit to the laboratory.
6. Ground water systems must analyze all ground water source samples collected under paragraph (3) of Rule 0400-45-01-.40 using one of the analytical methods listed in the following table for the presence of E. coli or enterococci.

Analytical Methods for Source Water Monitoring

Fecal Indicator1

Methodology

Method citation

E. coli

Colilert3

9223 B.2

Colisure3

9223 B.2

Membrane Filter Method with MI Agar

EPA Method 1604.4

m-ColiBlue24 Test5

E*Colite Test6

EC-MUG7

NA-MUG7

9221 F.2

9222 G.2

Enterococci

Multiple-Tube Technique

9230B.2

Membrane Filter Technique

9230C.2

Membrane Filter Technique

EPA Method 1600.8

Enterolert9

Analyses must be conducted in accordance with the documents listed below. The Director of the Federal Register approves the incorporation by reference of the documents listed in footnotes 2-11 in accordance with 5 U.S.C. 552(a) and 1 CFR part 51. Copies of the documents may be obtained from the sources listed below. Copies may be inspected at EPA's Drinking Water Docket, EPA West, 1301 Constitution Avenue, NW., EPA West, Room B102, Washington DC 20460 (Telephone: 202-566-2426); or at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030, or go to:

http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html.

Footnotes

1 The time from sample collection to initiation of analysis may not exceed 30 hours. The ground water system is encouraged but not required to hold samples below 10° C during transit.

2 Methods are described in Standard Methods for the Examination of Water and Wastewater 20th edition (1998) and copies may be obtained from the American Public Health Association, 1015 Fifteenth Street NW., Washington DC 20005-2605.

3 Medium is available through IDEXX Laboratories, Inc., One IDEXX Drive, West Brook, Maine 04092.

4 EPA Method 1604: Total Coliforms and Escherichia coli in Water by Membrane Filtration Using a Simultaneous Detection Technique (MI Medium); September 2002, EPA 821-R-02-024. Method is available at http://www.epa.gov/nerlccwww/1604sp02.pdf or from EPA's Water Resource Center (RC-4100T), 1200 Pennsylvania Avenue, NW., Washington DC 20460.

5 A description of the m-ColiBlue24 Test, "Total Coliforms and E. coli Membrane Filtration Method with m-ColiBlue24 Broth," Method No. 10029 Revision 2, August 17, 1999, is available from Hach Company, 100 Dayton Ave., Ames IA 50010 or from EPA's Water Resource Center (RC-4100T), 1200 Pennsylvania Avenue, NW., Washington DC 20460.

6 A description of the E*Colite Test, "Charm E*Colite Presence/Absence Test for Detection and Identification of Coliform Bacteria and Escherichia coli in Drinking Water, January 9, 1998, is available from Charm Sciences, Inc., 659 Andover St., Lawrence, MA 01843-1032 or from EPA's Water Resource Center (RC-4100T), 1200 Pennsylvania Avenue, NW., Washington DC 20460.

7 EC-MUG (Method 9221F) or NA-MUG (Method 9222G) can be used for E. coli testing step as described in 141.21(f)(6)(i) or (ii) after use of Standard Methods 9221 B, 9221 D, 9222 B, or 9222 C.

8 EPA Method 1600: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus Indoxyl-b-D-Glucoside Agar (mEI) EPA 821-R-02-022 (September 2002) is an approved variation of Standard Method 9230C. The method is available at http://www.epa.gov/nerlcwww/1600sp02.pdf or EPA's Water Resource Center (RC-4100T), 1200 Pennsylvania Avenue, NW., Washington DC 20460. The holding time and temperature for ground water samples are specified in footnote 1 above, rather than as specified in Section 8 of EPA Method 1600.

9 Medium is available through IDEXX Laboratories, Inc., One IDEXX Drive, Westbrook, Maine 04092. Preparation and use of the medium is set forth in the article "Evaluation of Enterolert for Enumeration of Enterococci in Recreational Waters," by Budnick, G.E., Howard, R.T, and Mayo, D.R., 1996, Applied and Environmental Microbiology, 62:3881-3884.

(i) Alternative testing methods for the fecal indicators listed in the table in Rule 0400-45-01-.14(10)(a) 6. are given in the following table:

Alternative for Analytical Testing for Source Monitoring Methods Water

Organism

Methodology

SM 21st Edition1

SM Online2

Other

E. coli

Colilert

9223 B

9223 B-97

Colisure

9223 B

9223 B-97

Colilert-18

9223 B

9223 B-97

Readycult®

Colitag

Readycult®3

Chromocult®

Modified ColitagT4
Chromocult®5

Enterococci

Multiple-Tube Technique

9230 B-04

Footnotes

1 Standard Methods for the Examination of Water and Wastewater, 21st edition (2005). Available from American Public Health Association, 800 I Street NW, Washington, DC 20001-3710.

2 Standard Methods Online are available at http://www.standardmethods.org. The year in which each method was approved by the Standard Methods Committee is designated by the last two digits in the method number. The methods listed are the only online versions that may be used.

3 Readycult® Method, "Readycult® Coliforms 100 Presence/Absence Test for Detection and Identification of Coliform Bacteria and Escherichia coli in Finished Waters," January, 2007. Version 1.1. Available from EMD Chemicals (affiliate of Merck KGaA,, Darmstadt, Germany), 480 S. Democrat Road, Gibbstown, NJ 08027-1297.

4 Modified ColitagTM Method. "Modified ColitagTM Test Method for the Simultaneous Detection of E. Coli and other Total Coliforms in Water (ATP D05-0035)," August 28, 2009. Available at http://www.nemi.gov or from CPI International, 5580 Skylane Boulevard, Santa Rosa, CA 95403.

5 Chromocult® Method, "Chromocult® Coliform Agar Presence/Absence Membrane Filter Test Method for Detection and Identification of Coliform Bacteria and Escherichia coli in Finished Waters," November, 2000. Version 1.0. EMD Chemicals (affiliate of Merck KGaA, Darmstadt, Germany), 480 S. Democrat Road, Gibbstown, NJ 08027-1297.

(b) Public Water system required to monitor for turbidity by this Chapter must use one of the methods listed in the following table:

TABLE 0400-45-01-.14(10)(b)

Turbidity4

Nephelometric Method

NephelometricMethod

Great Lakes Instruments

Hach FilterTrak

2130 B

180.11

Method 22

101333

Footnotes

1. "Methods for the Determination of Inorganic Substances in Environmental Samples'', EPA/600/R-93/100, August 1993. Available at NTIS, PB94-121811.

2. GLI Method 2, "Turbidity'', November 2, 1992, Great Lakes Instruments, Inc., 8855 North 55th Street, Milwaukee, Wisconsin 53223.

3. A description of the Hach FilterTrak Method 10133, "Determination of Turbidity by Laser Nephelometry,'' January 2000, Revision 2.0, can be obtained from; Hach Co., P.O. Box 389, Loveland, CO 80539-0389, telephone: 800-227-4224.

4. Styrene divinyl benzene beads (e.g. AMCO-AEPA-1 or equivalent) and stabilized formazin (e.g. Hach StablCal TM or equivalent) are acceptable substitutes for formazin.

1. Alternative testing methods for turbidity given in table 0400-45-01-.14(10)(b) are given in the following table:

TABLE 0400-45-01-.14(10)(b) 1.

Contaminant

Methodology

SM 21 st Edition1

Other

Turbidity

Nephelometric Method

2130 B

Laser Nephelometry (on-line)

Mitchell M52712

LED Nephelometry (on-line)

Mitchell M53313

LED Nephelometry (on-line)

AMI Turbiwell 4

LED Nephelometry (on-line)

Orion AQ4500 5

Footnotes

1 Standard Methods for the Examination of Water and Wastewater, 21st edition (2005). Available from American Public Health Association, 800 I Street NW, Washington, DC 20001- 3710

2 Mitchell Method M5271, Revision 1.1. "Determination of Turbidity by Laser Nephelometry," March 5, 2009. Available at http://www.nemi.gov or from Leck Mitchell, Ph.D., PE, 656 Independence Valley Dr., Grand Junction, CO 81507.

3 Mitchell Method M5331, Revision 1.1. "Determination of Turbidity by LED Nephelometry," March 5, 2009. Available at http://www.nemi.gov or from Leck Mitchell, Ph.D., PE, 656 Independence Valley Dr., Grand Junction, CO 81507.

4 AMI Turbiwell, "Continuous Measurement of Turbidity Using a SWAN AMI Turbiwell Turbidimeter," August 2009. Available at http://www.nemi.gov or from Markus Bernasconi, SWAN Analytische Instrumente AG, Studbachstrasse 13, CH-8340 Hinwil, Switzerland.

5 Orion Method AQ4500, Revision 1.0. "Determination of Turbidity by LED Nephelometry," May 8, 2009. Available at http://www.nemi.gov or from Thermo Scientific, 166 Cummings Center, Beverly, MA 01915, http://www.thermo.com.

(c) Public water systems required to monitor by this Chapter for any inorganic contaminants listed in the following table must utilize one of the approved methods for that contaminant listed in the following table:

Inorganic Contaminants Analytical Methods TABLE 0400-45-01-.14(10)(c)

Contaminant

Methodology 13

EPA

ASTM 3

SM 4 (18th, 19th ed.)

SM 4 (20th ed.)

SM Online 22

Other

1. Alkalinity

Titrimetric Electrometric titration

D1067-92, 02 B

2320 B

2320 B

2320 B-97 I-1030-85 5

2. Antimony

Inductively Coupled Plasma

(ICP)-Mass Spectrometry

200.82

Hydride-Atomic Absorption

D3697-92, 02

Atomic Absorption;Platform

200.92

Atomic Absorption; Furnace

3113 B

3113 B-99

3. Arsenic

ICP-Mass Spectrometry

200.82

Atomic Absorption;Platform

200.92

Atomic Absorption; Furnace

D2972-97, 03 C

3113 B

3113 B-99

Hydride Atomic Absorption

D2972-97, 03 B

3114 B

3114 B-97

4. Asbestos

Transmission Electron Microscopy

100.19

Transmission Electron

100.210

Microscopy

5. Barium

Inductively Coupled Plasma

200.72

3120 B

3120 B

3120 B-99

ICP-Mass Spectrometry

200.82

Atomic Absorption; Direct

3111D

3111 D-99

Atomic Absorption; Furnace

3113 B

3113 B-99

6. Beryllium

Inductively Coupled Plasma

200.72

3120 B

3120 B

3120 B-99

ICP-Mass Spectrometry

200.82

Atomic Absorption;Platform

200.92

Atomic Absorption; Furnace

D3645-97, 03 B

3113 B

3113 B-99

7. Cadmium

Inductively Coupled Plasma

200.72

ICP-Mass Spectrometry

200.82

Atomic Absorption;Platform

200.92

Atomic Absorption; Furnace

3113 B

3113 B-99

8. Calcium

EDTA titrimetric

D511-93, 03 A

3500-Ca D

3500-Ca B

3500-Ca B-97

Atomic Absorption; Direct Aspiration.

D511-93, 03 B

3111 B

3111 B-99

Inductively Coupled Plasma

200.72

3120 B

3120 B

3120 B-99

Ion Chromatography

D6919-03

9. Chromium

Inductively Coupled Plasma

200.72

3120 B

3120 B

3120 B-99

ICP-Mass Spectrometry

200.82

Atomic Absorption;Platform

200.92

Atomic Absorption; Furnace

3113 B

3113 B-99

10. Copper

Atomic Absorption; Furnace

D1688-95, 02 C

3113 B

3113 B-99

Atomic Absorption; Direct

D1688-95, 02 A

3111 B

3111 B-99

Aspiration.

Inductively Coupled Plasma

200.72

3120 B

3120 B

3120 B-99

ICP-Mass spectrometry

200.82

Atomic Absorption;Platform

200.92

11.Conductivity

Conductance

D1125-95

(Reapproved

1999) A

2510 B

2510 B

2510 B-97

12. Cyanide

Manual Distillation followed by

Spectrophotometric, Amenable.

Spectro-photometric Manual.

Spectro-photometric Semi-automated.

335.46

D2036-98 A

D2036-98 B

D2036-98 A

4500-CN- C

4500-CN- G

4500-CN-E

4500-CN- C

4500-CN-G

4500-CN-E

4500-CN- G-99

4500-CN- E-99

I-3300-855

Selective Electrode

4500-CN- F

4500-CN- F

4500-CN- F-99

UV, Distillation, Spectrophotometric.

Kelada-01

16

Micro Distillation, Flow Inj ection, Spectrophotometric.

QuikChem

10-204-00-1-X17

Ligand Exchange and

Amperometry19

D6888-04

OIA-1677,

DW19

13. Fluoride

Ion Chromatography

300.06,

300.118

D4327-97, 03

4110 B

4110 B

4110 B-00

Manual Distill; Color. SPADNS.

4500-F- B, D

4500-F- B, D

4500-F- B, D-

97

Manual Electrode

D1179-93, 99 B

4500-F- C

4500-F- C

4500-F- C-97

Automated Electrode

380-75WE11

Automated Alizarin

4500-F- E

4500-F- E

4500-F- E-97

129-71W11

Capillary Ion Electrophoresis

D6508, Rev. 222

14. Lead

Atomic Absorption; Furnace

D3559-96, 03 D

3113 B

3113 B-99

ICP-Mass spectrometry

Atomic

Absorption;Platform

Differential Pulse Anodic

200.82 200.92

Method

Stripping Voltametry

100115

15. Magnesium

Atomic Absorption ICP

200.72

D511-93, 03 B

3111 B 3120 B

3120 B

3111 B-99 3120 B-99

Complexation Titrimetric Methods

D511-93, 03 A

3500-Mg E

3500-Mg B

3500-Mg B-97

Ion Chromatography

D6919-03

16. Mercury

Manual, Cold Vapor

245.12

D3223-97, 02

3112 B

3112 B-99

Automated, Cold Vapor

245.21

ICP-Mass Spectrometry

200.82

17. Nickel

Inductively Coupled Plasma

200.72

3120 B

3120 B

3120 B-99

ICP-Mass Spectrometry

Atomic

Absorption;Platform

200.82 200.92

Atomic Absorption; Direct

3111 B

3111 B-99

Atomic Absorption; Furnace

3113 B

3113 B-99

18. Nitrate

Ion Chromatography

300.06 300.12

D4327-97, 03

4110 B

4110 B

4110 B-00

B-10118

Automated Cadmium Reduction

353.26

D3867-90 A

4500-NO3- F

4500-NO3-F

4500-NO3- F-00

Ion Selective Electrode

4500-NO3- D

4500-NO3-D

4500-NO3- D -00

6017

Manual Cadmium Reduction

D3867-90 B

4500-NO3- E

4500-NO3-E

4500-NO3- E-00

Capillary Ion Electrophoresis

D6508, Rev

222

19. Nitrite

Ion Chromatography

300.06 300.12

D4327-97, 03

4110 B

4110 B

4110 B-00

B-1011 8

Automated Cadmium Reduction

353.26

D3867-90 A

4500-NO3- F

4500-NO3-F

4500-NO3- F -00

Manual Cadmium Reduction

D3867-90 B

4500-NO3E

4500-NO3-E

4500-N O3- E-00

Spectrophotometric

4500-NO2 -B

4500-NO2-B

4500-NO2-B-00

Capillary Ion Electrophoresis

D6508, Rev.

222

20. Ortho-phosphate12

Colorimetric, Automated, Ascorbic Acid.

365.16

4500-P F

4500-P F

Colorimetric, ascorbic acid, single reagent.

D515-88 A

4500-P E

4500-P E

Colorimetric Phosphomolybdate; Automated-seg-

I-1601-855 I-2601-905

mented flow; Automated Discrete

I-2598-855

Ion Chromatography

300.06 300.118

D4327-97, 03

4110 B

4110 B

4110 B-00

Capillary Ion Electro-phoresis.

D6508, Rev.

222

21. pH

Electrometric

150.1,

150.21

D1293-95, 99

4500-H+ B

4500-H+ B

4500-H+ B -

00

22. Selenium

Hydride-Atomic Absorption

D3859-98, 03 A

3114 B

3114 B-97

ICP-Mass Spectrometry

200.82

Atomic Absorption;Platform

200.92

Atomic Absorption; Furnace

D3859-98, 03 B

3113 B

3113 B-99

23. Silica

Colorimetric, Molybdate

Blue

Automated-segmentedFlow

I-1700-855 I-2700-855

Colorimetric

D859-94, 00.

Molybdosilicate .

4500-Si D

4500-SiO2 C

4500-SiO2 C-97

Heteropoly blue

4500-Si E

4500-SiO2 D

4500-SiO2 D-97

Automated for Molyb-date-reactive Silica.

4500-Si F

4500-SiO2 E

4500-SiO2 E-97

Inductively Coupled Plasma

200.72

3120 B

3120 B

3120 B-99

24. Sodium

Inductively Coupled Plasma

200.72

Atomic Absorption; Direct Aspiration.

3111 B

3111 B-99

Ion Chromatography

D6919-03

25. Temperature

Thermometric

2550

2550

2550-00

26. Thallium

ICP-Mass Spectrometry

200.82

Atomic Absorption;Platform

200.92

Footnotes

1. "Methods for Chemical Analysis of Water and Wastes,'' EPA/600/4-79/020, March 1983. Available at NTIS, PB84-128677.

2. "Methods for the Determination of Metals in Environmental Samples-Supplement I,'' EPA/600/R-94/111, May 1994. Available at NTIS, PB95-125472.

3. Annual Book of ASTM Standards, 1994, 1996, 1999, or 2003, Vols. 11.01 and 11.02, ASTM International; any year containing the cited version of the method may be used. The previous versions of D1688-95A, D1688-95C (copper), D3559-95D (lead), D1293-95 (pH), D1125-91A (conductivity) and D859-94 (silica) are also approved. These previous versions D1688-90A, C; D3559-90D, D1293-84, D1125-91A and D859-88, respectively are located in the Annual Book of ASTM Standards, 1994, Vol. 11.01. Copies may be obtained from ASTM International, 100 Barr Harbor Drive, West Conshohocken, PA 19428.

4. Standard Methods for the Examination of Water and Wastewater, 18th edition (1992), 19th edition (1995), or 20th edition (1998). American Public Health Association, 1015 Fifteenth Street, NW., Washington, DC 20005. The cited methods published in any of these three editions may be used, except that the versions of 3111 B, 3111 D, 3113 B and 3114 B in the 20th edition may not be used.

5. Method I-2601-90, Methods for Analysis by the U.S. Geological Survey National Water Quality Laboratory-Determination of Inorganic and Organic Constituents in Water and Fluvial Sediment, Open File Report 93-125, 1993; For Methods I-1030-85; I-1601-85; I-1700-85; I-2598-85; I-2700-85; and I-3300-85 See Techniques of Water Resources Investigation of the U.S. Geological Survey, Book 5, Chapter A-1, 3rd edition., 1989; Available from Information Services, U.S. Geological Survey, Federal Center, Box 25286, Denver, CO 80225-0425.

6. "Methods for the Determination of Inorganic Substances in Environmental Samples,'' EPA/600/R-93/100, August 1993. Available at NTIS, PB94-120821.

7. The procedure shall be done in accordance with the Technical Bulletin 601 "Standard Method of Test for Nitrate in Drinking Water," July 1994, PN 221890-001, Analytical Technology, Inc. Copies may be obtained from ATI Orion, 529 Main Street, Boston, MA 02129.

8. Method B-1011, "Waters Test Method for Determination of Nitrite/Nitrate in Water Using Single Column Ion Chromatography,'' August 1987. Copies may be obtained from Waters Corporation, Technical Services Division, 34 Maple Street, Milford, MA 01757, Telephone: 508/482-2131, Fax: 508/482-3625.

9. Method 100.1, "Analytical Method For Determination of Asbestos Fibers in Water,'' EPA/600/4-83/043, EPA, September 1983. Available at NTIS, PB83-260471.

10. Method 100.2, "Determination of Asbestos Structure Over 10-±m In Length In Drinking Water,'' EPA/600/R-94/134, June 1994. Available at NTIS, PB94-201902.

11. Industrial Method No. 129-71W, "Fluoride in Water and Wastewater,'' December 1972, and Method No. 380-75WE, "Fluoride in Water and Wastewater,'' February 1976, Technicon Industrial Systems. Copies may be obtained from Bran & Luebbe, 1025 Busch Parkway, Buffalo Grove, IL 60089.

12. Unfiltered, no digestion or hydrolysis.

13. Because MDLs reported in EPA Methods 200.7 and 200.9 were determined using a 2x preconcentration step during sample digestion, MDLs determined when samples are analyzed by direct analysis (i.e., no sample digestion) will be higher. For direct analysis of cadmium and arsenic by Method 200.7, and arsenic by Method 3120 B, sample preconcentration using pneumatic nebulization may be required to achieve lower detection limits. Preconcentration may also be required for direct analysis of antimony, lead, and thallium by Method 200.9; antimony and lead by Method 3113 B; and lead by Method D3559-90D, unless multiple in-furnace depositions are made.

14. If ultrasonic nebulization is used in the determination of arsenic by Methods 200.7, 200.8, or SM 3120 B, the arsenic must be in the pentavalent state to provide uniform signal response. For Methods 200.7 and 3120 B, both samples and standards must be diluted in the same mixed acid matrix concentration of nitric and hydrochloric acid with the addition of 100 ± L of 30% hydrogen peroxide per 100 mL of solution. For direct analysis of arsenic with Method 200.8 using ultrasonic nebulization, samples and standards must contain 1 mg/L of sodium hypochlorite.

15. The description for Method Number 1001 for lead is available from Palintest, LTD, 21 Kenton Lands Road, P.O. Box 18395, Erlanger, KY 41018. Or from the Hach Company, P.O. Box 389, Loveland, CO 80539.

16. The description for the Kelada-01 Method, "Kelada Automated Test Methods for Total Cyanide, Acid Dissociable Cyanide, And Thiocyanate,'' Revision 1.2, August 2001, EPA # 821-B01-009 for cyanide is available from the National Technical Information Service (NTIS), PB 2001-108275, 5285 Port Royal Road, Springfield, VA 22161. The toll free telephone number is 800-553-6847. Note: A 450-W UV lamp may be used in this method instead of the 550-W lamp specified if it provides performance within the quality control (QC) acceptance criteria of the method in a given instrument. Similarly, modified flow cell configurations and flow conditions may be used in the method, provided that the QC acceptance criteria are met.

17. The description for the QuikChem Method 10-204-00-1-X, "Digestion and distillation of total cyanide in drinking and wastewaters using MICRO DIST and determination of cyanide by flow injection analysis,'' Revision 2.1, November 30, 2000, for cyanide is available from Lachat Instruments, 6645 W. Mill Rd., Milwaukee, WI 53218. Telephone: 414-358-4200.

18. "Methods for the Determination of Organic and Inorganic Compounds in Drinking Water,'' Vol. 1, EPA 815-R-00-014, August 2000. Available at NTIS, PB2000-106981.

19. Method OIA-1677, DW "Available Cyanide by Flow Injection, Ligand Exchange, and Amperometry,'' January 2004. EPA-821-R-04-001, Available from ALPKEM, A Division of OI Analytical, P.O. Box 9010, College Station, TX 77842-9010.

20. Sulfide levels below those detected using lead acetate paper may produce positive method interferences. Test samples using a more sensitive sulfide method to determine if a sulfide in-terference is present, and treat samples accordingly.

21. Standard Methods Online are available at http://www.standardmethods.org. The year in which each method was approved by the Standard Methods Committee is designated by the last two digits in the method number. The methods listed are the only online versions that may be used.

22. Method D6508, Rev. 2, "Test Method for Determination of Dissolved Inorganic Anions in Aqueous Matrices Using Capillary Ion Electrophoresis and Chromate Electrolyte,'' available from Waters Corp, 34 Maple St, Milford, MA, 01757, Telephone: 508/482-2131, Fax: 508/482-3625.

1. The inorganic contaminants from table 0400-45-01-.14(10)(c) that have alternative testing methods are given in the following table:

TABLE 0400-45-01-.14(10)(c) 1.

Contaminant

Methodology

EPA Method

SM 21 st Edition1

SM

Online2

ASTM 3

Other

Alkalinity

Titrimetric

2320 B

Antimony

Hydride - Atomic Absorption

D 3697-07

Atomic Absorption; Furnace

3113 B

Axially viewed inductively coupled plasma-atomic emission spectrometry (AVICP-AES)

200.5, Revision

4.24

Arsenic

Atomic Absorption; Furnace

3113 B

D 2972-08 C

Hydride Atomic Absorption

3114 B

D 2972-08 B

Axially viewed inductively coupled plasma-atomic emission spectrometry (AVICP-AES)

200.5,

Revision

4.2

Barium

Inductively Coupled Plasma

3120 B

Atomic Absorption; Direct

3111 D

Atomic Absorption; Furnace

3113 B

Axially viewed inductively coupled plasma-atomic emission spectrometry (AVICP-AES)

200.5,

Revision

4.2

Beryllium

Inductively Coupled Plasma

3120 B

Atomic Absorption; Furnace

3113 B

D 3645-08 B

Axially viewed inductively coupled plasma-atomic emission spectrometry (AVICP-AES)

200.5,

Revision

4.2

Cadmium

Atomic Absorption; Furnace

3113 B

Axially viewed inductively coupled plasma-atomic emission spectrometry (AVICP-AES)

200.5,

Revision

4.2

Calcium

EDTA titrimetric

3500-Ca B

D 511-09 A

Atomic Absorption; Direct Aspiration

3111 B

D 511-09 B

Inductively Coupled Plasma

3120 B

Axially viewed inductively coupled plasma-atomic emission spectrometry (AVICP-AES)

200.5,

Revision

4.2

Chromiuim

Inductively Coupled Plasma

3120 B

Atomic Absorption;

3113 B

Furnace

Axially viewed inductively coupled plasma-atomic emission spectrometry (AVICP-AES)

200.5,

Revision

4.2

Copper

Atomic Absorption; Furnace

3113 B

D 1688-07 C

Atomic Absorption; Direct Aspiration

3111 B

D 1688-07 A

Inductively Coupled Plasma

3120 B

Axially viewed inductively coupled plasma-atomic emission spectrometry (AVICP-AES)

200.5,

Revision

4.2

Conductivity

Conductance

2510 B

Cyanide

Manual Distillation followed by:

D2036-06 A

Spectro-photometric, Amenable

4500-CN -G

D2036-06 B

Spectro-photometric Manual

4500-CN -E

D2036-06 A

Selective Electrode

4500-CN -F

Gas

Chromatography/Mass Spectrometry Headspace

ME355.01 5

Fluoride

Ion Chromatography

4110 B

Manual Distillation; Colorimetric SPADNS

4500-F -B, D

Manual Electrode

4500-F - C

D1179-04 B

Automated Alizarin

4500-F - E

Lead

Atomic Absorption; Furnace

3113 B

D 3559-08 D

Axially viewed inductively coupled plasma-atomic emission spectrometry (AVICP-AES)

200.5,

Revision

4.2

Magnesium

Atomic Absorption

3111 B

D 511-09 B

Inductively Coupled Plasma

3120 B

Complexation Titrimetric Methods

3500-Mg B

D 511-09 A

Axially viewed inductively coupled plasma-atomic emission spectrometry (AVICP-AES)

200.5,

Revision

4.2

Mercury

Manual, Cold Vapor

3112 B

Nickel

Inductively Coupled Plasma

3120 B

Atomic Absorption; Direct

3111 B

Atomic Absorption; Furnace

3113 B

Axially viewed inductively coupled plasma-atomic emission spectrometry (AVICP-AES)

200.5,

Revision

4.2

Nitrate

Ion Chromatography

4110 B

Automated Cadmium Reduction

4500-NO3- F

Manual Cadmium Reduction

4500-NO3- E

Ion Selective Electrode

4500-NO2- B

Reduction/Colorimetric

Systea Easy (1 -

Reagent)6

Nitrite

Ion Chromatography

4110 B

Automated Cadmium Reduction

4500-NO3- F

Manual Cadmium Reduction

4500-NO3- E

Spectrophotometric

4500-NO2- B

Reduction/Colorimetric

Systea Easy (1 -

Reagent)6

Orthophosphate

Ion Chromatography

4110 B

Colorimetric, ascorbic acid, single reagent

4500-P E

4500-P E-99

Colorimetric, Automated, Ascorbic Acid

4500-P F

4500-P F-99

pH

Electrometric

4500-H +

B

Selenium

Hydride-Atomic Absorption

3114 B

D 3859-08 A

Atomic Absorption; Furnace

3113 B

D 3859-08 B

Axially viewed inductively coupled plasma-atomic emission spectrometry (AVICP-AES)

200.5,

Revision

4.2

Silica

Colorimetric

D859-05

Molybdosilicate

4500-SiO2 C

Heteropoly blue

4500-SiO2 D

Automated for

4500-

Molybdate-reactive Silica

SiO2 E

Axially viewed inductively coupled plasma-atomic emission spectrometry (AVICP-AES)

200.5,

Revision

4.2

Inductively Coupled Plasma

3120 B

Sodium

Atomic Absorption; Direct Aspiration

3111 B

Axially viewed inductively coupled plasma-atomic emission spectrometry (AVICP-AES)

200.5,

Revision

4.2

Temperature

Thermometric

2550

Footnotes

1 Standard Methods for the Examination of Water and Wastewater, 21st edition (2005). Available from American Public Health Association, 800 I Street NW, Washington, DC 20001- 3710

2 Standard Methods Online are available at http://www.standardmethods.org. The year in which each method was approved by the Standard Methods Committee is designated by the last two digits in the method number. The methods listed are the only online versions that may be used.

3 Available from ASTM International, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959 or http://astm.org. The methods listed are the only alternative versions that may be used.

4 EPA Method 200.5, Revision 4.2. "Determination of Trace Elements in Drinking Water by Axially Viewed Inductively Coupled Plasma-Atomic Emission Spectrometry." 2003. EPA/600/R-06/115. (Available at http://www.epa.gov/nerlcwww.ordmeth.htm. )

5 Method D99-003, Revision 3.0. "Free Chlorine Species (HOCl- and OCl-) by Test Strip," November 21, 2003. Available from Industrial Test Systems, Inc., 1875 Langston St., Rock Hill, SC 29730.

6 Systea Easy (1 - Reagent). "Systea Easy (1 - Reagent) Nitrate Method," February 4, 2009. Available at http://www.nemi.gov or from Systea Scientific, LLC., 900 Jorie Blvd., Suite 35, Oak Brook, IL 60523.

(d) Detection Limits for Inorganic Contaminants methodology specified below must be equal to or less than the requirements in the following:

TABLE 0400-45-01-.14(10)(d) Detection Limits for Inorganic Contaminants

Contaminant

MCL (mg/l)

Methodology

Detection limit (mg/1)

Antimony

0.006

Atomic Absorption Furnace

0.003

Atomic Absorption: Platform

0.00085

ICP-Mass Spectrometry

0.0004

Hydride-Atomic Absorption

0.001

Arsenic

0.016

Atomic Absorption Furnace

0.001

Atomic Absorption: Platform

Stabilized Temperature

70.0005

Atomic Absorption: Gaseous Hydride

0.001

ICP-Mass Spectrometry

80.0014

Asbestos

7 MFL

Transmission Electron Microscopy

0.01 MFL

Barium

2

Atomic Absorption; furnace technique

0.002

Atomic Absorption; Direct Aspiration

0.1

Inductively Coupled Plasma

0.002(0.001)

Beryllium

0.004

Atomic Absorption; Furnace

0.00025

Atomic Absorption; Platform

0.00002

Inductively Coupled Plasma

0.0003

ICP-Mass Spectrometry

0.0003

Cadmium

0.005

Atomic Absorption; furnace technique

0.0001

Inductively Coupled Plasma

0.001

Chromium

0.1

Atomic Absorption; furnace technique

0.001

Inductively Coupled Plasma

0.007(0.001)

Cyanide

0.2

Distillation, Spectrophotometric3

0.02

Distillation, Automated Spectrophotometric3

0.005

Distillation, Selective Electrode

0.05

Distillation, Amenable, Spectrophotometric4

0.02

Mercury

0.002

Manual Cold Vapor Technique

0.0002

Automated Cold Vapor Technique

0.0002

Nickel

0.1

Atomic Absorption; Furnace

0.001

Atomic Absorption; Platform

0.00065

Inductively Coupled Plasma2

0.005

ICP-Mass Spectrometry

0.0005

Nitrate

10 (as N)

Manual Cadmium Reduction

0.01

Automated Hydrazine Reduction

0.01

Automated Cadmium Reduction

0.05

Ion Selective Electrode

1

Ion Chromatography

0.01

Nitrite

1 (as N)

Spectrophotometric

0.01

Automated Cadmium Reduction

0.05

Manual Cadmium Reduction

0.01

Ion Chromatography

0.004

Selenium

0.05

Atomic Absorption; furnace

0.002

Atomic Absorption; gaseous hydride

0.002

Thallium

0.002

Atomic Absorption; Furnace

0.001

Atomic Absorption; Platform

0.00075

ICP-Mass Spectrometry

0.0003

Footnotes 1 MFL=million fibers per liter > 10 microns.

2 Using a 2X preconcentration step as noted in Method 200.7 Lower method detection limits (MDLs) may be achieved using a 4X preconcentration.

3 Screening method for total cyanides.

4 Measures "free" cyanides.

5 Lower MDLs are reported using stabilized temperature graphite furnace atomic absorption.

6 The value for arsenic is effective January 23, 2006. Until then the MCL is 0.05 mg/L.

7. The MDL reported for EPA method 200.9 (Atomic Absorption; Platform-Stabilized Temperature) was determined using a 2X concentration step during sample digestion. The MCL determined for samples analyzed using direct analyses (i.e, no sample digestion) will be higher. Using multiple depositions, EPA 200.9 is capable of obtaining MDL of 0.0001 mg/L.

8 Using selective ion monitoring, EPA Method 200.8 (ICP-MS) is capable of obtaining a MDL of 0.0001 mg/L.

1. Laboratories must achieve a method detection limit for lead of 0.001 mg/l according to the procedures in appendix B of part 136 of 40 CFR. This need only be accomplished if the laboratory will be processing source water composite samples under subpart (9)(a)1.(iv) of Rule 0400-45-01-.33.
(i) Lead: 0.001 mg/l (only if source water compositing is done under Rule 0400-45-01-.09 ); and
(ii) Copper: 0.001 mg/l or 0.020 mg/l when atomic absorption direct aspiration is used (only if source water compositing is done under Rule 0400-45-01-.09 ).
2. The Department has the authority to allow the use of previously collected monitoring data, provided that the laboratory is currently certified by EPA or the Department to perform analyses to the specifications required in this subparagraph and if the data were collected and analyzed in accordance with the requirements of this rule and Rule 0400-45-01-.33.
3. All lead levels measured between the PQL and the MDL must be either reported as measured or they can be reported as one-half the PQL (0.0025 mg/l). All levels below the lead MDL must be reported as zero; and
4. All copper levels measured between PQL and the MDL must be either reported as measured or they can be reported as one-half the PQL (0.025 mg/l). All levels below the copper MDL must be reported as zero.
(e) Laboratories must analyze PE samples within the following acceptance criteria:

Contaminant

Acceptance limit

Antimony

±30 at >=0.006 mg/l

Arsenic

±30 at >=0.003 mg/l

Asbestos

2 standard deviations based on study statistics

Barium

±15% at >=0.15 mg/l

Beryllium

±15% at >=0.001 mg/l

Cadmium

±20% at >=0.002 mg/l

Chromium

±15% at >=0.01 mg/l

Copper

±10% at >=0.050 mg/l1

Cyanide

±25% at >=0.1 mg/l

Fluoride

±10% at >=1 to 10 mg/l

Lead

± 30% >=0.005 mg/l2

Mercury

±30% at >=0.0005 mg/l

Nickel

±15% at >=0.01 mg/l

Nitrate

±10% at >=0.4 mg/l

Nitrite

±15% at >=0.4 mg/l

Selenium

±20% at >=0.01 mg/l

Thallium

±30% at >=0.002 mg/l
1. The practical quantitation level (PQL) for copper is 0.050 mg/l.
2. The PQL for lead is 0.005 mg/l.
(f) Sample collection for antimony, arsenic, asbestos, barium, beryllium, cadmium, chromium, cyanide, fluoride, mercury, nickel, nitrate, nitrite, selenium, and thallium under this Rule shall be conducted using the sample preservation, container, and maximum holding time procedures specified in the table below:

TABLE 0400-45-01-.14(10)(f)

Contaminant

Preservative1

Container2

Time3

Antimony

HNO3

P or G

6 months

Arsenic

Conc HNO3to pH<2

P or G

6 months

Asbestos

4°C

P or G

48 hours4

Barium

HNO3

P or G

6 months

Beryllium

HNO3

P or G

6 months

Cadmium

HNO3

P or G

6 months

Chromium

HNO3

P or G

6 months

Cyanide

4°C, NaOH

P or G

14 days

Fluoride

None

P or G

1 month

Mercury

HNO3

P or G

28 days

Nickel

HNO3

P or G

6 months

Nitrate

4°C

P or G

48 hours5

Nitrate-Nitrite 6

H2SO4

P or G

28 days

Nitrite

4°C

P or G

48 hours

Selenium

HNO3

P or G

6 months

Thallium

HNO3

P or G

6 months

Footnotes

1. For cyanide determinations samples must be adjusted with sodium hydroxide to pH 12 at the time off collection. When chilling is indicated the sample must be shipped and stored at 4°C or less. Acidification of nitrate or metals samples may be with a concentrated acid or a dilute (50% by volume) solution of the applicable concentrated acid. Acidification of samples for metals analysis is encouraged and allowed at the laboratory rather than at the time of sampling provided the shipping time and other instructions in Section 8.3 of EPA Methods 200.7 or 200.8 or 200.9 are followed.

2. P=plastic, hard or soft; G=glass, hard or soft.

3. In all cases samples should be analyzed as soon after collection as possible. Follow additional (if any) information on preservation, containers or holding times that is specified in method.

4. Instructions for containers, preservation procedures and holding times as specified in Method 100.2 must be adhered to for all compliance analyses including those conducted with Method 100.1.

5. If the sample is chlorinated, the holding time for an unacidified sample kept at 4°C is extended to 14 days.

6. Nitrate-Nitrite refers to a measurement of total nitrate.

(g) Certified Laboratories performing analyses for Public Water Systems as required by this Chapter must utilize an approved method for Organic Contaminants listed in table 0400-45-01-.14(10)(g) or the altenative testing methods in table A in this subparagraph:

TABLE 0400-45-01-.14(10)(g)

Contaminant

EPA method1

Standard Methods

ASTM

Other

1. Benzene

502.2, 524.2

2. Carbon tetrachloride

502.2, 524.2, 551.1

3. Chlorobenzene

502.2, 524.2

4. 1,2-Dichlorobenzene

502.2, 524.2

5. 1,4-Dichlorobenzene

502.2, 524.2

6. 1,2-Dichloroethane

502.2, 524.2

7. cis-Dichloroethylene

502.2, 524.2

8. trans-Dichloroethylene

502.2, 524.2

9. Dichloromethane

502.2, 524.2

10. 1,2-Dichloropropane

502.2, 524.2

11. Ethylbenzene

502.2, 524.2

12. Styrene

502.2, 524.2

13. Tetrachloroethylene

502.2, 524.2, 551.1

14. 1,1,1-Trichloroethane

502.2, 524.2, 551.1

15. Trichloroethylene

502.2, 524.2, 551.1

16. Toluene

502.2, 524.2

17. 1,2,4-Trichlorobenzene

502.2, 524.2

18. 1,1-Dichloroethylene

502.2, 524.2

19. 1,1,2-Trichloroethane

502.2, 524.2, 551.1

20. Xylenes (total)

502.2, 524.2

21. Vinyl chloride

502.2, 524.2

22. 2,3,7,8-TCDD (dioxin)

1613

23. 2,4-D4 (as acid, salts and esters)

515.2, 555, 515.1, 515.3, 515.4

D5317-93,98 (Reapproved 2003)

24. 2,4,5-TP 4 (Silvex)

515.2, 555, 515.1, 515.3, 515.4

D5317-93,98 (Reapproved 2003

25. Alachlor2

507, 525.2, 508.1, 505, 551.1

26. Atrazine2

507, 525.2, 508.1, 505, 551.1

Syngenta5 AG-

625

27. Benzo(a)pyrene

525.2, 550, 550.1

28. Carbofuran

531.1, 531.2

6610

29. Chlordane

508, 525.2, 508.1, 505

30. Dalapon

552.1, 515.1, 552.2, 515.3, 515.4, 552.3

31. Di(2-ethylhexyl)adipate

506, 525.2

32. Di(2-ethylhexyl)phthalate

506, 525.2

33. Dibromochloropropane (DBCP)

504.1, 551.1

34. Dinoseb4

515.2, 555, 515.1, 515.3, 515.4

35. Diquat

549.2

36. Endothall

548.1

37. Endrin

508, 525.2, 508.1, 505, 551.1

38. Ethylene dibromide (EDB)

504.1, 551.1

39. Glyphosate

547

6651

40. Heptachlor

508, 525.2, 508.1, 505, 551.1

41. Heptachlor Epoxide

508, 525.2, 508.1, 505, 551.1

42. Hexachlorobenzene

508, 525.2, 508.1, 505, 551.1

43. Hexachlorocyclopentadiene

508, 525.2, 508.1, 505, 551.1

44. Lindane

508, 525.2, 508.1, 505, 551.1

45. Methoxychlor

508, 525.2, 508.1, 505, 551.1

46. Oxamyl

531.1, 531.2

6610

47. PCBs3 (as decachlorobiphenyl)

508A

48. PCBs3 (as Aroclors)

508.1, 508, 525.2, 505

49. Pentachlorophenol

515.2, 525.2, 555, 515.1, 515.3, 515.4

D5317-93,98 (Reapproved 2003)

50. Picloram4

515.2, 555, 515.1, 515.3, 515.4

D5317-93,98 (Reapproved 2003)

51. Simazine2

507, 525.2, 508.1, 505, 551.1

52. Toxaphene

508, 508.1, 525.2, 505

Footnotes

1. Previously approved EPA methods remain available for compliance monitoring until June 1, 2001. EPA methods 502.2 Rev. 2.0, 505 Rev. 2.0, 507 Rev. 2.0, 508 Rev. 3.0, 531.1 Rev. 3.0 are in "Methods for the Determination of Organic Compounds in Drinking Water", December 1988, revised July 1991; methods 506 and 551 are in "Methods for the Determination of Organic Compounds in Drinking Water--Supplement I", July 1990; methods 515.2 Rev. 1.0 and 524.2 Rev. 4.0 are in "Methods for the Determination of Organic Compounds in Drinking Water--Supplement II,'' August 1992; and methods 504.1 Rev. 1.0, 508.1 Rev. 1.0, 525.2 Rev.1.0 are available from US EPA NERL, Cincinnati, OH 45268

2. Substitution of the detector specified in Method 505, 507, 508, or 508.1 for the purpose of achieving lower detection limits is allowed as follows: Either an electron capture or nitrogen phosphorus detector may be used provided all regulatory requirements and quality control criteria are met.

3. PCBs are qualitatively identified as Aroclors and measured for compliance purposes as decachlorobiphenyl. Users of Method 505 may have more difficulty in achieving the required detection limits than users of Methods 508.1, 525.2 or 508.

4. Accurate determination of the chlorinated esters requires hydrolysis of the sample as described in EPA Methods 515.1, 515.2, 515.3, 515.4, and 555 and ASTM Method D 5317-93, 98 (Reapproved 2003).

5. This method may not be used for the analysis of atrazine in any system where chlorine dioxide is used for drinking water treatment. In samples from all other systems, any result for atrazine generated by Method AG-625 that is greater than one-half the maximum contaminant level (MCL) (in other words, greater than 0.0015mg/L or 1.5µ/L) must be confirmed using another approved method for this contaminant and should use additional volume of the original sample collected for compliance monitoring. In instances where a result from Method AG-625 triggers such confirmatory testing, the confirmatory result is to be used to determine compliance.

TABLE A

The Organic Contaminants from table 0400-45-01-.14(10)(g) that have Alternative Testing Methods

Contaminant

Methodology

EPA Method

SM 21stEdition1

SM Online2

Benzene

Purge & Trap/Gas Chromatography/Mass Spectrometry (PT/GC/MS)

524.33

Carbon tetrachloride

PT/GC/MS

524.3

Chlorobenzene

PT/GC/MS

524.3

1,2-Dichlorobenzene

PT/GC/MS

524.3

1,4-Dichlorobenzene

PT/GC/MS

524.3

1,2-Dichloroethane

PT/GC/MS

524.3

cis-Dichloroethylene

PT/GC/MS

524.3

trans-Dichloroethylene

PT/GC/MS

524.3

Dichloromethane

PT/GC/MS

524.3

1,2-Dichloropropane

PT/GC/MS

524.3

Ethylbenzene

PT/GC/MS

524.3

Styrene

PT/GC/MS

524.3

Tetrachloroethylene

PT/GC/MS

524.3

1,1,1-Trichloroethane

PT/GC/MS

524.3

Trichloroethylene

PT/GC/MS

524.3

Toluene

PT/GC/MS

524.3

1,2,4-Trichlorobenzene

PT/GC/MS

524.3

1,1-Dichloroethylene

PT/GC/MS

524.3

1,1,2-Trichloroethane

PT/GC/MS

524.3

Xylenes (total)

PT/GC/MS

524.3

Vinyl chloride

PT/GC/MS

524.3

Carbofuran

High-performance liquid chromatography (HPLC) with post-column derivatization and fluorescence detection

6610 B

6610 B-04

Dalapon

Ion Chromatography Electrospray Ionization Tandem Mass Spectrometry (IC-ESI-MS/MS)

5574

6640 B

6640 B-01

Dibromochloropropane (DBCP)

PT/GC/MS

524.3

Ethyl dibromide (EDB)

PT/GC/MS

524.3

Oxamyl

High-performance liquid chromatography (HPLC) with post-column derivatization and fluorescence detection

6610 B

6610 B-04

Total Trihalomethanes

PT/GC/MS

524.3

Footnotes

1 Standard Methods for the Examination of Water and Wastewater, 21st edition (2005). Available from American Public Health Association, 800 I Street NW, Washington, DC 20001-3710

2. Standard Methods Online are available at http://www.standardmethods.org. The year in which each method was approved by the Standard Methods Committee is designated by the last two digits in the method number. The methods listed are the only online versions that may be used.

3. EPA Method 524.3, Version 1.0. "Measurement of Purgeable Organic Compounds in Water by Capillary Column Gas Chromatography/Mass Spectrometry," June 2009. EPA 815-B-09-009. Available at http://epa.gov/safewater/methods/analyticalmethods_ogwdw.html.

4. EPA Method 557. "Determination of Haloacetic Acids, Bromate, and Dalapon in Drinking Water by Ion Chromatography Electrospray Ionization Tandem Mass Spectrometry (IC-ESI-MS/MS)," September 2009, EPA 815-B-09-012. Available at http://epa.gov/safewater/methods/analyticalmethods_ogwdw.html.

1. To obtain certification for contaminants 1 through 20 listed in table 0400-45-01-.14(10)(g) laboratories must:
(i) Successfully analyze 80% of the contaminants included in the PE sample. To successfully analyze a contaminant a laboratory must achieve quantitative results which are: within ±40% of the actual amount in the PE sample when the actual amount is less than 0.010 mg/l, within ±20% of the actual amount in the PE sample when the actual amount is greater than or equal to 0.010 mg/l.
(ii) Achieve a method detection limit of 0.0005 mg/l, according to the procedures in 40 CFR part 136 Appendix B.
2. To obtain certification for vinyl chloride a laboratory must:
(i) Achieve quantitative results on PE samples which are within ±40% of the actual amount of vinyl chloride in the PE sample.
(ii) Achieve a method detection limit of 0.0005 mg/l, according to the procedures in 40 CFR part 136 Appendix B.
(iii) Achieve certification for contaminants 1 through 20 listed in table 0400-45-01-.14(10)(g).
3. To obtain certification for contaminants 22 through 52 listed in table 0400-45-01-.14(10)(g) certified laboratories must achieve quantitative results on PE samples within the following acceptance limits:

TABLE 0400-45-01-.14(10)(g) 3.

Contaminant

Acceptance limits (percent)

DBCP

+ 40

EDB

+ 40

Alachlor

+ 45

Atrazine

+ 45

Benzo[a]pyrene

2 standard deviations

Carbofuran

+ 45

Chlordane

+ 45

Dalapon

2 standard deviations

Di(2-ethylhexyl)adipate

2 standard deviations

Di(2-ethylhexyl)phthalate

2 standard deviations

Dinoseb

2 standard deviations

Diquat

2 standard deviations

Endothall

2 standard deviations

Endrin

+ 30

Glyphosate

2 standard deviations

Heptachlor

+ 45

Heptachlor Epoxide

+ 45

Hexachlorobenzene

2 standard deviations.

Hexachlorocyclopentadiene

2 standard deviations

Lindane

+ 45

Methoxychlor

+ 45

Oxamyl

2 standard deviations

PCBs (as Decachlorobiphenyl)

0 - 200

Picloram

2 standard deviations

Simazine

2 standard deviations

Toxaphene

+ 45

Aldicarb

2 standard deviations

Aldicarb sulfoxide

2 standard deviations

Aldicarb sulfone

2 standard deviations.

Pentachlorophenol

+ 50

2,3,7,8-TCDD (Dioxin)

2 standard deviations

2,4-D

+ 50

2,4,5-TP (Silvex)

+ 50
4. Analysis for PCBs shall be conducted as follows:
(i) Each system which monitors for PCBs shall analyze each sample using either Methods 508.1, 525.2, 508, or 505. Users of Method 505 may have more difficulty in achieving the required Aroclor detection limits than users of Methods 508.1, 525.2 or 508.
(ii) If PCBs (as one of seven Aroclors) are detected (as designated by table 0400-45-01-.14(10)(g) 4.(ii)) in any sample analyzed using Methods 505 or 508, the system shall reanalyze the sample using Method 508A to quantitate PCBs (as decachlorobiphenyl).

TABLE 0400-45-01-.14(10)(g) 4.(ii)

Aroclor

Detection Limit (mg/l)

1016

0.00008

1221

0.02

1232

0.0005

1242

0.0003

1248

0.0001

1254

0.0001

1260

0.0002
(iii) Compliance with the PCB MCL shall be determined based upon the quantitative results of analyses using Method 508A.
(h) Analytical methods used to determine compliance with paragraph (5) of Rule 0400-45-01-.06 shall be in accordance with table 0400-45-01-.14(10)(h).

TABLE 0400-45-01-.14(10)(h)

Reference (method or page number)

Contaminant

Methodology

EPA1

EPA2

EPA3

EPA4

SM5

ASTM6

USGS7

DOE8

Other

Naturally occurring:Gross alpha11and beta.

Evaporation

900.0

p 1

00-01

p 1

302, 7110 B

R-1120-76

Gross alpha11

Co-precipitation

00-02

7110 C

Radium 226

Radon emanation

903.1

p 16

Ra-04

p 19

7500-Ra C

D 3454-91

R-1141-76

Ra-05

N.Y.9

Radio chemical

903.0

p 13

Ra-03

304, 305, 7500-Ra B

D 2460-91

R-1140-76

GA14

Radium 228

Radio chemical

904.0

p 24

Ra-05

p 19

304, 7500-Ra D

R-1142-76

N. Y.9 N. J.10

Uranium12

Radio chemical

908.0

7500-U B

Fluorometric

908.1

7500-U C (17thEd.)

D 2907-91

R-1180-76 R-1181-76

U-04

ICP-MS

200.813

3125

D 5673-03

Alpha spectrometry

00-07

P 33

7500-U C (18th or 19thEd.)

D 3972-90

R-1182-76

U-02

Laser Phosophorimetry

D 5174-91

Man-made Radioactive cesium.

Radio chemical

901.0

p 4

7500-Cs B

D 2459-72

R-1111-76

Gamma ray spectrometry.

901.1

p 92

7120 (19thEd.)

D 3649-91

R-1110-76

4.5.2.3

Radioactive iodine

Radio chemistry

902.0

p 6 p 9

7500-I B 7500-I C 7500-I D

D 3649-91

Gamma ray spectrometry.

901.1

p 92

7120 (19thEd.)

D 4785-88

4.5.2.3

Radioactive Strontium 89, 90.

Radio chemical

905.0

p 29

Sr-04

p 65

303, 7500-Sr B

R-1160-76

Sr-01 Sr-02

Tritium

Liquid scintillation

906.0

p 34

H-02

p 87

306, 7500-3H B

D 4107-91

R-1171-76

Gamma emitters

Gamma ray

901.1

p 92

7120 (19thEd.)

D 3649-91

R-1110-76

4.5.2.3

Spectrometry

902.0 901.0

7500-Cs B 7500-I B

D 4785-88

The procedures shall be done in accordance with the documents listed below. The incorporation by reference of documents 1 through 10 was approved by the Director of the Federal Register in accordance with 5 U.S.C. 552(a) and 1 CFR part 51. Copies of the documents may be obtained from the sources listed below. Information reguarding obtaining these documents can be obtained from the Safe Drinking Water Hotline at 800-426-4691. Documents may be inspected at EPA's Drinking Water Docket, 401 M Street, SW., Washington, DC 20460 (Telephone: 202-260-3027); or at the Office of Federal Register, 800 North Capitol Street, NW., Suite 700, Washington, DC.

Footnotes

1. "Prescribed Procedures for Measurement of Radioactivity in Drinking Water", EPA 600/4-80-032, August 1980. Available at U.S. Department of Commerce, National Technical Information Service (NTIS), 5285 Port Royal Road, Springfield, VA 22161 (Telephone 800-553-6847), PB 80-224744.

2. "Interim Radiochemical Methodology for Drinking Water", EPA 600/4-75-008(revised), March 1976. Available at NTIS, ibid. PB 253258.

3. "Radiochemistry Procedures Manual", EPA 520/5-84-006, December 1987. Available at NTIS, ibid. PB 84-215581.

4. "Radiochemical Analytical Procedures for Analysis of Environmental Samples", March 1979. Available at NTIS, ibid. EMSL LV 053917.

5. "Standard Methods for the Examination of Water and Wastewater", 13th, 17th, 18th, 19th Editions, 1971, 1989, 1992, 1995. Available at American Public Health Association, 1015 Fifteenth Street N. W., Washington, D.C. 20005. All methods are in the 17th, 18th, and 19th editions except 7500-U C Fluorometric Uranium was discontinued after the 17th Edition, 7120 Gamma Emitters is only in the 19th Edition, and 302, 303, 304, 305 and 306 are only in the 13th Edition.

6. Annual Book of ASTM Standards, Vol. 11.02, 1994. Available at American Society for Testing and Materials, 100 Barr Harbor Drive, West Conshohocken, PA 19428.

7. "Methods for Determination of Radioactive Substances in Water and Fluvial Sediments", Chapter A5 in Book 5 of Techniques of Water-Resources Investigations of the United States Geological Survey, 1977. Available at U. S. Geological Survey (USGS) Information Services, Box 25286, Federal Center, Denver, CO 80225-0425.

8. "EML Procedures Manual", 27th Edition, Volume 1, 1990. Available at the Environmental Measurements Laboratory, U.S. Department of Energy (DOE), 376 Hudson Street, New York, NY 10014-3621.

9. "Determination of Ra-226 and Ra-228 (Ra-02)", January 1980, Revised June 1982. Available at Radiological Sciences Institute Center for Laboratories and Research, New York State Department of Health, Empire State Plaza, Albany, NY 12201.

10. "Determination of Radium 228 in Drinking Water", August 1980. Available at State of New Jersey, Department of Environmental Protection, Division of Environmental Quality, Bureau of Radiation and Inorganic Analysis Services, 9 Ewing Street, Trenton, NJ 08625.

11. Natural uranium and thorium-230 are approved as gross alpha calibration standards for gross alpha with co-precipitation and evaporation methods; americium-241 is approved with co-precipitation methods.

12. If uranium (U) is determined by mass, a 0.67 pCi/ug of uranium conversion factor must be used. This conservative factor is based on the 1:1 activity ratio of U-234 to U-238 that is characteristic of naturally occurring uranium.

13. "Determination of Trace Elements in Waters and Wastes by Inductively Coupled Plasma-Mass Spectrometry," Revision 5.4, which is published in "Methods for the Determination of Metals in Environmental Samples-Supplement I," EPA 600-R-94-111, May 1994. Available at NTIS, PB 95-125472.

14. "The Determination of Radium-226 and Radium-228 in Drinking Water by Gamma-ray Spectrometry Using HPGE or Ge(Li) Detectors,'' Revision 1.2, December 2004. Available from the Environmental Resources Center, Georgia Institute of Technology, 620 Cherry Street, Atlanta, GA 30332-0335, USA, Telephone: 404-894-3776. This method may be used to analyze for radium-226 and radium-228 in samples collected after January 1, 2005 to satisfy the radium-226 and radium-228 monitoring requirements specified at 40 CFR 141.26.

1. When the identification and measurement of radionuclides other than those listed in table 0400-45-01-.11(1), the following references are to be used, except in cases where alternative methods have been approved by the Department.
(i) Procedures for Radiochemical Analysis of Nuclear Reactor Aqueous Solutions, H. L. Krieger and S. Gold, EPA-RA-73-014, USEPA, Cincinnati, Ohio, May, 1973.
(ii) HASL Procedure Manual, Edited by John H. Harley, HASL 300, ERDA Health and Safety Laboratory, New York, NY., 1973.
2. The inorganic contaminants from table 0400-45-01-.14(10)(h) that have alternative testing methods are given in the following table:

TABLE 0400-45-01-.14(10)(h) 2

Contaminant

Methodology

SM 21 st Edition 1

ASTM 2

Naturally Occurring

Gross alpha and beta

Evaporation

7110 B

Gross alpha

Coprecipitation

7110 C

Radium 226

Radon emanation

7500-Ra C

D3454-05

Radiochemical

7500-Ra B

D2460-07

Radium 228

Radiochemical

7500-Ra D

Uranium

Radiochemical

7500-U B

ICP-MS

D5673-05

Alpha spectrometry

7500-U C

Laser Phosphorimetry

D5174-07

Man-Made:

Radioactive Cesium

Radiochemical

7500-Cs B

Gamma Ray Spectrometry

7120

D3649-06

Radioactive Iodine

Radiochemical

7500-I B

D3649-06

Gamma Ray Spectrometry

7120

D4785-08

Radioactive Strontium 89, 90

Radiochemical

7500-Sr B

Tritium

Liquid Scintillation

7500-3H B

D4107-08

Gamma Emitters

Gamma Ray Spectrometry

7120

7500-Cs B

7500-I B

D3649-06

D4785-08

Footnotes

1 Standard Methods for the Examination of Water and Wastewater, 21st edition (2005). Available from American Public Health Association, 800 I Street NW, Washington, DC 20001- 3710

2 Available from ASTM International, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959 or http://astm.org. The methods listed are the only alternative versions that may be used.

(i) Public Water Systems required to monitor disinfectant residuals by this Chapter must utilize one of the methods in the following table. In addition Water Systems may use of the ITS free chlorine test strip for the determination of free chlorine. Use of the test strips is described in Method D99-003, "Free Chlorine Species (HOCl- and OCl-) by Test Strip,'' Revision 3.0, November 21, 2003, available from Industrial Test Systems, Inc., 1875 Langston St., Rock Hill, SC 29730. Free and total chlorine residuals may be measured continuously by adapting a specified chlorine residual method for use with a continuous monitoring instrument provided the chemistry, accuracy, and precision remain the same. Instruments used for continuous monitoring must be calibrated with a grab sample measurement at least every five days, or with a protocol approved by the Department.

TABLE 0400-45-01-.14(10)(i)

Methodology

SM (19th or 20th ed)

SM

Online2

Other

Residual measured1

O3

Free Cl2

Combined

Cl2

Total Cl2

ClO

2

Amperometric Titration

4500-Cl D

4500-Cl-D-00

D 1253-033

X

X

X

Low Level

Amperometric

Titration

4500-Cl E

4500-Cl-E-00

X

DPD Ferrous Titrimetric

4500-Cl F

4500-Cl-F-00

X

X

X

DPD Colorimetric

4500-Cl G

4500-Cl-G-00

X

X

X

Syringaldazine (FACTS)

4500-Cl H

4500-Cl-H-00

X

Iodometric Electrode

4500-Cl I

4500-Cl-I-00

X

DPD

4500-ClO2D

X

Amperometric Method II

4500-ClO2E

4500 ClO2 E-00

X

Spectrophotometr ic

327.0 Rev1.14

X

Indigo Method

4500-O3 B

4500-O3

B-97

X

Footnotes

1. X indicates method is approved for measuring specified disinfectant residual. Free chlorine or total chlorine may be measured for demonstrating compliance with the chlorine MRDL and combined chlorine, or total chlorine may be measured for demonstrating compliance with the chloramine MRDL.

2. The Standard Methods Online version that is approved is indicated by the last two digits in the method number which is the year of approval by the Standard Method Committee. Standard Methods Online are available at http://www.standardmethods.org.

3. Annual Book of ASTM Standards, Vol. 11.01, 2004 ; ASTM International; any year containing the cited version of the method may be used. Copies of this method may be obtained from ASTM International, 100 Barr Harbor Drive, P.O. Box C700 West Conshohocken, PA 19428-2959.

4. EPA Method 327.0, Revision 1.1, "Determination of Chlorine Dioxide and Chlorite Ion in Drinking Water Using Lissamine Green B and Horseradish Peroxidase with Detection by Visible Spectrophotometry,'' USEPA, May 2005, EPA 815-R-05-008. Available online at http://www.epa.gov/safewater/methods/sourcalt.html.

1. Alternative testing methods for the disinfectant residuals given in table 0400-45-01-.14(10)(i) are given in the following table:

TABLE 0400-45-01-.14(10)(i) 1.

Residual

Methodology

SM 21 st Edition1

ASTM 2

Other

Free Chlorine

Amperometric Titration

4500-Cl D

D 1253-08

DPD Ferrous Titrimetric

4500-Cl F

DPD Colorimetric

4500-Cl G

Syringaldazine (FACTS)

4500-Cl H

On-line Chlorine Analyzer

EPA 334.0 3

Amperometric Sensor

Chlorosense 4

Total Chlorine

Amperometric Titration

4500-Cl D

D 1253-08

Amperometric Titration (Low level measurement)

4500-Cl E

DPD Ferrous Titrimetric

4500-Cl F

DPD Colorimetric

4500-Cl G

Iodometric Electrode

4500-Cl I

On-line Chlorine Analyzer

EPA 334.0 3

Amperometric Sensor

Chlorosense 4

Chlorine Dioxide

Amperometric Titration

4500-ClO2 C

Amperometric Titration

4500-ClO2 E

Ozone

Indigo Method

4500-O3 B

Footnotes

1 Standard Methods for the Examination of Water and Wastewater, 21st edition (2005). Available from American Public Health Association, 800 I Street NW, Washington, DC 20001- 3710

2 Available from ASTM International, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959 or http://astm.org. The methods listed are the only alternative versions that may be used.

3 EPA Method 334.0. "Determination of Residual Chlorine in Drinking Water Using an On-line Chlorine Analyzer," September 2009. EPA 815-B-09-013. Available at http://epa.gov/safewater/methods/analyticalmethods_ogwdw.html.

4 Chlorosense. "Measurement of Free and Total Chlorine in Drinking Water by Palintest Chlorosense," August 2009. Available at http://www.nemi.gov or from Palintest Ltd, 21 Kenton Lands Road, PO Box 18395, Erlanger, KY 41018.

(j) Analysis conducted to determine compliance with Rule 0400-45-01-.12 shall be made in accordance with the methods described in the following table:

TABLE 0400-45-01-.14(10)(j)

Contaminant

EPA

ASTM3

SM418thand 19th

ed.

SM420th ed.

SM7Online

Other

1. Aluminum

200.72

200.82

200.92

3120 B

3113 B

3111 D

3120 B

3120 B-99

3113 B-99

3111 D-99

2. Chloride

300.01

300.16

D4327-97, 03

D512-89 Reapproved 1999) B

4110 B

4500-Cl - D

4500-Cl-B

4110 B 4500-Cl - D

4500-Cl-B

4110 B- 00

4500-Cl - D-97

4500-Cl-B-97

D6508, Rev.

28

3. Color

2120 B

2120 B

2120 B-01

4. Foaming Agents

5540 C

5540 C

5540 C-00

5. Iron

200.72200.92

3120 B

3111 B

3113 B

3120 B

3120 B-99

3111 B-99

3113 B-99

6. Manganese

200.72200.82200.92

3120 B

3111 B

3113 B

3120 B

3120 B-99

3111 B-99

3113 B-99

7. Odor

2150 B

2150 B

2150 B-97

8. Silver

200.72

200.82

200.92

3120 B

3111 B

3113 B

3120 B

3120 B-99

3111 B-99

3113 B-99

I-3720-855

9. Sulfate

300.01

300.16

375.21

D4327-97, 03

D516-90, 02

4110 B

4500-SO42-F

4500-SO42-C,D

4500-SO42-E

4110 B

4500-SO42-F

4500-SO42-C,D

4500-SO42-E

4110 B-00

D6508, Rev.

28

10. Total Dissolved Solids

200.72

2540 C

2540 C

2540 C-97

11. Zinc

200.82

3120 B

3111 B

3120 B

3120 B-99

3111 B-99

Footnotes

1. "Methods for the Determination of Inorganic Substances in Environmental Samples,'' EPA/600/R-93-100, August 1993. Available at NTIS, PB94-120821.

2. "Methods for the Determination of Metals in Environmental Samples-Supplement I,'' EPA/600/R-94-111, May 1994. Available at NTIS, PB 95-125472.

3. Annual Book of ASTM Standards, 1994, 1996, 1999, or 2004, Vols. 11.01 and 11.02, ASTM International; any year containing the cited version of the method may be used. Copies may be obtained from the ASTM International, 100 Barr Harbor Drive, West Conshohocken, PA 19428.

4. Standard Methods for the Examination of Water and Wastewater, 18th edition (1992), 19th edition (1995), or 20th edition (1998). American Public Health Association, 1015 Fifteenth Street, NW., Washington, DC 20005. The cited methods published in any of these three editions may be used, except that the versions of 3111 B, 3111 D, and 3113 B in the 20th edition may not be used.

5. Method I-3720-85, Techniques of Water Resources Investigation of the U.S. Geological Survey, Book 5, Chapter A-1, 3rd ed., 1989. Available from Information Services, U.S. Geological Survey, Federal Center, Box 25286, Denver, CO 80225-0425.

6. "Methods for the Determination of Organic and Inorganic Compounds in Drinking Water,'' Vol. 1, EPA 815-R-00-014, August 2000. Available at NTIS, PB2000-106981.

7. Standard Methods Online are available at http://www.standardmethods.org. The year in which each method was approved by the Standard Methods Committee is designated by the last two digits in the method number. The methods listed are the only online versions that may be used.

8. Method D6508, Rev. 2, "Test Method for Determination of Dissolved Inorganic Anions in Aqueous Matrices Using Capillary Ion Electrophoresis and Chromate Electrolyte,'' available from Waters Corp, 34 Maple St., Milford, MA, 01757, Telephone: 508/482-2131, Fax: 508/482-3625.

1. The alternative methods for the analyses identified in Rule 0400-45-01-.14(10)(j) conducted to determine compliance with Rule 0400-45-01-.12 shall be made in accordance with the methods described in the following table:

TABLE 0400-45-01-.14(10)(j) 1.

Contaminant

Methodology

EPA Method

ASTM 1

SM 21 st Edition2

SM Online 3

Aluminum

Axially viewed inductively coupled plasma-atomic emission spectrometry (AVICP-AES)

200.5, Revision 4.24

Atomic

Absorption;

Direct

3111 D

Atomic

Absorption;

Furnace

3113 B

Inductively Coupled Plasma

3120 B

Chloride

Silver Nitrate Titration

D 512-04 B

4500-Cl - B

Ion Chromatography

4110 B

Potentiometric Titration

4500-Cl - D

Color

Visual Comparison

2120 B

Foaming Agents

Methylene Blue Active Substances (MBAS)

5540 C

Iron

Axially viewed inductively coupled plasma-atomic emission spectrometry (AVICP-AES)

200.5, Revision 4.2

Atomic

Absorption;

Direct

3111 B

Atomic

Absorption;

Furnace

3113 B

Inductively Coupled Plasma

3120 B

Manganese

Axially viewed inductively coupled plasma-atomic emission spectrometry (AVICP-AES)

200.5, Revision 4.2

Atomic

Absorption;

Direct

3111 B

Atomic

Absorption;

Furnace

3113 B

Inductively Coupled Plasma

3120 B

Odor

Threshold Odor Test

2150 B

Silver

Axially viewed inductively coupled plasma-atomic emission spectrometry (AVICP-AES)

200.5, Revision 4.2

Atomic

Absorption;

Direct

3111 B

Atomic

Absorption;

Furnace

3113 B

Inductively

3120 B

Coupled Plasma

Sulfate

Ion Chromatography

4110 B

Gravimetric with ignition of residue

4500-SO4 -2 C

4500-SO4 -2 C-97

Gravimetric with drying of residue

4500-SO4 -2 D

4500-SO4 -2 D-97

Turbidimetric method

4500-SO4 -2 E

4500-SO4 -2 E-97

Automated methylthymol blue method

4500-SO4 -2 F

4500-SO4 -2 F-97

Total Dissolved Solids

Total Dissolved Solids Dried at 180 deg C

2540 C

Zinc

Axially viewed inductively coupled plasma-atomic emission spectrometry (AVICP-AES)

200.5, Revision 4.2

Atomic Absorption; Direct Aspiration

3111 B

Inductively Coupled Plasma

3120 B

Footnotes

1 Available from ASTM International, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959 or http://astm.org. The methods listed are the only alternative versions that may be used.

2 Standard Methods for the Examination of Water and Wastewater, 21st edition (2005). Available from American Public Health Association, 800 I Street NW, Washington, DC 20001- 3710

3 Standard Methods Online are available at http://www.standardmethods.org. The year in which each method was approved by the Standard Methods Committee is designated by the last two digits in the method number. The methods listed are the only online versions that may be used.

4 EPA Method 200.5, Revision 4.2. "Determination of Trace Elements in Drinking Water by Axially Viewed Inductively Coupled Plasma-Atomic Emission Spectrometry." 2003. EPA/600/R-06/115. (Available at http://www.epa.gov/nerlcwww/ordmeth.htm.)

(k) Disinfection byproducts
1. Systems required to monitor by this Chapter for disinfection byproducts must utilize the approved methods in the following table:

TABLE 0400-45-01-.14(10)(k) 1.

Approved Methods for Disinfection Byproduct Compliance Monitoring

Contaminant and methodology1

EPA method

Standard method2

SM online9

ASTM method3

TTHM

P&T/GC/ElCD & PID

502.24

P&T/GC/MS

524.2

LLE/GC/ECD

551.1

HAA5

LLE (diazomethane)/GC/ECD

6251 B5

6251 B-94

SPE (acidic methanol)/GC/ECD

552.15

LLE (acidic methanol)/GC/ECD

552.2, 552.3

Bromate

Ion chromatography

300.1

D 6581-00

Ion chromatography & post column reaction

317.0 Rev 2.06,

326.06

IC/ICP-MS

321.86,7

Chlorite

Amperometric titration

4500-ClO2 E8

4500-ClO2 E-00 8

Spectrophotometry

327.0 Rev 1.18

Ion chromatography

300.0,

300.1, 317.0

Rev 2.0, 326.0.

D 6581-00

1P&T=purge and trap; GC=gas chromatography; ElCD=electrolytic conductivity detector; PID=photoionization detector; MS=mass spectrometer; LLE=liquid/liquid extraction; ECD=electron capture detector; SPE=solid phase extraction; IC=ion chromatography; ICP-MS=inductively coupled plasma/mass spectrometer.

2 19 th and 20th editions of Standard Methods for the Examination of Water and Wastewater, 1995 and 1998, respectively, American Public Health Association; either of these editions may be used.

3 Annual Book of ASTM Standards, 2001 or any year containing the cited version of the method, Vol 11.01.

4If TTHMs are the only analytes being measured in the sample, then a PID is not required.

5The samples must be extracted within 14 days of sample collection.

6Ion chromatography & post column reaction or IC/ICP-MS must be used for monitoring of bromate for purposes of demonstrating eligibility of reduced monitoring, as prescribed in Rule 0400-45-01-.36(6)(b) 3.(ii).

7Samples must be preserved at the time of sampling with 50 mg ethylenediamine (EDA)/L of sample and must be analyzed within 28 days.

8Amperometric titration or spectrophotometry may be used for routine daily monitoring of chlorite at the entrance to the distribution system, as prescribed in Rule 0400-45-01-.36(6)(b) 2.(i)(I). Ion chromatography must be used for routine monthly monitoring of chlorite and additional monitoring of chlorite in the distribution system, as prescribed in Rules 0400-45-01-.36(6)(b) 2.(i)(II) and (b)2.(ii).

9The Standard Methods Online version that is approved is indicated by the last two digits in the method number which is the year of approval by the Standard Method Committee. Standard Methods Online are available at http://www.standardmethods.org.

(i) Alternative testing methods for the disinfection by products given in table 0400-45-01-.14(10)(k) 1. are given in the following table:

TABLE 0400-45-01-.14(10)(k) 1.(i)

Contaminant

Methodology

EPA Method

ASTM 1

SM 21 st Edition2

TTHM

P&T/GC/MS

524.3 3

HAA5

LLE (diazomethane)/GC/ECD

6251 B

Ion Chromatography Electrospray Ionization Tandem Mass Spectrometry (IC-ESI-MS/MS)

557 4

Bromate

Two-Dimensional Ion Chromatography (IC)*

302.0 5

Ion Chromatography Electrospray Ionization Tandem Mass Spectrometry (IC-ESI-MS/MS)*

557 4

Chemically Supressed Ion Chromatography

D 6581-08 A

Electrolytically Supressed Ion Chromatography

D 6581-08 B

Chlorite

Chemically Supressed Ion Chromatography

D 6581-08 A

Electrolytically Supressed Ion Chromatography

D 6581-08 B

Chlorite - daily

Amperometric Titration

4500-ClO2 E

monitoring as prescribed in Rule 0400-45-01-.36(6)(b) 2.(i)(I)

Footnotes

1 Available from ASTM International, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959 or http://astm.org. The methods listed are the only alternative versions that may be used.

2 Standard Methods for the Examination of Water and Wastewater, 21st edition (2005). Available from American Public Health Association, 800 I Street NW, Washington, DC 20001- 3710

3 EPA Method 524.3, Version 1.0. "Measurement of Purgeable Organic Compounds in Water by Capillary Column Gas Chromatography/Mass Spectrometry," June 2009. EPA 815-B-09-009. Available at http://epa.gov/safewater/methods/analyticalmethods_ogwdw.html.

4 EPA Method 557. "Determination of Haloacetic Acids, Bromate, and Dalapon in Drinking Water by Ion Chromatography Electrospray Ionization Tandem Mass Spectrometry (IC-ESI-MS/MS)," September 2009. EPA 815-B-09-012. Available at http://epa.gov/safewater/methods/analyticalmethods_ogwdw.html.

5 EPA Method 302.0. "Determination of Bromate in Drinking Water using Two-Dimensional Ion Chromatography with Supressed Conductivity Detection," September 2009. EPA 815-B-09-014. Available at http://epa.gov/safewater/methods/analyticalmethods_ogwdw.html.

*Only IC and IC-ESI-MS/MS have an MRL <0.0010 mg/l and may be used for Bromate monitoring listed under EPA 815-B-09-014. Available at http://epa.gov/safewater/methods/analyticalmethods_ogwdw.html.

2. Laboratories must achieve quantitative results on the PE sample analyses that are within the following acceptance limits:

DBP

Acceptance limits

(percent of true

value)

Comments

TTHM

Chloroform

±20

Laboratory must meet all 4 individual THM acceptance limits in order to successfully pass a PE sample for TTHM

Bromodichloromethane

±20

Dibromochloromethane

±20

Bromoform

±20

HAA5

Monochloroacetic Acid

±40

Laboratory must meet the acceptance limits for all 5 of the HAA5 compounds in order to successfully pass a PE sample for HAA5

Dichloroacetic Acid

±40

Trichloroacetic Acid

±40

Monobromoacetic Acid

±40

Dibromoacetic Acid

±40

Chlorite

±30

Bromate

±30
3. Laboratories must report quantitative data for concentrations at least as low as the ones listed in the following table for all DBP samples analyzed for compliance with Rules 0400-45-01-.06, 0400-45-01-.36, 0400-45-01-.37, and 0400-45-01-.38:

DBP

Minimum reporting level (mg/L)1

Comments

TTHM2

Chloroform

0.0010

Bromodichloromethane

0.0010

Dibromochloromethane

0.0010

Bromoform

0.0010

HAA52

Monochloroacetic Acid

0.0020

Dichloroacetic Acid

0.0010

Trichloroacetic Acid

0.0010

Monobromoacetic Acid

0.0010

Dibromoacetic Acid

0.0010

Chlorite

0.020

Applicable to monitoring as prescribed in Rules 0400-45-01-.36(6)(b) 2(i)(II) and (b)2(ii).

Bromate

0.0050 or 0.00010

Laboratories that use EPA Methods 317.0 Revision 2.0, 326.0 or 321.8 must meet a 0.0010 mg/L MRL for bromate. The alternative methods for reduced monitoring under Rule 0400-45-01-.36(6)(b) 3.(ii)(II) meeting an MRL of < 0.0010 mg/L are EPA Method 302.0 and 557.

1 The calibration curve must encompass the regulatory minimum reporting level (MRL) concentration. Data may be reported for concentrations lower than the regulatory MRL as long as the precision and accuracy criteria are met by analyzing an MRL check standard at the lowest reporting limit chosen by the laboratory. The laboratory must verify the accuracy of the calibration curve at the MRL concentration by analyzing an MRL check standard with a concentration less than or equal to 110% of the MRL with each batch of samples. The measured concentration for the MRL check standard must be ±50% of the expected value, if any field sample in the batch has a concentration less than 5 times the regulatory MRL. Method requirements to analyze higher concentration check standards and meet tighter acceptance criteria for them must be met in addition to the MRL check standard requirement.

2 When adding the individual trihalomethane or haloacetic acid concentrations to calculate the TTHM or HAA5 concentrations, respectively, a zero is used for any analytical result that is less than the MRL concentration for that DBP, unless otherwise specified by the Department.

4. Additional analytical methods. Systems required to analyze parameters not included in subparagraph (i) and part (k)1. of this paragraph must use the following methods. A party approved by the EPA or the Department must measure these parameters.
(i) Alkalinity. All methods allowed in subparagraph (c) of this paragraph for measuring alkalinity.
(ii) Bromide. EPA Methods 300.0, 300.1, 317.0 Revision 2.0, 326.0, or ASTM D 6581-00.
(iii) Total Organic Carbon (TOC). Standard Method 5310 B or 5310 B-00 (High-Temperature Combustion Standard Method) or Standard Method 5310 C or 5310 C-00 (Persulfate-Ultraviolet or Heated-Persulfate Oxidation Method) or Standard Method 5310 D or 5310 D-00 (Wet-Oxidation Method) or EPA Method 415.3 Revision 1.1. Inorganic carbon must be removed from the samples prior to analysis. TOC samples may not be filtered prior to analysis. TOC samples must be acidified at the time of sample collection to achieve pH less than or equal to 2 with minimal addition of the acid specified in the method or by the instrument manufacturer. Acidified TOC samples must be analyzed within 28 days. The alternative testing methods for TOC are High Temperature Combustion, Standard Method 5310 B 21st edition (2005) or EPA Method 415.3, Revision 1.2; Persulfate-Ultraviolet or Heated Persulfate Oxidation, Standard Method 5310 C 21st edition (2005) or EPA Method 415.3, Revision 1.2; or Wet Oxidation, Standard Method 5310 D 21st edition (2005) or EPA Method 415.3, Revision 1.2.
(iv) Specific Ultraviolet Absorbance (SUVA). SUVA is equal to the UV absorption at 254 nm (UV254) (measured in m-1 divided by the dissolved organic carbon (DOC) concentration) (measured as mg/L). In order to determine SUVA, it is necessary to separately measure UV254 and DOC. When determining SUVA, systems must use the methods stipulated in item (I) of this subpart to measure DOC and the method stipulated in item (II) of this subpart to measure UV254. SUVA must be determined on water prior to the addition of disinfectants/oxidants by the system. DOC and UV254 samples used to determine a SUVA value must be taken at the same time and at the same location. The alternative testing method for SUVA is Calculation using DOC and UV254 data, EPA Method 415.3, Revision 1.2.
(I) Dissolved Organic Carbon (DOC). Standard Method 5310 B or 5310 B-00 (High-Temperature Combustion Method) or Standard Method 5310 C or 5310 C-00 (Persulfate-Ultraviolet or Heated-Persulfate Oxidation Method) or Standard Method 5310 D or 5310 D-00 (Wet-Oxidation Method) or EPA Method 415.3 Revision 1.1. DOC samples must be filtered through the 0.45 µm pore-diameter filter as soon as practical after sampling, not to exceed 48 hours. After filtration, DOC samples must be acidified to achieve pH less than or equal to 2 with minimal addition of the acid specified in the method or by the instrument manufacturer. Acidified DOC samples must be analyzed within 28 days of sample collection. Inorganic carbon must be removed from the samples prior to analysis. Water passed through the filter prior to filtration of the sample must serve as the filtered blank. This filtered blank must be analyzed using procedures identical to those used for analysis of the samples and must meet the following criteria: DOC < 0.5 mg/L. The alternative testing methods for DOC are High Temperature Combustion, Standard Method 5310 B 21st edition (2005) or EPA Method 415.3, Revision 1.2; Persulfate-Ultraviolet or Heated Persulfate Oxidation, Standard Method 5310 C 21st edition (2005) or EPA Method 415.3, Revision 1.2; or Wet Oxidation, Standard Method 5310 D 21st edition (2005) or EPA Method 415.3, Revision 1.2.
(II) Ultraviolet Absorption at 254 nm (UV254). Standard Method 5910 B or 5910 B-00 (Ultraviolet Absorption Method) or EPA Method 415.3 Revision 1.1. UV absorption must be measured at 253.7 nm (may be rounded off to 254 nm). Prior to analysis, UV254 samples must be filtered through a 0.45 µm pore-diameter filter. The pH of UV254 samples may not be adjusted. Samples must be analyzed as soon as practical after sampling, not to exceed 48 hours. The alternative testing method for UV254 is Spectrophotometry, Standard Method 5910 B 21 st edition (2005) or EPA Method 415.3, Revision 1.2.
(v) pH. All methods allowed in table 0400-45-01-.14(10)(c) for measuring pH.
(vi) Magnesium. All methods allowed in table 0400-45-01-.14(10)(c) for measuring magnesium.
(l) Cryptosporidium. Systems must analyze for Cryptosporidium using Method 1623: Cryptosporidium and Giardia in Water by Filtration/I MS/FA, 2005, United States Environmental Protection Agency, EPA-815-R-05-002 or Method 1622: Cryptosporidium in Water by Filtration/IMS/FA, 2005, United States Environmental Protection Agency, EPA-815-R-05-001, which are incorporated by reference. The Director of the Federal Register approves this incorporation by reference in accordance with 5 U.S.C. 552(a) and 1 CFR part 51. You may obtain a copy of these methods online from http://www.epa.gov/safewater/disinfection/lt2 or from the United States Environmental Protection Agency, Office of Ground Water and Drinking Water, 1201 Constitution Ave., NW, Washington, DC 20460 (Telephone: 800-426-4791). You may inspect a copy at the Water Docket in the EPA Docket Center, 1301 Constitution Ave., NW, Washington, DC, (Telephone: 202-566-2426) or at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030, or go to:

http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html.

1. Systems must analyze at least a 10 L sample or a packed pellet volume of at least 2 ml as generated by the methods listed in this subparagraph. Systems unable to process a 10 L sample must analyze as much sample volume as can be filtered by two filters approved by EPA for the methods listed in this subparagraph, up to a packed pellet volume of at least 2 ml.
2.
(i) Matrix spike (MS) samples, as required by the methods in this subparagraph, must be spiked and filtered by a laboratory approved for Cryptosporidium analysis under part 4 of this subparagraph.
(ii) If the volume of the MS sample is greater than 10 L, the system may filter all but 10 L of the MS sample in the field, and ship the filtered sample and the remaining 10 L of source water to the laboratory. In this case, the laboratory must spike the remaining 10 L of water and filter it through the filter used to collect the balance of the sample in the field.
3. Flow cytometer-counted spiking suspensions must be used for MS samples and ongoing precision and recovery (OPR) samples.
4. Systems must have Cryptosporidium samples analyzed by a laboratory that is approved under EPA's Laboratory Quality Assurance Evaluation Program for Analysis of Cryptosporidium in Water or a laboratory that has been certified for Cryptosporidium analysis by an equivalent State laboratory certification program.

Notes

Tenn. Comp. R. & Regs. 0400-45-01-.14
Original rule filed August 1, 2012; effective October 30, 2012. Rule was previously numbered 1200-05-01. Amendments filed November 19, 2018; effective 2/17/2019.

Authority: T.C.A. §§ 4-5-201, et seq.; 68-203-101, et seq.; and 68-221-701, et seq.

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