PURPOSE: This rule lists manuals containing acceptable analysis procedures for determination of contaminant levels.

Editor’s Note: The secretary of state has determined that the publication of this rule in its entirety would be unduly cumbersome or expensive. The entire text of the material referenced has been filed with the secretary of state. This material may be found at the Office of the Secretary of State or at the headquarters of the agency and is available to any interested person at a cost established by state law.

1. (1) Inorganic and Radiological Contaminants. Unless substitute methods are approved by the department, analysis shall be conducted in accordance with the methods listed in the following table. Criteria for analyzing arsenic, barium, beryllium, cadmium, calcium, chromium, copper, lead, nickel, selenium, sodium, and thallium with digestion or directly without digestion, and other analytical test procedures are contained in “Technical Notes on Drinking Water Methods,” EPA- 600/R-94-173, October 1994. This document also contains approved analytical test methods which remain available for compliance monitoring until July 1, 1996. These methods will not be available for use after July 1, 1996. This document is available from the National Technical Information Service, NTIS PB95-104766, U.S. Department of Commerce, 5285 Port Royal Road, Springfield, VA 22161. The toll-free number is 800- 553-6847. Contaminant

Aluminum

Antimony

Arsenic

Asbestos

Barium

Beryllium

Cadmium

Chloride

Chromium

Color

Copper Methodology Method (if appropriate) (if appropriate)

Inductively Coupled Plasma—Emission Spectroscopy

Inductively Coupled Plasma—Mass Spectrometry Atomic Absorption—Platform Technique

Atomic Absorption—Gaseous Hydride Atomic Absorption—Graphite Furnace Inductively Coupled Plasma—Mass Spectrometry Atomic Absorption—Platform Technique

Atomic Absorption—Graphite Furnace

Atomic Absorption—Gaseous Hydride

Atomic Absorption—Platform Inductively Coupled Plasma—Emission Spectroscopy

Inductively Coupled Plasma—Mass Spectrometry

Transmission Electron Microscopy

Inductively Coupled Plasma—Mass Spectrometry Atomic Absorption—Graphite Furnace Atomic Absorption—Direct Aspiration Inductively Coupled Plasma—Emission Spectroscopy

Atomic Absorption—Graphite Furnace

Atomic Absorption—Platform Inductively Coupled Plasma—Emission Spectroscopy

Inductively Coupled Plasma—Mass Spectrometry

Atomic Absorption—Graphite Furnace Atomic Absorption—Platform Inductively Coupled Plasma—Emission Spectroscopy Inductively Coupled Plasma—Mass Spectrometry

Atomic Absorption—Furnace Technique Atomic Absorption—Platform Inductively Coupled Plasma—Emission Spectroscopy

Inductively Coupled Plasma—Mass Spectrometry

Atomic Absorption—Furnace Technique

Atomic Absorption—Platform Reference

200.7 3120B 200.8 200.9 3113B 3111D

D3697-92 3113B 200.8 200.9

D2972-93C 3113B D2972-93B 3114B 200.9 200.7 3120B 200.8

100.1 100.2

200.8 3113B 3111D 200.7 3120B

D3645-93B 3113B 200.9 3120B 200.7 200.8

3113B 200.9 200.7 200.8

300.0 D4327-91 4500-Cl-D

3113B 200.9 200.7 3120B 200.8

2120B

D1688-90C 3113B 200.9 Contaminant

Copper (cont.)

Cyanide

Fluoride

Foaming Agents

Iron

Lead

Manganese

Mercury

Nickel Methodology Method (if appropriate) (if appropriate)

Atomic Absorption—Direct Aspiration

Inductively Coupled Plasma

Inductively Coupled Plasma—Mass Spectrometry

Manual distillation followed by— 1. Amenable Spectrophotometric

1. 2. Spectrophotometric—Manual
2. 3. Spectrophotometric— Manual—Semiautomated
3. 4. Selective Electrode

Colorimetric SPADNS, with distillation Ion Chromatography

Manual Electrode

Automated Alizarin Fluoride Blue, with distillation (complexone)

Automated Ion Selective Electrode

Atomic Absorption—Furnace Technique

Inductively Coupled Plasma—Mass Spectrometry Atomic Absorption—Platform Furnace

Manual cold vapor technique

Automated cold vapor technique Inductively Coupled Plasma—Mass Spectrometry

Atomic Absorption—Direct Aspiration Atomic Absorption—Platform Technique 10 CSR 60-5

Reference

D1688-90A 3111B 200.7 3120B 200.8

4500-CN-C D2036-91B 4500 CN-G D2036-91A 4500 CN-E 1-3300-85

335.4 4500 CN-F

4500 F-B&D 300.0 D4327-91 4110B D1179- 93B 4500 F-C

4500 F-E 129-71W 380-75WE

5540C

200.7 200.9 3120B 3111B 3113B

D3559-90D 3113B 200.8 200.9

200.7 200.8 200.9 3120B 3111B 3113B

245.1 D3223-91 3112B 245.2 200.8

3111B 200.9 Contaminant

Nickel (cont.)

Nitrate

Nitrite

Odor

Operational Monitoring— General Operational Monitoring— pH

Operational Monitoring— Residual Disinfectant Monitoring— Chlorine Dioxide

Operational Monitoring— Residual Disinfectant Monitoring— Free Chlorine

Combined Chlorine

Methodology Method (if appropriate) (if appropriate)

Inductively Coupled Plasma—Emission Spectroscopy

Inductively Coupled Plasma—Mass Spectrometry Atomic Absorption—Graphite Furnace

Manual Cadmium Reduction

Automated Cadmium Reduction

Ion Selective Electrode

Ion Chromatography

Spectrophotometric Automated Cadmium Reduction

Manual Cadmium Reduction

Ion Chromatography

pH Value

Amperometric Titration

DPD Method

Amperometric Titration DPD Ferrous Titrimetric DPD Colorimetric Syringaldazine (FACTS)

Amperometric Titration Amperometric Titration—low level measurement DPD Ferrous Titrimetric DPD Colorimetric Iodometric Electrode Reference

200.7 3120B 200.8 3113B

D3867-90B 4500 NO3-E 353.2 D3867-90A 4500 NO3-F 4500 NO3-D

300.0 B1011 4110B D4327-91

4500-NO3-B 353.2 D3867-90A 4500 NO3-F D3867-90B 4500-NO3-E 300.0 B1011 D4327-91 4110B

2150B

150.1 150.2 D1293-84 4500-H+-B

4500-ClO C 4500-ClO E 4500-ClO D

4500-Cl D 4500-Cl F 4500-Cl G 4500-Cl H

4500-Cl D 4500-Cl E 4500-Cl F 4500-Cl G 4500-Cl I Contaminant

Operational Monitoring— Lead and Copper Regulation

Operational Monitoring— Residual Disinfectant Monitoring— Ozone

Operational Monitoring— Temperature

Radionuclides Methodology (if appropriate) (if appropriate)

pH Electrometric

Conductivity

Calcium (EDTA Titrimetric)

(Inductively Coupled Plasma)

(Atomic Absorption—Direct Aspiration)

Alkalinity (Titrimetric)

(Electrometric Titration)

Orthophosphate (unfiltered, no digestion or hydrolysis) (Colorimetric, automated ascorbic acid)

(Colorimetric, ascorbic acid single reagent) (Colorimetric, phosphomolybdate, automated-segmented flow, automated discrete)

(Ion Chromatography)

Silica (Colorimetric, molybdate blue, automated-segmented flow)

(Colorimetric) (Molybdosilicate) (Heteropoly blue) (Automated method for molybdate-reatine silica) (Inductively Coupled Plasma)

Indigo

Thermometric

Examination of Water & Wastewater for Radioactivity 10 CSR 60-5

Method

150.1 150.2 D1293-84 4500-H+-B D1125-91A 2510B D511-93A 3500-Ca-D 200.7 3120B D511-93B 3111B D1067-92B 2320B I-1030-85

365.1 4500-P-F D515-88A 4500-P-E

I-1601-85 I-2601-90 I-2598-85 300.0 D4327-91

I-1700-85 I-2700-85 D859-88 4500-Si-D 4500-Si-E

4500-Si-F 200.7 3120B

4500-O B

2550B Reference Contaminant

Radionuclides (cont.)

Selenium

Silver

Sulfate

Thallium

Total Dissolved Solids

Turbidity

Great Lakes Instruments Method 2

Sodium

Zinc

1. (A) References for analytical methods in 10 CSR 60-5.010(1):

   1. 1. “Methods of Chemical Analysis of Water and Wastes,” EPA Environmental Monitoring and Support Laboratory, Cincinnati, OH 45268

(EPA-600/4-79-020), March 1983. Available from National Technical Information Service, PB84-128677. Methods 150.1, 150.2 and 246.2 are also available from U.S. EPA, EMSL, Cincinnati, OH 45268.

1. 2. Annual Book of ASTM Standards, Vols. 11.01 and 11.02, 1991, American Society for Testing and Materials, 1916 Race Street, Philadel-

phia, PA 19103.

1. 3. Standard Methods for the Examination of Water and Wastewater, 16th edition, American Public Health Association, American Water

Works Association, Water Pollution Control Federation, 1985.

1. 4. “Methods for Determination of Inorganic Substances in Water and Fluvial Sediments,” Techniques of Water-Resources Investigations

of the U.S. Geological Survey Books, Book 5, Chapter A1, Third Edition, 1989. Available at Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402.

1. 5. “Orion Guide to Water and Wastewater Analysis.” Form WeWWG/5880, p. 5, 1985. Orion Research, Inc., Cambridge, MA 02139.
2. 6. 200.7A “Inductively Coupled Plasma Atomic Emission Analysis of Drinking Water,” Appendix to Method 200.7, March 1987, U.S.

EPA, Environmental Monitoring and Support Laboratory, Cincinnati, OH 45268.

1. 7. “Analytical Method for Determination of Asbestos Fibers in Water,” Method 100.1, EPA-600/4-83-043, September 1983. Available

from National Technical Information Service, PB83-260471. Methodology Method (if appropriate) (if appropriate)

Gamma Spectrometry in Water Microquantities of Uranium in Water by Fluorometry Secondary Contaminants

Atomic Absorption—Hydride Generation

Atomic Absorption—Graphite Furnace

Atomic Absorption—Platform Inductively Coupled Plasma—Mass Spectrometry

Atomic Absorption—Graphite Furnace Inductively Coupled Plasma—Emission Spectroscopy Inductively Coupled Plasma—Mass Spectrometry Atomic Absorption—Platform Technique

Colorimetric—Methylthymol blue Gravimetric Turbidimetric Ion Chromatography

Atomic Absorption—Platform Technique Inductively Coupled—Plasma-Mass Spectrometry

Nephelometric

Inductively Coupled Plasma Atomic Absorption—Direct Aspiration Reference

D2459

D2907

D3859-93A 3114B D385-93 3113B 200.9 200.8

I-3720-85 200.7 200.8 200.9 3120B 3111B 3113B

375.2 4500 SO4-C, D 4500 SO4- F 300.0

D4327-91

200.9 200.8

2540C

2130B 180.1

200.7 3111B

200.8 3111B

1. 8. “Waters Test Method for the Determination of Nitrite/Nitrate in Water Using Single Column Ion Chromatography,” Method B-1011,

Millipore Corporation, Waters Chromatography Division, 34 Maple Street, Milford, MA 01757.

1. 9. “Fluoride in Water and Wastewater,” Industrial Method 129-71W, Technicon Industrial Systems, Tarrytown, NY 10591, December

1972.

1. 10. “Fluoride in Water and Wastewater,” Industrial Method No. 380-75WE, Technicon Industrial Systems, Tarrytown, NY 10591, Febru-

ary 1976.

1. 11. “Radiochemical Methodology for Drinking Water,” Environmental Monitoring Support Laboratory, EPA-600/4-75-008, U.S. EPA,

Cincinnati, OH 45268.

1. 12. “Procedures for Radiochemical Analysis of Nuclear Reactor Aqueous Solutions,” H.L. Krieger and S. Gold, EPA-R4-730014, U.S.

EPA, Cincinnati, OH, May 1973.

1. 13. HASL Procedure Manual, edited by John H. Harley, HASL 300, ERDA Health and Safety Laboratory, New York, NY, 1973.
2. 14. “Determination of and Trace Elements in Water and Wastes by Inductively Coupled Plasma-Mass Spectrometry,” Method 200.8, ver-

sion 4.3, August 1990, EPA, Environmental Monitoring and Systems Laboratory, Cincinnati, OH 45268. Available from ORD Publication, CERI, EPA, Cincinnati, OH 45268.

1. 15. “Determination of Metals and Trace Elements by Stabilized Temperature Graphite Furnace Atomic Absorption Spectrometry,” Method

200.9, version 1.1, August 1990, EPA, Environmental Monitoring and Systems Laboratory, Cincinnati, OH 45268.

1. 16. “Determination of Ozone in Water by the Indigo Method; A Submitted Standard Method,” Ozone Science and Engineering, Volume

4, pages 169–176, Pergamon Press Ltd., 1982.

1. 17. Standard Methods for the Examination of Water and Wastewater, 18th edition, American Public Health Association, American Water

Works Association, Water Pollution Control Federation, 1992.

1. 18. “Turbidity,” GLI Method 2, November 2, 1992, Great Lakes Instruments, Inc., 8855 North 55 Street, Milwaukee, WI 53223.
2. 19. Annual Book of ASTM Standards, Vols. 11.01 and 11.02, 1994, American Society for Testing and Materials, 1916 Race Street,

Philadelphia, PA 19103.

1. 20. “Determination of Metals and Trace Elements in Water and Wastes by Inductively Coupled Plasma-Mass Spectrometry” Method

200.8, August 1990, Revision 3.2 EPA EMSL. Available from U.S. EPA, EMSL Cincinnati, OH 45268.

1. 21. “Determination of Inorganic Ions in Water by Ion Chromatography” Method 300.8, December 1989, U.S. EPA EMSL. Available

from U.S. EPA, EMSL, Cincinnati, OH 45268.

1. 22. “Methods for the Determination of Metals in Environmental Samples—Supplement I, EPA-600/R-94-111, May 1994.” Available from

National Technical Information Service (NTIS) NTIS PB 94-184942, U.S. Department of Commerce, 5285 Port Royal Road, Springfield, VA 22161. The toll free number is (800) 553-6847.

1. 23. “Method 300. Determination of Inorganic Anions in Water by Ion Chromatography.” Inorganic Chemistry Branch, Environmental

Monitoring Systems Laboratory, August 1991.

1. 24. Available from the Books and Open-File Reports Section, United States Geological Survey, Federal Center, Box 25425, Denver, CO

80225-0425.

1. 25. “Methods for the Determination of Inorganic Substances in Environmental Samples,” EPA-600/R-93-100, August 1993. Available

from National Technical Information Service, PB94-121811.

1. 26. 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. Available from ATI, Orion, 529 Main Street, Boston, MA 02129.

1. 27. “Determination of Asbestos Structure over 10-cm in Length in Drinking Water,” Method 100.2, EPA-600/R-94-134, June 1994. Avail-

able from NTIS, PB94-201902. (2) Organic Contaminants. Unless substitute methods are approved, the following table includes acceptable analysis procedures for organic contaminants:

Contaminant

2,3,7,8-TCDD (Dioxin) 2,4-D

2,4,5-TP (Silvex) 515.1515.2, 3-Hydrodroxycarbofuran

Alachlor

Aldicarb

Aldicarb sulfoxide

Aldicarb sulfone

Aldrin

Atrazine

Benzo(a)pyrene

Butachlor

Carbaryl

Carbofuran

Chlordane

Dalapon

Di(2-ethylhexyl)adipate

Di(2-ethylhexyl)phthalate

Dibromochloropropane (DBCP)

Dicamba

Dieldrin Contaminant Dinoseb

Diquat

Method Endothall Endrin

515.1 515.2 Ethylene dibromide (EDB)

Glyphosate

531.1 6610 Heptachlor

525.2 Heptachlor epoxide 508.1 531.1

531.1 Hexachlorobenzene 531.1

Hexachlorocyclopentadiene

525.2 508.1 Lindane 525.2 508.1 525.2 Methomyl 550.1 Methoxychlor 525.2 531.1 Metolachlor 531.1 Metribuzin

525.2 Oxamyl (vydate) 508.1 515.1 Pentachlorophenol 552.1

525.2 Picloram 525.2 504.1 Polychlorinated biphenyls 515.1 515.2 Aroclors)

508 Aroclors) 508.1 508A (as deca- 525.2 chlorobiphenyl) Method Contaminant Propachlor 515.1 515.2 Simazine 549.1 548.1

Toxaphene

525.2 508.1 504.1 Total Trihalomethanes

Volatile Organic Chemicals (regulated and unregulated)

525.2 508.1 Footnotes 1) A nitrogen-phosphorous detector should be substituted for the electron capture detec- 525.2 tor in Method 505 (or another approved 508.1 method should be used) to determine alachlor, atrazine and simazine, if lower detection limits are required. 525.2 2) PCBs are qualitatively identified as Aro- 508.1 clors and measured for compliance purposes as decachlorobiphenyl. Each system which 525.2 monitors for PCBs shall analyze each sample using either Method 505 or Method 508. 508.1 3) Analyses of total trihalomethanes shall be conducted in accordance with these methods and “Technical Notes on Drinking Water 525.2 Methods,” EPA-600/R94-173, October 1994, 508.1 which is available at NTIS, PB95-104766. 531.1 4) In addition to Methods 502.2 and 524.2, analysis for bromodichloromethane, bromoform,* chlorodibromomethane, chloroform, 525.2 carbon tetrachloride, tetrachlorethylene, 508.1 1,1,1-trichloroethane, and trichloroethylene may also be conducted by EPA Method 551. 508.1 Analysis for 1,2,3-trichloropropane may be 525.2 conducted by Methods 502.1, 524.2 and 504.1. 508.1 525.2 References for analytical methods in 10 CSR 531.1 60-5.010(2): Methods 502.2, 505, 507, 508, 508A, 515.1 and 531.1 are in “Methods for 515.1 the Determination of Organic Compounds in 515.2 Drinking Water,” EPA-600/4-88-039, 525.2 December 1988, revised July 1991. Methods 506, 547, 550, 550.1 and 551 are in “Meth- 515.1 ods for the Determination of Organic Com- 515.2 pounds in Drinking Water—Supplement I,” EPA-600-4-90-020, July 1990. Methods 515.2, 524.2, 548.1, 549.1, 552.1 and 555 (as are in “Methods for the Determination of Organic Compounds in Drinking Water— Supplement II,” EPA-600/R-92-129, August (as 1992. Method 1613 is titled “Tetra-through Octa-Chlorinated Dioxins and Furans by Isotope-Dilution HRGC/HRMS,” EPA-821-B- 94-005, October 1994. These documents are Method

508.1 525.2

508.1 525.2

525.2 502.2 524.2

502.2 524.2 available from National Technical Information Service (NTIS) NTIS PB91-231480, PB91-146027, PB92-207703, and PB95- 104774, U.S. Department of Commerce, 5285 Port Royal Road, Springfield, VA 22161. The toll free number is (800) 553- 6847. Method 6651 shall be followed in accordance with the 18th edition of “Standard Methods for the Examination of Water and Wastewater,” 1992. Available from the American Public Health Association, 1015 Fifteenth Street NW, Washington, DC 20005. Method 6610 shall be followed in accordance with the “Supplement to the 18th Edition of Standard Methods for the Examination of Water and Wastewater,” 1994. Available from the American Public Health Association, 1015 Fifteenth Street NW, Washington, DC 20005. EPA Methods 504.1, 508.1 and 525.2 are available from U.S. EPA EMSL, Cincinnati, OH 45268. The phone number is (513) 569-7586. Other analytical test procedures are contained in Technical Notes on Drinking Water Methods, EPA-600/R-94-173, October 1994, NTIS PB95-104766.

502.1 Volatile halogenated organic chemicals in water by purge and trap gas chromatography 502.2 Volatile organic compounds in water by purge and trap capillary column gas chromatography with photoionization and electrolytic conductivity detectors in series 503.1 Volatile aromatic and unsaturated organic compounds in water by purge and trap gas chromatography 504.1 1,2-Dibromoethane (EDB), 1,2- Dibromo-3-chloropropane (DBCP), a n d 1 , 2 , 3 - Tr i c h l o r o p r o p a n e (123TCP) in Water by Microextraction and Gas Chromatography 505 Analysis of organohalide pesticides and commercial polychlorinated biphenyl products (Aroclors) in water by microextraction and gas chromatography 506 Determination of phthalate and adipate esters in drinking water by liquid-liquid extraction or liquid-solid extraction and gas chromatography with photoionization detection 507 Determination of nitrogenand phosphorus-containing pesticides in groundwater by gas chromatography with a nitrogen-phosphorus detector 508 Determination of chlorinated pesticides in water by gas chromatography with an electron capture detector 508.1 Determination of chlorinated pesticides, herbicides, and organohalides by liquid-solid extraction and electron capture gas chromatography 508A Screening for polychlorinated biphenyls by perchlorination and gas chromatography (for quantification if detected with Method 505 or 508) 515.1 Determination of chlorinated acids in water by gas chromatography with an electron capture detector, revision 5.0, May 1991 524.1 Measurement of purgeable organic compounds in water by purged column gas chromatography/mass spectrophotometry 524.2 Volatile organic chemicals in water by purge and trap capillary column gas chromatography/mass spectrophotometry 525.2 Determination of organic compounds in drinking water by liquidsolid extraction in capillary column gas chromatography/mass spectrometry 531.1 Measurement of N-methyl carbamoyloximes and N-methyl carbamates in water by direct aqueous injection HPLC with post-column derivatization 547 Analysis of glyphosate in drinking water by direct-aqueous-injection HPLC, with post-column derivatization 548 Determination of endothall in aqueous samples 549.1 Determination of diquat and paraquat in drinking water by liquidsolid extraction and high performance liquid chromatography with ultraviolet detection 550 Determination of polycyclic aromatic hydrocarbons in drinking water by liquid-liquid extraction and HPLC with coupled ultraviolet and fluorescence detection 550.1 Determination of polycyclic aromatic hydrocarbons in drinking water by liquid-solid extraction and HPLC with coupled ultraviolet and fluorescence detection 552 Determination of polycyclic aromatic hydrocarbons in drinking water by liquid-solid extraction and HPLC with coupled ultraviolet and fluorescence detection 551 Determination of chlorination disinfection byproducts and chlorinated solvents in drinking water by liquidliquid extraction and gas chromatography with electron-capture detection 555 Determination of chlorinated acids in water by high performance liquid chromatography with a photodiode 10 CSR 60-5

array ultraviolet detector

1613 “Tetra-through Octa-Chlorinated Dioxins and Furans by Isotope Dilution.” This method is available from U.S. EPA-OST, Sample Control Center, P.O. Box 1407, Alexandria, VA 22313. 6610 Carbamate pesticides 6651 Glyphosate herbicide

1. (3) Microbiological Contaminants. Unless substitute methods are approved, this section
2. (3) lists acceptable analysis procedures for microbiological contaminants. Contaminant Approved Manual or Procedure

3. (A) Escherichia coli. Public water systems must conduct analysis of Escherichia coli in accordance with one (1) of the (E. coli) following analytical methods:

   1. 1. EC medium supplemented with fifty (50) c/ml of 4-methylumbelliferyl-beta-D-glucuronide

4. (MUG) (final concentration). EC medium is described in Standard Methods for the Examination of Water and Wastewater, 1992, American Public Health Association, 18th edition, Method 9221E, p. 9–52, paragraph 1a. MUG may be added to EC medium before autoclaving. EC medium supplemented with fifty (50) c/ml of MUG is commercially available. At least ten (10) ml of EC medium supplemented with MUG must be used. The inner inverted fermentation tube may be omitted. The procedure for transferring a total coliform-positive culture to EC medium supplemented with MUG shall be as specified in 10 CSR 60-5.010(1)(B)2. for transferring a total coliform-positive culture to EC medium. Observe fluorescence with an ultraviolet light (366 nm) in the dark after incubating tube at 44.5 ± 0.2 degrees Celsius for 24 ± 2 hours;

   1. 2. Nutrient agar supplemented with 100 c/ml MUG (final concentration). Nutrient agar is described in Standard Methods for the Examination of Water and Wastewater, 1992, American Public Health Association, 18th edition, p. 9-47 to 9-48. This test is used to determine if a total coliform-positive sample, as determined by the membrane filter technique (MFT) or any other method in which a membrane filter is used, contains E. coli. Transfer the membrane filter containing a total coliform colony(ies) to nutrient agar supplemented with 100 c/ml (final concentration) MUG. After incubating the agar plate at thirty-five degrees Celsius (35°C) for four (4) hours, observe the colony(ies) under ultraviolet light (366 nm) in the dark for fluorescence. If fluorescence is visible, E. coli are present;
   2. 3. Minimal Medium ONPG-MUG (MMO-MUG) Test, as set forth in the article “National Field Evaluation of a 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 (4) hours (but not to exceed 28 hours total). And again test the medium for flouresecence. The MMO-MUG Test with hepes buffer in lieu of phosphate buffer is the only approved formulation for the detection of E. coli;
   3. 4. As an option to paragraph (3)(A)3. of this rule, 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. Observation of the results are described in 40 CFR 141.21(f)(6)(i); or
   4. 5. 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.

5. (B) Fecal Coliform. 1. Public water systems must conduct fecal coliform analysis in accordance with the following procedure: When the multiple-tube fermentation (MTF) technique or presence-absence (P-A) coliform test is used to test for total coliform, shake the lactose-positive presumptive tube or P-A vigorously and transfer the growth with a sterile three millimeter (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. For EPA-approved analytical methods which use a membrane filter, transfer the total coliformpositive culture by one (1) of the following methods: 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 membrane filter 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 coliformpositive colonies into EC medium. Gently shake the inoculated tubes of EC medium to insure adequate mixing and incubate in a waterbath at 44.5 ± 0.2 degrees Celsius 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 Standard Methods for the Examination of Water and Wastewater, 1992, American Public Health Association, 18th edition, Method 9221E, p. 9-2, paragraph 1a. Public water systems need only determine the presence or absence of fecal coliforms; a determination of fecal coliform density is not required. Only this method for fecal coliform is allowed for compliance with 10 CSR 60-4.020(5); or

   1. 2. Standard Methods for the Examination of Water and Wastewater, 1992, American Public Health Association, 18th edition.

      1. A. Fecal coliform most probable number (MPN) procedures, method 9221E, pages 9-52 to 9-53

(Note: A-1 Broth may be held up to three (3) months in a tightly closed screwcap tube at four degrees Celsius (4°C); Contaminant

1. (C) Heterotrophic Bacteria.
2. (D) Total Coliform.
3. (4) Sample collection for the contaminants listed in this rule must be conducted using the sample preservation, container and maximum holding time procedures specified in the following table. All other samples for contaminants in 10 CSR 60-5.010 shall be collected in accordance with procedures contained in the appropriate analytical method.

Contaminant Antimony Asbestos Barium Beryllium Cadmium Chromium Copper Preserved Unpreserved Cyanide Fluoride Lead Preserved Unpreserved Mercury Approved Manual or Procedure

1. B. Fecal coliform membrane filter procedure, method 9222D, pages 9-60 to 9-61.

Standard Methods for the Examination of Water and Wastewater, 1992, American Public Health Association, 18th edition, pour plate method, method 9215B. The time from sample collection to initiation of analysis may not exceed twenty-four (24) hours.

1. 1. The standard sample volume required for total coliform analysis, regardless of analytical method used, is one hundred milliliters (100 ml). The time from sample collection to initiation of analysis may not exceed forty-eight (48) hours. If the laboratory analyzes samples after thirty (30) hours and up to forty-eight (48) hours from sample collection, the laboratory shall indicate on the report of the analysis results that the data may be invalid because of excessive delay before sample processing.

2. 2. Standard Methods for the Examination of Water and Wastewater, 1992, American Public Health Association, 18th edition—

   1. A. Fermentation technique, method 9221A, B.

      1. (I) Lactose broth, as commercially available, may be used in lieu of lauryl tryptose broth, if

the system conducts at least twenty-five (25) parallel tests between this medium and lauryl tryptose broth using the water normally tested, and this comparison demonstrates that the false-positive rate for total coliforms, using lactose broth, is less than ten percent (10%).

1. (II) If inverted tubes are used to detect gas production, the media should cover these tubes at

least one-half (1/2) to two-thirds (2/3) after the sample is added.

1. (III) No requirement exists to run the completed phase on ten percent (10%) of all total col-

iform-positive confirmed tubes.

1. B. Membrane filter (MF) technique, method 9222A, B, C.

2. C. Presence-absence (P-A) coliform test, method 9221D.

   1. (I) Six-times formulation strength may be used if the medium is filter-sterilized rather than

autoclaved.

1. (II) No requirement exists to run the completed phase on ten percent (10%) of all total col-

iform-positive confirmed tubes.

1. D. ONPG-MUG Test (also known as the Autoanalysis Colilert System, method 9223).
2. E. Colisure test. The Colisure test must be incubated for twenty-eight (28) hours before exam-

ining the results. If an examination of the results at twenty-eight (28) hours is not convenient, then results may be examined at any time between twenty-eight (28) and forty-eight (48) hours. A description of the Colisure test may be obtained from the Millipore Corporation, Technical Service Department, 80 Ashby Road, Bedford, MA 01730.

Preservative Concentrated HNO3 to pH<2 Cool to 4°C Concentrated HNO3 to pH<2 Concentrated HNO3 to pH<2 Concentrated HNO3 to pH<2 Concentrated HNO3 to pH<2

Concentrated HNO3 to pH<2 NONE Cool to 4°C, NaOH to pH>12 None

Concentrated HNO3 to pH<2 NONE Concentrated HNO3 to pH<2 10 CSR 60-5

Container P or G P or G P or G P or G P or G P or G

P or G P or G P or G P or G

P or G P or G P or G Holding Time 6 months

6 months 6 months 6 months 6 months

6 months 14 days

1 month

6 months 14 days 28 days Contaminant Nickel Nitrate Chlorinated Nonchlorinated Nitrite Selenium Thallium

1. (A) If HNO cannot be used because of shipping restrictions, sample may be initially preserved by icing and immediately shipping to the laboratory. Upon receipt in the laboratory, the sample must be acidified with concentrated HNO3to pH<2 and held for sixteen

1. (16) hours before analysis. At time of analysis, sample container should be thoroughly rinsed with 1:1 HNO3; washings should be added to the sample.

   1. (B) P = Plastic, hard or soft.
   2. (C) G = Glass, hard or soft.
   3. (D) In all cases samples should be analyzed as soon after collection as possible.
   4. (E) For cyanide see method(s) for the information for preservation.
   5. (F) The system shall take each sample at the same sampling point unless conditions make another sampling point more representative of each source or treatment plant.
   6. (G) If a system draws water from more than one (1) source and the sources are combined before distribution, the system must sample at an entry point to the distribution system during periods of normal operating conditions (that is, when water is representative of all sources being used).
2. (5) The department may reduce the total number of samples a system must analyze by allowing the use of compositing. Composite samples from a maximum of five (5) sampling points are allowed provided that the detection limit of the method used for analysis is less than one-fifth (1/5) of the MCL. For a lower number of composited samples the allowable relationship between the detection limit and MCL will change proportionally. Compositing of samples must be done in the laboratory and the composite sample must be analyzed within fourteen (14) days of collection. If the population served by the system is greater than thirty-three hundred (>3300) persons, then compositing is permitted only at sampling points within a single system. In systems serving less than or equal to thirty-three hundred (3300) persons, the department may permit compositing among different systems provided the five (5)-sample limit is maintained. Preservative Container P or G Concentrated HNO3 to pH<2

Cool to 4°C P or G P or G Concentrated H2SO4 to pH<2 Cool to 4°C P or G P or G Concentrated HNO3 to pH<2 P or G Concentrated HNO3 to pH<2

1. (A) Compositing of samples may be Contaminant allowed for inorganic chemicals (IOCs) listed in 10 CSR 60-4.030(1) and synthetic organic chemicals (SOCs) listed in 10 CSR 60-4.040 and volatile organic chemicals (VOCs) listed in 10 CSR 60-4.010(2) and unregulated organic and inorganic chemicals listed in 10 CSR 60-4.110(2). Beryllium Atomic Absorption—Furnace
2. (B) If the concentration in the composite sample is greater than or equal to 0.0005 mg/l for any organic contaminant listed at 40 CFR 141.61(a), then a follow-up sample must be taken within fourteen (14) days at each sampling point included in the compos- Cadmium Atomic Absorption—Furnace ite. These samples must be analyzed for the contaminants which exceeded 0.0005 mg/l in the composite sample. Resampling is not Chromium Atomic Absorption—Furnace required for unregulated organic and inorganic chemicals listed in 10 CSR 60-4.110(2).
3. (C) If the concentration in the composite sample detects one (1) or more synthetic organic contaminants listed in paragraph (5)(D)2. of this rule, then a follow-up sample Copper must be taken within fourteen (14) days at each sampling point included in the composite. The follow-up sample must be analyzed for the contaminant(s) detected. Cyanide

4. (D) Detection limits.

   1. 1. Detection Limits for inorganic chem-

ical analytical methods are the following:

Detection Limits for Inorganic Contaminants

Detection Lead

Contaminant Method Limit (mg/l) Mercury Manual Cold Vapor Antimony Atomic Absorption—Furnace Technique 0.003 Atomic Absorption—Platform 0.0008 Inductively Coupled Plasma—Mass Spectrometry 0.0004 Nickel Atomic Absorption—Gaseous Hydride 0.001 Asbestos Transmission Electron Microscopy 0.01 million fibers per liter Nitrate Barium Atomic Absorption—Furnace Technique 0.0002 Atomic Absorption—Direct Aspiration 0.1 Holding Time 6 months

28 days 14 days 48 hours 6 months 6 months

Detection

Method Limit (mg/l)

Inductively Coupled Plasma Inductively Coupled Plasma (EPA method 200.7) (mg/l)

Technique Atomic Absorption—Platform Inductively Coupled Plasma Inductively Coupled Plasma— Mass Spectrometry

Technique Inductively Coupled Plasma

Technique Inductively Coupled Plasma Inductively Coupled Plasma (EPA Method 200.7A) All Methods Except Atomic Absorption Atomic Absorption With Direct Aspiration Distillation, Spectrophotometric (screen) Distillation, Automated Spectrophotometric (screen) Distillation, Selective Electrode (screen) Distillation, Amenable, Spectrophotometric (free) All Methods

Technique Automated Cold Vapor Technique

Atomic Absorption — Furnace Technique Atomic Absorption—Platform Inductively Coupled Plasma Inductively Coupled Plasma— Mass Spectrometry Manual Cadmium Reduction Automated Hydrazine Reduction 0.002 0.001

0.0002 0.00002 0.0003 0.0003

0.0001 0.001

0.001 0.007 0.001

0.0002 0.0002

0.02 0.005 0.02

0.02 0.001

0.0002 0.0002

0.001 0.0006 0.005

0.0005 0.01 0.01 Contaminant Method Automated Cadmium Reduction Ion Selective Electrode Ion Chromatography

Nitrite Spectrophotometric Automated Cadmium Reduction Manual Cadmium Reduction Ion Chromatography Selenium Atomic Absorption—Furnace Technique Atomic Absorption—Gaseous Hydride

Thallium Atomic Absorption—Furnace Technique Atomic Absorption—Platform 0.0007 Inductively Coupled Plasma— Mass Spectrometry

1. 2. Detection limits for SOCs are the fol-

lowing:

Contaminant

2,3,7,8-TCDD (Dioxin) 2,4-D 2,4,5-TP (Silvex) Alachlor Aldicarb Aldicarb sulfoxide Aldicarb sulfone Atrazine Benzo(a)pyrene Carbofuran Chlordane Dalapon Dibromochloropropane (DBCP) Di(2-ethylhexyl)adipate Di(2-ethylhexyl)phthalate Dinoseb Diquat Endothall Endrin Ethylene dibromide (EDB) Glyphosate Heptachlor Heptachlor epoxide Hexachlorobenzene Hexachlorocyclopentadiene Lindane Methoxychlor Oxamyl (Vydate) Pentachlorophenol Picloram Polychlorinated biphenyls (PCBs) (as decachlorobiphenyl) Aroclor 1016 Detection Limit (mg/l)

0.05 0.01

0.01 0.05 0.01 0.004

0.002

0.002 (mg/l)

0.001

0.0003

Detection Limit (mg/l) 0.000000005 0.0001 0.0002 0.0002 0.0005 0.0005 0.0008 0.0001 0.00002 0.0009 0.0002 0.001

0.00002 0.0006 0.0006 0.0002 0.0004 0.009 0.00001 0.00001 0.006 0.00004 0.00002 0.0001 0.0001 0.00002 0.0001 0.002 0.00004 0.0001

0.0001 0.00008 Detection Contaminant Limit (mg/l) Aroclor 1221 0.02 Aroclor 1232 0.0005 Aroclor 1242 0.0003 Aroclor 1248 0.0001 Aroclor 1254 0.0001 Aroclor 1260 0.0002 Simazine 0.00007 Toxaphene 0.001

1. 3. The detection limit for VOCs is

0.0005 mg/l.

1. (E) If duplicates of the original sample from each sampling point used in the composite are available, the system may use these duplicates instead of resampling. The duplicate must be analyzed and the results reported to the department within fourteen (14) days of collection.

2. (F) Compositing Samples Prior to Gas Chromatograph (GC) Analysis.

   1. 1. Add five milliliter (5 ml) or equal

larger amounts of each sample (up to five (5) samples are allowed) to a twenty-five milliliter (25 ml) glass syringe. Special precautions must be made to maintain zero headspace in the syringe.

1. 2. The samples must be cooled at four

degrees Centigrade (4°C) during this step to minimize volatilization losses.

1. 3. Mix well and draw out a five milliliter

(5 ml) aliquot for analysis.

1. 4. Follow sample introduction, purging

and desorption steps described in the method.

1. 5. If less than five (5) samples are used

for compositing, a proportionately small syringe may be used.

1. (G) Compositing Samples Prior to GC/Mass Spectrophotometer (MS) Analysis.

   1. 1. Inject five milliliter (5 ml) or equal

larger amounts of each aqueous sample (up to five (5) samples are allowed) into a twentyfive milliliter (25 ml) purging device using the sample introduction technique described in the method.

1. 2. The total volume of the sample in the

purging device must be twenty-five milliliters (25 ml).

1. 3. Purge and desorb as described in the

method.

1. (H) For lead and copper monitoring, composite samples from a maximum of five (5) sampling points per composite sample are allowed with prior approval of the department. The reportable value, as required in 10 CSR 60-7.020, for each of the samples in the composite is the concentration detected multiplied by the number of samples composited. If the concentration in the composite sample is less than the detection limit, the reportable value for each of the samples in the compos- 10 CSR 60-5

ite is the detection limit multiplied by the number of samples composited. If the ninetieth percentile concentration, calculated in accordance with 10 CSR 60-15.010(3)(C), exceeds the lead and copper action level established in 10 CSR 60-15.010(3)(A) and (B), each of the samples from which the composite was derived must be analyzed individually and reported as required in 10 CSR 60- 7.020.

AUTHORITY: section 640.100, RSMo (1994).* Original rule filed May 4, 1979, effective Sept. 14, 1979. Amended: Filed April 14, 1981, effective Oct. 11, 1981. Amended: Filed June 2, 1988, effective Aug. 31, 1988. Rescinded and readopted: Filed Dec. 4, 1990, effective July 8, 1991. Rescinded and readopted: Filed March 31, 1992, effective Dec. 3, 1992. Amended: Filed Aug. 4, 1992, effective May 6, 1993. Amended: Filed May 4, 1993, effective Jan. 13, 1994. Amended: Filed Feb. 1, 1996, effective Oct. 30, 1996. *Original authority 1939, amended 1978, 1981, 1982, 1988, 1992, 1993, 1995.