Wis. Admin. Code Department of Natural Resources NR 809.203

Current through October 28, 2024

Section NR 809.203 - Analytical requirements for synthetic organic contaminants

(1) DETECTION LIMITS. Detection as used in this section shall be defined as greater than or equal to the following concentrations for each contaminant:

Contaminant	Detection Limit (mg/L)
1. Alachlor	0.0002
2. Aldicarb	0.0005
3. Aldicarb sulfoxide	0.0005
4. Aldicarb sulfone	0.0008
5. Atrazine	0.0001
6. Benzo[a]pyrene	0.00002
7. Carbofuran	0.0009
8. Chlordane	0.0002
9. 2,4-D	0.0001
10. Dalapon	0.001
11. Dibromochloropropane	0.00002
12. Di(2-ethylhexyl)adipate	0.0006
13. Di(2-ethylhexyl)phthalate	0.0006
14. Dinoseb	0.0002
15. Diquat	0.0004
16. Endothall	0.009
17. Endrin	0.00001
18. Ethylene dibromide	0.00001
19. Glyphosate	0.006
20. Heptachlor	0.00004
21. Heptachlor epoxide	0.00002
22. Hexachlorobenzene	0.0001
23. Hexachlorocyclopentadiene	0.0001
24. Lindane	0.00002
25. Methoxychlor	0.0001
26. Oxamyl	0.002
27. Picloram	0.0001
28. Polychlorinated biphenyls (PCBs as decchlorobiphenyls)	0.0001
29. Pentachlorophenol	0.00004
30. Simazine	0.00007
31. Toxaphene	0.001
32. 2,3,7,8-TCDD (Dioxin)	0.000000005
33. 2,4,5-TP (Silvex)	0.0002

(2) ANALYTICAL METHODS. Analysis for the synthetic organic contaminants listed in s. NR 809.20 shall be conducted using the methods prescribed in Table CM.

Table CM

SDWA Approved Methodology for Synthetic Organic Contaminants

Contaminant	EPA Methods¹	SM⁹	SM Online¹⁰	ASTM	Other
Regulated Parameters:
Synthetic Organic Chemicals
2,3,7,8-TCDD (dioxin)	1613
2,4-D ² (as acids, salts and esters)	515.2, 555, 515.1, 515.3, 515.4			D5317-93, 98 (Reapproved 2003)
2,4,5-TP ² (Silvex)	515.2, 555, 515.1, 515.3, 515.4	6640 B,	6640 B-01, B-06¹¹	D5317-93, 98 (Reapproved 2003)
Alachlor	507, 525.2, 525.3² 508.1, 505⁸, 551.1
Atrazine ³	507, 525.2, 525.3 508.1, 505⁸, 551.1, 536				Syngenta⁴AG-625
Benzo(a)pyrene	525.2, 525.3, 550, 550.1
Carbofuran	531.1, 531.2	6610⁵ 6610 B	6610 B-04
Chlordane	508, 525.2, 525.3, 508.1, 505
Dalapon	552.1 515.1, 552.2, 515.3, 515.4, 552.3, 557	6640 B	6640 B-01, 06
Di(2-ethylhexyl)adipate	506, 525.2, 525.3
Di(2-ethylhexyl)phthalate	506, 525.2, 525.3
Dibromochloropropane (DBCP)	504.1, 551.1, 524.3⁹
Dinoseb	515.2, 555, 515.1, 515.3, 515.4	6640 B	6640 B-01, 06
Diquat	549.2
Endothall	548.1
Endrin	508, 525.2, 525.3, 508.1, 505, 551.1
Ethylene dibromide (EDB)	504.1, 551.1, 524.3
Glyphosate	547	6651⁶ 6651 B	6651 B-01, B-06
Heptachlor	508, 525.2, 525.3, 508.1, 505, 551.1
Heptachlor Epoxide	508, 525.2, 525.3, 508.1, 505, 551.1
Hexachlorobenzene	508, 525.2, 525.3, 508.1, 505, 551.1
Hexachlorocyclopentadiene	508, 525.2, 525.3, 508.1, 505, 551.1
Lindane	508, 525.2, 525.3, 508.1, 505, 551.1
Methoxychlor	508, 525.2, 525.3, 508.1, 505, 551.1
Oxamyl	531.1, 531.2	6610⁵ 6610 B	6610 B-04
PCBs (as decachlorobiphenyl)	508A⁷
(as Aroclors)	508.1, 508, 525.2, 525.3, 505
Pentachlorophenol	515.2, 525.2, 525.3, 555, 515.1, 515.3, 515.4			D5317-93, 98 (Reapproved 2003)
Picloram ²	515.2, 555, 515.1, 515.3, 515.4	6640 B	6640 B-01	D5317-93, 98 s (Reapproved 2003)
Simazine	507, 525.2, 525.3, 523, 536, 508.1, 505⁸, 551.1
Toxaphene	508, 508.1, 525.2, 525.3, 505
Unregulated Parameters:
Aldicarb	531.1, 531.2	6610⁵ 6610 B	6610 B-04
Aldicarb sulfone	531.1, 531.2	6610⁵ 6610 B	6610 B-04
Aldicarb Sulfoxide	531.1, 531.2	6610⁵ 6610 B	6610 B-04
Aldrin	505, 508, 525.2, 525.3, 508.1
Butachlor	507, 525.2, 525.3
Carbaryl	531.1, 531.2	6610⁵ 6610 B	6610 B-04
Dicamba	515.1, 555, 515.2, 515.3, 515.4	6640 B	6640 B-01, B-06
Dieldrin	505, 508, 525.2, 525.3, 508.1
3-Hydroxcarbofuran	531.1, 531.2	6610⁵ 6610 B	6610 B-04
Methomyl	531.1, 531.2	6610⁵ 6610 B	6610 B-04
Metolachlor	507, 525.2, 525.3, 508.1
Metribuzin	507, 525.2, 525.3, 508.1
Propachlor	507, 525.2, 525.3, 508.1

¹ EPA methods are available at http://epa.gov/safewater/methods/analyticalmethods_ogwdw.htm.

² 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).

³ 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.

⁴ 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 generated by Method AG-625 that is greater than one-half the maximum contaminant level (MCL) (in other words, greater than 0.0015 mg/L or 1.5 ì/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.

⁵ 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, or with the 19th edition of Standard Methods for the Examination of Water and Wastewater, 1995, APHA; either publication may be used. This incorporation by reference was approved by the Director of the Federal Register in accordance with 5 USC 552(a) and 1 CFR Part 51. Copies may be obtained from the American Public Health Association, 1015 Fifteenth Street, N.W., Washington, D.C., 2005. Other required analytical test procedures germane to conducting these analyses are contained in Technical Notes on Drinking Water Methods, EPA/600/R-94-173, October 1994, NTIS PB95-104766.

⁶ Method 6651 shall be followed in accordance with the "Standard Methods for the Examination of Water and Wastewater", 18th Edition, 1992, and 19th edition, 1995, American Public Health Association. This incorporation by reference was approved by the Director of the Federal Register in accordance with 5 U.S.C. 552(a) and 1 CFR Part 51. Copies may be obtained from the American Public Health Association, 1015 Fifteenth Street, N.W., Washington, D.C., 20005.

⁷ Method 505 or 508 can be used as a screen for PCBs. Method 508A shall be used to quantitate PCBs as decachlorobiphenyl if detected in Method 505 or 508. PCBs are qualitatively identified as Aroclors and measured for compliance purposes as decachlorobiphenyl.

⁸ A nitrogen-phosphorus detector should be substituted for the electron capture detector in Method 505 (or a different approved method should be used) to determine alachlor, atrazine and simizine, if lower detection limits are required.

⁹Standard Methods for the Examination of Water and Wastewater, 18^th edition (1992), 19^th edition (1995), 20^th edition (1998), 21^sd edition (2005), 22^nd edition (2012). Available from American Public Health Association, 800 I Street, NW., Washington, DC, 20001-3710.

¹⁰ 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) PCB ANALYSIS. Analysis for PCBs shall be conducted as follows:

(a) Each water supplier that monitors for PCBs shall have each sample analyzed by a laboratory certified under ch. NR 149 using Method 505, 508, 508.1 or 525.2 as specified in Table CM and must achieve the required detection limits in this subsection.

(b) If one or more of 7 PCB Aroclors are detected as designated in this paragraph in any sample analyzed using Methods 505 and 508, the sample shall be reanalyzed using Method 508A to quantitate PCBs as decachlorobiphenyl.

(c) Compliance with the PCB MCL shall be determined based upon the quantitative results of analyses using Method 508A.

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

(4) SAMPLE COLLECTION. Samples shall be collected using containers and preservatives, and meeting the holding times specified in Table D. When an approved method that is not included in Table D is used to analyze samples, samples shall be collected using containers and preservatives, and meeting the holding times specified in the approved method. In all cases, samples should be analyzed as soon after collection as possible.

Table D Sample Preservation, Holding Times, and Sampling Containers for Organic Parameters
Method	Preservative²	Sample Holding Time	Extract Holding Time and Storage Conditions	Suggested Sample Size	Type of Container
502.2²	Sodium Thiosulfate or Ascorbic Acid, 4°C, HCl pH<2	14 days	NA	40 - 120 mL	Glass with PTFE¹ Lined Septum
504.1	Sodium Thiosulfate, Cool, 4°C	14 days	4°C, 24 hours	40 mL	Glass with PTFE¹ Lined Septum
505	Sodium Thiosulfate, Cool, 4°C	14 days (7 days for Heptachlor)	4°C, 24 hours	40 mL	Glass with PTFE¹ Lined Septum
506	Sodium Thiosulfate, Cool, 4°C, Dark	14 days	4°C, Dark 14 days	1 L	Amber Glass with PTFE¹ Lined Septum
507	Sodium Thiosulfate, Cool, 4°C, Dark	14 days (See method for exceptions.)	4°C, Dark 14 days	I L	Amber Glass with PTFE¹ Lined Cap
508	Sodium Thiosulfate, Cool, 4°C, Dark	7 days (See method for exceptions.)	4°C, Dark 14 days	I L	Glass with PTFE¹Lined Cap
508A	Cool, 4°C	14 days	30 days	I L	Amber Glass with PTFE¹ Lined Cap
508.1	Sodium Sulfite, HCl pH<2, Cool, 4°C	14 days (See method for exceptions.)	30 days	I L	Glass with PTFE Lined Cap
515.1	Sodium Thiosulfate, Cool, 4°C, Dark	14 days	4°C, Dark 28 days	I L	Amber Glass with PTFE¹ Lined Cap
515.2	Sodium Thiosulfate or Sodium Sulfite, HCl pH<2 Cool, 4°C, Dark	14 Days	<=4°C, Dark 14 Days	I L	Amber Glass with PTFE¹ Lined Cap
515.3	Sodium Thiosulfate, Cool, 4°C, Dark	14 days	<=4°C, Dark 14 Days	50 mL	Amber Glass with PTFE¹ Lined Cap
515.4	Sodium Sulfite, Dark, Cool <=10°C for First 48 hrs, <=6°C thereafter	14 days	<=0°C 21 days	40 mL	Amber Glass with PTFE¹ Lined Cap
524.2²	Ascorbic Acid or Sodium Thiosulfate, HCl pH<2, Cool 4°C	14 days	NA	40 - 120 mL	Glass with PTFE¹Lined Septum
524.3²	Maleic and Ascorbic Acids pH<2, <=10°C for first 48 hrs., <=6 thereafter If only analyzing TTHM: Sodium Thiosulfate pH<2, <=10°C for first 48 hrs., <=6 thereafter	14 days	NA	40 - 120 mL	Amber Glass with PTFE¹ Lined Septum
525.2	Sodium Sulfite, Dark, Cool, 4°C, HCl pH<2	14 days (See method for exceptions)	<=4°C 30 days	1 L	Amber Glass with PTFE¹ Lined Cap
531.1, 6610	Sodium Thiosulfate, Monochloroacetic Acid pH<3, Cool, 4ºC	Cool 4°C from collection until storage at laboratory; <=10°C at the laboratory; 28 days	NA	60 mL	Glass with PTFE¹ Lined Septum
531.2	Sodium Thiosulfate, Potassium Dihydrogen Citrate Buffer pH<4, Dark <=10°C for first 48 hrs., <=6ºC thereafter	28 days	NA	40 mL	Glass with PTFE¹ Lined Septum
547	Sodium Thiosulfate, Cool, 4°C	14 days; 18 mos. Frozen	NA	60 mL	Glass with PTFE¹ Lined Septum
548.1	Sodium Thiosulfate, HCl pH 1.5 -2 if High Biological Activity, Cool, 4°C, Dark	7 days	<=4°C 14 days	>= 250 mL	Amber Glass with PTFE¹ Lined Septum
549.2	Sodium Thiosulfate, H₂SO₄ pH<2, if Biologically Active, Cool 4°C, Dark	7 days	21 days	>= 250 mL	High Density Amber Plastic or Silanized Amber Glass
550	Sodium Thiosulfate, Cool, 4°C, HCl pH<2	7 days	4°C, Dark 30 days	1 L	Amber Glass with PTFE¹ Lined Septum
550.1	Sodium Thiosulfate, Cool, 4°C, HCl pH<2	7 days	4°C, Dark 40 days	1 L	Amber Glass with PTFE¹ Lined Septum
551.1	Sodium Sulfite, Ammonium Chloride, pH 4.5-5.0 with Phosphate Buffer, Cool, 4°C	14 days	14 days <-10°C	>= 40 mL	Glass with PTFE¹Lined Septum
552.1	Ammonium Chloride, Cool, 4°C, Dark	28 days	<=4°C, Dark 48 hrs.	250 mL	Amber Glass with PTFE¹ Lined Cap
552.2	Ammonium Chloride, Cool, 4°C, Dark	14 days	<=4°C, Dark, 7 days <=-10°C, 14 days	50 mL	Amber Glass with PTFE¹ Lined Cap
555	Sodium Sulfite,HCl pH <=2,Dark, Cool, 4°C	14 days	NA	>= 100 mL	Glass wit PTFE¹Lined Cap
1613	Sodium Thiosulfate,Cool, 0 - 4°C, Dark	1 year	40 days recommended	1 L	Amber Glass with PTFE¹ Lined Cap

¹ Polytetrafluoroethylene. Teflon is a brand name of a PTFE product.

² Chlorinated samples need to be dechlorinated at the time of collection. Samplers should follow the dechlorinating procedures contained in the approved methods.

(5) LABORATORY CERTIFICATION. Analyses under this section shall only be conducted by laboratories that have received certification under ch. NR 149 or have been approved by EPA.

Wis. Admin. Code Department of Natural Resources NR 809.203

CR 09-073: cr. Register November 2010 No. 659, eff. 12-1-10.

Amended by, CR 15-049: am. (1), (2), renum. (2) Table C to Table CM and am, am. (3) (a), (4) (intro.), r. and recr. (4) Table D Register March 2016 No. 723, eff.4/1/2016

Amended by, CR 21-088: am. (1) Table, (2) Table CM, (4) Table D Register July 2022 No. 799, eff. 8-1-22; correction in Table CM, D made under s. 35.17, Stats., Register July 2022 No. 799, eff. 8/1/2022.