Sec. NR 809.203 - Analytical requirements for synthetic organic contaminants

§ 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

        

Syngenta4 AG-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 ?g/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.

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

10Standard 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 PTFE1 Lined 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 PTFE1 Lined 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 PTFE1 Lined 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 PTFE1 Lined 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.

(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)

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