Wis. Admin. Code Department of Natural Resources NR 809.52

Current through November 25, 2024

Section NR 809.52 - Analytical methods for radionuclides

(1) ANALYTICAL METHODS. Analyses conducted to determine compliance with ss. NR 809.50 and 809.51 shall be made in accordance with approved methods listed in Table N.

Table N

SDWA Approved Methodology for Radiological Measurements Reference (method or page number)

Parameter	Method	EPA¹	EPA²	EPA³	EPA 4	SM⁵	ASTM⁶	USGS⁷	DOE⁸	Others
						SM Online
Naturally Occurring:								R-1120-76	----
Gross alpha¹¹& beta	Evaporation	900.0	p1	00-01	p1	302, 7110 B		R-1120-76	----
						7110 B-00
Gross alpha¹¹	co-precipitation	----		00-02		7110 C	----	----	----
						7110 C-00
Radium 226	Radon emanation, Radiochemical	903.1 903.0	P 16 p13	Ra-04 Ra-03	p19	7500-Ra C 304,305, 7500-Ra B	D 3454-91 D 2460-90 D3454-05 D2460-07	R-1141-76 R-1140-76	Ra-05	N.Y.⁹
						7550-Ra C-01 7500-Ra B-01
Radium 228	Radiochemical	904.0	P 24	Ra-05	p19	304,7500 Ra D	----	R-1142-76	----	N.Y.⁹N.J.¹⁰
						7500-Ra D-01
Uranium¹²	Radiochemical	908.0				7500-UB	D 2907-91	R-1180-76	U-04 U-2
						7500-U B-00
	Fluorometric	908.1				7500-UC (17th Ed)	D 2907-97	R-1180-76 R-1181-76 R-1182-76	U-04
	Alpha spectrometry	----		00-07	p33	7500-UC (18th or 19th Ed)	D 3972-90 D3972-09	----	----
						7500-U C-00
	Laser Phosphorimetry	----				-	D5174-97, 02
	ICP-MS	200.8¹³				3125	D 5673-03 D5673-05, 10
Man-Made:
Radioactive							----
Strontium -89,90	Radiochemical	905.0	p 29	Sr-04	p65	303, 7500-Sr B	----	R1160-76	Sr-01 Sr-02
						7500-Sr B-01
Tritium	Liquid Scintillation	906.0	p 34	H-02	p 87	306, 7500-H B³		D 4107-91 D 4107-08	R 1171-76	----
						7500-3H B-00
Radioactive Cesium -	Radiochemical, Gamma ray spectrophotometry	901.0 901.1	p 4		p 92	7500-Cs B, 7120 (19th Ed.)	D 2459-72 D 3649-91 D3649-06	--- R-1110-76	4.5.2.3
Radioactive Iodine	Radiochemical, Gamma ray spectrophotometry	902.0 901.1	p 6 p 9		p 92	7500-I B 7500-I C 7500-I D 7120 (19th Ed)	D 3649-91 D 4785-88 D3649-06 D4785-08	----	4.5.2.3
						7500-I C-00, 7500-I D-00
Gamma Emitters	Gamma ray spectrometry	901.1 902.0 901.0			p 92	7120 (19th Ed.) 7500-Cs B 7500-I B	D 3649-91 D 4785-88 D3649-0 D4785-08	----	4.5.2.3
						7120-97

1 "Prescribed Procedures for Measurement of Radioactivity in Drinking Water", EPA-600/4-80/032. August, 1980. Available from the EMSL, Office of Research and Development, U.S. EPA, 26 W. Martin Luther King Drive, Cincinnati, Ohio, 45268.

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, 19^th, 20^th, 21^st, or 22^nd, edition, 1971, 1989, 1992, 1995, 1998, 2005, 2012, available at American Public Health Association, 800 I Street NW., Washington, DC. 20001-3710. Methods 302, 303, 304, 305 and 306 are only in the 13th edition. Methods 7110B, 7500-Ra B, 7500-Ra C, 7500-Ra D, 7500-U B, 7500-Cs B, 7500-I B, 7500-I C, 7500-I D, 7500-Sr B, and 7500-³H B are in the 17th, 18th, 19 th 20 th, 21 st, and 22 nd editions. Method 7110 C and 7500-U C Alpha spectrometry is in the 18th, 19^th, 20^th, 21^st, and 22^nd editions. Method 7500-U C Fluorometric Uranium is only in the 17th edition, Method 7120 is only in the 19th and 20th editions. Method 3125 is only in the 20th edition. 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.

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 A 5 in Book 5 of Techniques of Water Resources Investigations of the United States Geological Survey, 1997. 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 Analytical Services, 9 Ewing Street, Trenton, N.J. 08625.

11 Natural uranium and thorium-230 or 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/g of uranium conversion factor shall 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.

(2) DETECTION LIMITS. To determine compliance with s. NR 809.50(1), the detection limit may not exceed the concentrations in Table O.

Table O

Detection Limits for Gross Alpha Particle Activity,

Radium 226, Radium 228, and Uranium

Contaminant	Detection Limit
Gross alpha particle activity	3 pCi/l
Radium 226	1 pCi/l
Radium 228	1 pCi/l
Uranium	Reserve

(3) RESULTS ROUNDING. To judge compliance with the maximum contaminant levels listed in s. NR 809.50, averages of data shall be used and shall be rounded to the same number of significant figures as the maximum contaminant level for the substance in question.

(4) SENSITIVITY LIMITS. For the purpose of monitoring radionuclide concentrations in drinking water, the required sensitivity of the radioanalysis is defined in terms of a detection limit. The detection limit shall be that concentration which can be counted with a precision of plus or minus 100% at the 95% confidence level, 1.96 ó where ó is the standard deviation of the net counting rate of the sample.

(5) DETECTION LIMITS FOR MAN-MADE BETA PARTICLE AND PHOTON EMITTERS . To determine compliance with s. NR 809.51, the detection limits may not exceed the concentrations listed in Table P.

Table P

Detection Limits for Man-made Beta Particle

and Photon Emitters

Radionuclide	Detection Limit
Tritium	1,000 pCi/1
Strontium-89	10 pCi/1
Strontium-90	2 pCi/1
Iodine-131	1 pCi/1
Cesium-134	10 pCi/1
Gross beta	4 pCi/1
Other radionuclides	1/10 of the applicable limit

Note: Sections NR 809.50 to 809.52 are identical to the radioactivity standards of the department of health services in ch. DHS 157, Wis. Adm. Code, and to the National Interim Primary Drinking Water Regulations, 40 CFR part 141. These sections are adopted pursuant to s. 254.34, Stats.

(6) SAMPLE COLLECTION METHODS. Sample collection for radionuclide contaminants under s. NR 809.50 shall be conducted using the sample preservation, containers and maximum holding time procedures specified in Table Q. If a composite sample is prepared, a holding time cannot exceed 12 months. In all cases, samples should be analyzed as soon after collection as possible.

Table Q

Radionuclide sample preservation, containers and maximum holding time

Parameter	Preservative¹	Container²	Holding Time
Gross Alpha ...........	Conc. HCl or HNO₃ to pH <2 ......	P or G .........	6 mo
Gross beta ..............	Conc. HCl or HNO₃ to pH <2 ......	P or G .........	6 mo
Strontium-89 ...........	Conc. HCl or HNO₃ to pH <2 ......	P or G .........	6 mo
Strontium-90 ...........	Conc. HCl or HNO₃ to pH <2 ......	P or G .........	6 mo
Radium-226 ...........	Conc. HCl or HNO₃ to pH <2 ......	P or G .........	6 mo
Radium-228 ...........	Conc. HCl or HNO₃ to pH <2 ......	P or G .........	6 mo
Cesium-134 ...........	Conc. HCl to pH <2 .............	P or G .........	6 mo
Iodine-131 ............	None .........................	P or G .........	8 days
Tritium ................	None ..........................	G ............	6 mo
Uranium ..............	Conc. HCl or HNO3 to pH <2 ......	P or G .........	6 mo
Photon emitters .........	Conc. HCl or HNO3 to pH <2 ......	P or G .........	6 mo

1 It is recommended that the preservative be added to the sample at the time of collection unless suspended solids activity is to be measured. If the sample has to be shipped to a laboratory or storage area unpreserved, acidification of the sample (in its original container) may be delayed for a period not to exceed 5 days. A minimum of 16 hours shall elapse between acidification and analysis.

2 P = Plastic, hard or soft; G = Glass, hard or soft.

Wis. Admin. Code Department of Natural Resources NR 809.52

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

Amended by, CR 15-049: am. (1) Table N Register March 2016 No. 723, eff.4/1/2016