Code of Federal Regulations Title 40. Protection of Environment § 40.136.3, Table IB Identification of test procedures

Current as of January 02, 2025 | Updated by Findlaw Staff

Table IB—List of Approved Inorganic Test Procedures
Parameter	Methodology ⁵⁸	EPA ⁵²	Standard methods ⁸⁴	ASTM	USGS/AOAC/other
1. Acidity, as CaCO₃, mg/L	Electrometric endpoint or phenolphthalein endpoint		2310 B-2011	D1067-16	I-1020-85.²
2. Alkalinity, as CaCO₃, mg/L	Electrometric or Colorimetric titration to pH 4.5, Manual		2320 B-2011	D1067-16	973.43,³ I-1030-85.²
	Automatic	310.2 (Rev. 1974) ¹		․	I-2030-85.²
3. Aluminum—Total,⁴ mg/L	Digestion,⁴ followed by any of the following:		․
	AA direct aspiration ³⁶		3111 D-2011 or 3111 E-2011		I-3051-85.²
	AA furnace		3113 B-2010.
	STGFAA	200.9, Rev. 2.2 (1994)/		․
	ICP/AES ³⁶	200.5, Rev 4.2 (2003); ⁶⁸ 200.7, Rev. 4.4 (1994)	3120 B-2011	D1976-12	I-4471-97.⁵⁰
	ICP/MS	200.8, Rev. 5.4 (1994)	3125 B-2011	D5673-16	993.14,³ I-4472-97.⁸¹
	Direct Current Plasma (DCP) ³⁶		․	D4190-15	See footnote.³⁴
	Colorimetric (Eriochrome cyanine R)		3500-Al B-2011.
4. Ammonia (as N), mg/L	Manual distillation ⁶ or gas diffusion (pH > 11), followed by any of the following:	350.1, Rev. 2.0 (1993)	4500-NH₃ B-2011		973.49.³
	Nesslerization		․	D1426-15 (A)	973.49,³ I-3520-85.²
	Titration		4500-NH₃ C-2011.
	Electrode		4500-NH₃ D-2011 or E-2011	D1426-15 (B).
	Manual phenate, salicylate, or other substituted phenols in Berthelot reaction-based methods		4500-NH₃ F-2011		See footnote.⁶⁰
	Automated phenate, salicylate, or other substituted phenols in Berthelot reaction-based methods	350.1,³⁰ Rev. 2.0 (1993)	4500-NH₃ G-2011 4500-NH₃ H-2011		I-4523-85,² I-2522-90.⁸⁰
	Automated electrode		․		See footnote.⁷
	Ion Chromatography		․	D6919-17.
	Automated gas diffusion, followed by conductivity cell analysis		․		Timberline Ammonia-001.⁷⁴
	Automated gas diffusion followed by fluorescence detector analysis		․		FIAlab100.⁸²
5. Antimony—Total,⁴ mg/L	Digestion,⁴ followed by any of the following:		․
	AA direct aspiration ³⁶		3111 B-2011.
	AA furnace		3113 B-2010.
	STGFAA	200.9, Rev. 2.2 (1994).		․
	ICP/AES ³⁶	200.5, Rev 4.2 (2003); ⁶⁸ 200.7, Rev. 4.4 (1994)	3120 B-2011	D1976-12.
	ICP/MS	200.8, Rev. 5.4 (1994)	3125 B-2011	D5673-16	993.14,³ I-4472-97.⁸¹
6. Arsenic-Total,⁴ mg/L	Digestion,⁴ followed by any of the following:	206.5 (Issued 1978) ¹.		․
	AA gaseous hydride		3114 B-2011 or 3114 C-2011	D2972-15 (B)	I-3062-85.²
	AA furnace		3113 B-2010	D2972-15 (C)	I-4063-98.⁴⁹
	STGFAA	200.9, Rev. 2.2 (1994).		․
	ICP/AES ³⁶	200.5, Rev 4.2 (2003); ⁶⁸ 200.7, Rev. 4.4 (1994)	3120 B-2011	D1976-12.
	ICP/MS	200.8, Rev. 5.4 (1994)	3125 B-2011	D5673-16	993.14,³ I-4020-05.⁷⁰
	Colorimetric (SDDC)		3500-As B-2011	D2972-15 (A)	I-3060-85.²
7. Barium-Total,⁴ mg/L	Digestion,⁴ followed by any of the following:		․
	AA direct aspiration ³⁶		3111 D-2011		I-3084-85.²
	AA furnace		3113 B-2010	D4382-18.
	ICP/AES ³⁶	200.5, Rev 4.2 (2003); ⁶⁸ 200.7, Rev. 4.4 (1994)	3120 B-2011		I-4471-97.⁵⁰
	ICP/MS	200.8, Rev. 5.4 (1994)	3125 B-2011	D5673-16	993.14,³ I-4472-97.⁸¹
	DCP ³⁶		․		See footnote.³⁴
8. Beryllium—Total,⁴ mg/L	Digestion,⁴ followed by any of the following:		․
	AA direct aspiration		3111 D-2011 or 3111 E-2011	D3645-15 (A)	I-3095-85.²
	AA furnace		3113 B-2010	D3645-15 (B).
	STGFAA	200.9, Rev. 2.2 (1994).		․
	ICP/AES	200.5, Rev 4.2 (2003); ⁶⁸ 200.7, Rev. 4.4 (1994)	3120 B-2011	D1976-12	I-4471-97.⁵⁰
	ICP/MS	200.8, Rev. 5.4 (1994)	3125 B-2011	D5673-16	993.14,³ I-4472-97.⁸¹
	DCP		․	D4190-15	See footnote.³⁴
	Colorimetric (aluminon)		See footnote.⁶¹.
9. Biochemical oxygen demand (BOD₅), mg/L	Dissolved Oxygen Depletion		5210 B-2016 ⁸⁵		973.44,³ p. 17,⁹ I-1578-78,⁸ See footnote.¹⁰^,⁶³
10. Boron—Total,³⁷ mg/L	Colorimetric (curcumin)		4500-B B-2011		I-3112-85.²
	ICP/AES	200.5, Rev 4.2 (2003); ⁶⁸ 200.7, Rev. 4.4 (1994)	3120 B-2011	D1976-12	I-4471-97.⁵⁰
	ICP/MS	200.8, Rev. 5.4 (1994)	3125 B-2011	D5673-16	993.14.³
	DCP		․	D4190-15	S7ee footnote.³⁴
11. Bromide, mg/L	Electrode		․	D1246-16	I-1125-85.²
	Ion Chromatography	300.0, Rev 2.1 (1993) and 300.1, Rev 1.0 (1997)	4110 B-2011, C-2011, D-2011	D4327-17	993.30,³ I-2057-85.⁷⁹
	CIE/UV		4140 B-2011	D6508-15	D6508, Rev. 2.⁵⁴
12. Cadmium—Total,⁴ mg/L	Digestion,⁴ followed by any of the following:		․
	AA direct aspiration ³⁶		3111 B-2011 or 3111 C-2011	D3557-17 (A or B)	974.27,³ p. 37,⁹ I-3135-85 ² or I-3136-85.²
	AA furnace		3113 B-2010	D3557-17 (D)	I-4138-89.⁵¹
	STGFAA	200.9, Rev. 2.2 (1994).		․
	ICP/AES ³⁶	200.5, Rev 4.2 (2003); ⁶⁸ 200.7, Rev. 4.4 (1994)	3120 B-2011	D1976-12	I-1472-85 ² or I-4471-97.⁵⁰
	ICP/MS	200.8, Rev. 5.4 (1994)	3125 B-2011	D5673-16	993.14,³ I-4472-97.⁸¹
	DCP ³⁶		․	D4190-15	See footnote.³⁴
	Voltammetry ¹¹		․	D3557-17 (C).
	Colorimetric (Dithizone)		3500-Cd-D-1990.
13. Calcium—Total,⁴ mg/L	Digestion,⁴ followed by any of the following:		․
	AA direct aspiration		3111 B-2011	D511-14 (B)	I-3152-85.²
	ICP/AES	200.5, Rev 4.2 (2003); ⁶⁸ 200.7, Rev. 4.4 (1994)	3120 B-2011		I-4471-97.⁵⁰
	ICP/MS	200.8, Rev. 5.4 (1994)	3125 B-2011	D5673-16	993.14.³
	DCP		․		See footnote.³⁴
	Titrimetric (EDTA)		3500-Ca B-2011	D511-14 (A).
	Ion Chromatography		․	D6919-17.
14. Carbonaceous biochemical oxygen demand (CBOD₅), mg/L ¹²	Dissolved Oxygen Depletion with nitrification inhibitor		5210 B-2016 ⁸⁵		See footnote.³⁵⁶³
15. Chemical oxygen demand (COD), mg/L	Titrimetric	410.3 (Rev. 1978) ¹	5220 B-2011 or C-2011	D1252-06(12) (A)	973.46,³ p. 17,⁹ I-3560-85.²
	Spectrophotometric, manual or automatic	410.4, Rev. 2.0 (1993)	5220 D-2011	D1252-06(12) (B)	See footnotes.¹³¹⁴⁸³, I-3561-85.²
16. Chloride, mg/L	Titrimetric: (silver nitrate)		4500-Cl-B-2011	D512-12 (B)	I-1183-85.²
	(Mercuric nitrate)		4500-Cl-C-2011	D512-12 (A)	973.51,³ I-1184-85.²
	Colorimetric: manual		․		I-1187-85.²
	Automated (ferricyanide)		4500-Cl-E-2011		I-2187-85.²
	Potentiometric Titration		4500-Cl-D-2011.
	Ion Selective Electrode		․	D512-12 (C).
	Ion Chromatography	300.0, Rev 2.1 (1993) and 300.1, Rev 1.0 (1997)	4110 B-2011 or 4110 C-2011	D4327-17	993.30,³ I-2057-90.⁵¹
	CIE/UV		4140 B-2011	D6508-15	D6508, Rev. 2.⁵⁴
17. Chlorine-Total residual, mg/L	Amperometric direct		4500-Cl D-2011	D1253-14.
	Amperometric direct (low level)		4500-Cl E-2011.
	Iodometric direct		4500-Cl B-2011.
	Back titration ether end-point ¹⁵		4500-Cl C-2011.
	DPD-FAS		4500-Cl F-2011.
	Spectrophotometric, DPD		4500-Cl G-2011.
	Electrode		․		See footnote.¹⁶
17A. Chlorine-Free Available, mg/L	Amperometric direct		4500-Cl D-2011	D1253-14.
	Amperometric direct (low level)		4500-Cl E-2011.
	DPD-FAS		4500-Cl F-2011.
	Spectrophotometric, DPD		4500-Cl G-2011.
18. Chromium VI dissolved, mg/L	0.45-micron filtration followed by any of the following:		․
	AA chelation-extraction		3111 C-2011		I-1232-85.²
	Ion Chromatography	218.6, Rev. 3.3 (1994)	3500-Cr C-2011	D5257-17	993.23.³
	Colorimetric (diphenyl-carbazide)		3500-Cr B-2011	D1687-17 (A)	I-1230-85.²
19. Chromium—Total,⁴ mg/L	Digestion,⁴ followed by any of the following:		․
	AA direct aspiration ³⁶		3111 B-2011	D1687-17 (B)	974.27,³ I-3236-85.²
	AA chelation-extraction		3111 C-2011.
	AA furnace		3113 B-2010	D1687-17 (C)	I-3233-93.⁴⁶
	STGFAA	200.9, Rev. 2.2 (1994).		․
	ICP/AES ³⁶	200.5, Rev 4.2 (2003),⁶⁸ 200.7, Rev. 4.4 (1994)	3120 B-2011	D1976-12.
	ICP/MS	200.8, Rev. 5.4 (1994)	3125 B-2011	D5673-16	993.14,³ I-4020-05 ⁷⁰ I-4472-97.⁸¹
	DCP ³⁶		․	D4190-15	See footnote.³⁴
	Colorimetric (diphenyl-carbazide)		3500-Cr B-2011.
20. Cobalt—Total,⁴ mg/L	Digestion,⁴ followed by any of the following:		․
	AA direct aspiration		3111 B-2011 or 3111 C-2011	D3558-15 (A or B)	p. 37,⁹ I-3239-85.²
	AA furnace		3113 B-2010	D3558-15 (C)	I-4243-89.⁵¹
	STGFAA	200.9, Rev. 2.2 (1994).		․
	ICP/AES	200.7, Rev. 4.4 (1994)	3120 B-2011	D1976-12	I-4471-97.⁵⁰
	ICP/MS	200.8, Rev. 5.4 (1994)	3125 B-2011	D5673-16	993.14,³ I-4020-05 ⁷⁰ I-4472-97.⁸¹
	DCP		․	D4190-15	See footnote.³⁴
21. Color, platinum cobalt units or dominant wavelength, hue, luminance purity	Colorimetric (ADMI)		2120 F-2011 ⁷⁸.
	Platinum cobalt visual comparison		2120 B-2011		I-1250-85.²
	Spectrophotometric		․		See footnote ¹⁸
22. Copper—Total,⁴ mg/L	Digestion,⁴ followed by any of the following:		․
	AA direct aspiration ³⁶		3111 B-2011 or 3111 C-2011	D1688-17 (A or B)	974.27,³ p. 37,⁹ I-3270-85 ² or I-3271-85.²
	AA furnace		3113 B-2010	D1688-17 (C)	I-4274-89.⁵¹
	STGFAA	200.9, Rev. 2.2 (1994).		․
	ICP/AES ³⁶	200.5, Rev 4.2 (2003); ⁶⁸ 200.7, Rev. 4.4 (1994)	3120 B-2011	D1976-12	I-4471-97.⁵⁰
	ICP/MS	200.8, Rev. 5.4 (1994)	3125 B-2011	D5673-16	993.14,³ I-4020-05,⁷⁰, I-4472-97.⁸¹
	DCP ³⁶		․	D4190-15	See footnote.³⁴
	Colorimetric (Neocuproine)		3500-Cu B-2011.
	Colorimetric (Bathocuproine)		3500-Cu C-2011		See footnote.¹⁹
23. Cyanide—Total, mg/L	Automated UV digestion/distillation and Colorimetry		․		Kelada-01.⁵⁵
	Segmented Flow Injection, In-Line Ultraviolet Digestion, followed by gas diffusion amperometry		․	D7511-12(17).
	Manual distillation with MgCl₂, followed by any of the following:	335.4, Rev. 1.0 (1993) ⁵⁷	4500-CN-B-2016 and C-2016	D2036-09(15)(A), D7284-13(17)	10-204-00-1-X.⁵⁶
	Flow Injection, gas diffusion amperometry		․	D2036-09(15)(A) D7284-13(17).
	Titrimetric		4500-CN-D-2016	D2036-09(15)(A)	p. 22.⁹
	Spectrophotometric, manual		4500-CN-E-2016	D2036-09(15)(A)	I-3300-85.²
	Semi-Automated ²⁰	335.4, Rev. 1.0 (1993) ⁵⁷	4500-CN-N-2016		10-204-00-1-X,⁵⁶ I-4302-85.²
	Ion Chromatography		․	D2036-09(15)(A).
	Ion Selective Electrode		4500-CN-F-2016	D2036-09(15)(A).
24. Cyanide-Available, mg/L	Cyanide Amenable to Chlorination (CATC); Manual distillation with MgCl₂, followed by Titrimetric or Spectrophotometric		4500-CN-G-2016	D2036-09(15)(B).
	Flow injection and ligand exchange, followed by gas diffusion amperometry ⁵⁹		․	D6888-16	OIA-1677-09.⁴⁴
	Automated Distillation and Colorimetry (no UV digestion)		․		Kelada-01.⁵⁵
24.A Cyanide-Free, mg/L	Flow Injection, followed by gas diffusion amperometry		․	D7237-15 (A)	OIA-1677-09.⁴⁴
	Manual micro-diffusion and colorimetry		․	D4282-15.
25. Fluoride—Total, mg/L	Manual distillation,⁶ followed by any of the following:		4500-F-B-2011	D1179-16 (A).
	Electrode, manual		4500-F-C-2011	D1179-16 (B).
	Electrode, automated		․		I-4327-85.²
	Colorimetric, (SPADNS)		4500-F-D-2011.
	Automated complexone		4500-F-E-2011.
	Ion Chromatography	300.0, Rev 2.1 (1993) and 300.1, Rev 1.0 (1997)	4110 B-2011 or C-2011	D4327-17	993.30.³
	CIE/UV		4140 B-2011	D6508-15	D6508, Rev. 2.⁵⁴
26. Gold—Total,⁴ mg/L	Digestion,⁴ followed by any of the following:		․
	AA direct aspiration		3111 B-2011.
	AA furnace	231.2 (Issued 1978) ¹	3113 B-2010.
	ICP/MS	200.8, Rev. 5.4 (1994)	3125 B-2011	D5673-16	993.14.³
	DCP		․		See footnote.³⁴
27. Hardness—Total, as CaCO₃, mg/L	Automated colorimetric	130.1 (Issued 1971) ¹.		․
	Titrimetric (EDTA)		2340 C-2011	D1126-17	973.52B ³, I-1338-85.²
	Ca plus Mg as their carbonates, by any approved method for Ca and Mg (See Parameters 13 and 33), provided that the sum of the lowest point of quantitation for Ca and Mg is below the NPDES permit requirement for Hardness		2340 B-2011.
28. Hydrogen ion (pH), pH units	Electrometric measurement		4500-H ⁺ B-2011	D1293-99 (A or B)	973.41,³ I-1586-85.²
	Automated electrode	150.2 (Dec. 1982) ¹		․	See footnote,²¹ I-2587-85.²
29. Iridium—Total,⁴ mg/L	Digestion,⁴ followed by any of the following:		․
	AA direct aspiration		3111 B-2011.
	AA furnace	235.2 (Issued 1978) ¹.		․
	ICP/MS		3125 B-2011.
30. Iron—Total,⁴ mg/L	Digestion,⁴ followed by any of the following:		․
	AA direct aspiration ³⁶		3111 B-2011 o 3111 C-2011	D1068-15 (A)	974.27,³ I-3381-85.²
	AA furnace		3113 B-2010	D1068-15 (B).
	STGFAA	200.9, Rev. 2.2 (1994)		․
	ICP/AES ³⁶	200.5, Rev. 4.2 (2003); ⁶⁸ 200.7, Rev. 4.4 (1994)	3120 B-2011	D1976-12	I-4471-97.⁵⁰
	ICP/MS	200.8, Rev. 5.4 (1994)	3125 B-2011	D5673-16	993.14.³
	DCP ³⁶		․	D4190-15	See footnote.³⁴
	Colorimetric (Phenanthroline)		3500-Fe B-2011	D1068-15 (C)	See footnote.²²
31. Kjeldahl Nitrogen ⁵—Total, (as N), mg/L	Manual digestion ²⁰ and distillation or gas diffusion, followed by any of the following:		4500-N_org B-2011 or C-2011 and 4500-NH₃ B-2011	D3590-17 (A)	I-4515-91.⁴⁵
	Titration		4500-NH₃ C-2011		973.48.³
	Nesslerization		․	D1426-15 (A).
	Electrode		4500-NH₃ D-2011 or E-2011	D1426-15 (B).
	Semi-automated phenate	350.1, Rev. 2.0 (1993)	4500-NH₃ G-2011 4500-NH₃ H-2011
	Manual phenate, salicylate, or other substituted phenols in Berthelot reaction based methods		4500-NH₃ F-2011		See footnote.⁶⁰
	Automated gas diffusion, followed by conductivity cell analysis		․		Timberline Ammonia-001.⁷⁴
	Automated gas diffusion followed by fluorescence detector analysis		․		FIAlab 100.⁸²
	(04)Automated Methods for TKN that do not require manual distillation
	Automated phenate, salicylate, or other substituted phenols in Berthelot reaction based methods colorimetric (auto digestion and distillation)	351.1 (Rev. 1978) ¹		․	I-4551-78.⁸
	Semi-automated block digestor colorimetric (distillation not required)	351.2, Rev. 2.0 (1993)	4500-N_org D-2011	D3590-17 (B)	I-4515-91 ⁴⁵
	Block digester, followed by Auto distillation and Titration		․		See footnote.³⁹
	Block digester, followed by Auto distillation and Nesslerization		․		See footnote.⁴⁰
	Block Digester, followed by Flow injection gas diffusion (distillation not required)		․		See footnote.⁴¹
	Digestion with peroxdisulfate, followed by Spectrophotometric (2,6-dimethyl phenol)		․		Hach 10242.⁷⁶
	Digestion with persulfate, followed by Colorimetric		․		NCASI TNTP W10900.⁷⁷
32. Lead—Total,⁴ mg/L	Digestion,⁴ followed by any of the following:		․
	AA direct aspiration ³⁶		3111 B-2011 or 3111 C-2011	D3559-15 (A or B)	974.27,³ I-3399-85.²
	AA furnace		3113 B-2010	D3559-15 (D)	I-4403-89.⁵¹
	STGFAA	200.9, Rev. 2.2 (1994).		․
	ICP/AES ³⁶	200.5, Rev. 4.2 (2003); ⁶⁸ 200.7, Rev. 4.4 (1994)	3120 B-2011	D1976-12	I-4471-97.⁵⁰
	ICP/MS	200.8, Rev. 5.4 (1994)	3125 B-2011	D5673-16	993.14,³ I-4472-97.⁸¹
	DCP ³⁶		․	D4190-15	See footnote.³⁴
	Voltammetry ¹¹		․	D3559-15 (C).
	Colorimetric (Dithizone)		3500-Pb B-2011.
33. Magnesium—Total,⁴ mg/L	Digestion,⁴ followed by any of the following:		․
	AA direct aspiration		3111 B-2011	D511-14 (B)	974.27,³ I-3447-85.²
	ICP/AES	200.5, Rev. 4.2 (2003) ⁶⁸; 200.7, Rev. 4.4 (1994)	3120 B-2011	D1976-12	I-4471-97.⁵⁰
	ICP/MS	200.8, Rev. 5.4 (1994)	3125 B-2011	D5673-16	993.14.³
	DCP		․		See footnote.³⁴
	Ion Chromatography		․	D6919-17.
34. Manganese—Total,⁴ mg/L	Digestion,⁴ followed by any of the following:		․
	AA direct aspiration ³⁶		3111 B-2011	D858-17 (A or B)	974.27,³ I-3454-85.²
	AA furnace		3113 B-2010	D858-17 (C).
	STGFAA	200.9, Rev. 2.2 (1994)		․
	ICP/AES ³⁶	200.5, Rev. 4.2 (2003); ⁶⁸ 200.7, Rev. 4.4 (1994)	3120 B-2011	D1976-12	I-4471-97.⁵⁰
	ICP/MS	200.8, Rev. 5.4 (1994)	3125 B-2011	D5673-16	993.14,³ I-4472-97.⁸¹
	DCP ³⁶		․	D4190-15	See footnote.³⁴
	Colorimetric (Persulfate)		3500-Mn B-2011		920.203.³
	Colorimetric (Periodate)		․		See footnote.²³
35. Mercury—Total, mg/L	Cold vapor, Manual	245.1, Rev. 3.0 (1994)	3112 B-2011	D3223-17	977.22,³ I-3462-85.²
	Cold vapor, Automated	245.2 (Issued 1974) ¹.		․
	Cold vapor atomic fluorescence spectrometry (CVAFS)	245.7 Rev. 2.0 (2005) ¹⁷		․	I-4464-01.⁷¹
	Purge and Trap CVAFS	1631E ⁴³.		․
36. Molybdenum—Total,⁴ mg/L	Digestion,⁴ followed by any of the following:		․
	AA direct aspiration		3111 D-2011		I-3490-85.²
	AA furnace		3113 B-2010		I-3492-96.⁴⁷
	ICP/AES	200.7, Rev. 4.4 (1994)	3120 B-2011	D1976-12	I-4471-97.⁵⁰
	ICP/MS	200.8, Rev. 5.4 (1994)	3125 B-2011	D5673-16	993.14,³ I-4472-97.⁸¹
	DCP		․		See footnote.³⁴
37. Nickel—Total,⁴	Digestion,⁴ followed by any of the following:
mg/L
	AA direct aspiration ³⁶		3111 B-2011 or 3111 C-2011	D1886-14 (A or B)	I-3499-85 ²
	AA furnace		3113 B-2010	D1886-14 (C)	I-4503-89.⁵¹
	STGFAA	200.9, Rev. 2.2 (1994)		․
	ICP/AES ³⁶	200.5, Rev. 4.2 (2003); ⁶⁸ 200.7, Rev. 4.4 (1994)	3120 B-2011	D1976-12	I-4471-97.⁵⁰
	ICP/MS	200.8, Rev. 5.4 (1994)	3125 B-2011	D5673-16	993.14,³ I-4020-05 ⁷⁰ I-4472-97.⁸¹
	DCP ³⁶		․	D4190-15	See footnote.³⁴
38. Nitrate (as N), mg/L	Ion Chromatography	300.0, Rev. 2.1 (1993) and 300.1, Rev. 1.0 (1997)	4110 B-2011 or C-2011	D4327-17	993.30.³
	CIE/UV		4140 B-2011	D6508-15	D6508, Rev. 2.⁵⁴
	Ion Selective Electrode		4500-NO₃ D-2016.
	Colorimetric (Brucine sulfate)	352.1 (Issued 1971) ¹		․	973.50,³ 419D ¹⁷, p. 28.⁹
	Spectrophotometric (2,6-dimethylphenol)		․		Hach 10206 ⁷⁵
	Nitrate-nitrite N minus Nitrite N (See parameters 39 and 40)		․
39. Nitrate-nitrite (as N), mg/L	Cadmium reduction, Manual		4500-NO₃-E-2016	D3867-16 (B).
	Cadmium reduction, Automated	353.2, Rev. 2.0 (1993)	4500-NO₃-F-2016 4500-NO₃-I-2016	D3867-16 (A)	I-2545-90.⁵¹
	Automated hydrazine		4500-NO₃-H-2016.
	Reduction/Colorimetric		․		See footnote.⁶²
	Ion Chromatography	300.0, Rev. 2.1 (1993) and 300.1, Rev. 1.0 (1997)	4110 B-2011 or C-2011	D4327-17	993.30.³
	CIE/UV		4140 B-2011	D6508-15	D6508, Rev. 2.⁵⁴
	Enzymatic reduction, followed by automated colorimetric determination		․	D7781-14	I-2547-11.⁷²
					I-2548-11.⁷²
					N07-0003.⁷³
	Enzymatic reduction, followed by manual colorimetric determination		4500-NO₃-J-2018.
	Spectrophotometric (2,6-dimethylphenol)		․		Hach 10206.⁷⁵
40. Nitrite (as N), mg/L	Spectrophotometric: Manual		4500-NO₂-B-2011		See footnote.²⁵
	Automated (Diazotization)		․		I-4540-85,² See footnote.⁶² I-2540-90.⁸⁰
	Automated (*bypass cadmium reduction)	353.2, Rev. 2.0 (1993)	4500-NO₃-F-2016 4500-NO₃-I-2016	D3867-16 (A)	I-4545-85.²
	Manual (*bypass cadmium or enzymatic reduction)		4500-NO₃- E-2016, 4500-NO₃-J-2018	D3867-16 (B).
	Ion Chromatography	300.0, Rev. 2.1 (1993) and 300.1, Rev. 1.0 (1997)	4110 B-2011 or C-2011	D4327-17	993.30.³
	CIE/UV		4140 B-2011	D6508-15	D6508, Rev. 2.⁵⁴
	Automated (*bypass Enzymatic reduction)		․	D7781-14	I-2547-11 ⁷² I-2548-11 ⁷² N07-0003.⁷³
41. Oil and grease—Total recoverable, mg/L	Hexane extractable material (HEM): n-Hexane extraction and gravimetry	1664 Rev. A; 1664 Rev. B ⁴²	5520 B-2011 ³⁸.
	Silica gel treated HEM (SGT-HEM): Silica gel treatment and gravimetry	1664 Rev. A; 1664 Rev. B ⁴²	5520 B-2011 ³⁸ and 5520 F-2011 ³⁸.
42. Organic carbon—Total (TOC), mg/L	Combustion		5310 B-2014	D7573-09(17)	973.47,³ p. 14.²⁴
	Heated persulfate or UV persulfate oxidation		5310 C-2014 5310 D-2011	D4839-03(17)	973.47,³ p. 14.²⁴
43. Organic nitrogen (as N), mg/L	Total Kjeldahl N (Parameter 31) minus ammonia N (Parameter 4)		․
44. Ortho-phosphate (as P), mg/L	Ascorbic acid method:		․
	Automated	365.1, Rev. 2.0 (1993)	4500-P F-2011 or G-2011		973.56,³ I-4601-85,² I-2601-90.⁸⁰
	Manual, single-reagent		4500-P E-2011	D515-88 (A)	973.55.³
	Manual, two-reagent	365.3 (Issued 1978) ¹.		․
	Ion Chromatography	300.0, Rev. 2.1 (1993) and 300.1, Rev. 1.0 (1997)	4110 B-2011 or C-2011	D4327-17	993.30.³
	CIE/UV		4140 B-2011	D6508-15	D6508, Rev. 2.⁵⁴
45. Osmium—Total,⁴ mg/L	Digestion,⁴ followed by any of the following:		․
	AA direct aspiration		3111 D-2011.
	AA furnace	252.2 (Issued 1978) ¹.		․
46. Oxygen, dissolved, mg/L	Winkler (Azide modification)		4500-O (B-F)-2016	D888-12 (A)	973.45B,³ I-1575-78.⁸
	Electrode		4500-O G-2016	D888-12 (B)	I-1576-78.⁸
	Luminescence-Based Sensor		4500-O H-2016	D888-12 (C)	See footnote.⁶³ See footnote.⁶⁴
47. Palladium—Total,⁴ mg/L	Digestion,⁴ followed by any of the following:		․
	AA direct aspiration		3111 B-2011.
	AA furnace	253.2 (Issued 1978) ¹.		․
	ICP/MS		3125 B-2011.
	DCP		․		See footnote.³⁴
48. Phenols, mg/L	Manual distillation,²⁶ followed by any of the following:	420.1 (Rev. 1978) ¹	5530 B-2010	D1783-01(12).
	Colorimetric (4AAP) manual	420.1 (Rev. 1978) ¹	5530 D-2010 ²⁷	D1783-01(12) (A or B).
	Automated colorimetric (4AAP)	420.4 Rev. 1.0 (1993)		․
49. Phosphorus (elemental), mg/L	Gas-liquid chromatography		․		See footnote.²⁸
50. Phosphorus—Total, mg/L	Digestion,²⁰ followed by any of the following:		4500-P B (5)-2011		973.55.³
	Manual	365.3 (Issued 1978) ¹	4500-P E-2011	D515-88 (A).
	Automated ascorbic acid reduction	365.1 Rev. 2.0 (1993)	4500-P (F-H)-2011		973.56,³ I-4600-85.²
	ICP/AES ⁴³⁶	200.7, Rev. 4.4 (1994)	3120 B-2011		I-4471-97.⁵⁰
	Semi-automated block digestor (TKP digestion)	365.4 (Issued 1974) ¹		D515-88 (B)	I-4610-91.⁴⁸
	Digestion with persulfate, followed by Colorimetric		․		NCASI TNTP W10900.⁷⁷
51. Platinum—Total,⁴ mg/L	Digestion,⁴ followed by any of the following:		․
	AA direct aspiration		3111 B-2011.
	AA furnace	255.2 (Issued 1978) ¹.		․
	ICP/MS		3125 B-2011.
	DCP		․		See footnote.³⁴
52. Potassium—Total,⁴ mg/L	Digestion,⁴ followed by any of the following:		․
	AA direct aspiration		3111 B-2011		973.53,³ I-3630-85.²
	ICP/AES	200.7, Rev. 4.4 (1994)	3120 B-2011.
	ICP/MS	200.8, Rev. 5.4 (1994)	3125 B-2011	D5673-16	993.14.³
	Flame photometric		3500-K B-2011.
	Electrode		3500-K C-2011.
	Ion Chromatography		․	D6919-17.
53. Residue—Total, mg/L	Gravimetric, 103-105°		2540 B-2015		I-3750-85.²
54. Residue—filterable, mg/L	Gravimetric, 180°		2540 C-2015	D5907-13	I-1750-85.²
55. Residue—non-filterable (TSS), mg/L	Gravimetric, 103-105° post-washing of residue		2540 D-2015	D5907-13	I-3765-85.²
56. Residue—settleable, ml/L	Volumetric (Imhoff cone), or gravimetric		2540 F-2015.
57. Residue—Volatile, mg/L	Gravimetric, 550°	160.4 (Issued 1971) ¹	2540 E-2015		I-3753-85.²
58. Rhodium—Total,⁴ mg/L	Digestion,⁴ followed by any of the following:		․
	AA direct aspiration, or		3111 B-2011.
	AA furnace	265.2 (Issued 1978) ¹.		․
	ICP/MS		3125 B-2011.
59. Ruthenium—Total,⁴ mg/L	Digestion,⁴ followed by any of the following:		․
	AA direct aspiration, or		3111 B-2011.
	AA furnace	267.2 ¹.		․
	ICP/MS		3125 B-2011.
60. Selenium—Total,⁴ mg/L	Digestion,⁴ followed by any of the following:		․
	AA furnace		3113 B-2010	D3859-15 (B)	I-4668-98.⁴⁹
	STGFAA	200.9, Rev. 2.2 (1994).		․
	ICP/AES ³⁶	200.5, Rev 4.2 (2003); ⁶⁸ 200.7, Rev. 4.4 (1994)	3120 B-2011	D1976-12.
	ICP/MS	200.8, Rev. 5.4 (1994)	3125 B-2011	D5673-16	993.14,³ I-4020-05 ⁷⁰ I-4472-97.⁸¹
	AA gaseous hydride		3114 B-2011, or 3114 C-2011	D3859-15 (A)	I-3667-85.²
61. Silica—Dissolved,³⁷ mg/L	0.45-micron filtration followed by any of the following:		․
	Colorimetric, Manual		4500-SiO₂ C-2011	D859-16	I-1700-85.²
	Automated (Molybdosilicate)		4500-SiO₂ E-2011 or F-2011		I-2700-85.²
	ICP/AES	200.5, Rev. 4.2 (2003) ⁶⁸; 200.7, Rev. 4.4 (1994)	3120 B-2011		I-4471-97.⁵⁰
	ICP/MS	200.8, Rev. 5.4 (1994)	3125 B-2011	D5673-16	993.14.³
62. Silver—Total,⁴³¹ mg/L	Digestion,⁴²⁹ followed by any of the following:		․
	AA direct aspiration		3111 B-2011 or 3111 C-2011		974.27,³ p. 37,⁹ I-3720-85.²
	AA furnace		3113 B-2010		I-4724-89.⁵¹
	STGFAA	200.9, Rev. 2.2 (1994).		․
	ICP/AES	200.5, Rev. 4.2 (2003); ⁶⁸ 200.7, Rev. 4.4 (1994)	3120 B-2011	D1976-12	I-4471-97.⁵⁰
	ICP/MS	200.8, Rev. 5.4 (1994)	3125 B-2011	D5673-16	993.14,³ I-4472-97.⁸¹
	DCP		․		See footnote.³⁴
63. Sodium—Total,⁴ mg/L	Digestion,⁴ followed by any of the following:		․
	AA direct aspiration		3111 B-2011		973.54,³ I-3735-85.²
	ICP/AES	200.5, Rev. 4.2 (2003); ⁶⁸ 200.7, Rev. 4.4 (1994)	3120 B-2011		I-4471-97.⁵⁰
	ICP/MS	200.8, Rev. 5.4 (1994)	3125 B-2011	D5673-16	993.14.³
	DCP		․		See footnote.³⁴
	Flame photometric		3500-Na B-2011.
	Ion Chromatography		․	D6919-17.
64. Specific conductance, micromhos/cm at 25 °C	Wheatstone bridge	120.1 (Rev. 1982) ¹	2510 B-2011	D1125-95(99) (A)	973.40,³ I-2781-85.²
65. Sulfate (as SO₄), mg/L	Automated colorimetric	375.2, Rev. 2.0 (1993)	4500-SO₄ ² F-2011 or G-2011
	Gravimetric		4500-SO₄ ²-C-2011 or D-2011		925.54.³
	Turbidimetric		4500-SO₄ ²-E-2011	D516-16.
	Ion Chromatography	300.0, Rev. 2.1 (1993) and 300.1, Rev. 1.0 (1997)	4110 B-2011 or C-2011	D4327-17	993, I-4020-05 ⁷⁰.30₃
	CIE/UV		4140 B-2011	D6508-15	D6508, Rev. 2.⁵⁴
66. Sulfide (as S), mg/L	Sample Pretreatment		4500-S^2- B, C-2011.
	Titrimetric (iodine)		4500-S-F-2011		I-3840-85.²
	Colorimetric (methylene blue)		4500-S^2- D-2011.
	Ion Selective Electrode		4500-S-G-2011	D4658-15.
67. Sulfite (as SO₃), mg/L	Titrimetric (iodine-iodate)		4500-SO₃ ²-B-2011.
68. Surfactants, mg/L	Colorimetric (methylene blue)		5540 C-2011	D2330-02.
69. Temperature, °C	Thermometric		2550 B-2010		See footnote.³²
70. Thallium-Total,⁴ mg/L	Digestion,⁴ followed by any of the following:		․
	AA direct aspiration		3111 B-2011.
	AA furnace	279.2 (Issued 1978) ¹	3113 B-2010.
	STGFAA	200.9, Rev. 2.2 (1994).		․
	ICP/AES	200.7, Rev. 4.4 (1994)	3120 B-2011	D1976-12.
	ICP/MS	200.8, Rev. 5.4 (1994)	3125 B-2011	D5673-16	993.14,³ I-4471-97 ⁵⁰ I-4472-97.⁸¹
71. Tin-Total,⁴ mg/L	Digestion,⁴ followed by any of the following:		․
	AA direct aspiration		3111 B-2011		I-3850-78.⁸
	AA furnace		3113 B-2010.
	STGFAA	200.9, Rev. 2.2 (1994).		․
	ICP/AES	200.5, Rev. 4.2 (2003) ⁶⁸; 200.7, Rev. 4.4 (1994).		․
	ICP/MS	200.8, Rev. 5.4 (1994)	3125 B-2011	D5673-16	993.14.³
72. Titanium-Total,⁴ mg/L	Digestion,⁴ followed by any of the following:		․
	AA direct aspiration		3111 D-2011.
	AA furnace	283.2 (Issued 1978) ¹.		․
	ICP/AES	200.7, Rev. 4.4 (1994).		․
	ICP/MS	200.8, Rev. 5.4 (1994)	3125 B-2011	D5673-16	993.14.³
	DCP		․		See footnote.³⁴
73. Turbidity, NTU ⁵³	Nephelometric	180.1, Rev. 2.0 (1993)	2130 B-2011	D1889-00	I-3860-85 ²
					See footnote.⁶⁵
					See footnote.⁶⁶
					See footnote.⁶⁷
74. Vanadium-Total,⁴ mg/L	Digestion,⁴ followed by any of the following:		․
	AA direct aspiration		3111 D-2011.
	AA furnace		3113 B-2010	D3373-17.
	ICP/AES	200.5, Rev. 4.2 (2003); ⁶⁸ 200.7, Rev. 4.4 (1994)	3120 B-2011	D1976-12	I-4471-97 ⁵⁰
	ICP/MS	200.8, Rev. 5.4 (1994)	3125 B-2011	D5673-16	993.14,³ I-4020-05.⁷⁰
	DCP		․	D4190-15	See footnote.³⁴
	Colorimetric (Gallic Acid)		3500-V B-2011.
75. Zinc-Total,⁴ mg/L	Digestion,⁴ followed by any of the following:		․
	AA direct aspiration ³⁶		3111 B-2011 or 3111 C-2011	D1691-17 (A or B)	974.27,³ p. 37,⁹ I-3900-85.²
	AA furnace	289.2 (Issued 1978) ¹.		․
	ICP/AES ³⁶	200.5, Rev. 4.2 (2003); ⁶⁸ 200.7, Rev. 4.4 (1994)	3120 B-2011	D1976-12	I-4471-97.⁵⁰
	ICP/MS	200.8, Rev. 5.4 (1994)	3125 B-2011	D5673-16	993.14,³ I-4020-05 ⁷⁰ I-4472-97.⁸¹
	DCP ³⁶		․	D4190-15	See footnote.³⁴
	Colorimetric (Zincon)		3500 Zn B-2011		See footnote.³³
76. Acid Mine Drainage		1627 ⁶⁹.		․
Table IB Notes:

¹ Methods for Chemical Analysis of Water and Wastes, EPA-600/4-79-020. Revised March 1983 and 1979, where applicable. U.S. EPA.

² Methods for Analysis of Inorganic Substances in Water and Fluvial Sediments, Techniques of Water-Resource Investigations of the U.S. Geological Survey, Book 5, Chapter A1., unless otherwise stated. 1989. USGS.

³ Official Methods of Analysis of the Association of Official Analytical Chemists, Methods Manual, Sixteenth Edition, 4th Revision, 1998. AOAC International.

⁴ For the determination of total metals (which are equivalent to total recoverable metals) the sample is not filtered before processing. A digestion procedure is required to solubilize analytes in suspended material and to break down organic-metal complexes (to convert the analyte to a detectable form for colorimetric analysis). For non-platform graphite furnace atomic absorption determinations, a digestion using nitric acid (as specified in Section 4.1.3 of Methods for Chemical Analysis of Water and Wastes) is required prior to analysis. The procedure used should subject the sample to gentle acid refluxing, and at no time should the sample be taken to dryness. For direct aspiration flame atomic absorption (FLAA) determinations, a combination acid (nitric and hydrochloric acids) digestion is preferred, prior to analysis. The approved total recoverable digestion is described as Method 200.2 in Supplement I of “Methods for the Determination of Metals in Environmental Samples” EPA/600R-94/111, May, 1994, and is reproduced in EPA Methods 200.7, 200.8, and 200.9 from the same Supplement. However, when using the gaseous hydride technique or for the determination of certain elements such as antimony, arsenic, selenium, silver, and tin by non-EPA graphite furnace atomic absorption methods, mercury by cold vapor atomic absorption, the noble metals and titanium by FLAA, a specific or modified sample digestion procedure may be required, and, in all cases the referenced method write-up should be consulted for specific instruction and/or cautions. For analyses using inductively coupled plasma-atomic emission spectrometry (ICP-AES), the direct current plasma (DCP) technique or EPA spectrochemical techniques (platform furnace AA, ICP-AES, and ICP-MS), use EPA Method 200.2 or an approved alternate procedure (e.g., CEM microwave digestion, which may be used with certain analytes as indicated in Table IB); the total recoverable digestion procedures in EPA Methods 200.7, 200.8, and 200.9 may be used for those respective methods. Regardless of the digestion procedure, the results of the analysis after digestion procedure are reported as “total” metals.

⁵ Copper sulfate or other catalysts that have been found suitable may be used in place of mercuric sulfate.

⁶ Manual distillation is not required if comparability data on representative effluent samples are on file to show that this preliminary distillation step is not necessary; however, manual distillation will be required to resolve any controversies. In general, the analytical method should be consulted regarding the need for distillation. If the method is not clear, the laboratory may compare a minimum of 9 different sample matrices to evaluate the need for distillation. For each matrix, a matrix spike and matrix spike duplicate are analyzed both with and without the distillation step (for a total of 36 samples, assuming 9 matrices). If results are comparable, the laboratory may dispense with the distillation step for future analysis. Comparable is defined as < 20% RPD for all tested matrices). Alternatively, the two populations of spike recovery percentages may be compared using a recognized statistical test.

⁷ Industrial Method Number 379-75 WE Ammonia, Automated Electrode Method, Technicon Auto Analyzer II. February 19, 1976. Bran & Luebbe Analyzing Technologies Inc.

⁸ The approved method is that cited in Methods for Determination of Inorganic Substances in Water and Fluvial Sediments, Techniques of Water-Resources Investigations of the U.S. Geological Survey, Book 5, Chapter A1. 1979. USGS.

⁹ American National Standard on Photographic Processing Effluents. April 2, 1975. American National Standards Institute.

¹⁰ In-Situ Method 1003-8-2009, Biochemical Oxygen Demand (BOD) Measurement by Optical Probe. 2009. In-Situ Incorporated.

¹¹ The use of normal and differential pulse voltage ramps to increase sensitivity and resolution is acceptable.

¹² Carbonaceous biochemical oxygen demand (CBOD₅) must not be confused with the traditional BOD₅ test method which measures “total 5-day BOD.” The addition of the nitrification inhibitor is not a procedural option but must be included to report the CBOD₅ parameter. A discharger whose permit requires reporting the traditional BOD₅ may not use a nitrification inhibitor in the procedure for reporting the results. Only when a discharger's permit specifically states CBOD₅ is required can the permittee report data using a nitrification inhibitor.

¹³ OIC Chemical Oxygen Demand Method. 1978. Oceanography International Corporation.

¹⁴ Method 8000, Chemical Oxygen Demand, Hach Handbook of Water Analysis, 1979. Hach Company.

¹⁵ The back-titration method will be used to resolve controversy.

¹⁶ Orion Research Instruction Manual, Residual Chlorine Electrode Model 97-70. 1977. Orion Research Incorporated. The calibration graph for the Orion residual chlorine method must be derived using a reagent blank and three standard solutions, containing 0.2, 1.0, and 5.0 mL 0.00281 N potassium iodate/100 mL solution, respectively.

¹⁷ Method 245.7, Mercury in Water by Cold Vapor Atomic Fluorescence Spectrometry, EPA-821-R-05-001. Revision 2.0, February 2005. US EPA.

¹⁸ National Council of the Paper Industry for Air and Stream Improvement (NCASI) Technical Bulletin 253 (1971) and Technical Bulletin 803, May 2000.

¹⁹ Method 8506, Bicinchoninate Method for Copper, Hach Handbook of Water Analysis. 1979. Hach Company.

²⁰ When using a method with block digestion, this treatment is not required.

²¹ Industrial Method Number 378-75WA, Hydrogen ion (pH) Automated Electrode Method, Bran & Luebbe (Technicon) Autoanalyzer II. October 1976. Bran & Luebbe Analyzing Technologies.

²² Method 8008, 1,10-Phenanthroline Method using FerroVer Iron Reagent for Water. 1980. Hach Company.

²³ Method 8034, Periodate Oxidation Method for Manganese, Hach Handbook of Wastewater Analysis. 1979. Hach Company.

²⁴ Methods for Analysis of Organic Substances in Water and Fluvial Sediments, Techniques of Water-Resources Investigations of the U.S. Geological Survey, Book 5, Chapter A3, (1972 Revised 1987). 1987. USGS.

²⁵ Method 8507, Nitrogen, Nitrite-Low Range, Diazotization Method for Water and Wastewater. 1979. Hach Company.

²⁶ Just prior to distillation, adjust the sulfuric-acid-preserved sample to pH 4 with 1 + 9 NaOH.

²⁷ The colorimetric reaction must be conducted at a pH of 10.0 ± 0.2.

²⁸ Addison, R.F., and R.G. Ackman. 1970. Direct Determination of Elemental Phosphorus by Gas-Liquid Chromatography, Journal of Chromatography, 47(3):421-426.

²⁹ Approved methods for the analysis of silver in industrial wastewaters at concentrations of 1 mg/L and above are inadequate where silver exists as an inorganic halide. Silver halides such as the bromide and chloride are relatively insoluble in reagents such as nitric acid but are readily soluble in an aqueous buffer of sodium thiosulfate and sodium hydroxide to pH of 12. Therefore, for levels of silver above 1 mg/L, 20 mL of sample should be diluted to 100 mL by adding 40 mL each of 2 M Na₂S₂O₃ and NaOH. Standards should be prepared in the same manner. For levels of silver below 1 mg/L the approved method is satisfactory.

³⁰ The use of EDTA decreases method sensitivity. Analysts may omit EDTA or replace with another suitable complexing reagent provided that all method-specified quality control acceptance criteria are met.

³¹ For samples known or suspected to contain high levels of silver (e.g., in excess of 4 mg/L), cyanogen iodide should be used to keep the silver in solution for analysis. Prepare a cyanogen iodide solution by adding 4.0 mL of concentrated NH₄OH, 6.5 g of KCN, and 5.0 mL of a 1.0 N solution of I₂ to 50 mL of reagent water in a volumetric flask and dilute to 100.0 mL. After digestion of the sample, adjust the pH of the digestate to >7 to prevent the formation of HCN under acidic conditions. Add 1 mL of the cyanogen iodide solution to the sample digestate and adjust the volume to 100 mL with reagent water (NOT acid). If cyanogen iodide is added to sample digestates, then silver standards must be prepared that contain cyanogen iodide as well. Prepare working standards by diluting a small volume of a silver stock solution with water and adjusting the pH>7 with NH₄OH. Add 1 mL of the cyanogen iodide solution and let stand 1 hour. Transfer to a 100-mL volumetric flask and dilute to volume with water.

³² “Water Temperature-Influential Factors, Field Measurement and Data Presentation,” Techniques of Water-Resources Investigations of the U.S. Geological Survey, Book 1, Chapter D1. 1975. USGS.

³³ Method 8009, Zincon Method for Zinc, Hach Handbook of Water Analysis, 1979. Hach Company.

³⁴ Method AES0029, Direct Current Plasma (DCP) Optical Emission Spectrometric Method for Trace Elemental Analysis of Water and Wastes. 1986-Revised 1991. Thermo Jarrell Ash Corporation.

³⁵ In-Situ Method 1004-8-2009, Carbonaceous Biochemical Oxygen Demand (CBOD) Measurement by Optical Probe. 2009. In-Situ Incorporated.

³⁶ Microwave-assisted digestion may be employed for this metal, when analyzed by this methodology. Closed Vessel Microwave Digestion of Wastewater Samples for Determination of Metals. April 16, 1992. CEM Corporation

³⁷ When determining boron and silica, only plastic, PTFE, or quartz laboratory ware may be used from start until completion of analysis.

³⁸ Only use n-hexane (n-Hexane—85% minimum purity, 99.0% min. saturated C6 isomers, residue less than 1 mg/L) extraction solvent when determining Oil and Grease parameters—Hexane Extractable Material (HEM), or Silica Gel Treated HEM (analogous to EPA Methods 1664 Rev. A and 1664 Rev. B). Use of other extraction solvents is prohibited.

³⁹ Method PAI-DK01, Nitrogen, Total Kjeldahl, Block Digestion, Steam Distillation, Titrimetric Detection. Revised December 22, 1994. OI Analytical.

⁴⁰ Method PAI-DK02, Nitrogen, Total Kjeldahl, Block Digestion, Steam Distillation, Colorimetric Detection. Revised December 22, 1994. OI Analytical.

⁴¹ Method PAI-DK03, Nitrogen, Total Kjeldahl, Block Digestion, Automated FIA Gas Diffusion. Revised December 22, 1994. OI Analytical.

⁴² Method 1664 Rev. B is the revised version of EPA Method 1664 Rev. A. U.S. EPA. February 1999, Revision A. Method 1664, n-Hexane Extractable Material (HEM; Oil and Grease) and Silica Gel Treated n-Hexane Extractable Material (SGT-HEM; Non-polar Material) by Extraction and Gravimetry. EPA-821-R-98-002. U.S. EPA. February 2010, Revision B. Method 1664, n-Hexane Extractable Material (HEM; Oil and Grease) and Silica Gel Treated n-Hexane Extractable Material (SGT-HEM; Non-polar Material) by Extraction and Gravimetry. EPA-821-R-10-001.

⁴³ Method 1631, Revision E, Mercury in Water by Oxidation, Purge and Trap, and Cold Vapor Atomic Fluorescence Spectrometry, EPA-821-R-02-019. Revision E. August 2002, U.S. EPA. The application of clean techniques described in EPA's Method 1669: Sampling Ambient Water for Trace Metals at EPA Water Quality Criteria Levels, EPA-821-R-96-011, are recommended to preclude contamination at low-level, trace metal determinations.

⁴⁴ Method OIA-1677-09, Available Cyanide by Ligand Exchange and Flow Injection Analysis (FIA). 2010. OI Analytical.

⁴⁵ Open File Report 00-170, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Ammonium Plus Organic Nitrogen by a Kjeldahl Digestion Method and an Automated Photometric Finish that Includes Digest Cleanup by Gas Diffusion. 2000. USGS.

⁴⁶ Open File Report 93-449, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Chromium in Water by Graphite Furnace Atomic Absorption Spectrophotometry. 1993. USGS.

⁴⁷ Open File Report 97-198, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Molybdenum by Graphite Furnace Atomic Absorption Spectrophotometry. 1997. USGS.

⁴⁸ Open File Report 92-146, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Total Phosphorus by Kjeldahl Digestion Method and an Automated Colorimetric Finish That Includes Dialysis. 1992. USGS.

⁴⁹ Open File Report 98-639, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Arsenic and Selenium in Water and Sediment by Graphite Furnace-Atomic Absorption Spectrometry. 1999. USGS.

⁵⁰ Open File Report 98-165, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Elements in Whole-water Digests Using Inductively Coupled Plasma-Optical Emission Spectrometry and Inductively Coupled Plasma-Mass Spectrometry. 1998. USGS.

⁵¹ Open File Report 93-125, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Inorganic and Organic Constituents in Water and Fluvial Sediments. 1993. USGS.

⁵² Unless otherwise indicated, all EPA methods, excluding EPA Method 300.1, are published in U.S. EPA. May 1994. Methods for the Determination of Metals in Environmental Samples, Supplement I, EPA/600/R-94/111; or U.S. EPA. August 1993. Methods for the Determination of Inorganic Substances in Environmental Samples, EPA/600/R-93/100. EPA Method 300.1 is U.S. EPA. Revision 1.0, 1997, including errata cover sheet April 27, 1999. Determination of Inorganic Ions in Drinking Water by Ion Chromatography.

⁵³ Styrene divinyl benzene beads (e.g., AMCO-AEPA-1 or equivalent) and stabilized formazin (e.g., Hach StablCalTM or equivalent) are acceptable substitutes for formazin.

⁵⁴ Method D6508-15, Test Method for Determination of Dissolved Inorganic Anions in Aqueous Matrices Using Capillary Ion Electrophoresis and Chromate Electrolyte. 2015. ASTM

⁵⁵ Kelada-01, Kelada Automated Test Methods for Total Cyanide, Acid Dissociable Cyanide, and Thiocyanate, EPA 821-B-01-009, Revision 1.2, August 2001. U.S. EPA. 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.

⁵⁶ 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 2.2, March 2005. Lachat Instruments.

⁵⁷ When using sulfide removal test procedures described in EPA Method 335.4-1, reconstitute particulate that is filtered with the sample prior to distillation.

⁵⁸ Unless otherwise stated, if the language of this table specifies a sample digestion and/or distillation “followed by” analysis with a method, approved digestion and/or distillation are required prior to analysis.

⁵⁹ Samples analyzed for available cyanide using OI Analytical method OIA-1677-09 or ASTM method D6888-16 that contain particulate matter may be filtered only after the ligand exchange reagents have been added to the samples, because the ligand exchange process converts complexes containing available cyanide to free cyanide, which is not removed by filtration. Analysts are further cautioned to limit the time between the addition of the ligand exchange reagents and sample filtration to no more than 30 minutes to preclude settling of materials in samples.

⁶⁰ Analysts should be aware that pH optima and chromophore absorption maxima might differ when phenol is replaced by a substituted phenol as the color reagent in Berthelot Reaction (“phenol-hypochlorite reaction”) colorimetric ammonium determination methods. For example, when phenol is used as the color reagent, pH optimum and wavelength of maximum absorbance are about 11.5 and 635 nm, respectively—see, Patton, C.J. and S.R. Crouch. March 1977. Anal. Chem. 49:464-469. These reaction parameters increase to pH > 12.6 and 665 nm when salicylate is used as the color reagent—see, Krom, M.D. April 1980. The Analyst 105:305-316.

⁶¹ If atomic absorption or ICP instrumentation is not available, the aluminon colorimetric method detailed in the 19th Edition of Standard Methods for the Examination of Water and Wastewater may be used. This method has poorer precision and bias than the methods of choice.

⁶² Easy (1-Reagent) Nitrate Method, Revision November 12, 2011. Craig Chinchilla.

⁶³ Hach Method 10360, Luminescence Measurement of Dissolved Oxygen in Water and Wastewater and for Use in the Determination of BOD₅ and CBOD₅. Revision 1.2, October 2011. Hach Company. This method may be used to measure dissolved oxygen when performing the methods approved in Table IB for measurement of biochemical oxygen demand (BOD) and carbonaceous biochemical oxygen demand (CBOD).

⁶⁴ In-Situ Method 1002-8-2009, Dissolved Oxygen (DO) Measurement by Optical Probe. 2009. In-Situ Incorporated.

⁶⁵ Mitchell Method M5331, Determination of Turbidity by Nephelometry. Revision 1.0, July 31, 2008. Leck Mitchell.

⁶⁶ Mitchell Method M5271, Determination of Turbidity by Nephelometry. Revision 1.0, July 31, 2008. Leck Mitchell.

⁶⁷ Orion Method AQ4500, Determination of Turbidity by Nephelometry. Revision 5, March 12, 2009. Thermo Scientific.

⁶⁸ EPA Method 200.5, Determination of Trace Elements in Drinking Water by Axially Viewed Inductively Coupled Plasma-Atomic Emission Spectrometry, EPA/600/R-06/115. Revision 4.2, October 2003. U.S. EPA.

⁶⁹ Method 1627, Kinetic Test Method for the Prediction of Mine Drainage Quality, EPA-821-R-09-002. December 2011. U.S. EPA.

⁷⁰ Techniques and Methods Book 5-B1, Determination of Elements in Natural-Water, Biota, Sediment and Soil Samples Using Collision/Reaction Cell Inductively Coupled Plasma-Mass Spectrometry, Chapter 1, Section B, Methods of the National Water Quality Laboratory, Book 5, Laboratory Analysis, 2006. USGS.

⁷¹ Water-Resources Investigations Report 01-4132, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Organic Plus Inorganic Mercury in Filtered and Unfiltered Natural Water with Cold Vapor-Atomic Fluorescence Spectrometry, 2001. USGS.

⁷² USGS Techniques and Methods 5-B8, Chapter 8, Section B, Methods of the National Water Quality Laboratory Book 5, Laboratory Analysis, 2011 USGS.

⁷³ NECi Method N07-0003, “Nitrate Reductase Nitrate-Nitrogen Analysis,” Revision 9.0, March 2014, The Nitrate Elimination Co., Inc.

⁷⁴ Timberline Instruments, LLC Method Ammonia-001, “Determination of Inorganic Ammonia by Continuous Flow Gas Diffusion and Conductivity Cell Analysis,” June 2011, Timberline Instruments, LLC.

⁷⁵ Hach Company Method 10206, “Spectrophotometric Measurement of Nitrate in Water and Wastewater,” Revision 2.1, January 2013, Hach Company.

⁷⁶ Hach Company Method 10242, “Simplified Spectrophotometric Measurement of Total Kjeldahl Nitrogen in Water and Wastewater,” Revision 1.1, January 2013, Hach Company.

⁷⁷ National Council for Air and Stream Improvement (NCASI) Method TNTP-W10900, “Total (Kjeldahl) Nitrogen and Total Phosphorus in Pulp and Paper Biologically Treated Effluent by Alkaline Persulfate Digestion,” June 2011, National Council for Air and Stream Improvement, Inc.

⁷⁸ The pH adjusted sample is to be adjusted to 7.6 for NPDES reporting purposes.

⁷⁹ I-2057-85 U.S. Geological Survey Techniques of Water-Resources Investigations, Book 5, Chap. A11989, Methods for Determination of Inorganic Substances in Water and Fluvial Sediments, 1989.

⁸⁰ Methods I-2522-90, I-2540-90, and I-2601-90 U.S. Geological Survey Open-File Report 93-125, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory-Determination of Inorganic and Organic Constituents in Water and Fluvial Sediments, 1993.

⁸¹ Method I-1472-97, U.S. Geological Survey Open-File Report 98-165, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory-Determination of Inorganic and Organic Constituents in Water and Fluvial Sediments, 1998.

⁸² FIAlab Instruments, Inc. Method FIAlab 100, “Determination of Inorganic Ammonia by Continuous Flow Gas Diffusion and Fluorescence Detector Analysis”, April 4, 2018, FIAlab Instruments, Inc.

⁸³ MACHEREY-NAGEL GmbH and Co. Method 036/038 NANOCOLOR^® COD LR/HR, “Spectrophotometric Measurement of Chemical Oxygen Demand in Water and Wastewater”, Revision 1.5, May 2018, MACHEREY-NAGEL GmbH and Co. KG.

⁸⁴ Please refer to the following applicable Quality Control Sections: Part 2000 Methods, Physical and Aggregate Properties 2020 (2017); Part 3000 Methods, Metals, 3020 (2017); Part 4000 Methods, Inorganic Nonmetallic Constituents, 4020 (2014); Part 5000 Methods, and Aggregate Organic Constituents, 5020 (2017). These Quality Control Standards are available for download at www.standardmethods.org at no charge.

⁸⁵ Each laboratory may establish its own control limits by performing at least 25 glucose-glutamic acid (GGA) checks over several weeks or months and calculating the mean and standard deviation. The laboratory may then use the mean ± 3 standard deviations as the control limit for future GGA checks. However, GGA acceptance criteria can be no wider than 198 ± 30.5 mg/L for BOD₅. GGA acceptance criteria for CBOD must be either 198 ± 30.5 mg/L, or the lab may develop control charts under the following conditions:

• Dissolved oxygen uptake from the seed contribution is between 0.6-1.0 mg/L.

• Control charts are performed on at least 25 GGA checks with three standard deviations from the derived mean.

• The RSD must not exceed 7.5%.

• Any single GGA value cannot be less than 150 mg/L or higher than 250 mg/L.

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Cite this article: FindLaw.com - Code of Federal Regulations Title 40. Protection of Environment § 40.136.3, Table IB Identification of test procedures - last updated January 02, 2025 | https://codes.findlaw.com/cfr/title-40-protection-of-environment/cfr-sect-40-136-3-nr3/

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