EPA-EAD: 607: Nitrosamines in wastewater

Summary
Analytes
Revision
Data and Sites

Official Method Name

Method 607-Nitrosamines

Current Revision

40 CFR Part 136.3, Appendix A (Current Edition)

Media

WATER

Instrumentation

Gas Chromatography with Mass Spectrometry Detection

Method Subcategory

Organic

Method Source

EPA-EAD

Citation

EPA Method Guidance CD-ROM (includes MCAWW Methods, and most current EPA Methods)

Brief Method Summary

A measured volume of sample is extracted with methylene chloride. The methylene chloride extract is washed with dilute HCl and concentrated to a volume of 10 mL or less. After the extract has been exchanged to methanol it is separated by GC and the parameters are measured with a nitrogen-phosphorus detector.

Scope and Application

This is a gas chromatographic (GC) method applicable to the determination of N-Nitrosodimethylamine, N-Nitrosodiphenylamine, and N-Nitrosodi-n-propylamine in municipal and industrial discharges as provided under 40 CFR 136.1.

Applicable Concentration Range

Interferences

(A) Glassware: Must be scrupulously cleaned. Solvent rinsing should be followed by detergent washing with hot water, and rinses with tap water and distilled water. Glassware should then be drained dry and heated in a muffle furnace at 400^oC for 15-30 minutes. Solvent rinses with acetone and pesticide quality hexane may be substituted for the muffle furnace. Store glassware inverted or capped with aluminum foil.
(B) Co-extraction: The extraction process will sometimes extract certain analytes that may cause possible interference with the target compounds. A Florisil cleanup procedure is described in Section 11 of the method.
(C) Care must be exercised in the heating or concentrating of solutions containing N-Nitrosodiphenylamine in the presence of reactive amines due to the potential for transnitrosation reactions.

Quality Control Requirements

Initial demonstration of laboratory capability and an ongoing analysis of spiked samples to evaluate and document data quality.

Sample Handling

Grab samples must be collected in amber or foil-wrapped glass containers using conventional sampling practices, with the exception that the bottle must not be prerinsed with sample before collection.
Store samples away from light.
Samples should be iced or kept refrigerated at 4^oC from time of collection to time of extraction.

Maximum Holding Time

Extract within 7 days of collection.
Analyze within 40 days of extraction.

Relative Cost

$201 to $400

Sample Preparation Methods

This method has 3 analytes associated with it.

Analyte	Detection Level	Bias	Precision	Spiking Level
N-Nitrosodiphenylamine(86-30-6) Benzenamine, N-nitroso-N-phenyl N,N-diphenylnitrosamine N-Nitroso-N-phenylbenzenamine N-Nitrosodiphenylamine Nitrous diphenylamide	0.810 ug/L	69% Rec (ML)	39.00 % RSD (ML)	10.00 ug/L
NDMA(62-75-9) Dimethylnitrosamine Methamine, N-methyl-N-nitroso- Methanamine, N-methyl-N-nitroso N-Methyl-N-nitroso-methamine N-Methyl-N-nitrosomethanamine N-Nitrosodimethylamine NDMA	0.150 ug/L	40% Rec (ML)	38.75 % RSD (ML)	2.00 ug/L
NDPA(621-64-7) 1-Propanamine, N-nitroso-n-propyl- Di-n-propylamine,n-nitroso- Di-n-propylnitrosamine N-Nitrosodi-n-propylamine N-Nitrosodipropylamine NDPA	0.460 ug/L	95% Rec (ML)	24.20 % RSD (ML)	5.00 ug/L

Precision Descriptor Notes:
Detection Level Note:	The method detection limit (MDL) is defined as the minimum concentration of a substance that can be measured and reported with 99% confidence that the value is above zero. The MDL concentrations in Table 1 of the method were obtained using reagent water, however, similar results were achieved using representative wastewaters. The MDL actually acieved in a given analysis will vary depending on instrument sensitivity and matrix effects.

Precision Descriptor Notes:

Detection Level Note:

The method detection limit (MDL) is defined as the minimum concentration of a substance that can be measured and reported with 99% confidence that the value is above zero. The MDL concentrations in Table 1 of the method were obtained using reagent water, however, similar results were achieved using representative wastewaters. The MDL actually acieved in a given analysis will vary depending on instrument sensitivity and matrix effects.

Revision	PDF/Link
40 CFR Part 136.3, Appendix A (Current Edition)

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EPA-EAD: 607: Nitrosamines in wastewater

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