EPA-NERL: 521: Nitrosamines in water by SPE and GC/MS/MS

Summary
Analytes
Revision
Data and Sites

Official Method Name

DETERMINATION OF NITROSAMINES IN DRINKING WATER BY SOLID PHASE EXTRACTION AND CAPILLARY COLUMN GAS CHROMATOGRAPHY WITH LARGE VOLUME INJECTION AND CHEMICAL IONIZATION TANDEM MASS SPECTROMETRY (MS/MS)

Current Revision

Ver. 1.0, Sept. 2004

Media

WATER

Instrumentation

Gas Chromatography with Mass Spectrometry Detection

Method Subcategory

Organic

Method Source

EPA-NERL

Citation

Munch, J.W., and Bassett, M.V., 2004, Determination of nitrosamines in drinking water by solid phase extraction and capillary column gas chromatography with large volume injection and chemical ionization tandem mass spectrometry: U.S. Environmental Protection Agency Report EPA/600/R-05/054, Version 1.0, 47 p.

Brief Method Summary

Analytes and a surrogate analyte are extracted by passing a 0.5-L water sample through a solid phase extraction (SPE) cartridge containing 2 g of 80-120 mesh coconut charcoal (Sect. 7.2.7). The organic compounds are eluted from the solid phase with a small quantity of methylene chloride.

Scope and Application

This method provides procedures for the determination of nitrosamines in finished drinking water. The method may be applicable to untreated source waters and other types of water samples, but it has not been evaluated for these uses. The method is applicable to nitrosamines that are efficiently partitioned from the water sample onto a solid phase extraction (SPE) sorbent, and sufficiently volatile and thermally stable for gas chromatography.

Applicable Concentration Range

Interferences

See Section 4.0 of the method.

Quality Control Requirements

See Section 9 of the method.

Sample Handling

8.1 SAMPLE COLLECTION -- When sampling from a water tap, open the tap and allow the system to flush until the water temperature has stabilized (usually about 2 min). Adjust the flow to about 500 mL/min and collect samples from the flowing stream. The sample should nearly fill the bottle, but does not need to be headspace free. If the dechlorination agent has been added to the bottle prior to sampling (Sect. 8.2), be careful not to rinse it out during sample collection. Keep samples sealed from collection time until analysis. When sampling from an open body of water, fill the sample container with water from a representative area. Sampling equipment, including automatic samplers, must be free of plastic or rubber tubing, gaskets, and other parts that may leach interfering analytes into the water sample.

Maximum Holding Time

Samples must be extracted within 14 days of collection. Sample extracts may be stored for up to 28 days after sample extraction, when stored in amber vials at -15 degrees C or less, and protected from light.

Relative Cost

Sample Preparation Methods

This method has 7 analytes associated with it.

Analyte	Detection Level	Bias	Precision	Spiking Level
NDBA(924-16-3) 1-Butanamine, N-butyl-N-nitroso- Di-N-butylnitrosamine Dibutylnitrosamine N,N-Dibutylnitrosoamine N-Butyl-N-nitroso-1-butanamine N-Nitroso-dibutylamine N-Nitrosodi-n-butylamine NDBA	0.360 ng/L	N/A	N/A	1.00 ng/L
NDEA(55-18-5) Diethylnitrosamine Ethanamine, N-ethyl-N-nitroso- N-Nitrosodiethylamine N-ethyl-n-nitrosoethanamine NDEA	0.260 ng/L	N/A	N/A	1.00 ng/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	0.280 ng/L	N/A	N/A	1.00 ng/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	0.320 ng/L	N/A	N/A	1.00 ng/L
NMEA(10595-95-6) Ethanamine, N-methyl-N-nitroso Ethylmethylnitrosamine N,n-methylethylnitrosoamine N-Nitroso-N-methylethylamine N-Nitrosomethylethylamine N-methyl-n-nitrosoethanamine NMEA	0.280 ng/L	N/A	N/A	1.00 ng/L
NPIP(100-75-4) 1-Nitrosopiperidine N-Nitrosopiperidine NPIP Nitrospiperidine,n- No-pip Piperidine, 1-Nitroso- Pyridine, hexahydro-N-nitroso- n-nitrosohexahydro-Pyridine	0.660 ng/L	N/A	N/A	1.00 ng/L
NPYR(930-55-2) 1-Nitrosopyrrolidine N-Nitrosopyrrolidine NPYR Pyrrole, tetrahydro-N-nitroso- Pyrrolidine, 1-nitroso-	0.350 ng/L	N/A	N/A	1.00 ng/L

Precision Descriptor Notes:	See Section 17 for tables, diagrams, flow charts, and validation data.
Detection Level Note:	The Minimum Reporting Level (MRL) is the lowest analyte concentration that meets Data Quality Objectives (DQOs) that are developed based on the intended use of this method. The lowest concentration MRL (LCMRL) is a single laboratory determination of the lowest true concentration for which a future recovery is expected, with 99 percent confidence, to be between 50 and 150 percent recovery. Single laboratory LCMRLs for analytes in this method range from 1.2-2.1 ng/L, and are listed in Table 1.

Precision Descriptor Notes:

See Section 17 for tables, diagrams, flow charts, and validation data.

Detection Level Note:

The Minimum Reporting Level (MRL) is the lowest analyte concentration that meets Data Quality Objectives (DQOs) that are developed based on the intended use of this method. The lowest concentration MRL (LCMRL) is a single laboratory determination of the lowest true concentration for which a future recovery is expected, with 99 percent confidence, to be between 50 and 150 percent recovery. Single laboratory LCMRLs for analytes in this method range from 1.2-2.1 ng/L, and are listed in Table 1.

Revision	PDF/Link
Ver. 1.0, Sept. 2004

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EPA-NERL: 521: Nitrosamines in water by SPE and GC/MS/MS

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