Determination of N-nitrosodimethylamine at part-per-trillion levels in drinking waters and contaminated groundwaters
Abstract
N-nitrosodimethylamine is a high, carcinogenic manufacturing by-product of unsymmetrical dimethyl hydrazine a component of rocket fuel. Prior disposal practices resulted in the contamination of groundwater near certain military installations with both species. The current regulatory threshold promulgated by the US Environmental Protection Agency (EPA) for NDMA in surface waters designated for drinking is 0.7 ng NDMA/L (0.7 pptr)L. Existing procedures for determining NDMA in aqueous samples typically employ dichloromethane extraction followed by concentration to a final volume of 1 mL, and gas chromatographic analysis of a 2 {mu}L aliquot of concentrate using either a nitrogen-phosphorus detector (NPD), mass spectrometric detector, or chemiluminescent nitrogen detector (CLND). Such a protocol does not permit detection of NDMA at the desired health-based criterion unless high-resolution mass spectrometric (HRMS) detectors are employed. The analytical procedure described in this work employed an initial solid-phase extraction of groundwater samples with a preconditioned Empore C{sub 18} disk, used to remove interfering neutral species including di-isopropylmethane phosphonate (DIMP), prior to continuous overnight extraction.
- Authors:
- Publication Date:
- Research Org.:
- Oak Ridge National Lab., TN (United States)
- Sponsoring Org.:
- Department of Defense, Washington, DC (United States)
- OSTI Identifier:
- 164458
- Report Number(s):
- CONF-9505309-1
ON: DE96003024
- DOE Contract Number:
- AC05-84OR21400
- Resource Type:
- Technical Report
- Resource Relation:
- Conference: 18. annual conference on analysis of pollutants in the environment, Norfolk, VA (United States), 3-4 May 1995; Other Information: PBD: [1995]
- Country of Publication:
- United States
- Language:
- English
- Subject:
- 54 ENVIRONMENTAL SCIENCES; 40 CHEMISTRY; GROUND WATER; CONTAMINATION; CHEMICAL ANALYSIS; DRINKING WATER; WATER QUALITY; LIQUID FUELS; ROCKETS; MILITARY FACILITIES; AMINES; MASS SPECTROSCOPY; COMPILED DATA
Citation Formats
Tomkins, B.A., Griest, W.H., and Higgins, C.E. Determination of N-nitrosodimethylamine at part-per-trillion levels in drinking waters and contaminated groundwaters. United States: N. p., 1995.
Web. doi:10.2172/164458.
Tomkins, B.A., Griest, W.H., & Higgins, C.E. Determination of N-nitrosodimethylamine at part-per-trillion levels in drinking waters and contaminated groundwaters. United States. doi:10.2172/164458.
Tomkins, B.A., Griest, W.H., and Higgins, C.E. Fri .
"Determination of N-nitrosodimethylamine at part-per-trillion levels in drinking waters and contaminated groundwaters". United States.
doi:10.2172/164458. https://www.osti.gov/servlets/purl/164458.
@article{osti_164458,
title = {Determination of N-nitrosodimethylamine at part-per-trillion levels in drinking waters and contaminated groundwaters},
author = {Tomkins, B.A. and Griest, W.H. and Higgins, C.E.},
abstractNote = {N-nitrosodimethylamine is a high, carcinogenic manufacturing by-product of unsymmetrical dimethyl hydrazine a component of rocket fuel. Prior disposal practices resulted in the contamination of groundwater near certain military installations with both species. The current regulatory threshold promulgated by the US Environmental Protection Agency (EPA) for NDMA in surface waters designated for drinking is 0.7 ng NDMA/L (0.7 pptr)L. Existing procedures for determining NDMA in aqueous samples typically employ dichloromethane extraction followed by concentration to a final volume of 1 mL, and gas chromatographic analysis of a 2 {mu}L aliquot of concentrate using either a nitrogen-phosphorus detector (NPD), mass spectrometric detector, or chemiluminescent nitrogen detector (CLND). Such a protocol does not permit detection of NDMA at the desired health-based criterion unless high-resolution mass spectrometric (HRMS) detectors are employed. The analytical procedure described in this work employed an initial solid-phase extraction of groundwater samples with a preconditioned Empore C{sub 18} disk, used to remove interfering neutral species including di-isopropylmethane phosphonate (DIMP), prior to continuous overnight extraction.},
doi = {10.2172/164458},
journal = {},
number = ,
volume = ,
place = {United States},
year = {Fri Dec 01 00:00:00 EST 1995},
month = {Fri Dec 01 00:00:00 EST 1995}
}
-
The carcinogen N-nitrosodimethylamine (NDMA) may be quantitated routinely at ultratrace (ng/L) levels in drinking water or contaminated groundwater. NDMA is selectively detected using a chemiluminescent nitrogen detector (CLND) operated in its nitrosamine-selective mode. The reporting limit for this procedure, evaluated using two independent statistically unbiased protocols, is 2 ng of NDMA/L. A related procedure, employing an automatic sampler instead of the short-path thermal desorber, provides convenient analysis of heavily contaminated samples and exhibits a reporting limit (same protocols cited previously) of 110 ng of NDMA/L. When the two methods are used together in a `two-tiered` protocol, NDMA concentrations spanning 4more »
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Determinations of N-Nitrosodimethylamine (NDMA) at part-per-trillion (ng/L) concentrations in contaminated groundwaters and drinking waters featuring carbon-based membrane extraction disks
A new solid phase extraction procedure extracts N- Nitrosodimethylamine (NDMA) at part-per-trillion (ng/L) concentrations from aqueous samples using a C{sub 18} (reversed-phase) membrane extraction disk layered over a carbon-based extraction disk. The reversed-phase disk removes nonpolar water-insoluble neutrals and is set aside; the carbon-based disk is extracted with a small volume of dichloromethane. NDMA is quantitated in the organic extract using a gas chromatograph equipped with both a short-path thermal desorber and a chemiluminescent nitrogen detector (CLND). The Method Detection Limit for the procedure is 2 ng of NDMA/L; the analyte recovery is approximately 57%. A related procedure substitutes amore » -
Determinations of N-nitrosodimethylamine at part-per-trillion concentrations in contaminated groundwaters and drinking waters featuring carbon-based membrane extraction disks
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