USGS-NWQL: O-1124-94: Nitroaromatic compounds in water by HPLC

Summary
Analytes
Revision
Data and Sites

Official Method Name

Extraction of nitroaromatic compounds from water by polystyrene divinylbenzene cartridge and determination by high-performance liquid chromatography

Current Revision

1994

Media

WATER

Instrumentation

High Performance Liquid Chromatography with Photodiode-Array Detection

Method Subcategory

Organic

Method Source

USGS-NWQL

Citation

Lindley, C.E., Burkhardt, M.R.,and DeRussseau, S.N., 1994, Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory -- Extraction of nitroaromatic compounds from water by polystyrene divinylbenzene cartridge and determination by high-performance liquid chromatography: U.S. Geological Survey Open-File Report 94-62

Brief Method Summary

Analytes are extracted from filtered (0.7-um pore diameter GF/F) using conditioned SPE cartridges. The sample is poured through the reservoir onto the cartridge. The nitroaromatic components are desorbed from the cartridge with acetonitrile immediately after sample extraction to reduce loss of the more volatile nitroaromatic compounds. They are then brought up to volume with reagent-grade water and an aliquot is saved for analysis using reverse phase HPLC with ultraviolet photodiode array detection.

Scope and Application

This method covers the determination of explosive ingredients and selected degradation products in groundwater, surface water, and lysimeter samples.

Applicable Concentration Range

0.11 to 0.32 ug/L (based on 1- liter sample size)

Interferences

(A) Polystyrene divinylbenzene material containing uncrosslinked prepolymer (U.S. Army Toxic and Hazardous Materials Agency, written commun., 1991, p. 5; Jenkins and others, 1992, p. 2): Thorough cleaning of material is essential. (B) Non-target analytes including organic compounds having nonpolar, hydrophobic character that are introduced or any naturally occurring: Quality control samples including standards and matrix spikes.

Quality Control Requirements

Laboratory blanks, reagent blanks, spiked samples, duplicate samples, continuing calibration standards, and matrix spikes.

Sample Handling

Filtered (0.7 um GF/F) samples submitted in 1-L amber-glass pesticide bottles sealed with a Teflon-lined cap and chilled until extraction.

Maximum Holding Time

7 days from collection to extraction; 21 days from extraction to analysis.

Relative Cost

$201 to $400

Sample Preparation Methods

Extraction with polystyrene divinylbenzene SPE cartridges and subsequent elution with acetonitrile.

This method has 13 analytes associated with it.

Analyte	Detection Level	Bias	Precision	Spiking Level
2,4,6-Trinitrotoluene(118-96-7) 1-Methyl-2,4,6-trinitrobenzene 2,4,6-Trinitrotoluene Trinitrotoluene Tritol (explosive)	0.110 ug/L	94% Rec	4.00 % RSD	1.00 ug/L
2,4-Dinitrotoluene(121-14-2) 1-Methyl-2,4-dinitrobenzene 2,4-DNT 2,4-Dinitrotoluene 2,4-Dinitrotoluol Benzene, 1-methyl-2,4-dinitro Benzene,2-methyl-2,4-dinitro- Dinitrobenzene,1-methyl-2,4- Dinitrotoluene, 2,4 Methyl-2,4-dinitrobenzene,1- Toluene, 2,4-dinitro-	0.180 ug/L	77% Rec	6.00 % RSD	1.00 ug/L
2,6-Dinitrotoluene(606-20-2) 2,6-DNT 2,6-Dinitrotoluene Benzene, 2-methyl-1,3-dinitro- Benzene,1-methyl-2,6-dinitro- Dinitrobenzene,1-methyl-2,6-	0.210 ug/L	75% Rec	7.00 % RSD	1.00 ug/L
2-Amino-4,6-dinitrotoluene(35572-78-2) 2-Amino-4,6-dinitrotoluene 2-Methyl-3,5-dinitrobenzenamine 3,5-Dinitro-o-toluidine BRN 2377515 CCRIS 5187	0.130 ug/L	101% Rec	4.00 % RSD	1.00 ug/L
3,5-Dinitroaniline(618-87-1) 3,5-Dinitroaniline BRN 0648811 CCRIS 3109 NSC 284	0.320 ug/L	91% Rec	10.00 % RSD	1.00 ug/L
3-Nitrotoluene(99-08-1) 3-Nitrotoluene Benzene, 1-methyl-3-nitro- NSC 9578 Nitrotoluene, all isomers m-Nitrotoluene	0.130 ug/L	84% Rec	4.00 % RSD	1.00 ug/L
4-Amino-2,6-dinitrotoluene(19406-51-0) 3,5-Dinitro-4-methylaniline 4-Amino-2,6-dinitrotoluene 4-Amino-2,6-dinitrotoluene NSC 25010	0.260 ug/L	71% Rec	8.00 % RSD	1.00 ug/L
4-Nitrotoluene(99-99-0) 1-Methyl-4-nitrobenzene 4-Methylnitrobenzene 4-Nitrotoluene 4-Nitrotoluol Benzene, 1-methyl-4-nitro- p-Methylnitrobenzene p-Nitrotoluene	0.290 ug/L	84% Rec	9.00 % RSD	1.00 ug/L
Cyclonite(121-82-4) 1,3,5-Trinitrohexahydro-1,3,5-triazine Cyclonite Hexahydro-1,3,5-trinitro 1,3,5-triazine Hexogen (Explosive) RDX	0.140 ug/L	94% Rec	5.00 % RSD	1.00 ug/L
Nitrobenzene(98-95-3) Benzene, nitro- EPA Pesticide Chemical Code 056501 Essence of mirbane Essence of myrbane Mirbane oil Mononitrobenzene Nitrobenzene Nitrobenzol Oil of mirbane Oil of myrbane RCRA waste number U169	0.180 ug/L	90% Rec	6.00 % RSD	1.00 ug/L
Octogen(2691-41-0) 1,3,5,7-Tetranitro-1,3,5,7-tetraazacyclooctane BRN 0361386 HMX Octahydro-1,3,5,7-tetranitro 1,3,5,7-tetrazocine Octogen Tetramethylenetetranitramine	0.120 ug/L	101% Rec	4.00 % RSD	1.00 ug/L
o-Nitrotoluene(88-72-2) 2-Nitrotoluene Benzene, 1-methyl-2-nitro- o-Nitrotoluene	0.240 ug/L	81% Rec	8.00 % RSD	1.00 ug/L
sym-Trinitrobenzene(99-35-4) 1,3,5-Trinitrobenzene Benzene, 1,3,5-trinitro- Benzite TNB sym-Trinitrobenzene	0.190 ug/L	91% Rec	6.00 % RSD	1.00 ug/L

Precision Descriptor Notes:	Sets of reagent-water samples, surface-water samples collected from Clear Creek at Prospect Park in Wheat Ridge, CO, and ground-water samples collected in Jefferson County, CO, were used to test method performance. Each of the three water matrices was split into two subsamples. At least seven aliquots of approximately 1 L from each subsample were individually fortified at about 1 ug/L, and the other subsample at about 100 ug/L. The samples were analyzed by two analysts at the USGS National Water Quality Laboratory, using one HPLC instrument.
Detection Level Note:	The MDLs for individual analytes were determined by multiplying the standard deviation from the results of seven replicates by the Student's t-value for a 99 percent confidence level, as given in the USEPA procedure for determination of the method detection limit (U.S. Environmental Protection Agency, 1990).

Precision Descriptor Notes:

Sets of reagent-water samples, surface-water samples collected from Clear Creek at Prospect Park in Wheat Ridge, CO, and ground-water samples collected in Jefferson County, CO, were used to test method performance. Each of the three water matrices was split into two subsamples. At least seven aliquots of approximately 1 L from each subsample were individually fortified at about 1 ug/L, and the other subsample at about 100 ug/L. The samples were analyzed by two analysts at the USGS National Water Quality Laboratory, using one HPLC instrument.

Detection Level Note:

The MDLs for individual analytes were determined by multiplying the standard deviation from the results of seven replicates by the Student's t-value for a 99 percent confidence level, as given in the USEPA procedure for determination of the method detection limit (U.S. Environmental Protection Agency, 1990).

Revision	PDF/Link
1994

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USGS-NWQL: O-1124-94: Nitroaromatic compounds in water by HPLC

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