EPA-RCA: 8330B: Explosives by HPLC

Summary
Analytes
Revision
Data and Sites

Official Method Name

Nitroaromatics, Nitramines, and Nitrate Esters by High Performance Liquid Chromatography (HPLC)

Current Revision

Revision 2, October 2006

Media

VARIOUS

Instrumentation

High Performance Liquid Chromatography

Method Subcategory

Organic

Method Source

EPA-RCA

Citation

SW-846 Online: Test Methods for Evaluating Solid Waste, Physical/Chemical Methods

Brief Method Summary

This method is applicable for trace analysis of explosives and propellant residues by high performance liquid chromatography (HPLC) using a dual wavelength ultraviolet (UV) detector in a water, soil, or sediment matrix. All of the compounds listed in this method are either used in the manufacture of explosives or propellants, or they are the degradation products of compounds used for that purpose. Samples are prepared for analysis by HPLC-UV using the appropriate sample preparation technique (solid phase extraction by 3535A or solvent extraction by 8330B) and, if necessary, sample cleanup procedures. Method 8330 provides a salting-out extraction procedure for low concentration (ppt or ng/L) of explosives residues in surface or ground water. Direct injection of diluted and filtered water samples can be used for water samples of higher concentration. Soil and sediment samples are extracted using acetonitrile in an ultrasonic bath, filtered and chromatographed. The detection limits, ranges, and interferences depend on the target compound.

Scope and Application

Trace analysis of explosives and propellant residues in water, soils and sediment by HPLC using a dual wavelength UV detector.

Applicable Concentration Range

Interferences

Solvents, reagents, glassware, and other sample processing hardware may yield artifacts and/or interferences to sample analysis. All these materials must be demonstrated to be free from interferences under the conditions of the analysis by analyzing method blanks. 2,4-DNT and 2,6-DNT elute at similar retention times on C-18 columns using the separation conditions described in this method (retention time difference of 0.2 minutes). A large concentration of one isomer (generally 2,4-DNT) may mask the response of the other isomer. If it is not apparent that both isomers are present (or are not detected), an isomeric mixture should be reported. Tetryl decomposes rapidly in methanol/water solutions, as well as with heat. All aqueous samples expected to contain tetryl should be diluted with acetonitrile prior to filtration and acidified to pH < 3 with aqueous sodium bisulfate. All samples expected to contain tetryl should not be exposed to temperatures above room temperature. Degradation products of tetryl appear as a shoulder on the 2,4,6-TNT peak using the C18 separation. Peak heights rather than peak areas should be used when tetryl is present in concentrations that are significant relative to the concentration of 2,4,6-TNT.

Quality Control Requirements

Any reagent blanks, matrix spikes, or replicate samples should be subjected to exactly the same analytical procedures as those used on actual samples. Refer to Chapter One for specific quality control procedures and Method 3500 for extraction and sample preparation procedures.

Sample Handling

See the introductory material to this chapter, Organic Analytes, Sec 4.1, SW-846

Maximum Holding Time

See introductory material, Organic analytes, Sec. 4.1.

Relative Cost

$201 to $400

Sample Preparation Methods

See intro. material, Sec 4.1, SW-846.

This method has 21 analytes associated with it.

Analyte	Detection Level	Bias	Precision
1,3-Dinitrobenzene(99-65-0) 1,3-Dinitrobenzene 1,3-Dinitrobenzol 2,4-Dinitrobenzene 2,6-Dinitrobenzene Benzene, 1,3-dinitro- Binitrobenzene DNB m-Dinitrobenzene	N/A	102% Rec	6.60 % RSD
2,4,6-Trinitrotoluene(118-96-7) 1-Methyl-2,4,6-trinitrobenzene 2,4,6-Trinitrotoluene Trinitrotoluene Tritol (explosive)	N/A	105% Rec	7.60 % RSD
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-	N/A	101% Rec	5.80 % RSD
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-	N/A	N/A	N/A
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	N/A	102% Rec	9.10 % RSD
3,5-Dinitroaniline(618-87-1) 3,5-Dinitroaniline BRN 0648811 CCRIS 3109 NSC 284	N/A	N/A	N/A
3-Nitrotoluene(99-08-1) 3-Nitrotoluene Benzene, 1-methyl-3-nitro- NSC 9578 Nitrotoluene, all isomers m-Nitrotoluene	N/A	97% Rec	12.40 % RSD
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	N/A	N/A	N/A
4-Nitrotoluene(99-99-0) 1-Methyl-4-nitrobenzene 4-Methylnitrobenzene 4-Nitrotoluene 4-Nitrotoluol Benzene, 1-methyl-4-nitro- p-Methylnitrobenzene p-Nitrotoluene	N/A	96% Rec	18.10
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	N/A	106% Rec	8.70 % RSD
Hexamethylenetriperoxidediamine(283-66-9) HMTD Hexamethylene triperoxide diamine Hexamethylenetriperoxidediamine	N/A	N/A	N/A
Nitramine(479-45-8) 2,4,6,N-Tetranitro-N-methylaniline 2,4,6-Tetryl 2,4,6-Trinitro-N-methyl-N-nitroaniline 2,4,6-Trinitrophenyl-N-methylnitramine 2,4,6-Trinitrophenylmethylnitroamine Aniline, N-methyl-N,2,4,6-tetranitro- (8CI) Benzenamine, N-methyl-N,2,4,6-tetranitro- NSC 2166 Nitramine	N/A	93% Rec	16.40 % RSD
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	N/A	N/A	N/A
Nitroglycerin(55-63-0) 1,2,3-Propanetriol, trinitrate NG Nitroglycerin	N/A	N/A	N/A
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	N/A	106% Rec	10.50 % RSD
Organics, semivolatile(E-12884) Organics, semivolatile Semi-volatile organics Semivolatile organics	N/A	N/A	N/A
Pentaerythritol tetranitrate(78-11-5) 1,3-Dinitrato-2,2-bis(nitratomethyl)propane LX 16 (explosive) PETN Pentaerythritol tetranitrate	N/A	N/A	N/A
Triacetone triperoxide(17088-37-8) Acetone peroxide trimer TATP TCAP Triacetone triperoxide triacetonetriperoxide	N/A	N/A	N/A
Volatile organic compounds(E-12419) Organic compounds, volatile VOCs Volatile organic compounds	N/A	N/A	N/A
o-Nitrotoluene(88-72-2) 2-Nitrotoluene Benzene, 1-methyl-2-nitro- o-Nitrotoluene	N/A	102% Rec	9.10 % RSD
sym-Trinitrobenzene(99-35-4) 1,3,5-Trinitrobenzene Benzene, 1,3,5-trinitro- Benzite TNB sym-Trinitrobenzene	N/A	119% Rec	7.60 % RSD

Precision Descriptor Notes:	20 samples
Detection Level Note:	The detection limits, ranges, and interferences depend on the target compound.

Revision	PDF/Link
Revision 2, October 2006

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EPA-RCA: 8330B: Explosives by HPLC

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