EPA Method 8330B

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EPA Method 8330B:
Explosives by HPLC. Official Name: Nitroaromatics, Nitramines, and Nitrate Esters by High Performance Liquid Chromatography (HPLC)

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

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

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.

QC 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.

Maximum Holding Time:
See introductory material, Organic analytes, Sec. 4.1.

Media:
VARIOUS

Subcategory:
Organic

Sample Prep:
See intro. material, Sec 4.1, SW-846.

Precision:
20 samples

Detection:
The detection limits, ranges, and interferences depend on the target compound.

Revision Number:
Revision 2, October 2006