EPA Method 8331 Tetrazene by Reverse Phase High Performance Liquid Chromatography (HPLC) - Revision 0
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40D31222B7404A4C8B8CD996A8E30080 |
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0.08 |
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页数： |
11 |
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日期： |
2003-1-16 |
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CD-ROM 8331 - 1 Revision 0,September 1994,METHOD 8331,TETRAZENE BY REVERSE PHASE,HIGH PERFORMANCE LIQUID CHROMATOGRAPHY (HPLC),1.0 SCOPE AND APPLICATION,1.1 This method is intended for the analysis of tetrazene, an explosive,residue, in soil and water. This method is limited to use by analysts,experienced in handling and analyzing explosive materials. The following,compounds can be determined by this method:,___________________________________________________________________________,Compound CAS Noa,___________________________________________________________________________,Tetrazene 31330-63-9,___________________________________________________________________________,a Chemical Abstracts Service Registry number,1.2 Tetrazene degrades rapidly in water and methanol at room temperature.,Special care must be taken to refrigerate or cool all solutions throughout the,analytical process.,1.3 Tetrazene, in its dry form, is extremely explosive. Caution must be,taken during preparation of standards.,1.4 The estimated quantitation limit (EQL) of Method 8331 for determining,the concentration of tetrazene is approximately 7 μg/L in water and approximately,1 mg/kg in soil.,1.5 This method is restricted to use by or under the supervision of,analysts experienced in the use of HPLC, skilled in the interpretation of,chromatograms, and experienced in handling explosive materials. Each analyst,must demonstrate the ability to generate acceptable results with this method.,2.0 SUMMARY OF METHOD,2.1 A 10 mL water sample is filtered, eluted on a C-18 column using ion,pairing reverse phase HPLC, and quantitated at 280 nm.,2.2 2 g of soil are extracted with 55:45 v/v methanol-water and,1-decanesulfonic acid on a platform shaker, filtered, and eluted on a C-18 column,using ion pairing reverse phase HPLC, and quantitated at 280 nm.,CD-ROM 8331 - 2 Revision 0,September 1994,3.0 INTERFERENCES,3.1 No interferences are known. Tetrazene elutes early, however, and if,a computing integrator is used for peak quantification, the baseline setting may,have to be set to exclude baseline aberrations. Baseline setting is particularly,important at low concentrations of analyte.,4.0 APPARATUS AND MATERIALS,4.1 HPLC system,4.1.1 HPLC - Pump capable of achieving 4000 psi.,4.1.2 100 μL loop injector.,4.1.3 Variable or fixed wavelength detector capable of reading,280 nm.,4.1.4 C-18 reverse phase HPLC column, 25 cm x 4.6 mm (5 μm),(Supelco LC-18, or equivalent).,4.1.5 Digital integrator - HP 3390A (or equivalent),4.1.6 Strip chart recorder.,4.2 Other apparatus,4.2.1 Platform orbital shaker.,4.2.2 Analytical balance - + 0.0001 g.,4.2.3 Desiccator.,4.3 Materials,4.3.1 Injection syringe - 500 μL.,4.3.2 Filters - 0.5 μm Millex-SR and 0.5 μm Millex-HV, disposable,or equivalent.,4.3.3 Pipets - volumetric, glass, Class A.,4.3.4 Scintillation vials - 20 mL, glass.,4.3.5 Syringes - 10 mL.,4.3.6 Volumetric flasks, Class A - 100 mL, 200 mL.,4.3.7 Erlenmeyer flasks with ground glass stoppers - 125 mL.,CD-ROM 8331 - 3 Revision 0,September 1994,4.4 Preparation,4.4.1 Prepare all materials as described in Chapter 4 for volatile,organics.,5.0 REAGENTS,5.1 HPLC grade chemicals shall be used in all tests. It is intended that,all reagents shall conform to the specifications of the Committee on Analytical,Reagents of the American Chemical Society, where such specifications are,available. Other grades may be used, provided it is first ascertained that the,reagent is of sufficiently high purity to permit its use without lowering the,accuracy of the determination.,5.2 General,5.2.1 Methanol, CH3OH - HPLC grade.,5.2.2 Organic-free reagent water - All references to water in this,method refer to organic-free reagent water, as defined in Chapter One.,5.2.3 1-Decanesulfonic acid, sodium salt, C10H21SO3Na - HPLC grade.,5.2.4 Acetic acid (glacial), CH3COOH - reagent grade.,5.3 Standard Solutions,5.3.1 Tetrazene - Standard Analytical Reference Material.,5.3.2 Stock standard solution - Dry tetrazene to constant weight,in a vacuum desiccator in the dark. (Tetrazene is extremely explosive in,the dry state. Do not dry more reagent than is necessary to prepare stock,solutions.) Place about 0.0010 g (weighed to 0.0001 g) into a 100-ml,volumetric flask and dilute to volume with methanol. Invert flask several,times until tetrazene is dissolved. Store in freezer at -10EC. Stock,solution is about 100 mg/L. Replace stock standard solution every week.,5.3.3 Intermediate standard solutions,5.3.3.1 Prepare a 4 mg/L standard by diluting the stock,solution 1/25 v/v with methanol.,5.3.3.2 Pipet 0.5, 1.0, 2.0, 5.0, 10.0, and 20.0 mL of the,4 mg/L standard solution into ……
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