EPA Method 13B Determination Of Total Fluoride Emissions From Stationary Sources (Specific Ion Electrode Method)
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F37B1C30865B42F8BF3B9234C20D240F |
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0.03 |
页数: |
12 |
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日期: |
2000-2-12 |
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874,METHOD 13B - DETERMINATION OF TOTAL FLUORIDE EMISSIONS,FROM STATIONARY SOURCES,(SPECIFIC ION ELECTRODE METHOD),NOTE: This method does not include all of the,specifications (e.g., equipment and supplies) and procedures,(e.g., sampling and analytical) essential to its,performance. Some material is incorporated by reference,from other methods in this part. Therefore, to obtain,reliable results, persons using this method should have a,thorough knowledge of at least the following additional test,methods: Method 1, Method 2, Method 3, Method 5, and,Method 13A.,1.0 Scope and Application.,1.1 Analytes.,Analyte CAS No. Sensitivity,Total fluorides,as Fluorine 7782-41-4 Not determined,1.2 Applicability. This method is applicable for the,determination of fluoride (F-) emissions from sources as,specified in the regulations. It does not measure,fluorocarbons, such as Freons.,1.3 Data Quality Objectives. Adherence to the,requirements of this method will enhance the quality of the,data obtained from air pollutant sampling methods.,875,2.0 Summary.,Gaseous and particulate F- are withdrawn,isokinetically from the source and collected in water and on,a filter. The total F- is then determined by the specific,ion electrode method.,3.0 Definitions. [Reserved],4.0 Interferences.,Grease on sample-exposed surfaces may cause low Fresults,because of adsorption.,5.0 Safety.,5.1 Disclaimer. This method may involve hazardous,materials, operations, and equipment. This test method does,not purport to address all of the safety problems associated,with its use. It is the responsibility of the user of this,test method to establish appropriate safety and health,practices and to determine the applicability of regulatory,limitations prior to performing this test method.,5.2 Corrosive Reagents. The following reagents are,hazardous. Personal protective equipment and safe,procedures are useful in preventing chemical splashes. If,contact occurs, immediately flush with copious amounts of,water at least 15 minutes. Remove clothing under shower and,decontaminate. Treat residual chemical burn as thermal,burn.,876,5.2.1 Sodium Hydroxide (NaOH). Causes severe damage,to eye tissues and to skin. Inhalation causes irritation to,nose, throat, and lungs. Reacts exothermically with limited,amounts of water.,5.2.2 Sulfuric Acid (H2SO4). Rapidly destructive to,body tissue. Will cause third degree burns. Eye damage may,result in blindness. Inhalation may be fatal from spasm of,the larynx, usually within 30 minutes. May cause lung,tissue damage with edema. 1 mg/m3 for 8 hours will cause,lung damage or, in higher concentrations, death. Provide,ventilation to limit inhalation. Reacts violently with,metals and organics.,6.0 Equipment and Supplies.,6.1 Sample Collection and Sample Recovery. Same as,Method 13A, Sections 6.1 and 6.2, respectively.,6.2 Sample Preparation and Analysis. The following,items are required for sample preparation and analysis:,6.2.1 Distillation Apparatus, Bunsen Burner, Electric,Muffle Furnace, Crucibles, Beakers, Volumetric Flasks,Erlenmeyer Flasks or Plastic Bottles, Constant Temperature,Bath, and Balance. Same as Method 13A, Sections 6.3.1 to,6.3.9, respectively.,6.2.2 Fluoride Ion Activity Sensing Electrode.,877,6.2.3 Reference Electrode. Single junction, sleeve,type.,6.2.4 Electrometer. A pH meter with millivolt-scale,capable of ± 0.1-mv resolution, or a specific ion meter made,specifically for specific ion electrode use.,6.2.5 Magnetic Stirrer and Tetrafluoroethylene (TFE),Fluorocarbon-Coated Stirring Bars.,6.2.6 Beakers. Polyethylene, 100-ml.,7.0 Reagents and Standards.,Unless otherwise indicated, all reagents are to,conform to the specifications established by the Committee,on Analytical Reagents of the American Chemical Society,where such specifications are available. Otherwise, use the,best available grade.,7.1 Sample Collection and Sample Recovery. Same as,Method 13A, Sections 7.1 and 7.2, respectively.,7.2 Sample Preparation and Analysis. The following,reagents and standards are required for sample analysis:,7.2.1 Calcium Oxide (CaO). Certified grade,containing 0.005 percent F- or less.,7.2.2 Phenolphthalein Indicator. Dissolve 0.1 g,phenolphthalein in a mixture of 50 ml of 90 percent ethanol,and 50 ml water.,7.2.3 Sodium Hydroxide (NaOH), Pellets.,878,7.2.4 Sulfuric Acid (H2SO4), Concentrated.,7.2.5 Filters. Whatman No. 541, or equivalent.,7.2.6 Water. Same as Section 7.1.2 of Method 13A.,7.2.7 Sodium Hydroxide, 5 M. Dissolve 20 g of NaOH,in 100 ml of water.,7.2.8 Sulfuric Acid, 25 Percent (v/v). Mix 1 part of,concentrated H2SO4 with 3 parts of water.,7.2.9 Total Ionic Strength Adjustment Buff……
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