EPA Method 13A Determination Of Total Fluoride Emissions From Stationary Sources (Spadns Zirconium Lake Method)

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24908C6093E64ECFAEDF1E0364C352AF

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0.24

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30

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日期:

2000-2-12

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844,METHOD 13A - DETERMINATION OF TOTAL FLUORIDE EMISSIONS,FROM STATIONARY SOURCES,(SPADNS ZIRCONIUM LAKE 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, and Method 5.,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the quality of the,data obtained from air pollutant sampling methods.,2.0 Summary.,Gaseous and particulate F- are withdrawn,isokinetically from the source and collected in water and on,845,a filter. The total F- is then determined by the SPADNS,Zirconium Lake Colorimetric method.,3.0 Definitions. [Reserved],4.0 Interferences.,4.1 Chloride. Large quantities of chloride will,interfere with the analysis, but this interference can be,prevented by adding silver sulfate into the distillation,flask (see Section 11.3). If chloride ion is present, it,may be easier to use the specific ion electrode method of,analysis (Method 13B).,4.2 Grease. Grease on sample-exposed surfaces may,cause low F- results due to adsorption.,5.0 Safety.,5.1 Disclaimer. This method may involve hazardous,materials, operations, and equipment. This test method may,not 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,846,water at least 15 minutes. Remove clothing under shower and,decontaminate. Treat residual chemical burn as thermal,burn.,5.2.1 Hydrochloric Acid (HCl). Highly toxic. Vapors,are highly irritating to eyes, skin, nose, and lungs,causing severe damage. May cause bronchitis, pneumonia, or,edema of lungs. Exposure to concentrations of 0.13 to 0.2,percent can be lethal in minutes. Will react with metals,producing hydrogen.,5.2.2 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.,5.2.3 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. A schematic of the sampling,train used in performing this method is shown in Figure,847,13A-1; it is similar to the Method 5 sampling train except,that the filter position is interchangeable. The sampling,train consists of the following components:,6.1.1 Probe Nozzle, Pitot Tube, Differential Pressure,Gauge, Filter Heating System, Temperature Sensor, Metering,System, Barometer, and Gas Density Determination Equipment.,Same as Method 5, Sections 6.1.1.1, 6.1.1.3 through 6.1.1.7,6.1.1.9, 6.1.2, and 6.1.3, respectively. The filter heating,system and temperature sensor are needed only when moisture,condensation is a problem.,6.1.2 Probe Liner. Borosilicate glass or 316,stainless steel. When the filter is located immediately,after the probe, a probe heating system may be used to,prevent filter plugging resulting from moisture,condensation, but the temperature in the probe shall not be,allowed to exceed 120 ± 14 EC (248 ± 25 EF).,6.1.3 Filter Holder. With positive seal against,leakage from the outside or around the filter. If the,filter is located between the probe and first impinger, use,borosilicate glass or stainless steel with a 20-mesh,stainless steel screen filter support and a silicone rubber,gasket; do not use a glass frit or a sintered metal filter,support. If the filter is l……

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