EPA Method 15A Determination Of Total Reduced Sulfur Emissions From Sulfur Recovery Plants In Petroleum Refineries

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FE2B7F29878742FB82A5B15C2975D613

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日期:

2000-2-12

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943,METHOD 15A - DETERMINATION OF TOTAL REDUCED SULFUR EMISSIONS,FROM SULFUR RECOVERY PLANTS,IN PETROLEUM REFINERIES,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 6, Method 15, and Method 16A.,1.0 Scope and Application.,1.1 Analytes.,Analyte CAS No. Sensitivity,Reduced sulfur compounds None assigned Not determined,1.2 Applicability. This method is applicable for the,determination of emissions of reduced sulfur compounds from,sulfur recovery plants where the emissions are in a reducing,atmosphere, such as in Stretford units.,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.,944,2.0 Summary of Method.,2.1 An integrated gas sample is extracted from the,stack, and combustion air is added to the oxygen,(O2)-deficient gas at a known rate. The reduced sulfur,compounds [including carbon disulfide (CS2), carbonyl,sulfide (COS), and hydrogen sulfide (H2S)] are thermally,oxidized to sulfur dioxide (SO2), which is then collected in,hydrogen peroxide as sulfate ion and analyzed according to,the Method 6 barium-thorin titration procedure.,3.0 Definitions. [Reserved],4.0 Interferences.,4.1 Reduced sulfur compounds, other than CS2, COS,and H2S, that are present in the emissions will also be,oxidized to SO2, causing a positive bias relative to,emission standards that limit only the three compounds,listed above. For example, thiophene has been identified in,emissions from a Stretford unit and produced a positive bias,of 30 percent in the Method 15A result. However, these,biases may not affect the outcome of the test at units where,emissions are low relative to the standard.,4.2 Calcium and aluminum have been shown to interfere,in the Method 6 titration procedure. Since these metals,have been identified in particulate matter emissions from,945,Stretford units, a Teflon filter is required to minimize,this interference.,4.3 Dilution of the hydrogen peroxide (H2O2) absorbing,solution can potentially reduce collection efficiency,causing a negative bias. When used to sample emissions,containing 7 percent moisture or less, the midget impingers,have sufficient volume to contain the condensate collected,during sampling. Dilution of the H2O2 does not affect the,collection of SO2. At higher moisture contents, the,potassium citrate-citric acid buffer system used with Method,16A should be used to collect the condensate.,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 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 for at least 15 minutes. Remove clothing under shower,946,and decontaminate. Treat residual chemical burns as thermal,burns.,5.2.1 Hydrogen Peroxide (H2O2). Irritating to eyes,skin, nose, and lungs.,5.2.2 Sodium Hydroxide (NaOH). Causes severe damage,to eyes and 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. 3 mg/m3 will cause lung damage in,uninitiated. 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. The sampling train used in,performing this method is shown in Figure 15A-1, and,component parts are discussed below. Modifications to this,sampling train are acceptable provided that the system,performance check is met.,947,6.1.1 Probe. 6.4-mm (?-in.) OD Teflon tubing,sequentially wrapped with heat-resistant fiber strips, a,rubberized heating tape (wit……

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