EPA Method 16A Determination Of Total Reduced Sulfur Emissions From Stationary Sources (Impinger Technique)

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9DF99ECB82914C8CB61BE396D33B3566

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日期:

2000-2-12

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983,METHOD 16A - DETERMINATION OF TOTAL REDUCED SULFUR EMISSIONS,FROM STATIONARY SOURCES (IMPINGER TECHNIQUE),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, and Method 16.,1.0 Scope and Application.,1.1 Analytes.,Analyte CAS No. Sensitivity,Total reduced sulfur (TRS),including:,Dimethyl disulfide,[(CH3)2S2],Dimethyl sulfide,[(CH3)2S],Hydrogen sulfide,[H2S],Methyl mercaptan,[CH4S],N/A,62-49-20,75-18-3,7783-06-4,74-93-1,See,Section 13.1,Reduced sulfur (RS),including,H2S,Carbonyl sulfide,[COS],Carbon disulfide,[CS2],Reported as:,Sulfur dioxide (SO2),N/A,7783-06-4,463-58-1,75-15-0,7449-09-5,984,1.2 Applicability. This method is applicable for,the determination of TRS emissions from recovery boilers,lime kilns, and smelt dissolving tanks at kraft pulp mills,reduced sulfur compounds (H2S, carbonyl sulfide, and carbon,disulfide from sulfur recovery units at onshore natural gas,processing facilities, and from other sources when specified,in an applicable subpart of the regulations. The flue gas,must contain at least 1 percent oxygen for complete,oxidation of all TRS to SO2.,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 of Method.,2.1 An integrated gas sample is extracted from the,stack. SO2 is removed selectively from the sample using a,citrate buffer solution. TRS compounds are then thermally,oxidized to SO2, collected in hydrogen peroxide as sulfate,and analyzed by the Method 6 barium-thorin titration,procedure.,3.0 Definitions. [Reserved],4.0 Interferences.,4.1 Reduced sulfur compounds other than those,regulated by the emission standards, if present, may be,measured by this method. Therefore, carbonyl sulfide, which,985,is partially oxidized to SO2 and may be present in a lime,kiln exit stack, would be a positive interferant.,4.2 Particulate matter from the lime kiln stack gas,(primarily calcium carbonate) can cause a negative bias if,it is allowed to enter the citrate scrubber; the particulate,matter will cause the pH to rise and H2S to be absorbed,prior to oxidation. Furthermore, if the calcium carbonate,enters the hydrogen peroxide impingers, the calcium will,precipitate sulfate ion. Proper use of the particulate,filter described in Section 6.1.3 will eliminate this,interference.,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,986,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.,5.3 Hydrogen Sulfide (H2S). A flammable, poisonous,gas with the odor of rotten eggs. H2S is extremely,hazardous and can cause collapse, coma, and death within a,few seconds of one or two inhalations at sufficient,concentrations. Low concentrations irritate the mucous,membranes and may cause nausea, dizziness, and headache,after exposure.,6.0 Equipment and Supplies.,987,6.1 Sample Collection. The sampling train is shown,in Figure 16A-1 and component parts are discussed below.,Modifications to this……

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