EPA Method 16B Determination Of Total Reduced Sulfur Emissions From Stationary Sources
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ECEEAAD70BC04ED598C90280730079C0 |
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0.05 |
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12 |
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日期: |
2000-2-12 |
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1023,METHOD 16B - DETERMINATION OF TOTAL REDUCED SULFUR,EMISSIONS FROM STATIONARY SOURCES,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,knowledge of at least the following additional test methods:,Method 6C, Method 16, and Method 16A.,1.0 Scope and Application.,1.1 Analytes.,Analyte CAS No.,Total reduced sulfur (TRS),including:,Dimethyl disulfide (DMDS),[(CH3)2S2],Dimethyl sulfide (DMS), [(CH3)2S],Hydrogen sulfide (H2S),Methyl mercaptan (MeSH), [CH4S],N/A,62-49-20,75-18-3,7783-06-4,74-93-1,Reported as:,Sulfur dioxide (SO2) 7449-09-5,1.2 Applicability. This method is applicable for,determining TRS emissions from recovery furnaces (boilers),lime kilns, and smelt dissolving tanks at kraft pulp mills,and from other sources when specified in an applicable,subpart of the regulations. The flue gas must contain at,1024,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. The SO2 is removed selectively from the sample using,a citrate buffer solution. The TRS compounds are then,thermally oxidized to SO2 and analyzed as SO2 by gas,chromatography (GC) using flame photometric detection (FPD).,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,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,before oxidation. Proper use of the particulate filter,1025,described in Section 6.1.3 of Method 16A, will eliminate,this interference.,4.3 Carbon monoxide (CO) and carbon dioxide (CO2),have substantial desensitizing effects on the FPD even after,dilution. Acceptable systems must demonstrate that they,have eliminated this interference by some procedure such as,eluting these compounds before the SO2. Compliance with,this requirement can be demonstrated by submitting,chromatograms of calibration gases with and without CO2 in,diluent gas. The CO2 level should be approximately 10,percent for the case with CO2 present. The two,chromatograms should show agreement within the precision,limits of Section 13.0.,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 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,1026,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.,6.1 Sample Collection. The sampling train is shown in,Figure 16B-1. Modifications to the apparatus are accepted,provided the system performance check in Section 8.4.1 is,met.,6.1.1 Probe, Probe Brush, Particulate Filter, SO2,Scrubber, Combustion Tube, and Furnace. Same as in Method,16A, Sections 6.1.1 to 6.1.6.,6.1.2 Sampling Pump. Leakless Teflon-coated diaphragm,type or equivalent.,6.2 Analysis.,6.2.1 Dilution System (optional), Gas Chromatograph,Oven, Temperature Gauges, Flow System, Flame Photometric,Detector, Electrometer, Power Supply, Recorder, Calibration,System, Tube Chamber, Flow System, and Constant Temperature,Bath. Same as in Method 16, Sections 6.2.1, 6.2.2, and 6.3.,6.2.2 Gas Chromatograph Columns. Same as in Method,16, Section 6.2.3. Other columns with demonstrated ability,to resolve SO2 and be free from known interferences are,acceptable alternatives. Single column systems such as a,1027,7-ft Carbsorb B HT 100 column have been found satisfactory,in resolving SO2 from CO2.,7.0 Reagent……
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