EPA Method 16 Semicontinuous Determination Of Sulfur Emissions From Stationary Sources
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ID： |
A15FF73742BB4715A6378C6D7100F5DA |
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文件大小(MB)： |
0.06 |
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页数： |
18 |
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文件格式： |
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日期： |
2000-2-12 |
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文本摘录（文本识别可能有误，但文件阅览显示及打印正常，pdf文件可进行文字搜索定位）：
966,METHOD 16 - SEMICONTINUOUS DETERMINATION OF 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,thorough knowledge of at least the following additional test,methods: Method 1, Method 4, Method 15, and Method 16A.,1.0 Scope and Application.,1.1 Analytes.,Analyte CAS No. Sensitivity,Dimethyl disulfide,[(CH3)2S2],62-49-20 50 ppb,Dimethyl sulfide,[(CH3)2S],75-18-3 50 ppb,Hydrogen sulfide,[H2S],7783-06-4 50 ppb,Methyl mercaptan,[CH4S],74-93-1 50 ppb,1.2 Applicability. This method is applicable for the,determination of total reduced sulfur (TRS) compounds from,recovery furnaces, lime kilns, and smelt dissolving tanks at,kraft pulp mills and fuel gas combustion devices at,petroleum refineries.,967,NOTE: The method described below uses the principle,of gas chromatographic (GC) separation and flame photometric,detection (FPD). Since there are many systems or sets of,operating conditions that represent useable methods of,determining sulfur emissions, all systems which employ this,principle, but differ only in details of equipment and,operation, may be used as alternative methods, provided that,the calibration precision and sample line loss criteria are,met.,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 A gas sample is extracted from the emission,source and an aliquot is analyzed for hydrogen sulfide,(H2S), methyl mercaptan (MeSH), dimethyl sulfide (DMS), and,dimethyl disulfide (DMDS) by GC/FPD. These four compounds,are known collectively as TRS.,3.0 Definitions. [Reserved],4.0 Interferences.,4.1 Moisture. Moisture condensation in the sample,delivery system, the analytical column, or the FPD burner,block can cause losses or interferences. This is prevented,by maintaining the probe, filter box, and connections at a,968,temperature of at least 120 EC (248 EF). Moisture is,removed in the SO2 scrubber and heating the sample beyond,this point is not necessary when the ambient temperature is,above 0 EC (32 EF). Alternatively, moisture may be,eliminated by heating the sample line, and by conditioning,the sample with dry dilution air to lower its dew point,below the operating temperature of the GC/FPD analytical,system prior to analysis.,4.2 Carbon Monoxide (CO) and Carbon Dioxide (CO2).,CO and CO2 have a substantial desensitizing effect on the,flame photometric detector even after dilution. Acceptable,systems must demonstrate that they have eliminated this,interference by some procedure such as eluting these,compounds before any of the compounds to be measured.,Compliance with this requirement can be demonstrated by,submitting chromatograms of calibration gases with and,without CO2 in the 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 10.2.,4.3 Particulate Matter. Particulate matter in gas,samples can cause interference by eventual clogging of the,analytical system. This interference is eliminated by using,the Teflon filter after the probe.,969,4.4 Sulfur Dioxide (SO2). Sulfur dioxide is not a,specific interferant but may be present in such large,amounts that it cannot effectively be separated from the,other compounds of interest. The SO2 scrubber described in,Section 6.1.3 will effectively remove SO2 from the sample.,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. 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.,6.1. Sample Collection. The following items are,needed for sample collection.,6.1.1 Probe. Teflon or Teflon-lined stainless steel.,The probe must be heated to preven……
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