EPA Method 29 Determination Of Metals Emissions From Stationary Sources

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2011-5-20

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1461,METHOD 29 - DETERMINATION OF METALS 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 5 and Method 12.,1.0 Scope and Application.,1.1 Analytes.,Analyte CAS No.,Antimony (Sb) 7440-36-0,Arsenic (As) 7440-38-2,Barium (Ba) 7440-39-3,Beryllium (Be) 7440-41-7,Cadmium (Cd) 7440-43-9,Chromium (Cr) 7440-47-3,Cobalt (Co) 7440-48-4,Copper (Cu) 7440-50-8,Lead (Pb) 7439-92-1,Manganese (Mn) 7439-96-5,Mercury (Hg) 7439-97-6,Nickel (Ni) 7440-02-0,Phosphorus (P) 7723-14-0,Selenium (Se) 7782-49-2,Silver (Ag) 7440-22-4,1462,Analyte CAS No.,Thallium (Tl) 7440-28-0,Zinc (Zn) 7440-66-6,1.2 Applicability. This method is applicable to the,determination of metals emissions from stationary sources.,This method may be used to determine particulate emissions,in addition to the metals emissions if the prescribed,procedures and precautions are followed.,1.2.1 Hg emissions can be measured, alternatively,using EPA Method 101A of Appendix B, 40 CFR Part 61. Method,101-A measures only Hg but it can be of special interest to,sources which need to measure both Hg and Mn emissions.,2.0 Summary of Method.,2.1 Principle. A stack sample is withdrawn,isokinetically from the source, particulate emissions are,collected in the probe and on a heated filter, and gaseous,emissions are then collected in an aqueous acidic solution,of hydrogen peroxide (analyzed for all metals including Hg),and an aqueous acidic solution of potassium permanganate,(analyzed only for Hg). The recovered samples are digested,and appropriate fractions are analyzed for Hg by cold vapor,atomic absorption spectroscopy (CVAAS) and for Sb, As, Ba,Be, Cd, Cr, Co, Cu, Pb, Mn, Ni, P, Se, Ag, Tl, and Zn by,inductively coupled argon plasma emission spectroscopy,1463,(ICAP) or atomic absorption spectroscopy (AAS). Graphite,furnace atomic absorption spectroscopy (GFAAS) is used for,analysis of Sb, As, Cd, Co, Pb, Se, and Tl if these elements,require greater analytical sensitivity than can be obtained,by ICAP. If one so chooses, AAS may be used for analysis of,all listed metals if the resulting in-stack method detection,limits meet the goal of the testing program. Similarly,inductively coupled plasma-mass spectroscopy (ICP-MS) may be,used for analysis of Sb, As, Ba, Be, Cd, Cr, Co, Cu, Pb, Mn,Ni, Ag, Tl and Zn.,3.0 Definitions. [Reserved],4.0 Interferences.,4.1 Iron (Fe) can be a spectral interference during,the analysis of As, Cr, and Cd by ICAP. Aluminum (Al) can,be a spectral interference during the analysis of As and Pb,by ICAP. Generally, these interferences can be reduced by,diluting the analytical sample, but such dilution raises the,in-stack detection limits. Background and overlap,corrections may be used to adjust for spectral,interferences. Refer to Method 6010 of Reference 2 in,Section 16.0 or the other analytical methods used for,details on potential interferences to this method. For all,GFAAS analyses, use matrix modifiers to limit interferences,and matrix match all standards.,1464,5.0 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,water at least 15 minutes. Remove clothing under shower and,decontaminate. Treat residual chemical burn as thermal,burn.,5.2.1 Nitric Acid (HNO3). Highly corrosive to eyes,skin, nose, and lungs. Vapors cause bronchitis, pneumonia,or edema of lungs. Reaction to inhalation may be delayed as,long as 30 hours and still be fatal. Provide ventilation to,limit exposure. Strong oxidizer. Hazardous reaction may,occur with organic materials such as solvents.,5.2.2 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,1465,the larynx, usually within 30 minutes. May cause lung,tissue damage……

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