EPA Method 12 Determination Of Inorganic Lead Emissions From Stationary Sources

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4C1138317942414991DBBA3B3C005CB9

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日期:

2000-2-12

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816,METHOD 12 - DETERMINATION OF INORGANIC LEAD,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 2, Method 3, and Method 5.,1.0 Scope and Application.,1.1 Analytes.,Analyte CAS No. Sensitivity,Inorganic Lead Compounds,as lead (Pb) 7439-92-1,see Section,13.3,1.2 Applicability. This method is applicable for the,determination of inorganic lead emissions from stationary,sources, only as specified in an applicable subpart of the,regulations.,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obtained from air pollutant sampling methods.,2.0 Summary of Method.,2.1 Particulate and gaseous Pb emissions are,withdrawn isokinetically from the source and are collected,817,on a filter and in dilute nitric acid. The collected,samples are digested in acid solution and are analyzed by,atomic absorption spectrophotometry using an air/acetylene,flame.,3.0 Definitions. [Reserved],4.0 Interferences.,4.1 Copper. High concentrations of copper may,interfere with the analysis of Pb at 217.0 nm. This,interference can be avoided by analyzing the samples at,283.3 nm.,4.2 Matrix Effects. Analysis for Pb by flame atomic,absorption spectrophotometry is sensitive to the chemical,composition and to the physical properties (e.g., viscosity,pH) of the sample. The analytical procedure requires the,use of the Method of Standard Additions to check for these,matrix effects, and requires sample analysis using the,Method of Standard Additions if significant matrix effects,are found to be present.,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,818,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 Hydrogen Peroxide (H2O2). Irritating to eyes,skin, nose, and lungs.,5.2.2 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.,6.0 Equipment and Supplies.,6.1 Sample Collection. A schematic of the sampling,train used in performing this method is shown in Figure 12-1,in Section 18.0; it is similar to the Method 5 train. The,following items are needed for sample collection:,6.1.1 Probe Nozzle, Probe Liner, Pitot Tube,Differential Pressure Gauge, Filter Holder, Filter Heating,819,System, Temperature Sensor, Metering System, Barometer, and,Gas Density Determination Equipment. Same as Method 5,Sections 6.1.1.1 through 6.1.1.7, 6.1.1.9, 6.1.2, and 6.1.3,respectively.,6.1.2 Impingers. Four impingers connected in series,with leak-free ground glass fittings or any similar leakfree,noncontaminating fittings are needed. For the first,third, and fourth impingers, use the Greenburg-Smith design,modified by replacing the tip with a 1.3 cm (1/2 in.) ID,glass tube extending to about 1.3 cm (1/2 in.) from the,bottom of the flask. For the second impinger, use the,Greenburg-Smith design with the standard tip.,6.1.3 Temperature Sensor. Place a temperature,sensor, capable of measuring temperature to within 1EC (2EF),at the outlet of the fourth impinger for monitoring,purposes.,6.2 Sample Recovery. The following items are needed,for sample recovery:,6.2.1 Probe-Liner and Probe-Nozzle Brushes, Petri,Dishes, Graduated Cylinder and/or Balance, Plastic Storage,Containers, and Funnel and Rubber Policeman. Same as Method,5, Sections 6.2.1 and 6.2.4 through 6.2.7, respectively.,6.2.2 Wash Bottles. Glass (2).,6.2.3 Sample Storage Containers. Chemically,resistant, borosilicate glass bottles, for 0.1 N nitric ……

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