EPA Method 105 Determination Of Mercury In Wastewater Treatment Plant Sewage Sludges
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FD33BAC8E4E14CE88F1152C252978066 |
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0.03 |
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11 |
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日期: |
2000-2-12 |
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1796,METHOD 105 - DETERMINATION OF MERCURY IN,WASTEWATER TREATMENT PLANT SEWAGE SLUDGES,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 also have,a thorough knowledge of at least the following additional,test methods: Method 101 and Method 101A.,1.0 Scope and Application.,1.1 Analytes.,Analyte CAS No. Sensitivity,Mercury (Hg) 7439-97-6 Dependent upon,spectrophotometer and recorder,1.2 Applicability. This method is applicable for the,determination of total organic and inorganic Hg content in,sewage sludges.,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of the,data obtained from air pollutant sampling methods.,2.0 Summary of Method.,2.1 Time-composite sludge samples are withdrawn from,the conveyor belt subsequent to dewatering and before,incineration or drying. A weighed portion of the sludge is,1797,digested in aqua regia and is oxidized by potassium,permanganate (KMnO4). Mercury in the digested sample is,then measured by the conventional spectrophotometric coldvapor,technique.,3.0 Definitions. [Reserved],4.0 Interferences. [Reserved],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 at least 15 minutes. Remove clothing under shower and,decontaminate. Treat residual chemical burn as thermal,burn.,5.2.1 Hydrochloric Acid (HCl). Highly toxic. Vapors,are highly irritating to eyes, skin, nose, and lungs,causing severe damage. May cause bronchitis, pneumonia, or,1798,edema of lungs. Exposure to concentrations of 0.13 to 0.2,percent can be lethal to humans in a few minutes. Provide,ventilation to limit exposure. Reacts with metals,producing hydrogen gas.,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 and Mixing. The following,items are required for collection and mixing of the sludge,samples:,6.1.1 Container. Plastic, 50-liter.,6.1.2 Scoop. To remove 950-ml (1 quart.) sludge,sample.,6.1.3 Mixer. Mortar mixer, wheelbarrow-type, 57,liter (or equivalent) with electricity-driven motor.,6.1.4 Blender. Waring-type, 2-liter.,6.1.5 Scoop. To remove 100-ml and 20-ml samples of,blended sludge.,6.1.6 Erlenmeyer Flasks. Four, 125-ml.,1799,6.1.7 Beakers. Glass beakers in the following sizes:,50 ml (1), 200 ml (1), 400 ml (2).,6.2 Sample Preparation and Analysis. Same as Method,101, Section 6.3, with the addition of the following:,6.2.1 Hot Plate.,6.2.2 Desiccator.,6.2.3 Filter Paper. S and S No. 588 (or equivalent).,6.2.4 Beakers. Glass beakers, 200 ml and 400 ml (2,each).,7.0 Reagents and Standards.,NOTE: Unless otherwise indicated, it is intended that,all reagents conform to the specifications established by,the Committee on Analytical Reagents of the American,Chemical Society, where such specifications are available;,otherwise, use the best available grade.,7.1 Sample Analysis. Same as Method 101A, Section,7.2, with the following additions and exceptions:,7.1.1 Hydrochloric Acid. The concentrated HCl,specified in Method 101A, Section 7.2.4, is not required.,7.1.2 Aqua Regia. Prepare immediately before use.,Carefully add one volume of concentrated HNO3 to three,volumes of concentrated HCl.,8.0 Sample Collection, Preservation, Storage, and,Transport.,1800,8.1 Sludge Sampling. Withdraw equal volume,increments of sludge [for a total of at least 15 liters (16,quarts)] at intervals of 30 min over an 8-hr period, and,combine in a rigid plastic container.,8.2 Sludge Mixing. Transfer the entire 15-liter,sample to a mortar mixer. Mix the sample for a minimum of,30 min at 30 rpm. Take six 100-ml portions……
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