1、Designation: D 4874 95 (Reapproved 2006)Standard Test Method forLeaching Solid Material in a Column Apparatus1This standard is issued under the fixed designation D 4874; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of l
2、ast revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method is a standard laboratory procedure forgenerating aqueous leachate from materials using a columnappara
3、tus. It provides a leachate suitable for organic analysis ofsemivolatile and nonvolatile compounds as well as inorganicanalyses.1.2 The column apparatus is designed and constructed ofmaterials chosen to enhance the leaching of low concentrationsof semivolatile and nonvolatile organic constituents as
4、 well asto maximize the leaching of metallic species from the solid.Analysis of column effluent provides information on theleaching characteristics of material under the conditions usedin the test.1.3 This test method provides for the passage of an aqueousfluid through materials of known mass in a s
5、aturated up-flowmode.1.4 It is intended that the sample used in the procedure bephysically, chemically, and biologically representative of thematerial.1.5 This test method does not produce results that can beused as the sole basis for (1) engineering design of a disposalsite, or (2) the characteriza
6、tion of wastes based on theirleaching characteristics.1.6 This test method has the following limitations:1.6.1 Maximum particle size is 10 mm (0.4 in.). Particle sizereduction is not recommended. Large-diameter material (cin-ders, rocks, and so forth) should be removed prior to packingthe column to
7、ensure adequate compaction.1.6.2 Test materials containing densely immiscible organicmaterial may result in phase separation and lead to columnplugging.1.6.3 This test method does not differentiate between dis-solved constituents and sub-70-m particulates that passthrough the pores of the end plates
8、.1.6.4 This test method is not applicable to the leachabilitycharacterization of materials with regard to volatile com-pounds.1.6.5 This test method is not applicable to the characteriza-tion of materials that dissolve in water to a degree thatsignificantly impacts the void volume in the column or t
9、hedetermination of the specific gravity of the material.1.7 Application of this test method to materials with initiallow permeability, or to those that lose permeability over thecourse of the test, may result in long testing periods.1.8 The values stated in SI units are to be regarded as thestandard
10、. The values given in parentheses are in approximateinch-pound equivalents.1.9 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determin
11、e the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2C 819 Test Method for Specific Surface Area of Carbon orGraphite3D 422 Test Method for Particle-Size Analysis of SoilsD 698 Test Methods for Laboratory Compaction Character-istics of Soil Using Sta
12、ndard Effort (12,400 ft-lbf/ft3(600kN-m/m3)D 854 Test Methods for Specific Gravity of Soil Solids byWater PycnometerD 1125 Test Methods for Electrical Conductivity and Re-sistivity of WaterD 1129 Terminology Relating to WaterD 1293 Test Methods for pH of WaterD 1498 Practice for Oxidation-Reduction
13、Potential of WaterD 1888 Methods of Test for Particulate and DissolvedMatter in Water3D 2216 Test Methods for Laboratory Determination of Wa-ter (Moisture) Content of Soil and Rock by MassD 2434 Test Method for Permeability of Granular Soils(Constant Head)D 3370 Practices for Sampling Water from Clo
14、sed ConduitsD 3694 Practices for Preparation of Sample Containers andfor Preservation of Organic ConstituentsD 4253 Test Methods for Maximum Index Density and Unit1This test method is under the jurisdiction of ASTM Committee D34 on WasteManagement and is the direct responsibility of Subcommittee D34
15、.01.04 on WasteLeaching Techniques.Current edition approved May 1, 2006. Published May 2006. Originallyapproved in 1989. Last previous edition approved in 2001 as D 4874 95(2001).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org.
16、 For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Withdrawn.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.Weight of Soils Using a Vibratory TableE 691 Practice fo
17、r Conducting an Interlaboratory Study toDetermine the Precision of a Test Method3. Terminology3.1 Definition:3.1.1 reagent wateras defined in SW-846, Method 1311,5.2.43.1.2 void volumethe volume between the solid particlesin a bed of granular material. Also called the interstitialvolume.3.2 Several
18、terms used in this test method are defined inTerminology D 1129.4. Significance and Use4.1 This test method is intended to provide an aqueousleaching of a material in a dynamic partitioning manner.4.2 Specific operating conditions for the column can beselected to satisfy the objectives of individual
19、 studies. Anunderstanding of the fundamental principles governing columnleaching is necessary in the selection of appropriate conditions.References (1-3)5provide useful information on these prin-ciples.4.3 The column apparatus is constructed of materials thatpermit the generation of a leachate which
20、 is suitable for lowconcentration organic analysis for semivolatile and nonvolatilecompounds as well as inorganic species.5. Apparatus (See Fig. 1)5.1 Columns:5.1.1 The column body is constructed of glass pipe, 300 mm(12 in.) in length, with an inside diameter of 100 mm (4 in.).The cylinder wall mus
21、t be of sufficient thickness, approxi-mately 6 mm (14 in.), to withstand the operating pressure.4SW-846, 3rd ed., Method 1311, Available from USEPA, Office of Solid Wasteand Emergency Response, Washington, DC 20460.5The boldface numbers in parentheses refer to the list of references at the end ofthi
22、s standard.FIG. 1 Column ApparatusD 4874 95 (2006)25.1.2 End plates are constructed of stainless steel. They areattached by means of eight, 6-mm (14-in.) threaded rods or anyother means which ensures a leakproof seal.5.1.3 Gaskets, one at each end of the column, are con-structed of chemically inert
23、materials, and are as thin aspossible while still providing a good seal. The gasket diametershould overlap the inside column diameter by 3 mm (18 in.) toprevent the gasket from being forced out while under pressure.Techniques other than gaskets for providing a seal between thecolumn and end plates a
24、re allowed provided the technique usedis specified in the report.5.1.4 Flow distribution disks must be constructed of sin-tered stainless steel, with a nominal pore diameter of 70 m.The disk thickness shall be 6 mm (14 in.), with a diameter equalto the inside diameter of the column, approximately 10
25、0 mm (4in.). The disk shall have eight evenly spaced grooves; each ofwhich is 3 mm (18 in.) wide, 3 mm deep and 50 mm (2 in.)long. These grooves shall be positioned in a ray originatingfrom the center of the disk.5.1.5 Tubing used in the apparatus shall be of inert materi-als, for example, glass, st
26、ainless steel, polytetrafluoroethylenelined. The outer diameter shall be 6 mm (14 in.).5.1.6 Substitution of materials of construction of the columnor any of its parts is acceptable, as long as it is demonstratedthat levels of contamination for analyte(s) of interest are equalto or less than those s
27、pecified. Any modification of theapparatus as described in this test method must be justified,documented, and delineated in the report.5.2 Pressurized Reservoir Vessel, which is used to containthe leaching fluid, is constructed with requirements similar tothose of the leaching column with the follow
28、ing exceptions: (1)no diffusion disks are used, and (2) it is equipped with a topport for refilling the fluid.5.3 Balance, 10-kg capacity, with a 1-g sensitivity.5.4 Compressed Gas Source, prepurified nitrogen or argonwith a two-stage delivery regulator (0 to 350 kPa) (0 to 50psig), and a pressure g
29、age capable of measuring the pressure inthe head space of the liquid reservoir to within 67 kPa (1 psig).6. Reagents and Materials6.1 American Chemical Society (ACS) Reagent gradechemicals or equivalent are preferred.66.2 Other grades of chemicals may be used, provided thatthe reagent is of sufficie
30、ntly high purity to permit its usewithout compromising the objectives of the testing.6.3 Demonstration of acceptability through reagent blankdata at or below the quantitation limits for all analytes ofinterest is required.6.4 Unless otherwise indicated, references to reagent watermean water as defin
31、ed in SW-846, Method 1311, 5.2. Seereagent water under the terminology section of this test method(3.1.1).NOTE 1Reagent water is defined in SW-846 as water in which aninterferant is not observed at or above the methods detection limit of theanalyte(s) of interest.7. Safety Precaution7.1 General oper
32、ating pressure should not exceed 275.8 kPa(40 psig) with materials as defined herein. Other inert materialsare available that can be used to manufacture the column whichwill withstand pressures above 275.8 kPa (40 psig).8. Sampling8.1 Sampling must be performed so as to obtain a represen-tative samp
33、le of the material.8.2 Where no specific sampling methods are available,sampling methods for materials of physical form similar to thematerial shall be used.8.3 Aminimum sample of 5000 g, or three column volumes,whichever is larger, shall be sent to the laboratory for eachcolumn.8.4 Samples must be
34、kept in closed containers appropriateto the sample type and otherwise protected if necessary prior totesting to prevent sample contamination or constituent changeor loss. Where it is desired to test biologically or chemicallyactive samples in their existing state, any sample storagerequired should b
35、e at 4C (Practice D 3370) and the leachingshould be started within8hofsample collection. Whereappropriate, the tester may modify a test portion beforeleaching to simulate the results of biological or chemicalactivity in the field. Record the storage conditions, samplingprocedures, handling practices
36、, and any abnormal samplingconditions in the report.9. Preparation of Apparatus9.1 The assembled apparatus is shown in Fig. 1.9.2 Column Preparation:9.2.1 Before use, clean all parts of the test apparatus thatwill contact the waste material, leaching fluid, or productleachate.9.2.1.1 Clean the sinte
37、red disks by boiling them for 15 minin reagent water, followed by a backflush with reagent water.Then saturate the disks with concentrated sulfuric acid andsoak until all residues are removed. Then vacuum or pressureremove the excess acid with reagent water. Next, pump or draweither acetone or metha
38、nol through the disks, followed byeither hexane or methylene chloride. Permit disks to air dry.9.2.1.2 Clean the column apparatus by washing it with anonionic surfactant soap and water. Rinse with tap water andfollow with a reagent water rinse. Then rinse it with eitheracetone or methanol, followed
39、by a rinse with either hexane ormethylene chloride. Permit the apparatus to air dry.9.3 Assemble the apparatus as depicted in Figs. 1 and 2.Weigh the dried, clean empty column, including end caps andother fittings necessary to contain the waste, and record themass. This is the tare of the apparatus.
40、 Record the insidediameter and height of that part of the column to be filled withwaste (that is, the column cylinder). If, following columnsaturation, the tester wishes to check the degree of saturation,6Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washingt
41、on, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.D 4874 95 (20
42、06)3it will first be necessary to determine the mass of water that canbe contained in the porous flow distribution disks, end plates,and fittings.10. Procedure10.1 Preconditioning:10.1.1 Prepare a test portion of waste in a manner thatsimulates the state the waste is in or will be in as it undergoes
43、leaching in the field. Preparation of the test portion mayinclude such factors as curing, and adjustment of moisturecontent and density. For such adjustments, the followingprocedures can be used where appropriate.10.1.2 Moisture Content Adjust the moisture content tothat defined in the disposal scen
44、ario by dewatering or addingreagent water to the material. Increase moisture content to thatdefined in the disposal scenario by addition of reagent water.Note and record the volume of reagent water added. If theconcentration of any trace analyte of concern found in thereagent water exceeds the repor
45、ting (quantitation) limit for thevolume added, note this on the report form. Decrease moisturecontent by determining scenario temperature (normally lessthan 60C) and drying the material at the temperature for aspecified time interval. Determine actual moisture content ofthe waste as it is placed in
46、the column using Test MethodD 2216 and an appropriate drying temperature. Note andrecord the drying temperature used. Record the moisturecontent.10.1.3 DensityDensity is to be adjusted by vibration (seeTest Method D 4253) or compaction (see Test Method D 698)to the anticipated field density. Pack th
47、e waste material in thecolumn so that uniform density is achieved. This can bechecked by visual observation of the waste in the transparentcolumn.10.1.4 CuringAging may be necessary for those materialsthat undergo physical or chemical changes with time in order toobtain a specimen (test portion) rep
48、resentative of the desiredconditions. Curing may be accomplished in the field beforetesting in the column to produce a physical and chemical staterepresentative of the waste as it undergoes leaching in the field.Note and record field conditions of temperature, humidity, andatmospheric pressure. Reco
49、rd the duration of the curing pro-cess and report with the test data.10.1.5 Particle Size Ensure that the particle size distribu-tion of the waste as placed in the column is representative ofthat expected in field placement. Interpretation of results isbased in part on a knowledge of the particle size distributionand surface area of the material. Maximum particle diametermust not exceed110 of the inside diameter of the column.Particle size reduction is not recommended. An evaluation ofthe particle characteristics of size distribution and surface areamay be usefu
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