1、Designation: D4874 95 (Reapproved 2014)Standard Test Method forLeaching Solid Material in a Column Apparatus1This standard is issued under the fixed designation D4874; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of las
2、t revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () 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 columnapparatus
3、. 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 we
4、ll 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 satu
5、rated 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 characterizatio
6、n 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(cinders, rocks, and so forth) should be removed prior topacking the column to ensur
7、e 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.1.6.
8、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 thedet
9、ermination 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. The
10、 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 determine the
11、 applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2C819 Test Method for Specific Surface Area of Carbon orGraphite (Withdrawn 1987)3D422 Test Method for Particle-Size Analysis of SoilsD698 Test Methods for Laboratory Compaction Character-istics of Soil
12、Using Standard Effort (12 400 ft-lbf/ft3(600kN-m/m3)D854 Test Methods for Specific Gravity of Soil Solids byWater PycnometerD1125 Test Methods for Electrical Conductivity and Resis-tivity of WaterD1129 Terminology Relating to WaterD1293 Test Methods for pH of WaterD1498 Test Method for Oxidation-Red
13、uction Potential ofWaterD1888 Methods Of Test for Particulate and Dissolved Matterin Water (Withdrawn 1989)31This test method is under the jurisdiction of ASTM Committee D34 on WasteManagement and is the direct responsibility of Subcommittee D34.01.04 on WasteLeaching Techniques.Current edition appr
14、oved May 1, 2014. Published May 2014. Originallyapproved in 1989. Last previous edition approved in 2006 as D4874 95(2006).DOI: 10.1520/D4874-95R14.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandar
15、ds volume information, refer to the standards Document Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1D2216 Test Meth
16、ods for Laboratory Determination of Water(Moisture) Content of Soil and Rock by MassD2434 Test Method for Permeability of Granular Soils(Constant Head)D3370 Practices for Sampling Water from Closed ConduitsD3694 Practices for Preparation of Sample Containers andfor Preservation of Organic Constituen
17、tsD4253 Test Methods for Maximum Index Density and UnitWeight of Soils Using a Vibratory TableE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method3. Terminology3.1 Definitions:3.1.1 reagent wateras defined in SW-846, Method 1311,5.2.43.1.2 void volumethe v
18、olume between the solid particlesin a bed of granular material. Also called the interstitialvolume.3.2 Several terms used in this test method are defined inTerminology D1129.4. Significance and Use4.1 This test method is intended to provide an aqueousleaching of a material in a dynamic partitioning
19、manner.4.2 Specific operating conditions for the column can beselected to satisfy the objectives of individual studies. Anunderstanding of the fundamental principles governing columnleaching is necessary in the selection of appropriate conditions.References (1-3)5provide useful information on these
20、prin-ciples.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 ofthis standard.FIG. 1 Column ApparatusD4874 95 (2014)24.3 The column apparatus is constr
21、ucted of materials thatpermit the generation of a leachate which 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,
22、 with an inside diameter of 100 mm (4 in.).The cylinder wall must be of sufficient thickness, approxi-mately 6 mm (14 in.), to withstand the operating pressure.5.1.2 End plates are constructed of stainless steel. They areattached by means of eight, 6-mm (14-in.) threaded rods or anyother means which
23、 ensures a leakproof seal.5.1.3 Gaskets, one at each end of the column, are con-structed of chemically inert 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 o
24、ut while under pressure.Techniques other than gaskets for providing a seal between thecolumn and end plates are 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
25、thickness shall be 6 mm (14 in.), with a diameter equalto the inside diameter of the column, approximately 100 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 t
26、he center of the disk.5.1.5 Tubing used in the apparatus shall be of inertmaterials, for example, glass, stainless steel, polytetrafluoro-ethylene lined. 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
27、as it is demonstratedthat levels of contamination for analyte(s) of interest are equalto or less than those specified. 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 conta
28、inthe leaching fluid, is constructed with requirements similar tothose of the leaching column with the following 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, pr
29、epurified nitrogen or argonwith a two-stage delivery regulator (0 to 350 kPa) (0 to 50psig), and a pressure gauge capable of measuring the pressurein the head space of the liquid reservoir to within 67 kPa (1psig).6. Reagents and Materials6.1 American Chemical Society (ACS) Reagent gradechemicals or
30、 equivalent are preferred.66.2 Other grades of chemicals may be used, provided thatthe reagent is of sufficiently 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 a
31、nalytes ofinterest is required.6.4 Unless otherwise indicated, references to reagent watermean water as defined 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 obser
32、ved at or above the methods detection limit of theanalyte(s) of interest.7. Safety Precaution7.1 General operating 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 pressur
33、es above 275.8 kPa (40 psig).8. Sampling8.1 Sampling must be performed so as to obtain a represen-tative sample 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
34、three column volumes,whichever is larger, shall be sent to the laboratory for eachcolumn.8.4 Samples must be 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
35、to test biologically or chemicallyactive samples in their existing state, any sample storagerequired should be at 4C (Practice D3370) and the leachingshould be started within8hofsample collection. Whereappropriate, the tester may modify a test portion beforeleaching to simulate the results of biolog
36、ical or chemicalactivity in the field. Record the storage conditions, samplingprocedures, handling practices, and any abnormal samplingconditions in the report.6Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of re
37、agents 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.D4874 95 (2014)39. Preparation of Apparatus9.1 The assemb
38、led 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 sintered disks by boiling them for 15 minin reagent water, followed by a backflush with reagent wa
39、ter.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 methanol through the disks, followed byeither hexane or methylene chloride. Permit disks to air dr
40、y.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 by a rinse with either hexane ormethylene chloride. Permit the apparatus to air dry.9.3 Assem
41、ble 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. Record the insidediameter and height of that part of the column to be filled withwaste (that
42、 is, the column cylinder). If, following columnsaturation, the tester wishes to check the degree of saturation,it 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 Prepar
43、e a test portion of waste in a manner thatsimulates the state the waste is in or will be in as it undergoesleaching 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 use
44、d where appropriate.10.1.2 Moisture ContentAdjust the moisture content tothat defined in the disposal scenario 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 wa
45、ter added. If theconcentration of any trace analyte of concern found in thereagent water exceeds the reporting (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 t
46、emperature for aspecified time interval. Determine actual moisture content ofthe waste as it is placed in the column using Test MethodD2216 and an appropriate drying temperature. Note and recordthe drying temperature used. Record the moisture content.FIG. 2 Packing ConfigurationD4874 95 (2014)410.1.
47、3 DensityDensity is to be adjusted by vibration (seeTest Method D4253) or compaction (see Test Method D698)tothe anticipated field density. Pack the 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
48、CuringAging may be necessary for those materialsthat undergo physical or chemical changes with time in order toobtain a specimen (test portion) representative of the desiredconditions. Curing may be accomplished in the field beforetesting in the column to produce a physical and chemical statereprese
49、ntative of the waste as it undergoes leaching in the field.Note and record field conditions of temperature, humidity, andatmospheric pressure. Record the duration of the curing pro-cess and report with the test data.10.1.5 Particle SizeEnsure 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
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