ASTM D4874-95(2014)
(Test Method)Standard Test Method for Leaching Solid Material in a Column Apparatus (Withdrawn 2021)
Standard Test Method for Leaching Solid Material in a Column Apparatus (Withdrawn 2021)
SIGNIFICANCE AND USE
4.1 This test method is intended to provide an aqueous leaching of a material in a dynamic partitioning manner.
4.2 Specific operating conditions for the column can be selected to satisfy the objectives of individual studies. An understanding of the fundamental principles governing column leaching is necessary in the selection of appropriate conditions. References (1-3)5 provide useful information on these principles.
4.3 The column apparatus is constructed of materials that permit the generation of a leachate which is suitable for low concentration organic analysis for semivolatile and nonvolatile compounds as well as inorganic species.
SCOPE
1.1 This test method is a standard laboratory procedure for generating aqueous leachate from materials using a column apparatus. It provides a leachate suitable for organic analysis of semivolatile and nonvolatile compounds as well as inorganic analyses.
1.2 The column apparatus is designed and constructed of materials chosen to enhance the leaching of low concentrations of semivolatile and nonvolatile organic constituents as well as to maximize the leaching of metallic species from the solid. Analysis of column effluent provides information on the leaching characteristics of material under the conditions used in the test.
1.3 This test method provides for the passage of an aqueous fluid through materials of known mass in a saturated up-flow mode.
1.4 It is intended that the sample used in the procedure be physically, chemically, and biologically representative of the material.
1.5 This test method does not produce results that can be used as the sole basis for (1) engineering design of a disposal site, or (2) the characterization of wastes based on their leaching characteristics.
1.6 This test method has the following limitations:
1.6.1 Maximum particle size is 10 mm (0.4 in.). Particle size reduction is not recommended. Large-diameter material (cinders, rocks, and so forth) should be removed prior to packing the column to ensure adequate compaction.
1.6.2 Test materials containing densely immiscible organic material may result in phase separation and lead to column plugging.
1.6.3 This test method does not differentiate between dissolved constituents and sub-70-μm particulates that pass through the pores of the end plates.
1.6.4 This test method is not applicable to the leachability characterization of materials with regard to volatile compounds.
1.6.5 This test method is not applicable to the characterization of materials that dissolve in water to a degree that significantly impacts the void volume in the column or the determination of the specific gravity of the material.
1.7 Application of this test method to materials with initial low permeability, or to those that lose permeability over the course of the test, may result in long testing periods.
1.8 The values stated in SI units are to be regarded as the standard. The values given in parentheses are in approximate inch-pound equivalents.
1.9 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
WITHDRAWN RATIONALE
This test method was a standard laboratory procedure for generating aqueous leachate from materials using a column apparatus.
Formerly under the jurisdiction of Committee D34 on Waste Management, this test method was withdrawn in May 2021. This standard is being withdrawn without replacement due to its limited use by industry.
General Information
Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D4874 − 95 (Reapproved 2014)
Standard Test Method for
Leaching Solid Material in a Column Apparatus
This standard is issued under the fixed designation D4874; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 1.6.4 This test method is not applicable to the leachability
characterization of materials with regard to volatile com-
1.1 This test method is a standard laboratory procedure for
pounds.
generating aqueous leachate from materials using a column
1.6.5 This test method is not applicable to the characteriza-
apparatus.Itprovidesaleachatesuitablefororganicanalysisof
tion of materials that dissolve in water to a degree that
semivolatile and nonvolatile compounds as well as inorganic
significantly impacts the void volume in the column or the
analyses.
determination of the specific gravity of the material.
1.2 The column apparatus is designed and constructed of
1.7 Application of this test method to materials with initial
materials chosen to enhance the leaching of low concentrations
low permeability, or to those that lose permeability over the
of semivolatile and nonvolatile organic constituents as well as
course of the test, may result in long testing periods.
to maximize the leaching of metallic species from the solid.
1.8 The values stated in SI units are to be regarded as the
Analysis of column effluent provides information on the
standard. The values given in parentheses are in approximate
leaching characteristics of material under the conditions used
inch-pound equivalents.
in the test.
1.9 This standard does not purport to address all of the
1.3 This test method provides for the passage of an aqueous
safety concerns, if any, associated with its use. It is the
fluid through materials of known mass in a saturated up-flow
responsibility of the user of this standard to establish appro-
mode.
priate safety and health practices and determine the applica-
1.4 It is intended that the sample used in the procedure be
bility of regulatory limitations prior to use.
physically, chemically, and biologically representative of the
2. Referenced Documents
material.
2.1 ASTM Standards:
1.5 This test method does not produce results that can be
C819 Test Method for Specific Surface Area of Carbon or
used as the sole basis for (1) engineering design of a disposal
Graphite (Withdrawn 1987)
site, or (2) the characterization of wastes based on their
D422 Test Method for Particle-Size Analysis of Soils
leaching characteristics.
D698 Test Methods for Laboratory Compaction Character-
1.6 This test method has the following limitations:
istics of Soil Using Standard Effort (12 400 ft-lbf/ft (600
1.6.1 Maximumparticlesizeis10mm(0.4in.).Particlesize
kN-m/m ))
reduction is not recommended. Large-diameter material
D854 Test Methods for Specific Gravity of Soil Solids by
(cinders, rocks, and so forth) should be removed prior to
Water Pycnometer
packing the column to ensure adequate compaction.
D1125 Test Methods for Electrical Conductivity and Resis-
1.6.2 Test materials containing densely immiscible organic
tivity of Water
material may result in phase separation and lead to column
D1129 Terminology Relating to Water
plugging.
D1293 Test Methods for pH of Water
1.6.3 This test method does not differentiate between dis- D1498 Test Method for Oxidation-Reduction Potential of
solved constituents and sub-70-µm particulates that pass Water
through the pores of the end plates. D1888 MethodsOfTestforParticulateandDissolvedMatter
in Water (Withdrawn 1989)
1 2
This test method is under the jurisdiction of ASTM Committee D34 on Waste For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Management and is the direct responsibility of Subcommittee D34.01.04 on Waste contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Leaching Techniques. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved May 1, 2014. Published May 2014. Originally the ASTM website.
approved in 1989. Last previous edition approved in 2006 as D4874 – 95(2006). The last approved version of this historical standard is referenced on
DOI: 10.1520/D4874-95R14. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4874 − 95 (2014)
D2216 Test Methods for Laboratory Determination of Water 3.1.2 void volume—the volume between the solid particles
(Moisture) Content of Soil and Rock by Mass in a bed of granular material. Also called the interstitial
D2434 Test Method for Permeability of Granular Soils volume.
(Constant Head)
3.2 Several terms used in this test method are defined in
D3370 Practices for Sampling Water from Closed Conduits
Terminology D1129.
D3694 Practices for Preparation of Sample Containers and
for Preservation of Organic Constituents
4. Significance and Use
D4253 Test Methods for Maximum Index Density and Unit
4.1 This test method is intended to provide an aqueous
Weight of Soils Using a Vibratory Table
leaching of a material in a dynamic partitioning manner.
E691 Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method
4.2 Specific operating conditions for the column can be
selected to satisfy the objectives of individual studies. An
3. Terminology
understanding of the fundamental principles governing column
leaching is necessary in the selection of appropriate conditions.
3.1 Definitions:
References (1-3) provide useful information on these prin-
3.1.1 reagent water—as defined in SW-846, Method 1311,
ciples.
5.2.
The boldface numbers in parentheses refer to the list of references at the end of
this standard.
SW-846, 3rd ed., Method 1311, Available from USEPA, Office of Solid Waste
and Emergency Response, Washington, DC 20460.
FIG. 1 Column Apparatus
D4874 − 95 (2014)
4.3 The column apparatus is constructed of materials that 6. Reagents and Materials
permit the generation of a leachate which is suitable for low
6.1 American Chemical Society (ACS) Reagent grade
concentration organic analysis for semivolatile and nonvolatile 6
chemicals or equivalent are preferred.
compounds as well as inorganic species.
6.2 Other grades of chemicals may be used, provided that
the reagent is of sufficiently high purity to permit its use
5. Apparatus (See Fig. 1)
without compromising the objectives of the testing.
5.1 Columns:
6.3 Demonstration of acceptability through reagent blank
5.1.1 Thecolumnbodyisconstructedofglasspipe,300mm
data at or below the quantitation limits for all analytes of
(12 in.) in length, with an inside diameter of 100 mm (4 in.).
interest is required.
The cylinder wall must be of sufficient thickness, approxi-
1 6.4 Unless otherwise indicated, references to reagent water
mately 6 mm ( ⁄4 in.), to withstand the operating pressure.
mean water as defined in SW-846, Method 1311, 5.2. See
5.1.2 End plates are constructed of stainless steel. They are
reagent water under the terminology section of this test method
attached by means of eight, 6-mm ( ⁄4-in.) threaded rods or any
(3.1.1).
other means which ensures a leakproof seal.
NOTE 1—Reagent water is defined in SW-846 as water in which an
5.1.3 Gaskets, one at each end of the column, are con-
interferant is not observed at or above the method’s detection limit of the
structed of chemically inert materials, and are as thin as
analyte(s) of interest.
possible while still providing a good seal. The gasket diameter
should overlap the inside column diameter by 3 mm ( ⁄8 in.) to
7. Safety Precaution
prevent the gasket from being forced out while under pressure.
7.1 General operating pressure should not exceed 275.8 kPa
Techniques other than gaskets for providing a seal between the
(40psig)withmaterialsasdefinedherein.Otherinertmaterials
columnandendplatesareallowedprovidedthetechniqueused
areavailablethatcanbeusedtomanufacturethecolumnwhich
is specified in the report.
will withstand pressures above 275.8 kPa (40 psig).
5.1.4 Flow distribution disks must be constructed of sin-
tered stainless steel, with a nominal pore diameter of 70 µm.
8. Sampling
Thediskthicknessshallbe6mm( ⁄4in.),withadiameterequal
8.1 Sampling must be performed so as to obtain a represen-
totheinsidediameterofthecolumn,approximately100mm(4
tative sample of the material.
in.). The disk shall have eight evenly spaced grooves; each of
1 8.2 Where no specific sampling methods are available,
which is 3 mm ( ⁄8 in.) wide, 3 mm deep and 50 mm (2 in.)
sampling methods for materials of physical form similar to the
long. These grooves shall be positioned in a ray originating
material shall be used.
from the center of the disk.
5.1.5 Tubing used in the apparatus shall be of inert 8.3 Aminimumsampleof5000g,orthreecolumnvolumes,
materials, for example, glass, stainless steel, polytetrafluoro- whichever is larger, shall be sent to the laboratory for each
ethylene lined. The outer diameter shall be 6 mm ( ⁄4 in.). column.
5.1.6 Substitutionofmaterialsofconstructionofthecolumn
8.4 Samples must be kept in closed containers appropriate
or any of its parts is acceptable, as long as it is demonstrated
to the sample type and otherwise protected if necessary prior to
that levels of contamination for analyte(s) of interest are equal
testing to prevent sample contamination or constituent change
to or less than those specified. Any modification of the
or loss. Where it is desired to test biologically or chemically
apparatus as described in this test method must be justified,
active samples in their existing state, any sample storage
documented, and delineated in the report.
required should be at 4°C (Practice D3370) and the leaching
should be started within8hof sample collection. Where
5.2 Pressurized Reservoir Vessel, which is used to contain
appropriate, the tester may modify a test portion before
the leaching fluid, is constructed with requirements similar to
leaching to simulate the results of biological or chemical
thoseoftheleachingcolumnwiththefollowingexceptions:(1)
activity in the field. Record the storage conditions, sampling
no diffusion disks are used, and (2) it is equipped with a top
procedures, handling practices, and any abnormal sampling
port for refilling the fluid.
conditions in the report.
5.3 Balance, 10-kg capacity, with a 1-g sensitivity.
5.4 Compressed Gas Source, prepurified nitrogen or argon
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
with a two-stage delivery regulator (0 to 350 kPa) (0 to 50
listed by the American Chemical Society, see Analar Standards for Laboratory
psig), and a pressure gauge capable of measuring the pressure
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
in the head space of the liquid reservoir to within 67 kPa (1
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
psig). MD.
D4874 − 95 (2014)
9. Preparation of Apparatus itwillfirstbenecessarytodeterminethemassofwaterthatcan
be contained in the porous flow distribution disks, end plates,
9.1 The assembled apparatus is shown in Fig. 1.
and fittings.
9.2 Column Preparation:
9.2.1 Before use, clean all parts of the test apparatus that 10. Procedure
will contact the waste material, leaching fluid, or product
10.1 Preconditioning:
leachate.
10.1.1 Prepare a test portion of waste in a manner that
9.2.1.1 Clean the sintered disks by boiling them for 15 min
simulates the state the waste is in or will be in as it undergoes
in reagent water, followed by a backflush with reagent water.
leaching in the field. Preparation of the test portion may
Then saturate the disks with concentrated sulfuric acid and
include such factors as curing, and adjustment of moisture
soak until all residues are removed. Then vacuum or pressure
content and density. For such adjustments, the following
removetheexcessacidwithreagentwater.Next,pumpordraw
procedures can be used where appropriate.
either acetone or methanol through the disks, followed by
10.1.2 Moisture Content—Adjust the moisture content to
either hexane or methylene chloride. Permit disks to air dry.
that defined in the disposal scenario by dewatering or adding
9.2.1.2 Clean the column apparatus by washing it with a
reagent water to the material. Increase moisture content to that
nonionic surfactant soap and water. Rinse with tap water and
defined in the disposal scenario by addition of reagent water.
follow with a reagent water rinse. Then rinse it with either
Note and record the volume of reagent water added. If the
acetone or methanol, followed by a rinse with either hexane or
concentration of any trace analyte of concern found in the
methylene chloride. Permit the apparatus to air dry.
reagent water exceeds the reporting (quantitation) limit for the
9.3 Assemble the apparatus as depicted in Figs. 1 and 2. volume added, note this on the report form. Decrease moisture
Weigh the dried, clean empty column, including end caps and content by determining scenario temperature (normally less
other fittings necessary to contain the waste, and record the than 60°C) and drying the material at the temperature for a
mass. This is the tare of the apparatus. Record the inside specified time interval. Determine actual moisture content of
diameter and height of that part of the column to be filled with the waste as it is placed in the column using Test Method
waste (that is, the column cylinder). If, following column D2216 and an appropriate drying temperature. Note and record
saturation, the tester wishes to check the degree of saturation, the drying temperature used. Record the moisture content.
FIG. 2 Packing Configuration
D4874 − 95 (2014)
10.1.3 Density—Density is to be adjusted by vibration (see 10.3.4 Determination of the Void Volume—Void volume is
Test Method D4253) or compaction (seeTest Method D698)to estimated from the measurement of specific gravity of the
the anticipated field density. Pack the waste material in the solids in accordance with Test Method D854, the mass of the
column so that uniform density is achieved. This can be wet solids placed into the column, the moisture content of the
checked by visual observation of the waste in the transparent material in accordance with Test Method D2216, and the
column. volume of the column. Althou
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