ASTM D4874-95
(Test Method)Standard Test Method for Leaching Solid Material in a Column Apparatus
Standard Test Method for Leaching Solid Material in a Column Apparatus
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.
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Designation: D 4874 – 95
Standard Test Method for
Leaching Solid Material in a Column Apparatus
This standard is issued under the fixed designation D 4874; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope determination of the specific gravity of the material.
1.7 Application of this test method to materials with initial
1.1 This test method is a standard laboratory procedure for
low permeability, or to those that lose permeability over the
generating aqueous leachate from materials using a column
course of the test, may result in long testing periods.
apparatus. It provides a leachate suitable for organic analysis of
1.8 The values stated in SI units are to be regarded as the
semivolatile and nonvolatile compounds as well as inorganic
standard. The values given in parentheses are in approximate
analyses.
inch-pound equivalents.
1.2 The column apparatus is designed and constructed of
1.9 This standard does not purport to address all of the
materials chosen to enhance the leaching of low concentrations
safety concerns, if any, associated with its use. It is the
of semivolatile and nonvolatile organic constituents as well as
responsibility of the user of this standard to establish appro-
to maximize the leaching of metallic species from the solid.
priate safety and health practices and determine the applica-
Analysis of column effluent provides information on the
bility of regulatory limitations prior to use.
leaching characteristics of material under the conditions used
in the test.
2. Referenced Documents
1.3 This test method provides for the passage of an aqueous
2.1 ASTM Standards:
fluid through materials of known mass in a saturated up-flow
C 819 Test Method for Specific Surface Area of Carbon or
mode.
Graphite
1.4 It is intended that the sample used in the procedure be
D 422 Test Method for Particle Size Analysis of Soils
physically, chemically, and biologically representative of the
D 698 Test Method for Laboratory Compaction Character-
material.
istics of Soil Using Standard Effort (12 400 ft-lbf/ft ) (600
1.5 This test method does not produce results that can be
kN-m/m )
used as the sole basis for (1) engineering design of a disposal
D 854 Test Method for Specific Gravity of Soils
site, or (2) the characterization of wastes based on their
D 1125 Test Methods for Electrical Conductivity and Re-
leaching characteristics.
sistivity of Water
1.6 This test method has the following limitations:
D 1129 Terminology Relating to Water
1.6.1 Maximum particle size is 10 mm (0.4 in.). Particle size
D 1293 Test Methods for pH of Water
reduction is not recommended. Large-diameter material (cin-
D 1498 Practice for Oxidation-Reduction Potential of Wa-
ders, rocks, and so forth) should be removed prior to packing
ter
the column to ensure adequate compaction.
D 1888 Test Methods for Particulate and Dissolved Matter
1.6.2 Test materials containing densely immiscible organic
in Water
material may result in phase separation and lead to column
D 2216 Test Method for Laboratory Determination of Water
plugging.
(Moisture) Content of Soil and Rock
1.6.3 This test method does not differentiate between dis-
D 2434 Test Method for Permeability of Granular Soils
solved constituents and sub-70-μm particulates that pass
(Constant Head)
through the pores of the end plates.
D 3370 Practices for Sampling Water
1.6.4 This test method is not applicable to the leachability
D 3694 Practice for Preparation of Sample Containers and
characterization of materials with regard to volatile com-
for Preservation of Organic Constituents
pounds.
D 4253 Test Methods for Maximum Index Density and Unit
1.6.5 This test method is not applicable to the characteriza-
Weight of Soils Using a Vibratory Table
tion of materials that dissolve in water to a degree that
E 691 Practice for Conducting an Interlaboratory Study to
significantly impacts the void volume in the column or the
Discontinued, see 1988 Annual Book of ASTM Standards, Vol 15.01.
This test method is under the jurisdiction of ASTM Committee D-34 on Waste
Annual Book of ASTM Standards, Vol 04.08.
Management and is the direct responsibility of Subcommittee D34.02 on Physical
Annual Book of ASTM Standards, Vol 11.01.
and Chemical Characterization.
Discontinued, see 1990 Annual Book of ASTM Standards, Vol 11.01.
Current edition approved Oct. 10, 1995. Published December 1995. Originally
Annual Book of ASTM Standards, Vol 11.02.
published as D 4874 – 89. Last previous edition D 4874 – 89.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
D 4874
FIG. 1 Column Apparatus
Determine the Precision of a Test Method leaching is necessary in the selection of appropriate conditions.
References (1-3) provide useful information on these prin-
3. Terminology
ciples.
3.1 Definition: 4.3 The column apparatus is constructed of materials that
3.1.1 reagent water—as defined in SW-846, Method 1311, permit the generation of a leachate which is suitable for low
5.2. concentration organic analysis for semivolatile and nonvolatile
3.1.2 void volume—the volume between the solid particles compounds as well as inorganic species.
in a bed of granular material. Also called the interstitial
5. Apparatus (See Fig. 1)
volume.
5.1 Columns:
3.2 Several terms used in this test method are defined in
Terminology D 1129. 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.).
4. Significance and Use
The cylinder wall must be of sufficient thickness, approxi-
mately 6 mm ( ⁄4 in.), to withstand the operating pressure.
4.1 This test method is intended to provide an aqueous
leaching of a material in a dynamic partitioning manner. 5.1.2 End plates are constructed of stainless steel. They are
attached by means of eight, 6-mm ( ⁄4-in.) threaded rods or any
4.2 Specific operating conditions for the column can be
selected to satisfy the objectives of individual studies. An other means which ensures a leakproof seal.
5.1.3 Gaskets, one at each end of the column, are con-
understanding of the fundamental principles governing column
structed of chemically inert materials, and are as thin as
Annual Book of ASTM Standards, Vol 14.02.
8 9
SW-846, 3rd ed., Method 1311, Available from USEPA, Office of Solid Waste The boldface numbers in parentheses refer to the list of references at the end of
and Emergency Response, Washington, DC 20460. this standard.
D 4874
possible while still providing a good seal. The gasket diameter (40 psig) with materials as defined herein. Other inert materials
should overlap the inside column diameter by 3 mm ( ⁄8 in.) to are available that can be used to manufacture the column which
prevent the gasket from being forced out while under pressure. will withstand pressures above 275.8 kPa (40 psig).
Techniques other than gaskets for providing a seal between the
8. Sampling
column and end plates are allowed provided the technique used
8.1 Sampling must be performed so as to obtain a represen-
is specified in the report.
5.1.4 Flow distribution disks must be constructed of sin- tative sample of the material.
8.2 Where no specific sampling methods are available,
tered stainless steel, with a nominal pore diameter of 70 μm.
The disk thickness shall be 6 mm ( ⁄4 in.), with a diameter equal sampling methods for materials of physical form similar to the
material shall be used.
to the inside diameter of the column, approximately 100 mm (4
in.). The disk shall have eight evenly spaced grooves; each of 8.3 A minimum sample of 5000 g, or three column volumes,
whichever is larger, shall be sent to the laboratory for each
which is 3 mm ( ⁄8 in.) wide, 3 mm deep and 50 mm (2 in.)
long. These grooves shall be positioned in a ray originating column.
8.4 Samples must be kept in closed containers appropriate
from the center of the disk.
5.1.5 Tubing used in the apparatus shall be of inert materi- to the sample type and otherwise protected if necessary prior to
testing to prevent sample contamination or constituent change
als, for example, glass, stainless steel, polytetrafluoroethylene
lined. The outer diameter shall be 6 mm ( ⁄4 in.). or loss. Where it is desired to test biologically or chemically
active samples in their existing state, any sample storage
5.1.6 Substitution of materials of construction of the column
or any of its parts is acceptable, as long as it is demonstrated required should be at 4°C (Practice D 3370) and the leaching
that levels of contamination for analyte(s) of interest are equal should be started within8hof sample collection. Where
appropriate, the tester may modify a test portion before
to or less than those specified. Any modification of the
apparatus as described in this test method must be justified, leaching to simulate the results of biological or chemical
activity in the field. Record the storage conditions, sampling
documented, and delineated in the report.
5.2 Pressurized Reservoir Vessel, which is used to contain procedures, handling practices, and any abnormal sampling
conditions in the report.
the leaching fluid, is constructed with requirements similar to
those of the leaching column with the following exceptions: (1)
9. Preparation of Apparatus
no diffusion disks are used, and (2) it is equipped with a top
9.1 The assembled apparatus is shown in Fig. 1.
port for refilling the fluid.
9.2 Column Preparation:
5.3 Balance, 10-kg capacity, with a 1-g sensitivity.
9.2.1 Before use, clean all parts of the test apparatus that
5.4 Compressed Gas Source, prepurified nitrogen or argon
will contact the waste material, leaching fluid, or product
with a two-stage delivery regulator (0 to 350 kPa) (0 to 50
leachate.
psig), and a pressure gage capable of measuring the pressure in
9.2.1.1 Clean the sintered disks by boiling them for 15 min
the head space of the liquid reservoir to within 67 kPa (1 psig).
in reagent water, followed by a backflush with reagent water.
6. Reagents and Materials
Then saturate the disks with concentrated sulfuric acid and
6.1 American Chemical Society (ACS) Reagent grade
soak until all residues are removed. Then vacuum or pressure
chemicals or equivalent are preferred.
remove the excess acid with reagent water. Next, pump or draw
6.2 Other grades of chemicals may be used, provided that
either acetone or methanol through the disks, followed by
the reagent is of sufficiently high purity to permit its use
either hexane or methylene chloride. Permit disks to air dry.
without compromising the objectives of the testing.
9.2.1.2 Clean the column apparatus by washing it with a
6.3 Demonstration of acceptability through reagent blank
nonionic surfactant soap and water. Rinse with tap water and
data at or below the quantitation limits for all analytes of
follow with a reagent water rinse. Then rinse it with either
interest is required.
acetone or methanol, followed by a rinse with either hexane or
6.4 Unless otherwise indicated, references to reagent water
methylene chloride. Permit the apparatus to air dry.
mean water as defined in SW-846, Method 1311, 5.2. See
9.3 Assemble the apparatus as depicted in Figs. 1 and 2.
reagent water under the terminology section of this test method
Weigh the dried, clean empty column, including end caps and
(3.1.1).
other fittings necessary to contain the waste, and record the
mass. This is the tare of the apparatus. Record the inside
NOTE 1—Reagent water is defined in SW-846 as water in which an
diameter and height of that part of the column to be filled with
interferant is not observed at or above the method’s detection limit of the
analyte(s) of interest.
waste (that is, the column cylinder). If, following column
saturation, the tester wishes to check the degree of saturation,
7. Safety Precaution
it will first be necessary to determine the mass of water that can
7.1 General operating pressure should not exceed 275.8 kPa
be contained in the porous flow distribution disks, end plates,
and fittings.
Reagent Chemicals, American Chemical Society Specifications, American
10. Procedure
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
10.1 Preconditioning:
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
10.1.1 Prepare a test portion of waste in a manner that
and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
MD. simulates the state the waste is in or will be in as it undergoes
D 4874
FIG. 2 Packing Configuration
leaching in the field. Preparation of the test portion may conditions. Curing may be accomplished in the field before
include such factors as curing, and adjustment of moisture testing in the column to produce a physical and chemical state
content and density. For such adjustments, the following representative of the waste as it undergoes leaching in the field.
procedures can be used where appropriate. Note and record field conditions of temperature, humidity, and
10.1.2 Moisture Content—Adjust the moisture content to atmospheric pressure. Record the duration of the curing pro-
that defined in the disposal scenario by dewatering or adding cess and report with the test data.
reagent water to the material. Increase moisture content to that 10.1.5 Particle Size—Ensure that the particle size distribu-
defined in the disposal scenario by addition of reagent water. tion of the waste as placed in the column is representative of
Note and record the volume of reagent water added. If the that expected in field placement. Interpretation of results is
concentration of any trace analyte of concern found in the based in part on a knowledge of the particle size distribution
reagent water exceeds the reporting (quantitation) limit for the and surface area of the material. Maximum particle diameter
volume added, note this on the report form. Decrease moisture must not exceed ⁄10 of the inside diameter of the column.
content by determining scenario temperature (normally less Particle size reduction is not recommended. An evaluation of
than 60°C) and drying the material at the temperature for a the particle characteristics of size distribution and surface area
specified time interval. Determine actual moisture content of may be useful. Test Methods D 422 and C 819 should be used
the waste as i
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