ASTM D4646-87(2001)
(Test Method)Standard Test Method for 24-h Batch-Type Measurement of Contaminant Sorption by Soils and Sediments
Standard Test Method for 24-h Batch-Type Measurement of Contaminant Sorption by Soils and Sediments
SCOPE
1.1 This test method describes a procedure for determining the sorption affinity of waste solutes by unconsolidated geologic material in aqueous suspension. The waste solute may be derived from a variety of sources such as wells, underdrain systems, or laboratory solutions such as those produced by waste extraction tests like the Method D3987 shake extraction method.
1.2 This test method is applicable in screening and providing relative rankings of a large number of geomedia samples for their sorption affinity in aqueous leachate/geomedia suspensions. This test method may not exactly simulate sorption characteristics that would occur in unperturbed geologic settings.
1.3 While this procedure may be applicable to both organic and inorganic constituents, care must be taken with respect to the stability of the particular constituents and their possible losses from solution by such processes as degradation by microbes, light, or hydrolysis. This test method should not be used for volatile chemical constituents (see 6.1).
1.4 This standard does not purport to address all of the safety problems 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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NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
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Designation: D 4646 – 87 (Reapproved 2001)
Standard Test Method for
24-h Batch-Type Measurement of Contaminant Sorption by
Soils and Sediments
This standard is issued under the fixed designation D 4646; 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 Term Batch Method
1.1 This test method describes a procedure for determining
3. Terminology
the sorption affinity of waste solutes by unconsolidated geo-
3.1 Definitions—For definition of terms used in this test
logic material in aqueous suspension. The waste solute may be
method refer to Terminology D 1129.
derived from a variety of sources such as wells, underdrain
3.1.1 solute—chemical species (for example, ion, molecule,
systems, or laboratory solutions such as those produced by
etc.) in solution.
waste extraction tests like the Method D 3987 shake extraction
3.1.2 sorbate—chemical species sorbed by a sorbent.
method.
3.1.3 sorbent—a substance that sorbs the solute from solu-
1.2 This test method is applicable in screening and provid-
tion (for example, soil, sediment, till, etc.).
ing relative rankings of a large number of geomedia samples
3.1.4 sorption—depletion of an amount of solute initially
for their sorption affinity in aqueous leachate/geomedia sus-
present in solution by a sorbent.
pensions. This test method may not exactly simulate sorption
3.1.5 sorption affınity—the relative degree of sorption that
characteristics that would occur in unperturbed geologic set-
occurs by a geomedia.
tings.
3.1.6 unconsolidated geologic material (geomedia)—a
1.3 While this procedure may be applicable to both organic
loosely aggregated solid natural material of geologic origin (for
and inorganic constituents, care must be taken with respect to
example, soil, sediment, till, etc.).
the stability of the particular constituents and their possible
3.2 Definitions of Terms Specific to This Standard:
losses from solution by such processes as degradation by
3.2.1 distribution coeffıcient, K —is defined identically to
d
microbes, light, or hydrolysis. This test method should not be
R , except it is considered to be an equilibrium value and
d
used for volatile chemical constituents (see 6.1).
independent of the concentration of solute (that is, linear
1.4 This standard does not purport to address all of the
sorption curve).
safety concerns, if any, associated with its use. It is the
3.2.2 distribution ratio (R )—the ratio of the concentration
d
responsibility of the user of this standard to establish appro-
of solute sorbed on the soil or other geomedia divided by its
priate safety and health practices and determine the applica-
concentration in solution. A 24-h R is the analogous ratio
d
bility of regulatory limitations prior to use.
evaluated after 24 h of contact of the solute with the geomedia.
2. Referenced Documents The R value is calculated as follows:
d
2.1 ASTM Standards: ~mass of solute sorbed per unit mass of geomedia!
R 5
d
D 1129 Terminology Relating to Water mass of solute in solution per unit volume of solution!
~
μg/g
D 1193 Specification for Reagent Water
μg/mL
D 2216 Test Method for Laboratory Determination of Water
3 mL
(Moisture) Content of Soil and Rock
5 (1)
g
D 3987 Test Method for Shake Extraction of Solid Waste
The dimensions of R reduce to units of volume per mass. It
with Water
d
is convenient to express R in units of millilitres (or cubic
D 4319 Test Method for Distribution Ratios by the Short-
d
centimetres) of solution per gram of geomedia. Dissimilar R
d
values may be obtained if different initial solute concentrations
This test method is under the jurisdiction of ASTM Committee D34 on Waste are used, depending on the sorption behavior of the solute and
Management and is the direct responsibility of Subcommittee D34.01.06 on
the properties of the geomedia (that is, nonlinear sorption
Analytical Methods.
curve). This concentration dependency may be absent where
Current edition approved March 3, 1987. Published April 1987. Originally
the solute concentrations are sufficiently low or the character-
published as ES 10 – 85. Last previous edition ES 10 – 85.
Annual Book of ASTM Standards, Vol 11.01.
istics of the particular solute-sorbent combination yield R
d
Annual Book of ASTM Standards, Vol 04.08.
values that are independent of the concentration of solute (that
Annual Book of ASTM Standards, Vol 11.04.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D 4646
is, linear sorption curve). 7. Apparatus
7.1 Agitation Equipment—The agitation equipment to be
4. Summary of Test Method
used is the rotary solid waste extractor specified in Test
4.1 Distilled water, natural water, waste leachate, or other
Method D 3987.
aqueous solution containing a known concentration of a solute
7.2 Phase Separation Equipment—A filtration apparatus
is mixed with a known amount of unconsolidated geologic
made of materials compatible with the solutions being filtered
material (geomedia) for 24 h. Changes in solute concentrations
and equipped with a 0.45-μm pore size membrane filter, or a
are used to calculate a distribution ratio (R ).
d
constant temperature centrifuge capable of separating particles
with diameters greater than 0.1 μm (see Section 9). If organic
5. Significance and Use
compounds are being measured, the filtration apparatus, cen-
5.1 This test method is meant to allow for a rapid (24 h)
trifuge tubes etc., should be compatible with the compounds
index of a geomedia’s sorption affinity for given chemicals or
being measured (that is, glass or stainless steel). Sorption of
leachate constituents. A large number of samples may be run
solute onto the filtration membrane may be significant for some
using this test method to determine a comparative ranking of
solutes, and must be evaluated by the use of blanks through all
those samples, based upon the amount of solute sorbed by the
steps of the procedure.
geomedia, or by various geomedia or leachate constituents.
7.3 Containers—Round, wide-mouth bottles compatible
The 24-h time is used to make the test convenient and also to
with the rotary extractor (Test Method D 3987) and of compo-
minimize microbial degradation which may be a problem in
sition suitable to the nature of the solute(s) under investigation
longer-timed procedures. Due to this time constraint, the final
and the analysis to be performed will be used. For nonvolatile
(24-h) concentration should not be confused with that of an
inorganic constituents, high-density, linear polyethylene bottles
equilibrium or steady-state concentration. While R values are
d
should be used with the size of the bottle dictated by sample
directly applicable for screening and comparative ranking
size, and the need for the solution to occupy 70 to 80 % of the
purposes, their use in predictive field applications generally
container volume (that is, 125 mL, 250 mL, or 2-L bottles for
requires the assumption that R =K ; the validity of this
d d
sample sizes of 5, 10, or 70 g respectively). For nonvolatile
assumption must be carefully evaluated by qualified personnel.
organic constituents, TFE-fluorocarbon, glass bottles, or stain-
5.2 While this test method may be useful in determining
less steel containers with water-tight closures made of chemi-
24-h R values for nonvolatile organic constituents, interlabo-
d
cally inert materials should be used with size requirements
ratory testing has been carried out only for the nonvolatile
being the same as for nonvolatile inorganics. Containers should
inorganic species, arsenic and cadmium. However, the proce-
be cleaned in a manner consistent with the analyses to be
dure has been tested for single laboratory precision with
performed. Samples of the solutions to be analyzed should be
polychlorinated biphenyls (PCBs) and is believed to be useful
stored in similar chemically compatible bottles.
for all stable and nonvolatile inorganic, and organic constitu-
7.4 Balance, having a minimum capacity of 70 g and a
ents. This test method is not considered appropriate for volatile
sensitivity of 60.005 g shall be used.
constituents.
5.3 The 24-h time limit may be sufficient to reach a
8. Reagents
steady-state R . However, to report this determination as a
d
8.1 Purity of Reagents—Reagent grade chemicals shall be
steady-state R (that is, R =K ), the relevant time studies must
d d d
used in all tests. Unless otherwise indicated, it is intended that
be carried out to document the development of steady-state
all reagents shall conform to the specifications of the American
conditions within the 24-h time period. Tests exceeding the
Chemical Society, where such specifications are available.
24-h time period are beyond the scope of this test method.
Other grades may be used, provided it is first ascertained that
Refer to Test Method D 4319, for an alternate procedure of
the reagent is of sufficiently high purity to permit its use
longer duration.
without lessening the accuracy of the determination.
8.2 Purity of Water— Unless otherwise indicated, refer-
6. Interferences
ences to water shall be understood to mean Type IV reagent
6.1 When dealing with solutes of unknown stability either in
water of Specification D 1193.
contact with the geomedia or when used as blanks, care must
be taken to determine if volatilization, hydrolysis, photodeg-
9. Procedure
radation, microbial degradation, oxidation-reduction (that is,
9.1 Geomedia samples are spread out on a flat surface, no
3+ 6+
Cr to Cr ) or other physicochemical processes are operating
more than 2 to 3 cm deep, and allowed to air dry for 7 days or
at a significant rate within the time frame of the procedure
...
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