ASTM D4646-03(2008)
(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
SIGNIFICANCE AND USE
This test method is meant to allow for a rapid (24 h) index of a geomedia's sorption affinity for given chemicals or leachate constituents. A large number of samples may be run using this test method to determine a comparative ranking of those samples, based upon the amount of solute sorbed by the geomedia, or by various geomedia or leachate constituents. The 24-h time is used to make the test convenient and also to minimize microbial degradation which may be a problem in longer-timed procedures. While Kd values are directly applicable for screening and comparative ranking purposes, their use in predictive field applications generally requires the assumption that Kd be a fixed value.
While this test method may be useful in determining 24-h Kd values for nonvolatile organic constituents, interlaboratory testing has been carried out only for the nonvolatile inorganic species, arsenic and cadmium. However, the procedure has been tested for single laboratory precision with polychlorinated biphenyls (PCBs) and is believed to be useful for all stable and nonvolatile inorganic, and organic constituents. This test method is not considered appropriate for volatile constituents.
The 24-h time limit may be sufficient to reach a steady-state Kd. However, to report this determination as a steady-state Kd, this test method should be conducted for intermediate times (for example, 12, 18 and 22 h) to ensure that the soluble concentrations in the solution have reached a steady state by 24 h. Refer to Test Method D 4319 for an alternate procedure of longer duration.
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 Test Method D 3987 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 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 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: D4646 − 03(Reapproved 2008)
Standard Test Method for
24-h Batch-Type Measurement of Contaminant Sorption by
Soils and Sediments
This standard is issued under the fixed designation D4646; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope D1193Specification for Reagent Water
D2216Test Methods for Laboratory Determination ofWater
1.1 This test method describes a procedure for determining
(Moisture) Content of Soil and Rock by Mass
the sorption affinity of waste solutes by unconsolidated geo-
D3987Practice for Shake Extraction of Solid Waste with
logic material in aqueous suspension.The waste solute may be
Water
derived from a variety of sources such as wells, underdrain
D4319Test Method for Distribution Ratios by the Short-
systems, or laboratory solutions such as those produced by
Term Batch Method (Withdrawn 2007)
waste extraction tests like the Test Method D3987 shake
extraction method.
3. Terminology
1.2 This test method is applicable in screening and provid-
3.1 Definitions:
ing relative rankings of a large number of geomedia samples
3.1.1 Fordefinitionoftermsusedinthistestmethodreferto
for their sorption affinity in aqueous leachate/geomedia sus-
Terminology D1129.
pensions. This test method may not exactly simulate sorption
3.1.2 solute—chemical species (for example, ion, molecule,
characteristics that would occur in unperturbed geologic set-
etc.) in solution.
tings.
3.1.3 sorbate—chemical species sorbed by a sorbent.
1.3 While this procedure may be applicable to both organic
3.1.4 sorbent—a substance that sorbs the solute from solu-
and inorganic constituents, care must be taken with respect to
tion (for example, soil, sediment, till, etc.).
the stability of the particular constituents and their possible
losses from solution by such processes as degradation by
3.1.5 sorption—depletion of an amount of solute initially
microbes, light, or hydrolysis. This test method should not be present in solution by a sorbent.
used for volatile chemical constituents (see 6.1).
3.1.6 sorption affınity—the relative degree of sorption that
1.4 The values stated in SI units are to be regarded as occurs by a geomedia.
standard. No other units of measurement are included in this
3.1.7 unconsolidated geologic material (geomedia)—a
standard.
looselyaggregatedsolidnaturalmaterialofgeologicorigin(for
1.5 This standard does not purport to address all of the example, soil, sediment, till, etc.).
safety concerns, if any, associated with its use. It is the
3.2 Definitions of Terms Specific to This Standard:
responsibility of the user of this standard to establish appro-
3.2.1 distribution coeffıcient, K —theratiooftheconcentra-
d
priate safety and health practices and determine the applica-
tion of solute sorbed on the soil or other geomedia divided by
bility of regulatory limitations prior to use.
its concentration in solution. A 24-h K is the analogous ratio
d
evaluatedafter24hofcontactofthesolutewiththegeomedia.
2. Referenced Documents
3.2.1.1 Discussion—The dimensions of K reduce to units
d
2.1 ASTM Standards:
of volume per mass. It is convenient to express K in units of
d
D1129Terminology Relating to Water
millilitres (or cubic centimetres) of solution per gram of
geomedia. Dissimilar K values may be obtained if different
d
This test method is under the jurisdiction ofASTM Committee D34 on Waste
initial solute concentrations are used, depending on the sorp-
Management and is the direct responsibility of Subcommittee D34.01.04 on Waste
tion behavior of the solute and the properties of the geomedia
Leaching Techniques.
(that is, nonlinear sorption curve). This concentration depen-
Current edition approved Oct. 1, 2008. Published December 2008. Originally
approvedasES10–85.Lastpreviouseditionapprovedin2003asD4646–03.DOI: dency may be absent where the solute concentrations are
10.1520/D4646-03R08.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contactASTM Customer Service at service@astm.org. ForAnnual Book ofASTM
Standards volume information, refer to the standard’s Document Summary page on The last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4646 − 03 (2008)
sufficiently low or the characteristics of the particular solute- difference is greater than the expected precision of the method
sorbentcombinationyield K valuesthatareindependentofthe (10%), then the K value generated may be unreliable and
d d
concentration of solute (that is, linear sorption curve). must be carefully evaluated.
7. Apparatus
4. Summary of Test Method
4.1 Distilled water, natural water, waste leachate, or other 7.1 Agitation Equipment—The agitation equipment to be
used is the rotary solid waste extractor specified in Test
aqueous solution containing a known concentration of a solute
is mixed with a known amount of unconsolidated geologic Method D3987.
material (geomedia) for 24 h.After 24 h, equilibrium between
7.2 Phase Separation Equipment—A filtration apparatus
the solid and solution phase is presumed to occur. The
made of materials compatible with the solutions being filtered
concentration of solute remaining in solution is measured and
and equipped with a 0.45-µm pore size membrane filter, or a
the amount of solute adsorbed is calculated. Given that the
constant temperature centrifuge capable of separating particles
mass of solid phase is known, the distribution coefficient for
with diameters greater than 0.1 µm (see Section 9). If organic
the specified experimental conditions can then be calculated.
compounds are being measured, the filtration apparatus, cen-
trifuge tubes etc., should be compatible with the compounds
5. Significance and Use
being measured (that is, glass or stainless steel). Sorption of
5.1 This test method is meant to allow for a rapid (24 h)
soluteontothefiltrationmembranemaybesignificantforsome
index of a geomedia’s sorption affinity for given chemicals or
solutes, and must be evaluated by the use of blanks through all
leachate constituents. A large number of samples may be run
steps of the procedure.
using this test method to determine a comparative ranking of
7.3 Containers—Round, wide-mouth bottles compatible
those samples, based upon the amount of solute sorbed by the
with the rotary extractor (Test Method D3987) and of compo-
geomedia, or by various geomedia or leachate constituents.
sition suitable to the nature of the solute(s) under investigation
The 24-h time is used to make the test convenient and also to
and the analysis to be performed will be used. For nonvolatile
minimize microbial degradation which may be a problem in
inorganicconstituents,high-density,linearpolyethylenebottles
longer-timed procedures. While K values are directly appli-
d
should be used with the size of the bottle dictated by sample
cable for screening and comparative ranking purposes, their
size, and the need for the solution to occupy 70 to 80% of the
use in predictive field applications generally requires the
container volume (that is, 125 mL, 250 mL, or 2-L bottles for
assumption that K be a fixed value.
d
sample sizes of 5, 10, or 70 g respectively). For nonvolatile
5.2 While this test method may be useful in determining
organic constituents, TFE-fluorocarbon, glass bottles, or stain-
24-h K values for nonvolatile organic constituents, interlabo-
d
less steel containers with water-tight closures made of chemi-
ratory testing has been carried out only for the nonvolatile
cally inert materials should be used with size requirements
inorganic species, arsenic and cadmium. However, the proce-
beingthesameasfornonvolatileinorganics.Containersshould
dure has been tested for single laboratory precision with
be cleaned in a manner consistent with the analyses to be
polychlorinated biphenyls (PCBs) and is believed to be useful
performed. Samples of the solutions to be analyzed should be
for all stable and nonvolatile inorganic, and organic constitu-
stored in similar chemically compatible bottles.
ents.Thistestmethodisnotconsideredappropriateforvolatile
7.4 Balance, having a minimum capacity of 70 g and a
constituents.
sensitivity of 60.005 g shall be used.
5.3 The 24-h time limit may be sufficient to reach a
8. Reagents
steady-state K . However, to report this determination as a
d
steady-state K , this test method should be conducted for
d
8.1 Purity of Reagents—Reagent grade chemicals shall be
intermediatetimes(forexample,12,18and22h)toensurethat
used in all tests. Unless otherwise indicated, it is intended that
thesolubleconcentrationsinthesolutionhavereachedasteady
allreagentsshallconformtothespecificationsoftheAmerican
state by 24 h. Refer to Test Method D4319 for an alternate
Chemical Society, where such specifications are available.
procedure of longer duration.
Other grades may be used, provided it is first ascertained that
the reagent is of sufficiently high purity to permit its use
6. Interferences
without lessening the accuracy of the determination.
6.1 Whendealingwithsolutesofunknownstabilityeitherin
8.2 Purity of Water—Unlessotherwiseindicated,references
contact with the geomedia or when used as blanks, care must
to water shall be understood to meanType IVreagent water of
be taken to determine if volatilization, hydrolysis,
Specification D1193.
photodegradation
...
This document is not anASTM standard and is intended only to provide the user of anASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation:D4646–87(Reapproved 1993) Designation:D4646–03 (Reapproved 2008)
Standard Test Method for
24-h Batch-Type Measurement of Contaminant Sorption by
Soils and Sediments
This standard is issued under the fixed designation D4646; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. 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 Test Method D3987 shake extraction method.
1.2 Thistestmethodisapplicableinscreeningandprovidingrelativerankingsofalargenumberofgeomediasamplesfortheir
sorptionaffinityinaqueousleachate/geomediasuspensions.Thistestmethodmaynotexactlysimulatesorptioncharacteristicsthat
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
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 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.
2. Referenced Documents
2.1 ASTM Standards:
D1129 Terminology Relating to Water
D1193 Specification for Reagent Water
D2216 Test Methods for Laboratory Determination of Water (Moisture) Content of Soil and Rock by Mass
D3987 Test Method for Shake Extraction of Solid Waste with Water
D4319 Test Method for Distribution Ratios by the Short-Term Batch Method
3. Terminology
3.1 Definitions—For definition of terms used in this test method refer to Terminology D1129.
3.1.1 solute—chemical species (for example, ion, molecule, etc.) in solution.
3.1.2 sorbate—chemical species sorbed by a sorbent.
3.1.3 sorbent—a substance that sorbs the solute from solution (for example, soil, sediment, till, etc.).
3.1.4 sorption—depletion of an amount of solute initially present in solution by a sorbent.
3.1.5 sorption affınity—the relative degree of sorption that occurs by a geomedia.
3.1.6 unconsolidated geologic material (geomedia)—a loosely aggregated solid natural material of geologic origin (for
example, soil, sediment, till, etc.).
3.2 Definitions of Terms Specific to This Standard:
3.2.1 distribution coeffıcient, K —isdefinedidenticallyto R ,exceptitisconsideredtobeanequilibriumvalueandindependent
d d
of the concentration of solute (that is, linear sorption curve).
3.2.2distribution ratio (R )—the ratio of the concentration of solute sorbed on the soil or other geomedia divided by its
d
concentration in solution. A 24-h R is the analogous ratio evaluated after 24 h of contact of the solute with the geomedia.
K
d
This test method is under the jurisdiction of ASTM Committee D34 on Waste Management and is the direct responsibility of Subcommittee D34.01.06 on Analytical
Methods.
Current edition approved March 3, 1987. Published April 1987. Originally published as ES10–85. Last previous edition ES10–85.
Current edition approved Oct. 1, 2008. Published December 2008. Originally approved as ES10–85. Last previous edition approved in 2003 as D4646–03.
Annual Book of ASTM Standards, Vol 11.01.
ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,orcontactASTMCustomerServiceatservice@astm.org.ForAnnualBookofASTMStandards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D4646–03 (2008)
3.2.1.1 Discussion—The dimensions of RK value is calculated as follows:
d
~massofsolutesorbedperunitmassofgeomedia! µg/g mL
R 5 5 5 (1)
d
~massofsoluteinsolutionperunitvolumeofsolution! µg/mL g
The dimensions of R reduce to units of volume per mass. It is convenient to express R in units of millilitres (or cubic
d K
d
centimetres) of solution per gram of geomedia. Dissimilar R values may be obtained if different initial solute concentrations are
K
d
used, depending on the sorption behavior of the solute and the properties of the geomedia (that is, nonlinear sorption curve).This
concentrationdependencymaybeabsentwherethesoluteconcentrationsaresufficientlyloworthecharacteristicsoftheparticular
solute-sorbent combination yield R values that are independent of the concentration of solute (that is, linear sorption curve).
K
d
4. Summary of Test Method
4.1Distilledwater,naturalwater,wasteleachate,orotheraqueoussolutioncontainingaknownconcentrationofasoluteismixed
with a known amount of unconsolidated geologic material (geomedia) for 24 h. Changes in solute concentrations are used to
calculate a distribution ratio (R ).
d
4.1 Distilled water, natural water, waste leachate, or other aqueous solution containing a known concentration of a solute is
mixed with a known amount of unconsolidated geologic material (geomedia) for 24 h.After 24 h, equilibrium between the solid
and solution phase is presumed to occur. The concentration of solute remaining in solution is measured and the amount of solute
adsorbed is calculated. Given that the mass of solid phase is known, the distribution coefficient for the specified experimental
conditions can then be calculated.
5. Significance and Use
5.1 Thistestmethodismeanttoallowforarapid(24h)indexofageomedia’ssorptionaffinityforgivenchemicalsorleachate
constituents.Alarge number of samples may be run using this test method to determine a comparative ranking of those samples,
based upon the amount of solute sorbed by the geomedia, or by various geomedia or leachate constituents. The 24-h time is used
to make the test convenient and also to minimize microbial degradation which may be a problem in longer-timed procedures. Due
to this time constraint, the final (24-h) concentration should not be confused with that of an equilibrium or steady-state
concentration. While RK values are directly applicable for screening and comparative ranking purposes, their use in predictive
d
field applications generally requires the assumption that R =K ; the validity of this assumption must be carefully evaluated by
d K
d
qualified personnel. be a fixed value.
5.2 While this test method may be useful in determining 24-h R values for nonvolatile organic constituents, interlaboratory
K
d
testing has been carried out only for the nonvolatile inorganic species, arsenic and cadmium. However, the procedure has been
tested for single laboratory precision with polychlorinated biphenyls (PCBs) and is believed to be useful for all stable and
nonvolatile inorganic, and organic constituents. This test method is not considered appropriate for volatile constituents.
5.3 The 24-h time limit may be sufficient to reach a steady-state R . However, to report this determination as a steady-state
K
d
R (that is, R =K ), the relevant time studies must be carried out to document the development of steady-state conditions within
K d d
d
the 24-h time period.Tests exceeding the 24-h time period are beyond the scope of this test method. Refer toTest Method D4319,
for an alternate procedure of longer duration. , this test method should be conducted for intermediate times (for example, 12, 18
and 22 h) to ensure that the soluble concentrations in the solution have reached a steady state by 24 h. Refer to Test Method D
4319 for an alternate procedure of longer duration.
6. Interferences
6.1 When dealing with solutes of unknown stability either in contact with the geomedia or when used as blanks, care must be
takentodetermineifvolatilization,hydrolysis,photodegradation,microbialdegradation,oxidation-reduction(thatis,(forexample,
3+ 6+
Cr to Cr ) or other physicochemical processes are operating at a significant rate within the time frame of the procedure. The
stabilityandhencelossfromsolutionmayaffecttheoutcomeofthisprocedureiftheaforementionedreactionsaresignificant.The
compatibility of the method and the solute of interest may be assessed by determining the differences between the initial solute
concentration (see 9.8) and the final blank concentration of the solute (see 9.15). If this difference is greater than the expected
precision of the method (10%), then the R value generated may be unreliable and must be carefully evaluated.
K
d
7. Apparatus
7.1 Agitation Equipment—The agitation equipment to be used is the rotary solid waste extractor specified in Test Method
D3987.
7.2 Phase Separation Equipment —A filtration apparatus made of materials compatible with the solutions being filtered and
equipped with a 0.45-µm pore size membrane filter, or a constant temperature centrifuge capable of separating particles with
diameters greater than 0.1 µm (see Section 9). If organic compounds are being measured, the filtration apparatus, centrifuge tubes
Annual Book of ASTM Standards, Vol 04.08.
Diamondstone, B. T., Burke, R. W., and Garner, E. L., “Improved Leach Measurements on Solid Wastes,” ASTM Standardization News, June 1982, pp. 28–33.
D4646–03 (2008)
etc., should be compatible with the compounds being measured (that is, glass or stainless steel). Sorption of solute onto the
filtration membrane may be significant for some solutes, and must be evaluated by the use of blanks through all steps of the
procedure.
7.3 Containers—Round, wide-mouth bottles compatible with the rotary extractor (Test Method D3987) and of composition
suitable to the nature of the solute(s) under investigation and the analysis to be performed will be us
...
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