METHOD 13151
MASS TRANSFER RATES OF CONSTITUENTS IN MONOLITHIC OR COMPACTED
GRANULAR MATERIALS USING A SEMI-DYNAMIC TANK LEACHING PROCEDURE
SW-846 is not intended to be an analytical training manual. Therefore, method
procedures are written based on the assumption that they will be performed by analysts who are
formally trained in at least the basic principles of chemical analysis and in the use of the subject
technology.
In addition, SW-846 methods, with the exception of required methods used for the
analysis of method-defined parameters, are intended to be guidance methods that contain
general information on how to perform an analytical procedure or technique, which a laboratory
can use as a basic starting point for generating its own detailed standard operating procedure
(SOP), either for its own general use or for a specific project application. Performance data
included in this method are for guidance purposes only and must not be used as absolute
quality control (QC) acceptance criteria for purposes of laboratory QC or accreditation.
1.0 SCOPE AND APPLICATION
1.1	This method is designed to provide the mass transfer rates (release rates) of
inorganic analytes contained in a monolithic or compacted granular material, under diffusion-
controlled release conditions, as a function of leaching time. Observed diffusivity and tortuosity
may be estimated through analysis of the resulting leaching test data.
1.2	This method is suitable to a wide range of solid materials which may be in
monolithic form (e.g., cements, solidified wastes) or may be compacted granular materials (e.g.,
soils, sediments and stacked granular wastes) which behave as a monolith, in that the
predominant water flow is around the material and release is controlled by diffusion to the
boundary. The method is not required by federal regulations to determine whether waste
passes or fails the toxicity characteristic as defined at 40 CFR 261.24.
1.3	This leaching characterization method provides intrinsic material parameters for
release of inorganic species under mass transfer controlled leaching conditions. This test
method is intended as a means for obtaining a series of eluents which may be used to estimate
the diffusivity of constituents and physical retention parameters of the solid material under
specified laboratory conditions.
1.4	This method is not applicable to characterize the release of organic analytes
with the exception of general dissolved organic carbon.
1.5	This method is a characterization method and does not provide a solution
considered to be representative of eluate under field conditions. This method is similar in
structure and use to predecessor methods such as MT001.1 (see Ref. 1), NEN 7345 (see Ref.
2), ANSI/ANS 16.1 (see Ref. 3), and ASTM C1308 (see Ref. 4). However, this method differs
from previous methods in that: 1) leaching intervals are modified to improve QC; 2) sample
preparation accounts for mass transfer from compacted granular samples; and, 3) mass transfer
may be interpreted by more complex release models that account for physical retention of the
1 This method has been derived from the MT001 and MT002 procedures (Ref. 1). The method is
analogous to the monolithic mass transfer methods NEN 7345 (Ref. 2) developed under Dutch regulation
and CEN/TS 15863 (Ref. 15) developed for the Comite Europeen de Normalisation (CEN).
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porous medium and chemical retention at the pore wall through geochemical speciation
modeling.
1.6	The geometry of monolithic samples may be rectangular (e.g., bricks or tiles),
cubes, wafers or cylinders. Samples may also have a variety of faces exposed to eluent,
forming anything from 1-dimensional (1-D) through 3-dimensional (3-D) mass transfer cases. In
all cases, a minimum sample size of 5 cm in the direction of mass transfer must be employed
and the liquid-surface-area ratio (L/A) must be maintained at 9  1 mL/cm2.
Monolithic samples should be suspended or held in the leaching fluid such that at least
98% of the entire sample surface area is exposed to eluent and the bulk of the eluent (e.g., a
minimum of 2 cm between any exposed surface and the vessel wall) is in contact with the
exposed sample surface. Figure 1 provides examples of appropriate sample holders and
leaching configurations for 3-D and 1-D cases.
1.7	Compacted granular materials are granular solids, screened to pass through a
2-mm sieve, compacted following a modified Proctor compaction effort (see Ref. 5). The
sample geometry must be open-faced cylinders due to limitations of mechanical packing.
However, the diameter and height of the sample holder may be altered to correspond
appropriately with the diameter and volume of the leaching vessel. In all cases, the sample size
of at least 5 cm in the direction of mass transfer must be employed and the L/A must be
maintained at 9  1 mL/cm2.
The sample should be positioned at the bottom of the leaching vessel with a minimum of
5 cm of distance between the solid-liquid interface and the top of the vessel. The distance
between the non-leaching faces (i.e., outside of the mold surfaces) and the leaching vessel wall
should be minimized to < 0.5 cm, such that the majority of the eluent volume is on top of the
sample. Figure 2 shows an example of a holder and leaching configuration for a compacted
granular sample.
1.8	The solvent system used in this characterization method is reagent water.
Other systems (e.g., groundwater, seawater, and simulated liquids) may be used to infer
material performance under specific environmental conditions. However, interaction between
the eluent and the solid matrix may result in precipitation and pore blocking, which may interfere
with characterization or complicate data interpretation.
1.9	Prior to employing this method, analysts are advised to consult the base
method for each type of procedure that may be employed in the overall analysis (e.g., Methods
9040, 9045 and 9050, and the determinative methods for the target analytes) for additional
information on QC procedures, development of QC acceptance criteria, calculations, and
general guidance. Analysts also should consult the disclaimer statement at the front of the
manual and the information in Chapter Two for: 1) guidance on the intended flexibility in the
choice of methods, apparatus, materials, reagents, and supplies; and, 2) the responsibilities of
the analyst for demonstrating that the techniques employed are appropriate for the analytes of
interest, in the matrix of interest, and at the levels of concern.
In addition, analysts and data users are advised that, except where explicitly specified in
a regulation, the use of SW-846 methods is not mandatory in response to federal testing
requirements. The information contained in this method is provided by the Environmental
Protection Agency (EPA or the Agency) as guidance to be used by the analyst and the
regulated community in making judgments necessary to generate results that meet the data
quality objectives for the intended application.
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1.10 This method is restricted to use by, or under supervision of, properly
experienced and trained personnel. Each analyst must demonstrate the ability to generate
acceptable results with this method.
2.0 SUMMARY OF METHOD
This method comprises leaching of continuously water-saturated monolithic or
compacted granular material in an eluent-filled tank with periodic renewal of the leaching
solution. The vessel and sample dimensions are chosen such that the sample is fully immersed
in the leaching solution. Monolithic samples may be cylinders or parallelepipeds, while granular
materials are compacted into cylindrical molds at optimum moisture content using modified
Proctor compaction methods (see Ref. 5). In either case, the exposure of a regular geometric
area to the eluent is recommended. Samples are contacted with reagent water at a specified
L/A. The leaching solution is exchanged with fresh reagent water at nine pre-determined
intervals (see NOTE below). The sample is freely drained and the mass is recorded to monitor
the amount of eluent absorbed into the solid matrix at the end of each leaching interval. The
eluate pH and specific conductance is measured for each time interval and analytical samples
are collected and preserved accordingly based on the determinative methods to be performed.
Eluate concentrations are plotted as a function of time, as a mean interval flux, and as a
cumulative release as a function of time. These data are used to estimate mass transfer
parameters (i.e., observed diffusivity) for each constituent of potential concern (COPC). A
flowchart for performing this method is shown in Figure 3.
NOTE: The leaching schedule may be extended for additional exchanges with individual
intervals of 14 days to provide more information about longer-term release.
3.0 DEFINITIONS
3.1	Constituent of potential concern (COPC) - A chemical species of interest,
which may or may not be regulated, but may be characteristic of release-controlling properties
of the sample geochemistry.
3.2	Release - The dissolution or partitioning of a COPC from the solid phase to the
aqueous phase during laboratory testing (or under field conditions). In this method, mass
release is expressed in units of mg COPC/kg dry solid material.
3.3	Liquid-to-surface area ratio (L/A) - The ratio representing the total liquid volume
used in the leaching interval to the external geometric surface area of the solid material. L/A is
typically expressed in units of mL of eluent/cm2 of exposed surface area.
3.4	Observed mass diffusivity - The apparent, macroscopic rate of release due to
mass transfer from a solid into a liquid as measured using a leaching test under conditions
where mass transfer controls release. The observed diffusivity accounts for all physical and
chemical retention factors influencing mass transfer and is typically expressed in units of cm2/s.
3.5	Effective mass diffusivity - The intrinsic rate of mass transfer in a porous
medium accounting for physical retention. The effective mass diffusivity is typically expressed
in units of cm2/s.
3.6	Physical retention factor - A mass transfer rate term that describes the
retardation of diffusion due to intrinsic physical properties of a porous medium (e.g., effective
porosity, tortuosity).
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3.7	Chemical retention factor - A mass transfer rate term that describes the
chemical processes (e.g., dissolution/precipitation, adsorption/desorption, complexation)
occurring at the pore water interface with the solid mineral phases within the porous structure of
the solid material.
3.8	Eluent - The solution used to contact the solid material in a leaching test. The
eluent is usually free of COPCs but may contain other species used to control the test
conditions of the extraction.
3.9	Eluate - The solution collected as an extract from a leaching test that contains
the eluent plus constituents leached from the solid phase.
3.10	Refer to Chapter One and Chapter Three, and the manufacturer's instructions
for definitions that may be relevant to this procedure.
4.0 INTERFERENCES
4.1	Solvents, reagents, glassware, and other sample processing hardware may
yield artifacts and/or interferences to sample analysis. All of these materials must be
demonstrated to be free from interferences under the conditions of the analysis by analyzing
method blanks. Specific selection of reagents and purification of solvents by distillation in all-
glass systems may be necessary. Refer to each method to be used for specific guidance on
QC procedures and to Chapters Three and Four for general guidance on glassware cleaning.
Also refer to Methods 9040, 9045, and 9050 and the determinative methods to be used for
information regarding potential interferences.
4.2	The reaction of atmospheric gases can influence the measured concentrations
of constituents in eluates. For example, reaction of carbon dioxide with eluents from highly
alkaline or strongly reducing materials will result in neutralization of eluate pH and precipitation
of carbonates. Leaching vessels, especially those used when testing highly alkaline materials,
should be designed to be airtight in order to minimize the reaction of samples with atmospheric
gases.
4.3	Use of certain solvent systems may lead to precipitation at the material surface
boundary, which may reduce mass transport rates. For example, exposure of cement-based
materials to seawater leads to sealing of the porous block (see Ref. 6).
5.0 SAFETY
5.1	This method does not address all safety issues associated with its use. The
laboratory is responsible for maintaining a safe work environment and a current awareness file
of Occupational Safety and Health Administration (OSHA) regulations regarding the safe
handling of the chemicals specified in this method. A reference file of material safety data
sheets (MSDSs) should be available to all personnel involved in these analyses.
5.2	During preparation and processing of extracts and/or eluents/eluates, some
waste materials may generate heat or evolve potentially harmful gases when contacted with
acids and bases. Adequate prior knowledge of the material being tested should be used to
establish appropriate personal protection and workspace ventilation.
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6.0 EQUIPMENT AND SUPPLIES
The mention of trade names or commercial products in this manual is for illustrative
purposes only, and does not constitute an EPA endorsement or exclusive recommendation for
use. The products and instrument settings cited in SW-846 methods represent those products
and settings used during the method development or subsequently evaluated by the Agency.
Glassware, reagents, supplies, equipment, and settings other than those listed in this manual
may be employed provided that method performance appropriate for the intended application
has been demonstrated and documented.
This section does not list common laboratory glassware (e.g., beakers and flasks) that
might be used.
6.1 Sample holder
6.1.1	Monolithic samples
6.1.1.1	A mesh or structured holder constructed of an inert
material such as high density polyethylene (HDPE) or other material resistant to
high and low pH is recommended.
6.1.1.2	The holder should be designed such that at least 98%
of the external surface area of the sample may be exposed to eluent.
6.1.1.3	The holder should be designed to match the geometry
of the mass transfer such that the bulk of the eluent may be in contact with the
sample and the exposed surfaces of the sample centered within the leaching
fluid.
NOTE: In the case of 1-D mass transfer from the axial face of a cylindrical
sample, the outer diameter (OD) of the holder should be matched as
closely as possible to the inner diameter (ID) of the leaching vessel so
that the majority of the eluent is above the sample (e.g., in contact with
the exposed material surface), while allowing for easy placement and
removal of the holder in the leaching vessel (see Figure 1).
6.1.2	Compacted granular samples
6.1.2.1	A cylindrical mold constructed of an inert material such
as HDPE or other material resistant to high and low pH is recommended.
6.1.2.2	The holder should be capable of withstanding the
compaction force required to prepare the sample (see Sec. 11.3) without
breaking or distorting.
NOTE: The outer diameter of the holder for a compacted granular sample
should be matched as closely as possible to the inner diameter of the
leaching vessel so that the majority of the eluent is above the sample
(e.g., in contact with the exposed material surface) while allowing for
easy placement and removal of the holder in the leaching vessel.
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6.2 Leaching vessel
6.2.1	A straight-sided container constructed of a material resistant to high
and low pH is recommended. Jars or buckets composed of HDPE, polycarbonate (PC),
polypropylene (PP), or polyvinyl chloride (PVC) are recommended when evaluating the
mobility of inorganic species.
6.2.2	The leaching vessel should have an airtight seal that can sustain
long periods of standing without gas exchange with the atmosphere.
6.2.3	The container must be of sufficient volume to accommodate both
the solid sample and an eluent volume based on an L/A of 9  1 ml_ /cm2 sample surface
area. Ideally, the vessel should be sized such that the headspace is minimized within
the tolerance of the L/A.
6.3 Leaching setup
Example photos of three possible leaching equipment arrangements for monolithic and
compacted granular samples are shown in Figures 1 and 2, respectively. The equipment used
in the each of these cases is described below.
6.3.1	Figure 1a shows a monolithic sample 3-D configuration with the
following accessories:
Sample holder - PP sink washers, 43-mm OD, 37-mm ID, 6-mm high, with four
holes drilled at the quadrants to accept 2-mm OD nylon string knotted at the top
Sample stand - PVC pipe, 47-mm OD, 51-mm high, cut to have four legs
approximately 8-mm wide and 30-mm high
Leaching Vessel - PP bucket, 140-mm ID at top, 120-mm ID at bottom,
200-mm high (Berry Plastics #T51386CP3, VWR Scientific, or equivalent)
6.3.2	Figure 1b shows a monolithic sample 1-D configuration with the
following accessories:
Sample holder - Polyethylene (PE) mold, 54-mm OD, 100-mm high
(MA Industries, Peach Tree City, GA, or equivalent), with the test sample cured in mold
and cut to 51-mm high
Leaching vessel -250-mL PC jar, 60-mm ID, 100-mm high (Nalgene #2116-
0250, Fisher Scientific, or equivalent)
6.3.3	Figure 2 shows a compacted granular sample 1-D Configuration
with the following accessories:
Sample holder - PE mold, 100-mm OD, 200-mm high, (MA Industries, Peach
Tree City, GA, or equivalent) cut to 63-mm high with three tabs drilled for 0.7-mm fishing
line knotted at the top
Leaching vessel - 1000-mL PC jar, 110-mm ID at top, 130-mm high (Nalgene
#2116-1000, Fisher Scientific, or equivalent)
Glass beads, borosilicate - 2-mm diameter
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6.4	Filtration apparatus - Pressure or vacuum filtration apparatus composed of
appropriate materials to maximize the collection of extracts and minimize the loss of COPCs
(Nalgene #300-4000 or equivalent)
6.5	Filtration membranes - Composed of hydrophilic polypropylene or equivalent
material with an effective pore size of 0.45 |jm (e.g., Andwin Scientific GH Polypro 28143-288 or
equivalent)
6.6	pH meter - Laboratory model with the capability for temperature compensation
(e.g., Accumet 20, Fisher Scientific or equivalent) and a minimum resolution of 0.1 pH units
6.7	pH combination electrode - Composed of chemically resistant materials
6.8	Conductivity meter - Laboratory model (e.g., Accumet 20, Fisher Scientific or
equivalent), with a minimum resolution of 5% of the measured value
6.9	Conductivity electrodes - Composed of chemically resistant materials
6.10	Proctor compactor (for compacted granular samples only) - Equipped with a
slide hammer capable of dropping a 4.5-kg weight over a 0.46-m interval (see Ref. 5 for further
details)
7.0 REAGENTS AND STANDARDS
7.1	Reagent-grade chemicals, at a minimum, should be used in all tests. Unless
otherwise indicated, all reagents should conform to the specifications of the Committee on
Analytical Reagents of the American Chemical Society (ACS), where such specifications are
available. Other grades may be used, provided the reagent is of sufficiently high purity to permit
its use without lessening the accuracy of the determination. Inorganic reagents and extracts
should be stored in plastic to prevent interaction of constituents from glass containers.
7.2	Reagent water - Reagent water must be interference-free. All references to
water in this method refer to reagent water unless otherwise specified.
7.3	Other reagents may be used in place of reagent water on a case-specific basis.
8.0 SAMPLE COLLECTION, PRESERVATION, AND STORAGE
8.1	See Chapter Three, "Inorganic Analytes," and Chapter 4, "Organic Analytes,"
for sample collection and preservation instructions.
8.2	Both plastic and glass containers are suitable for the collection of samples. All
sample containers must be prewashed with a metal-free detergent and triple-rinsed with nitric
acid and reagent water, depending on the history of the container. For further information, see
Chapter Three.
9.0 QUALITY CONTROL
9.1 Refer to Chapter One for guidance on quality assurance (QA) and quality control
(QC) protocols. When inconsistencies exist between QC guidelines, method-specific QC
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criteria take precedence over both technique-specific criteria and Chapter One criteria, and
technique-specific QC criteria take precedence over Chapter One criteria. Any effort involving
the collection of analytical data should include development of a structured and systematic
planning document, such as a quality assurance project plan (QAPP) or a sampling and
analysis plan (SAP), which translates project objectives and specifications into directions for
those who will implement the project and assess the results.
Each laboratory should maintain a formal QA program. The laboratory should also
maintain records to document the quality of the data generated. Development of in-house QC
limits for each method is encouraged. Use of instrument-specific QC limits is encouraged,
provided such limits will generate data appropriate for use in the intended application. All data
sheets and QC data should be maintained for reference or inspection.
9.2	In order to demonstrate the purity of reagents and sample contact surfaces,
method blanks should be tested for each leaching interval. Refer to Chapter One for specific
QC procedures.
9.3	The analysis of extracts should follow appropriate QC procedures, as specified
in the determinative methods for the COPCs. Refer to Chapter One for specific QC procedures.
9.4	Initial demonstration of proficiency (IDP)
Leachate methods are not amenable to typical IDPs when reference materials with
known values are not available. However, prior to using this method an analyst should have
documented proficiency in the skills required for successful implementation of the method. For
example, skill should be demonstrated in the use of an analytical balance, the determination of
pH using Methods 9040 and 9045 and the determination of conductance using Method 9050.
10.0 CALIBRATION AND STANDARDIZATION
10.1	The balance should be calibrated and certified, at a minimum, annually or in
accordance with laboratory policy.
10.2	Prior to measurement of eluate pH, the pH meter should be calibrated using a
minimum of two standards that bracket the range of pH measurements. Refer to Methods 9040
and 9045 for additional guidance.
10.3	Prior to measurement of eluate conductivity, the meter should be calibrated
using at least one standard at a value greater than the range of conductivity measurements.
Refer to Method 9050 for additional guidance.
11.0 PROCEDURE
A flowchart of this method is presented in Figure 3. Microsoft Excel data templates are
available to aid in collecting and archiving of laboratory and analytical data.2
11.1 Preparatory Procedures - Determination of solids and moisture content
2 These Excel templates form the basis for uploading method data into the data management program,
TM	TM
LeachXS Lite . Both the data templates and LeachXS Lite are available at
http://vanderbilt.edu/leachinq.
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The moisture and solids content of the sample material are used to relate leaching
results to dry-material masses. When preparing compacted granular samples for testing, the
moisture content or solid content is used to determine the optimum moisture content following
the modified Proctor test. This method calculates moisture content on the basis of the "wet" or
"as-tested" sample.
WARNING: The drying oven should be contained in a hood or otherwise properly ventilated.
Significant laboratory contamination or inhalation hazards may result when drying
heavily contaminated samples. Consult the laboratory safety officer for
proper handling procedures prior to drying samples that may contain volatile,
hazardous, flammable, or explosive materials.
11.1.1	Place 5 -10 g of solid sample material into a tared dish or crucible.
Dry the sample to a constant mass at 105  2 C. Check for constant mass by returning
the dish to the drying oven for 24 hours, cooling to room temperature in a desiccator and
re-weighing. The two mass readings should agree within the larger of 0.2% or 0.02 g.
NOTE: The oven-dried sample is not used for the extraction and should be properly
disposed of once the dry mass is determined.
11.1.2	Calculate and report the solids content as follows:
SC = dry
M test
Where: SC = solids content of "as-tested" material (g-dry/g)
Mdry = mass of dry material specified in the method (g-dry)
Mtest = mass of "as-tested" solid equivalent to the dry-material mass (g)
11.1.3 Calculate and report the moisture content (wet basis) as follows:
ur _ ^test ~~ Mdry
wet " M
1 nest
Where: MCwet = moisture content on a wet basis (gH2o/g)
Mdry = mass of dry material specified in the method (g-dry)
Mtest = mass of "as-tested" solid equivalent to the dry-material mass (g)
11.2 Preparation of monolithic samples
11.2.1	If the material to be tested is granular, disregard this section and
proceed to Sec. 11.3.
11.2.2	A representative sample of monolithic material should be obtained
by molding material components in place (e.g., cementitious media) or by coring or
cutting a sample from a larger existing specimen.
11.2.3 The geometry of monolithic samples may be rectangular (e.g.,
bricks or tiles), cubes, wafers, or cylinders. Samples may also have a variety of faces
exposed to eluent forming 1-, 2-, or 3-D mass transfer cases. Examples of monolithic
sample leaching setups are shown in Figure 1.
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11.2.4	A minimum sample size of 5 cm in the direction of mass transfer
must be employed and the L/A must be maintained at 9  1 mL/cm2.
NOTE: Since the sample holder and leaching vessel must correspond to the
specifications in Sec. 6.1, it is often easier to modify the sample size and
geometry rather than the holder and vessel dimensions.
11.2.5	Proceed to Sec. 11.4.
11.3 Preparation of compacted granular samples
Compacted granular materials, in most cases, must be open-faced cylinders due to the
limitations of mechanical packing. However, the diameter and height of the sample holder may
be altered to work appropriately with the diameter and volume of the leaching vessel. In all
cases, a minimum sample size of 5 cm in the direction of mass transfer must be employed and
the L/A must be maintained at 9  1 mL/cm2.
Granular samples are compacted into the sample holder using a variation on the
modified Proctor compaction (see Ref. 5) to include the use of 6-cm high-test molds. Shorter or
taller molds (or packing depths) may be used as long as the compaction effort of 56,000 ft-1bf/ft3
is achievable. The number of packing layers should be maintained at the five layers specified in
Ref. 5. However, the number of blows per layer in a 4-in diameter mold may be changed
according to the follow formula:
Where: h is the measured height of the sample mold (ft).
Thus, for the mold height of 4.584 in (0.382 ft) specified in the ASTM procedure, 25 blows per
each of 5 layers are required. When a 6-cm (0.196 ft) mold height is used (as suggested in this
method), 13 blows per each of 5 layers are required to obtain the same compaction effort.
The granular sample should be compacted at a moisture content corresponding to 90% of the
modified Proctor optimum packing density in order to provide a uniform approach to obtaining a
sample density that approximates field conditions. Optimum moisture content refers to the
amount of moisture or fractional mass of water (gH2o/g material) in the granular sample that is
present at the optimum packing density (g-dry material/cm3). Optimum packing density is
defined in Ref. 5. The optimum moisture content of the test material is determined from a pre-
test that measures the packing density of granular materials compacted at different levels of
moisture content.
11.3.1 Pre-test to determine optimum moisture content
The pre-test is conducted as a series of five batch-wise packing trials with
consecutive increases in moisture content until the maximum packing density has been
surpassed. The optimum moisture content is determined as the maximum of a third-
order polynomial fit through the graph of dry-packing density as a function of moisture
content (wet basis).
56,000 ft-lbf blow
65.2 x hh\ow
ft3 1.5 ft x 10 lbf 5 layer
layer
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11.3.1.1 Place 1500 g of "as received" material into a pail or
bowl and mix well by hand to homogenize. As an alternative to hand mixing, a
mechanical paddle mixer may be used.
NOTE: The pre-test may be conducted from a bulk supply of solid material
(e.g., 10 kg total for five batches) as long as the starting mass for each
trial is recorded and incremental water additions are used.
11.3.1.2	Mix a known amount of tap water with the bulk material
in the pail or bowl until homogenized based on visual inspection. For the first
point in the pre-test, no water needs to be added.
NOTE: The amount of water added should be enough to increase the moisture
content in approximately 3 - 5% increments. Smaller additions may be
needed in order to provide finer resolution of the packing density as a
function of the moisture content curve.
11.3.1.3	Calculate the new moisture content (wet basis) for the
trial as follows:
MCi
Mtest X MCwet + Wadded
Msl + W>ad,d
Where:
MC(wet) = moisture content on a wet basis of the pre-test trial (gH2o/g)
Mtest = mass of "as-tested" solid equivalent to the dry-material mass (g)
MO(Wet) = moisture content on a wet basis of the "as-tested" material
(9H2o/g)
Wadded = mass of water added to the "as-tested" material (gH2o/g)
11.3.1.4	Compact approximately 1000 g of material into a tared
10-cm diameter mold into three consecutive layers of material. The compacted
mass should have a level, flat surface as a top face.
11.3.1.5	Measure and record the height, diameter, and mass of
the resulting compacted material.
11.3.1.6	Calculate and record the packing density (dry basis) as
follows:
_ m x SC f2V
Ppack "T71T d
Where:
Ppack = packing density (dry basis) (g-dry/cm3)
m = mass of the compacted sample (g)
SC = solids content of "as-tested" granular material (g-dry/g)
d = measured diameter of the compacted sample (cm)
h = measured height of the compacted sample (cm)
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11.3.1.7	Repeat Sec. 11.3.1.1 - 11.3.1.6 for four subsequent
trials until the value of the calculated packing density decreases.
11.3.1.8	Plot the packing density as a function of moisture
content. Figure 4 shows an example of a packing density curve.
11.3.1.9	Determine the optimum moisture content at the
maximum of the packing density curve. This value may be read directly from
the graph or determined by the maximum of a third-order polynomial fit through
the five pre-test data points (see the Microsoft Excel Template).
11.3.2 Compacted granular test sample preparation
11.3.2.1	Using the optimum moisture content determined in
Sec. 11.3.1.9, calculate the amount of "as-received" material that is required to
pack the sample holder to within 3 mm of the rim of the holder.
Where:
Mtest = mass of "as tested" solid equivalent to the dry-material mass (g)
p0pt = optimal packing density (dry basis) (g-dry/cm3)
determined in Sec. 11.3.1.9
h = measured height of the sample mold (cm)
SC = solids content of "as-tested" granular material (g-dry/g)
d = measured diameter of the sample mold (cm)
11.3.2.2	Adjust the moisture content of the "as-received"
material to the optimum moisture content using reagent water and mix until
homogenized.
11.3.2.3	Pack the sample material into the sample holder using
the modified Proctor compaction as described in Ref. 5.
11.3.2.4	Place a monolayer of borosilicate glass beads (Sec.
6.3.3) on the exposed sample surface to minimize scouring and mass loss
during testing.
11.3.2.5	Begin the leach test procedure promptly or cover the
sample with plastic wrap to minimize moisture loss to the atmosphere.
11.4 Leaching procedure
This protocol is a semi-dynamic, tank-leaching procedure (see schematic in Figure 5)
where the sample is exposed to eluate for a series of leaching intervals interspersed with eluent
exchanges. The chemical composition of each eluate is determined and mass transfer from the
bulk solid is determined as a function of cumulative leaching time. The schedule of leaching
intervals for this method is shown in Table 1.
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11.4.1	Pre-test measurements - For the surface area calculation, measure
and record the dimensions of the test specimen. This should include the diameter and
height for a cylinder; length, width, and depth for a parallelepiped; or diameter of
exposed surface for a compacted granular sample.
11.4.2	Measure and record the mass of the specimen. This value should
be monitored for each eluent exchange.
11.4.3	If a holder is used, place the specimen in the monolith holder.
11.4.4	Measure and record the mass of the specimen and holder, if
applicable.
11.4.5	The recommended temperature for conducting this method is room
temperature (20  2 C). When conducted at temperature readings or variations other
than those recommended, record the ambient temperature at each eluent renewal.
11.5 Eluent exchange
11.5.1	Fill a clean leaching vessel with the required volume of reagent
water based on an L/A of 9  1 mL/cm2. Record the amount of eluent used.
11.5.2	Carefully place the specimen or the specimen and holder in the
leaching vessel (Figure 6a) so that the sample is centered in the eluent (see Figure 6b).
Submersion should be gentle enough so that the physical integrity of the monolith is
maintained and scouring of the solid is minimized.
11.5.3	Cover the leaching vessel with the airtight lid and place in a safe
location until the end of the leaching interval. Table 1 shows the schedule of leaching
intervals and cumulative release times for this method.
NOTE: Eluates of alkaline materials may be susceptible to neutralization through
reaction with carbon dioxide. Precautions (e.g., ensuring airtight vessels or
purging headspace) should be taken to minimize the effect of carbonation on
eluates that may sit stationary for more than one week.
11.5.4	Prior to the end of the leaching interval, repeat Sec. 11.5.1 in order
to prepare a vessel for the next leaching interval.
11.5.5	At the end of the leaching interval (see Table 1), carefully remove
the specimen or the specimen and holder from the vessel (Figure 6c). Drain the
liquid from the surface of the specimen into the eluate for approximately 20 sec.
11.5.6	Measure and record the mass of the specimen or the mass of the
specimen and holder (Figure 6d).
NOTE: The change in sample mass between intervals is an indication of the potential
absorption of eluent by the matrix (mass gain) or erosion of the matrix (mass
loss). In the case where a holder is used, moisture may condense on the holder
during the leaching interval and sample absorption may not be evident.
NOTE: Mass gain may also be indicative of carbonate precipitation if the vessel is not
tightly sealed and carbon dioxide is absorbed from the atmosphere.
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11.5.7	Place the specimen or the specimen and holder into the clean
leaching vessel filled with new eluent as prepared in Sec. 11.5.4.
11.5.8	Cover the new leaching vessel with the airtight lid and place in a
safe location until the end of the leaching interval.
11.6 Eluate processing
11.6.1	Measure and record the pH, specific conductivity, and oxidation
reduction potential (ORP) of the eluate of the decanted eluate from the previous leaching
interval (see Methods 9040, 9045, and 9050).
NOTE: Measurement of pH, conductivity, and ORP should be taken within 15 minutes of
eluent exchange (Sec. 11.5) to avoid neutralization of the solution due to
exposure to carbon dioxide, especially when alkaline materials are tested.
NOTE: The measurement of ORP is optional, but strongly recommended, especially
when testing materials where oxidation is likely to change the chemistry of
COPCs.
11.6.2	Filter the remaining eluate through a 0.45-|jm membrane (Sec. 6.5).
11.6.3	Immediately preserve and store the volume(s) of eluate required for
chemical analysis. Preserve all analytical samples in a manner that is consistent with
the determinative chemical analyses to be performed.
11.6.4	Collect all subsequent eluate by repeating the eluent exchange and
eluate processing procedures in Sees. 11.5 and 11.6.
12.0 DATA ANALYSIS AND CALCULATIONS
12.1 Data reporting
12.1.1	Figure 7 shows an example of a data sheet which may be used to
report the concentration results of this method. At a minimum, the basic test report
should include the following:
a)	Name of the laboratory
b)	Laboratory technical contact information
c)	Date and time at the start of the test
d)	Name or code of the solid material
e)	Material description (including monolithic or compacted granular)
f)	Moisture content of material used (gH2o/g)
g)	Dimensions (cm) and geometry of sample used
h)	Mass of solid material used (g)
i)	Mass of sample and holder at start of test (g)
j) Eluate type (e.g., reagent water)
k) Eluate-specific information (see Sec. 12.1.2 below)
12.1.2	The minimum set of data that should be reported for each eluate
includes:
a) Eluate sample ID
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b)	Target eluent exchange date and time
c)	Actual eluent exchange date and time
d)	Volume of eluent used (ml_)
e)	Mass of sample and holder (g)
f)	Measured eluate pH
g)	Measured eluate conductivity (mS/cm)
h)	Measured ORP (mV) (optional)
i)	Concentration of all COPCs
j) Analytical QC qualifiers as appropriate
12.2 Data presentation
12.2.1	Interval concentrations
12.2.1.1	At the conclusion of the schedule of leaching intervals
(see Table 1), the concentration of COPCs in each eluate may be plotted as a
function of cumulative leaching time. An example of this is shown in Figure 8
for mass transport from a monolithic field sample of fixated scrubber sludge and
lime.
12.2.1.2	If data is available from Method 1313, interval
concentrations and Method 1313 data may be plotted on the same graph as a
function of eluate pH. This QC step is conducted in order to determine whether
the concentration of COPCs approached equilibrium in any leaching interval
(i.e., the driving force for mass transport from the matrix may not be constant,
which is a common assumption of dynamic-tank leach testing). Figure 9 shows
this type of graph for the release from a field sample of fixated scrubber sludge
and lime.
12.2.2	Interval mass release
At the conclusion of the schedule of leaching intervals (see Table 1), the
interval mass released can be calculated for each leaching interval as follows:
A
Where:
M t. = mass released during the current leaching interval, i (mg/m2)
Ci = constituent concentration in the eluate for interval i (mg/L)
Vi = eluate volume in interval i (L)
A = specimen external geometric surface area exposed to
the eluent (m2)
12.2.3 Mean interval flux
The flux of a COPC in an interval may be plotted as a function of the
generalized mean of the square root of cumulative leaching time (^T). An example of a
flux graph is show in Figure 10 for the release from a field sample of fixated scrubber
sludge with lime. This graph may be used to interpret the mechanism of release (see
Ref. 7 for further details).
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12.2.3.1 The flux across the exposed surface of the sample can
be calculated by dividing the interval mass release by the interval duration as
follows:
Fj
Where:
F| = flux for interval, i (mg/m2s)
M|= mass released during the current leaching interval, i (mg/m2)
ti = cumulative time at the end of the current leaching interval, i (s)
tM = cumulative time at the end of the previous leaching interval, i-1 (s)
12.2.3.2 The time used to plot each interval mass is the
generalized mean of the square root of the cumulative leaching time using the
cumulative time at the end of the ith interval, th and the cumulative time at the
end of the previous interval, tM.
11 = generalized mean leaching time for the current interval, i (s)
t| = cumulative time at the end of the current leaching interval, i (s)
tM = cumulative time at the end of the previous leaching interval, i-1 (s)
NOTE: If the concentrations of a COPC in the eluates approach that shown in
Method 1313 for liquid-solid equilibrium, the flux curve will show the
pattern in Figure 10 with intervals of the same duration having the same
flux value. When the eluate concentration approaches saturation, the
driving force for mass transfer approaches zero, interval flux is limited,
and intervals with like durations will display similar flux limitations.
12.2.4 Cumulative release
summed to provide the cumulative mass release as a function of leaching time.
Figure 11 shows the cumulative release curves for a field sample of fixated
scrubber sludge with lime.
12.2.4.2 Interpretation of the cumulative release of constituents
is illustrated using the analytical solution for simple radial diffusion from a
cylinder into an infinite bath presented by Crank (see Ref. 6).
v
y
Where:
12.2.4.1 The interval release calculated in 12.2.2 can be
i/
72
Mt = 2pC0
v
71
J
Where:
Mt = cumulative mass released during leaching interval i (mg/m2)
p = density of the "as-tested" sample (kg/m3)
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C0 = concentration of available COPC in the solid matrix (mg/kg)
Dobs = observed diffusivity (m2/s)
t = leaching time (s)
When transformed to a log-log scale, the analytical solution
presented by Crank becomes linear with the square root of time.
log[Mt ] = log
2pC0
( pobs \/2
V 71 /
1
-t
2
Thus, under the assumptions of the analytical solution presented by
Crank, the mass release should be proportional to the square root of time. A
line showing the square root of time is plotted in Figure 11 along with the data.
Since flux is the derivative of release, a similar treatment of flux as a function of
leaching time using the simple diffusion model would be proportional to the
negative square root of time as shown in Figure 10.
Models other than the simple diffusion model presented by Crank
may also be used to interpret mass release. For example, the Shrinking
Unreacted Core Model (see Ref. 8) and the Coupled Dissolution-Diffusion
Model (see Ref. 9) incorporate chemical release parameters (e.g., as derived
from Method 1313 data) into the model to better estimate release mechanisms
and predictions (see Ref. 7 for further details).
12.2.5 Observed diffusivity
An observed diffusivity for each COPC can be determined using the logarithm
of the cumulative release plotted versus the logarithm of time. In the case of a diffusion-
controlled mechanism, this plot is expected to be a straight line with a slope of 0.5. An
observed diffusivity can then be determined for each leaching interval where the slope is
0.50  0.15 (see Refs. 10 and 11) by the following:
DbS -rr
i = Tt
M,
2PCo(Vti A-1 )
Where:
Dbs = observed diffusivity of a COPC for leaching interval i (m2/s)
Mt. = mass released during leaching interval i (mg/m2)
t| = cumulative contact time at the end of the current leaching interval, i (s)
tM = cumulative contact time at the end of the previous leaching interval, i-1 (s)
p = sample density (dry basis) (kg-dry/m3)
Co = initial leachable content (i.e., available release potential) (mg/kg)
The mean observed diffusivity for each COPC is then determined by taking the
average of the interval observed diffusivities. It should be reported with the computed
uncertainty (i.e., standard deviation).
NOTE: Since the analysis presented above assumes a diffusion process, only those
interval mass transfer coefficients corresponding to leaching intervals with slopes
of 0.50 0.15 are included in the overall average mass-transfer coefficient.
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12.3
Data representation by constituent
A concise representation of all relevant data for a single constituent may be presented
as shown in Figure 12 for arsenic from a field core of fixated scrubber sludge with lime (FSSL)
material. The data shows eluate pH generation as a function of leaching time (Figure 12a),
comparison between eluate concentrations and Method 1313 data as a function of eluate pH
(Figure 12b), constituent flux as a function of generalized mean cumulative leaching time
(Figure 12c), and constituent release as a function of cumulative leaching time (Figure 12d).
12.4 Interpolation/extrapolation to target time values
The collected time dependence data may be interpolated or extrapolated to the nearest
target cumulative time (It) value for purposes of comparing different data sets (e.g., test
replicates of the same or different materials). The most transparent and straightforward
method is linear interpolation/extrapolation of data after log10 transformation.
12.4.1	Log10 transformation
Collected concentration values are transformed by taking the log10 of the
measured concentration at each test position, i:
Q = log10(Ci)
Where:
Ci = log10-transformed concentration at test position i (log10[mg/L])
q = the concentration measured at test position i (mg/L)
12.4.2	Linear interpolation/extrapolation
Given a set of coordinate data {(It ,Cj): i = 1,...n} sorted by increasing order
according to It value (e.g., It-i < It2 <  < Itn), an interpolated/extrapolated log10-
transformed concentration at a known It target is calculated as:
Cj = a j + bj'Itj
Where:
CT = the concentration at target It value, ItT (log10[s])
aT and bT are coefficients of the linear interpolation/extrapolation equation.
ItT = a target cumulative time value
Depending on the values of observed It values relative to target It values, the
calculations of the coefficients aT and bT in the equation may differ according to the
following algorithm:
	If ItT < Iti, then bT = (C2 - Ci) / (It2 - ItO and aT = C2 - bTIt2 (extrapolation from
the two points with closest It values)
	If ItT > Itn, then bT =(Cn - Cn-i) / (Itn - Itn-i) and aT = Cn - bT Itn (extrapolation
from the two points with closest It values)
	If Itj-! < ItT < Itj, then bT = (C, - Cj-0 / (It, - Itj-0 and aT = y, - bT Itj
(interpolation from the two closest points surrounding ItT)
NOTE: Interpolation or extrapolation of data should only be conducted within a distance
of 20% of the target It value. Since the allowable US tolerance about a target
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L/S value is variable (see Table 1), interpolation/extrapolation should not create
data at a target It value where collected data is missing.
13.0 METHOD PERFORMANCE
13.1	Performance data and related information are provided in SW-846 methods
only as examples and guidance. The data do not represent required performance criteria for
users of the methods. Instead, performance criteria should be developed on a project-specific
basis, and the laboratory should establish in-house QC performance criteria for the application
of this method. Performance data must not be used as absolute QC acceptance criteria for
laboratory QC or accreditation.
13.2	Interlaboratory validation of this method was conducted using a solidified waste
analog (material code SWA) and a contaminated smelter site soil (material code CFS).
Repeatability and reproducibility was determined for mean interval flux excluding the first wash-
off interval (see Table 2) and for cumulative mass released after 63 days of leaching (see Table
3). More details on the interlaboratory validation may be found in Ref. 14.
13.3	References 1 and 7 may provide additional guidance and insight on the use,
performance, and application of this method.
14.0 POLLUTION PREVENTION
14.1	Pollution prevention encompasses any technique that reduces or eliminates the
quantity and/or toxicity of waste at the point of generation. Numerous opportunities for pollution
prevention exist in laboratory operations. The EPA has established a preferred hierarchy of
environmental management techniques that places pollution prevention as the management
option of first choice. Whenever feasible, laboratory personnel should use pollution prevention
techniques to address their waste generation. When wastes cannot be feasibly reduced at the
source, the Agency recommends recycling as the next best option.
14.2	For information about pollution prevention that may be applicable to
laboratories and research institutions consult Less is Better: Laboratory Chemical Management
for Waste Reduction, a free publication available from the ACS, Committee on Chemical Safety,
http://portal.acs.Org/portal/fileFetch/C/WPCP 012290/pdf/WPCP 012290.pdf.
15.0 WASTE MANAGEMENT
The EPA requires that laboratory waste management practices be conducted consistent
with all applicable rules and regulations. Laboratories are urged to protect air, water, and land
by minimizing and controlling all releases from hoods and bench operations, complying with the
letter and spirit of any sewer discharge permits and regulations, and by complying with all solid
and hazardous waste regulations, particularly the hazardous waste identification rules and land
disposal restrictions. For further information on waste management, consult The Waste
Management Manual for Laboratory Personnel available from the ACS at the web address listed
in Sec. 14.2.
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16.0 REFERENCES
1.	D.S. Kosson, H.A. van der Sloot, F. Sanchez and A.C. Garrabrants, "An Integrated
Framework for Evaluating Leaching in Waste Management and Utilization of Secondary
Materials," Environmental Engineering Science, 19(3) 159-204, 2002.
2.	NEN 7345, "Leaching Characteristics of Solid Earth and Stony Materials - Leaching
Tests - Determination of the Leaching of Inorganic Constituents from Molded and
Monolithic Materials with the Diffusion Test," Dutch Standardization Institute, Delft, The
Netherlands, 1995.
3.	ANSI/ANS 16.1, "American National Standard Measurement of the Leachability of
Solidified Low-Level Radioactive Wastes by a Short-term Test Procedure," American
Nuclear Society, La Grange Park, IL, 1986.
4.	ASTM D1308-95, "Standard Method for Accelerated Leach Test for Diffusive Releases
from Solidified Waste and a Computer Program to Model Diffusive, Fractional Leaching
from Cylindrical Waste Forms," ASTM International, West Conshohocken, PA, 2001.
5.	ASTM D1557-07, "Standard Method for Laboratory Compaction Characteristics of Soil
Using Modified Effort (56,000 ft-lbf/ft3 (2,700 kN-m/m3))," ASTM International, West
Conshohocken, PA.
6.	D.E. Hockley and H.A. van der Sloot, "Long-term Processes in a Stabilized Coal Waste
Block Exposed to Seawater," Environmental Science and Technology, 25(8), 1408-1414,
1991.
7.	A.C. Garrabrants, D.S. Kosson, H.A. van der Sloot, F. Sanchez and O. Hjelmar,
"Background Information for the Leaching Environmental Assessment Framework
(LEAF) Test Methods," EPA/600/R-10-170, U.S. Environmental Protection Agency,
Washington, DC, December 2010.
8.	Crank, Mathematics of Diffusion, Oxford University Press, London, 1986.
9.	Hinsenveld, and P.L. Bishop "Use of the shrinking core/exposure model to describe the
leachability from cement stabilized wastes," in Stabilization and Solidification of
Hazardous, Radioactive, and Mixed Wastes, 3rd Volume, ASTM STP 1240, T.M. Gilliam
and C.C. Wiles (eds), American Society for Testing and Materials, Philadelphia, PA,
1996.
10.	Sanchez, "Etude de la lixiviation de milieux poreux contenant des especes solubles:
Application au cas des dechets solidifies par Hants hydrauliques," doctoral thesis, Institut
National des Sciences Appliquees de Lyon, Lyon, France, 1996.
11.	International Ash Working Group (IAWG), Municipal Solid Waste Incinerator Residues,
Elsevier Science Publishers, Amsterdam, the Netherlands, 1997.
12.	J. de Groot, and H. A. van der Sloot, "Determination of Leaching Characteristics of
Waste Materials Leading to Environmental Product Certification," in Solidification and
Stabilization of Hazardous, Radioactive, and Mixed Wastes, 2nd Volume, ASTM STP
1123, T.M. Gilliam and C.C. Wiles (eds), American Society for Testing and Materials,
Philadelphia, PA, 1992.
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13.	A.C. Garrabrants and D.S. Kosson, "Leaching Processes and Evaluation Tests for
Inorganic Constituents Release from Cement-Based Matrices," in
Solidification/Stabilization of Hazardous, Radioactive and Mixed Wastes, R. Spence and
C. Shi (eds.), CRC Press, 2005.
14.	A.C. Garrabrants, D.S. Kosson, R. DeLapp, P. Kariher, P.F.A.B. Seignette, H.A. van der
Sloot, L. Stefanski, and M. Baldwin, "Interlaboratory Validation of the Leaching
Environmental Assessment (LEAF) Method 1314 and Method 1315," Draft, U.S.
Environmental Protection Agency, Washington DC, April 2012.
15.	CEN/TS 15863, Characterization of waste - Leaching Behaviour Tests - Dynamic
Monolithic Leaching Test with Periodic Leachant Renewal, Comite Europeen de
Normalisation, Brussels, Belgium, 2009.
17.0 TABLES, DIAGRAMS, FLOWCHARTS, AND VALIDATION DATA
The following pages contain the tables and figures referenced by this method.
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TABLE 1
SCHEDULE OF ELUATE RENEWALS
Interval Label
Interval
Duration
(h)
Interval
Duration
(d)
Cumulative
Leaching Time
(d)
T01
2.0  0.25
-
0.08
T02
23.0  0.5
-
1.0
T03
23.0  0.5
-
2.0
T04
-
5.0  0.1
7.0
T05
-
7.0  0.1
14.0
T06
-
14.0  0.1
28.0
T07
-
14.0  0.1
42.0
T08
-
7.0  0.1
49.0
T09
-
14.0  0.1
63.0
NOTE: This schedule may be extended for additional 14-day contact intervals
to provide more information regarding longer-term release.
TABLE 2
METHOD PRECISON FOR MEAN INTERVAL FLUX (2nd - 9th Intervals)
Repeatability	Reproducibility
Analyte
Symbol
SWA
%RSDr
CFS
%RSDr
SWA
%RSDr
CFS
%RSDr
Aluminum
Al
7.3
13.3
25.3
25.3
Antimony
Sb
9.2
14.8
21.8
23.8
Arsenic
As
19.9
-
31.1
-
Barium
Ba
13.2
7.5
44.8
18.3
Boron
B
10.8
7.2
27.3
27.1
Cadmium
Cd
-
7.6
-
23.2
Calcium
Ca
8.1
6.6
28.7
26.0
Chromium
Cr
10.2
-
23.8
-
Lead
Pb
-
4.3
-
19.8
Potassium
K
12.4
10.8
28.8
40.1
Selenium
Se
10.9
13.3
30.8
32.4
Vanadium
V
8.5
11.3
22.3
30.6
Mat
erial Mean
11%
10%
29%
27%
Overall Mean
11
%
28%
NOTE: First interval is removed from mean interval flux because of variances associated with
wash-off of surface contaminants that do not pertain to the method precision.
Data taken from Reference 14.
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TABLE 3
METHOD PRECISON FOR CUMULATIVE RELEASE AFTER 63 DAYS
Repeatability	Reproducibility
Analyte
Symbol
SWA
%RSDr
CFS
%RSDr
SWA
%RSDr
CFS
%RSDr
Aluminum
Al
5.4
5.3
23.6
22.9
Antimony
Sb
6.9
5.9
19.7
14.4
Arsenic
As
15.9
-
31.0
-
Barium
Ba
7.5
3.9
35.6
16.5
Boron
B
8.4
3.7
22.6
25.7
Cadmium
Cd
-
4.8
-
18.4
Calcium
Ca
4.6
3.2
23.9
24.6
Chromium
Cr
7.7
-
17.7
-
Lead
Pb
-
1.6
-
12.0
Potassium
K
10.8
6.3
24.8
44.4
Selenium
Se
8.7
3.6
26.7
20.5
Vanadium
V
5.7
4.2
21.1
22.8
Mat
erial Mean
8%
4%
25%
22%
Overall Mean
6%
23%
Data taken from Reference 14.
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FIGURE 1
EXAMPLES OF MONOLITHIC SAMPLE HOLDERS
a) 3-D Configuration
Nylon
Test Sample

47 mm OD
3 mm wait
51 mm high
Sample Holder
b) 1-D Configuration
Sample, Holder and Stand
3-D Leaching Setup
Test Sample
PP Mo
100 mm hig
Empty Sample Holder
Full Sample Holder
1-D Leaching Setup
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FIGURE 2
EXAMPLE COMPACTED GRANULAR SAMPLE HOLDER AND SETUP
/ Fishing line
0.7 mm diameter
Empty Sample Holder
Compacted Sample
1-D Leaching Setup
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FIGURE 3
METHOD FLOWCHART
Material of
Interest
Solids/Moisture Content
(Section 11.1)
Is the
material
monolithic?
Compaction Pre-Test
(Section 11.3.1)
no
yes

Sample Preparation
(Sec. 11.2)
Sample Preparation
(Section 11.3.2)
Leaching Procedure
(Sec. 11.4)
Pre-Test Measurements (Sec. 11.4.1)
Eluant Exchange (Sec. 11.5)
Eluate Processing (Sec. 11.6)
Extract Analysis
Documentation and
Graphing
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FIGURE 4
EXAMPLE CURVE OF PACKING DENSITY AS A FUNCTION OF MOISTURE CONTENT
y = 55.975X3 - 65.036x2 + 1.8352
r2 = 0.983
2.65
maximum density
2 60
3 2.55

1 2.50
ai
245
optimum moisti
0,120 gH2o/S
t
2.35
2.30
0
00
0.05
0.10
0.20
0.25
Moisture Content fflmo/g]
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FIGURE 5
SCHEMATIC OF SEMI-DYNAMIC MASS TRANSFER TEST PROCESS
1 Sample
n Leaching Intervals
Monolith
(allfaces exposed)
Compacted Granular
(1 circular face exposed)
or
1
JL
c


A
1

V
7

Li
^7^At2^7 ^7 Atn
QJ
5P	ro
=	>
TO	*-
_Z	CD
U
x .E
c
ro ^
oi a!
-O
V
iCT
A
n

V
7



I
mn
N
analytical
samples
Figure obtained and modified from Ref. 11.
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FIGURE 6
EXAMPLE LEACHING PROCEDURE STEPS
Start of Leaching Interval
Sample Centered in Eluant {top view)
Removing Sample for Exchange
Mass of Sample and Holder
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FIGURE 7
EXAMPLE DATA REPORTING FORMAT
ABC Laboratories
123 Main Street
Anytown, USA
Contact: John Smith
(555) 111-1111
Material Code
EPA METHOD 1315
Report of Analysis
XYZ
Client Contact: Susan Jones
(555) 222-2222
Particle Size: 88% passing 2-mm sieve

Material Type: Coal Combustion Fly Ash
Mass used in Column:
860 g


Date Received: 10/1/20xx



Moisture Content:
0.002 gH2o/g


Test Sta rt Date: 11/1 /20xx



Sample Geometry:
Cylinder


Report Date: 12/1/20xx



Sample Diameter
10.0 cm






Sample Depth:
60.3 cm


Test Type: Compacted Granular

Mass of Sample & Holder
1020 g


Eluent: ASTM Type II Water


Lab Temperature:
21  2 C

Test







Position
Replicate
Value
Units

Method
Note

T01
A







Eluate Sample ID
XYZ-1315-T01-A





Exchange Date 1
1/1/20xx






Target Exchange Time
12:00
PM





Actual Exchange Time
12:15
PM





Mass of Sample & Holder
1026
g





Eluate Mass
730.4
g





Eluate pH
8.82
-

EPA 9040



Eluate Conductivity
5.4
mS/c

EPA 9050



Eluate ORP
NA
mv








QC


Dilution

Chemical Analysis
Value
Units
Flag
Method
Date
Factor

Al
4.72
mg/L

EPA 6020
11/7/20xx
1000

As
0.12
mg/L

EPA 6020
11/7/20xx
10

CI
5.42
mg/L

EPA 9056
11/9/20xx
1
Test







Position
Replicate
Value
Units

Method
Note

T02
A







Eluate Sample ID
XYZ-1315-T02-A





Exchange Date 1
1/1/20xx






Target Exchange Time
12:00
PM





Actual Exchange Time
12:18
PM





Mass of Sample & Holder
1027
g





Eluate Mass
725.0
g





Eluate pH
9.15
-

EPA 9040



Eluate Conductivity
2.8
mS/c

EPA 9050



Eluate ORP
NA
mv








QC


Dilution

Chemical Analysis
Value
Units
Flag
Method
Date
Factor

Al
2.99
mg/L

EPA 6020
11/7/20xx
1000

As
0.21
mg/L

EPA 6020
11/7/20xx
10

CI
4.20
mg/L
U
EPA 9056
11/7/20xx
1
QC Flag Key: U Value below lower limit of quantitation as reported (< "LLOQ")
1315-30
Revision 0
January 2013

-------
FIGURE 8
EXAMPLE INTERVAL CONCENTRATION GRAPHS
1000
100
J
ro 10
0.1
0.01
u


AF
OF
SSL-A
SSL-B

2

a




:

	

	1	1	'	


1000
100
0.1
0.01
1000
20 40 60 80
Leaching Time [days]


AFSSL-A
OFSSL-B
U





6
a




	




c)
20 40 60
Leaching Time [days]
80
D)
E
3
"O
U
b)
E
3
^5
ro
c
ro
>
10
0.1
0.01


AFSSL-A
OFSSL-B








1



UA
o
O"

0 o
~
DA
i * 1
a
 * 
20 40 60 80
Leaching Time [days]
1000
0.1
0.01


AFSSL-A
OFSSL-B

a

Q
:



I


	
	1	1	L	
* 1 
1 ' ' 1 1

d)
20 40 60
Leaching Time [days]
80
NOTE: Orange lines represent cumulative release if all eluate extracts were at the quantitation limit
(dashed) and detection limit (solid). Chemical analyses below the detection limit are shown at
% the detection limit value.
1315-31
Revision 0
January 2013

-------
FIGURE 9
EXAMPLE OF SATURATION CHECK BETWEEN INTERVAL CONCENTRATIONS
AND METHOD 1313 DATA
100000
10000
_ 1000
_l
a 100
o
10
1
0.1
0.01
c
cu
3)
On
n


~ Method 1313 
AFSSL-A

~


rOOL-D









hni






IUI_









:	

	
	

	
	
- -"-H

H-'-H

H-'-H
H-'-H
H-J-J-
a)
100000
10000
IT 1000
100
0 2 4 6 8 10 12 14
Eluate pH
2,
E
3
"E
_Q)
a>
V)
10
1
0.1
0.01



~ Method 1313
AFSSL-A
OFSftl -R
: 1=0
r
5






Wi











IB
















c)
4 6 8 10 12 14
Eluate pH
1000
100 -!

E
~o
w
O
0.1
0.01
- Qd
D


~ Method 1313
A FSSL-A
OFSSL-B
I

~




:
C

nn


:




[LjU]

:



A

' ' '
I 1 1 1 l
H-'-H
l 1 ' ' 1
MJ>
| i i i | i i i i

b)
m
n.
E
_3
fB
tz
>
100000
10000
' 1000 -fc
100 -I
10 -t
1
0.1
0.01
~
~
0
4 6 8 10 12 14
Eluate pH
O
~ Method 1313
AFSSL-A
OFSSL-B
~
~
-=3
~ 4
3
I
   i    i 
d)
4 6 8
Eluate pH
10 12 14
NOTE: Orange lines represent cumulative release if all eluate extracts were at the quantitation limit
(dashed) and detection limit (solid). Chemical analyses below the detection limit are shown at
1/2 the detection limit value.
1315-32
Revision 0
January 2013

-------
FIGURE 10
EXAMPLE INTERVAL FLUX GRAPHS
1.E-03
1.E-04
1.E-05 -t
E,
x
~
c
CD
in
< 1.E-08
1.E-09
 6" -
^ A




Q slope

= -1/2
*r-J
 -


:

-

-j AFSSL-A
 OFSSL-B
	 			i_

v
. i ..in.
' IM'"l
	1i iinn,
a)
0.01 0.1 1 10 100
Mean Interval [days]
1.E-04
tn
N
E
"3>
X
3
C
0)
CO
e)
1.E-08
1.E-09
: ir--
V .


; -

^slope-
A <
o
= -1/2
"k
: \
\


\-
\_

I AFSSL-A
; OFSSL-B
, 		
- 1,1	1 ""'!
0.01 0.1 1 10 100
Mean Interval [days]
{/)
N
E
"ro
X
3
b)
1.E-05
1.E-06
1.E-07 - e
~ 1.E-08 -
1.E-09
1	1 ' I 1 ! M 1 r
i/>o
/
r




:Iope = -1/2
, -r>J l


* o
\
V.
3 I



	
: AFSSL-A
- OFSSL-B
 itiii i i i i mi
1 1 1 11 111
pocl
0.01 0.1 1 10 100
Mean Interval [days]
1.E-03
X
w
E
o>

X
D
Li.
E
~
03
c
A3
>
d)
1.E-07
1.E-08
1.E-09
L  slope = -1/2


!

fl'Q^
: -

! \
; \

-

I

"X
	1	11JLLL1
AFSSL-A
: OFSSL-B
_ i i i 11 Hq i i i i mi|
	ji i 11 iiij
0.01 0.1 1 10 100
Mean Interval [days]
NOTE: Orange data represent cumulative release if all eluate extracts were at the quantitation limit
(dashes) and detection limit (solid line).
1315-33
Revision 0
January 2013

-------
FIGURE 11
INTERVAL FLUX AT ELUATE SATURATION
1,000

100
1
2
3
m
m
 10
X
B

N,
Equal-
ly inter
i ;
...J	,1	,1		t,	I	I	I,,,, I,, ,1,, ,f,, 1,4	1	1	.1	1.,,, ,1, ,1,, 1,, 1,1	1	f,	1	1,, ,i,, I,, 1, A,
0.01
0.1
10
100
Mean Flux Time [days]
NOTE: This figure assumes that the concentration in the eluate approaches saturation during the
leaching interval (i.e., the driving force for diffusion approaches zero). When the leaching
solution is saturated, the resulting mass release and interval flux is constant for intervals
of the same duration.
1315-34
Revision 0
January 2013

-------
FIGURE 12
EXAMPLE CUMULATIVE RELEASE GRAPHS
1000
100
10
1
0.001
- A FSSL-A
-r OFSSL-B


.
n
o
CD 0.1
oc
E
=3
E
~o
CCS
O
E
*~)
JE
0)
(/)
OS
_0)
0
a:
E
3
03
C
03
>
w
d)
0.01
b)
0.001
1000
100
10
1
0.1
0.01
0.001
A FSSL-A
OFSSL-B
slope -1/2

1-
"t-
	I 	
0.01
0.1 1 10 100
I Leaching Time [days]



: A FSSL-A
OFSSL-B



1

:
\ slope:
= 1/2

- ^
.

m




i i i i mi
0.01 0.1 1 10 100
I Leaching Time [days]
NOTE: Orange data represent cumulative release if all eluate extracts were at the quantitation limit
(dashes) and detection limit (solid line).
1315-35
Revision 0
January 2013

-------
FIGURE 13
DATA REPRESENTATION BY CONSTITUENT (QUAD FORMAT)
11
10 -
i
Q.
&
to
LU
O
~
o
~
2a
9
8 -
AFSSL-A
OFSSL-B
J	1	1 I I 1 1
20 40 60 80
I Leaching Time [days]
1.E-03
1.E-04
1.E-05
1.E-06
o 1.E-07
c
0)
(fi
 1.E-08
1.E-09
c)
CM
E
o>
E^
x
3
: 6





0 slope = -1/2
A-l-J
; -




\-
-




-
-[ ArSSL-A
j OFSSL-B
	1	
	1 I I inn
	 	
0.01 0.1 1 10
Mean Interval [days]
100
100000
10000
, 1000
100
10
0.01
: Q]
~


~ Method 1313-1
AFSSL-A
DFSSL-B

~








%
~rnn







'S














	
- -j-j-h
1 ' ' 1
1 ' '
' ' '
P-'-H
1 1 " 1

b)
0 2 4 6 8 10 12 14
Eluate pH
E
o:
E
o>
in
CD

tn

<
W
d)
1000
100
10
0.1
o.oi i

A FSSL-A
OFSSL-B



-

*>'-b

:



j slope =
:
1/2 ^  ~4,

1





- ~	-




1 1 1 1 llll
0.01 0.1 1	10 100
 Leaching Time [days]
NOTE: Orange data represent cumulative release if all eluate extracts were at the quantitation
limit (dashes) and detection limit (solid line).
1315-36
Revision 0
January 2013

-------