EPA/600/R-10/170 

November 2010 

Background Information for the Leaching Environmental 

Assessment Framework (LEAF) Test Methods 
EPA-600/R-10/170 

November 2010

Background Information for the Leaching Environmental 

Assessment Framework (LEAF) Test Methods 

Andrew C. Garrabrants1, David S. Kosson1, Hans A. van der Sloot2, 

Florence Sanchez1

, Ole Hjelmar3

1 Vanderbilt University 

Department of Civil and Environmental Engineering 

Nashville, TN 

2 Energy Research Centre of the Netherlands 

Environmental Risk Assessment Group 

Petten, the Netherlands 

and 

Van der Sloot Consultancy 

Langedijk, the Netherlands 

3 DHI 

Hørsholm, Denmark 

Category III / Applied Research 

Contract No. EP-C-09-027 

Work Assignment No. 1-7 

Prepared for: 

Susan A. Thorneloe 

U.S. Environmental Protection Agency 

Office of Research and Development 

National Risk Management Research Laboratory 

Air Pollution Prevention and Control Division 

Research Triangle Park, NC 27711
i 

Foreword

The U.S. Environmental Protection Agency (EPA) is charged by Congress with protecting 

the Nation’s land, air, and water resources. Under a mandate of national environmental laws, 

the Agency strives to formulate and implement actions leading to a compatible balance 

between human activities and the ability of natural systems to support and nurture life. To 

meet this mandate, EPA’s research program is providing data and technical support for 

solving environmental problems today and building a science knowledge base necessary to 

manage our ecological resources wisely, understand how pollutants affect our health, and 

prevent or reduce environmental risks in the future. 

The National Risk Management Research Laboratory (NRMRL) is the Agency’s center for 

investigation of technological and management approaches for preventing and reducing risks 

from pollution that threaten human health and the environment. The focus of the 

Laboratory’s research program is on methods and their cost-effectiveness for prevention and 

control of pollution to air, land, water, and subsurface resources; protection of water quality 

in public water systems; remediation of contaminated sites, sediments, and ground water; 

prevention and control of indoor air pollution; and restoration of ecosystems. NRMRL 

collaborates with both public and private sector partners to foster technologies that reduce the 

cost of compliance and to anticipate emerging problems. NRMRL’s research provides 

solutions to environmental problems by: developing and promoting technologies that protect 

and improve the environment; advancing scientific and engineering information to support 

regulatory and policy decisions; and providing the technical support and information transfer 

to ensure implementation of environmental regulations and strategies at the national, state, 

and community levels. 

This publication has been produced as part of the Laboratory’s strategic long-term research 

plan. It is published and made available by EPA’s Office of Research and Development to 

assist the user community and to link researchers with their clients. 

 

 Sally Gutierrez, Director 

National Risk Management Research Laboratory 
ii 

ACKNOWLEDGEMENTS 

The information presented in this document is based on the collaborative research of 

Vanderbilt University, the Energy Research Centre of the Netherlands, DHI (Demark), U.S. 

EPA’s Office of Research and Development and Office of Resource Conservation and 

Recovery with additional support provided by ARCADIS-US. The authors thank P. Kariher, 

R. Delapp, L.H. Turner and P. Seignette for analytical and data management support, and M. 

Baldwin, G. Helms, and S. Thorneloe for guidance and significant contributions to the 

research reported in this documented. 
iii 

 

ABSTRACT 

The U.S. Environmental Protection Agency Office of Resource Conservation and Recovery 

has initiated the review and validation process for four leaching tests under consideration for 

inclusion into SW-846: 

Method 1313*

 “Liquid-Solid Partitioning as a Function of Extract pH for Constituents in 

Solid Materials using a Parallel Batch Extraction Procedure” 

Method 1314*

 “Liquid-Solid Partitioning as a Function of Liquid-Solid Ratio for 

Constituents in Solid Materials using an Up-flow Percolation Column Procedure” 

Method 1315*

 “Mass Transfer Rates of Constituents in Monolithic or Compacted 

Granular Materials using a Semi-dynamic Tank Leaching Procedure” 

Method 1316*

 “Liquid-Solid Partitioning as a Function of Liquid-Solid Ratio for 

Constituents in Solid Materials using a Parallel Batch Extraction Procedure” 

*

 Method identification numbers are subject to change. 

These protocols are derived from published leaching methods contained in the Leaching 

Environmental Assessment Framework (LEAF), an integrated set of testing methods, data 

management tools, and report support utilities that can be used to support a wide range of 

environmental management decisions. The methods comprise a suite of available leaching 

tests, including batch, column and tank tests, which may be interpreted individually or 

integrated to provide characteristic leaching behavior of a solid material over a range of 

potential release scenarios. LEAF also includes tools for visualizing leaching data and 

significantly facilitating data management through the LeachXS LiteTM expert leaching 

system software program. 

LEAF represents a considerable shift in leaching assessment methodology from current 

approaches which are typically based on single-point pH tests and not necessarily reflective 

of management conditions. Thus, this document provides the required background necessary 

to understand the development, application, and use of these four test methods. The 

document includes sections on an overview of the leaching process, selection of test 

parameters, and estimates of the time, material and costs required. 

Subsequent reports in this series will focus on (i) the inter-laboratory validation of the LEAF 

test methods, (ii) the relationship between LEAF testing results and field leaching 

observations, and (iii) applications of the LEAF testing approach for evaluating use and 

disposal options of coal combustion residues. 
iv 

 

ABBREVIATIONS 

CEN European Committee for Standardization 

COPC Constituent of Potential Concern 

DOC Dissolve Organic Carbon 

EC Electrical Conductivity [mS/cm] 

ECN Energy research Centre of the Netherlands 

EPA United States Environmental Protection Agency 

FNU Formazin Nephelometric Unit 

ISO International Standardization Organization 

LEAF Leaching Environmental Assessment Framework 

L/S Liquid-to-Solid Ratio [mL/g, dry mass basis] 

L/A Liquid-to-Surface Area Ratio [mL/cm2

, geometric surface area basis] 

LSP Liquid-Solid Partitioning 

MC Moisture Content [g water/g wet mass basis] 

ORP Oxidation/Reduction Potential [mV] 

PAH Polycyclic Aromatic Hydrocarbon 

pD Diffusivity [m2

/s] in terms of the negative logarithm (-log[m2/s]) 

POM Particulate Organic Matter 

PTFE Polytetrafloroethylene 

RCF Relative Centrifugal Force 

SAB Science Advisory Board 

SC Solids Content 

TCLP Toxicity Characteristic Leaching Procedure 

TOC Total Organic Carbon 
v 

 

TABLE OF CONTENTS 

Acknowledgements ........................................................................................................... ii

Abstract ............................................................................................................................iii

Abbreviations ................................................................................................................... iv

Table of Contents .............................................................................................................. v

List of Figures ................................................................................................................viii

List of Tables.................................................................................................................... ix

1 Introduction .............................................................................................................. 1

2 Leaching overview ................................................................................................... 2

3 Leaching Assessment Framework............................................................................ 5

3.1 Leaching Tests .................................................................................................. 6

3.1.1 Influence of pH on Equilibrium .................................................................. 7

3.1.2 Influence of Liquid-to-Solid Ratio on Equilibrium..................................... 7

3.1.3 Influence of Mass Transfer Rates................................................................ 8

4 Method Summaries and Justification of Test Parameters ........................................ 8

4.1 Preliminary Version of Method 1313 ............................................................... 9

4.1.1 Method Summary ........................................................................................ 9

4.1.2 Constituents of Potential Concern............................................................. 10

4.1.3 Target pH Values....................................................................................... 10

4.1.4 Eluent Composition................................................................................... 11

4.1.5 Minimum Dry Mass Equivalent ................................................................ 12

4.1.6 Particle Size, Liquid-To-Solid Ratio and Contact Time ........................... 13

4.1.7 Temperature............................................................................................... 18

4.1.8 Agitation.................................................................................................... 18

4.1.9 Filtration .................................................................................................... 18

4.2 Preliminary Version of Method 1314 ............................................................. 19

4.2.1 Method Summary ...................................................................................... 19

4.2.2 Particle Size............................................................................................... 19
vi 

4.2.3 Constituents of Potential Concern............................................................. 20

4.2.4 Eluent Composition................................................................................... 21

4.2.5 Minimum Column Dimensions ................................................................. 21

4.2.6 Solids Packing ........................................................................................... 21

4.2.7 Sand Layers ............................................................................................... 21

4.2.8 Pre-Equilibration ....................................................................................... 22

4.2.9 Flow Rate .................................................................................................. 22

4.2.10 Temperature............................................................................................... 23

4.2.11 Filtration and Centrifugation ..................................................................... 23

4.2.12 Eluate Collection and Compositing for Analytical Samples..................... 23

4.3 Preliminary Version of Method 1315 ............................................................. 25

4.3.1 Method Summary ...................................................................................... 25

4.3.2 Constituents of Potential Concern............................................................. 25

4.3.3 Sample Preparation and Geometry............................................................ 26

4.3.4 Eluent Composition................................................................................... 27

4.3.5 Liquid-To-Surface Area Ratio................................................................... 28

4.3.6 Tank-Sample Geometry ............................................................................ 28

4.3.7 Temperature............................................................................................... 29

4.3.8 Eluent Exchange Sequence ....................................................................... 29

4.3.9 Filtration .................................................................................................... 32

4.4 Preliminary Version of Method 1316 ............................................................. 33

4.4.1 Method Summary ...................................................................................... 33

4.4.2 Constituents of Potential Concern............................................................. 33

4.4.3 Eluent Composition................................................................................... 33

4.4.4 Minimum Dry Mass Equivalent ................................................................ 34

4.4.5 Specified Liquid-To-Solid Ratios ............................................................. 35

4.4.6 Particle Size, Liquid-To-Solid Ratio, and Contact Time .......................... 35

4.4.7 Temperature............................................................................................... 41

4.4.8 Agitation.................................................................................................... 41

4.4.9 Filtration .................................................................................................... 41
vii 

5 Estimates of Laboratory Processing Time, Material Requirements and 

Supply/Equipment Costs ........................................................................................ 44

5.1 Labor/Processing Time ................................................................................... 44

5.2 Material Requirements.................................................................................... 52

5.3 Supplies and Equipment ................................................................................. 52

6 References .............................................................................................................. 54

Appendix A. Preliminary Version of Method 1313 

Appendix B. Preliminary Version of Method 1314 

Appendix C. Preliminary Version of Method 1315 

Appendix D. Preliminary Version of Method 1316 

Appendix E. Details of Time, Materials, and Cost Estimates by Method 
viii 

LIST OF FIGURES 

Figure 1. Internal and external factors influencing the leaching process (modified from 

Garrabrants and Kosson, 2005). ................................................................................................4

Figure 2. Contact time required for a species with an observed diffusivity of 10-13 m

2

/s to 

reach 90% of equilibrium ( ) based on mass transport as functions of particle 

diameter and fractional solubility ( ). Figure modified from Garrabrants, 1997. ......16

Figure 3. Contact time required for a particle of 0.3 mm diameter to reach 90% of 

equilibrium ( ) as function of diffusivity and fractional solubility ( ). 

Figure modified from Garrabrants, 1997. ...............................................................................17

Figure 4. Evaluation of depth of depletion C(x,t)/Co=0.8 as a function of diffusion 

coefficient (pD is the negative logarithm of the diffusion coefficient)...................................27

Figure 5. Hypothetical internal mass flux assuming the exchange intervals in the tank leach 

test were long enough to results in equilibrium between solid and bulk liquid phases: (a) 

common test methods and (b) Method 1315. ..........................................................................31

Figure 6. Contact time required for a species with an observed diffusivity of 10-13 m

2

/s to 

reach 90% of equilibrium ( ) based on mass transport as functions of particle 

diameter and fractional solubility ( ). Figure modified from Garrabrants, 1997. ......39

Figure 7. Contact time required for a particle of 0.3 mm diameter to reach 90% of 

equilibrium ( ) as function of diffusivity and fractional solubility ( ). 

Figure modified from Garrabrants, 1997. ...............................................................................40

Figure 8. Gantt Style Chart of A Typical Method 1313 Processing Schedule.......................46

Figure 9. Gantt Style Chart of a Typical Method 1314 Processing Schedule. .......................48

Figure 10. Gantt Style Chart of a Typical Method 1315 Processing Schedule. .....................49

Figure 11. Gantt Style Chart of a Typical Method 1316 Processing Schedule. .....................51
ix 

LIST OF TABLES 

Table 1. Rationale for Method 1313 Final pH Targets...........................................................10

Table 2. Extraction parameters as function of maximum particle size. .................................17

Table 3. Suggested Solid Amounts for Method 1316. ...........................................................35

Table 4. Extraction Parameters as Function of Maximum Particle Size................................41

Table 5. Comparison of Test Specifications for Preliminary Versions of Methods 1313, 

1314, 1315, and 1316. .............................................................................................................42

Table 6. Summary of Estimates for Labor Time and Total Processing Time........................44

Table 7. Summary of Solid Materials Required for Test Methods ........................................52

Table 8. Summary of Estimated Supply and Equipment Costs (as of July 2010) .................53
1 

1 INTRODUCTION 

The U.S. Environmental Protection Agency (U.S. EPA) Office of Resource Conservation and 

Recovery has initiated the review and validation process for four leaching tests under 

consideration for inclusion in its analytical chemistry guidance, SW-846.1 These protocols 

are derived from published leaching methods (Kosson et al. 2002) and international standards 

in various states of development and validation on wastes (CEN/TS 14405 2004; CEN/TS 

14429 2005; CEN/TS 14997 2005; CEN/TS 15863 2009), construction products (CEN/TS-2 

2009; CEN/TS-3 2009), and soils (ISO/TS 21268-3 2007; ISO/TS 21268-4 2007; ISO/DIS 

12782 parts 1-5 2010) with further collaborative development between Vanderbilt 

University, the Energy research Centre of the Netherlands (ECN) and DHI in Denmark. 

The four test methods supported in this document provide the required materials leaching 

information for the Leaching Environmental Assessment Framework (LEAF). These 

methods have been used as the basis for evaluation of process variables in the leaching of 

coal combustion residues (Sanchez et al. 2006; Sanchez et al. 2008; Kosson et al. 2009; 

Thorneloe et al. 2010); however, broader application of these test methods can be used to 

estimate constituent leaching from a wide range of solid materials in the context of disposal, 

beneficial use in construction applications, and evaluation of treatment effectiveness. 

LEAF is an integrated set of testing methods, data management and visualization tools, and 

report support utilities that can be used to support a wide range of environmental 

management decisions. Within the framework, testing characterizes the leaching behavior of 

a material under equilibrium and dynamic conditions through the use of a suite of four broadbased test methods including batch, column and tank tests. The results of these tests may be 

interpreted individually or integrated to provide characteristic leaching behavior of a solid 

material over a range of potential release scenarios. The methods are applicable to a wide 

range of solid materials, including combustion residues, soils, sediments, construction 

materials, industrial process residues, for estimation of constituent release, with a focus to 

date on inorganics, in the context of disposal, beneficial use in construction applications, and 

evaluation of treatment effectiveness, and remediation. Data management, comparison of 

test results to previously characterized materials and report output support is greatly 

facilitated by the LeachXS LiteTM expert leaching system software program.2

 

1

These methods have not been incorporated into, nor endorsed by, SW-846 to date but are in the review and 

evaluation process. 

2

 The development of LeachXSTM Lite is the result of collaboration between EPA, Vanderbilt University, the 

Energy research Centre of the Netherlands and DHI (Denmark). The LeachXS Lite program, LEAF test 

methods and data management templates are available free of charge at www.vanderbilt.edu/leaching. 
2 

Due to the shift in leaching assessment methodology that these methods represent, this 

document is intended to provide the background necessary to understand the development 

basis for the four preliminary versions of methods under consideration for adoption into SW846. The document includes sections on the selection of test parameters and estimates of the 

time, materials and costs associated with conducting a full characterization of a solid 

material. 

Preliminary versions of the methods are provided in separate appendices as follows: 

Appendix A –Method 1313*

 “Liquid-Solid Partitioning as a Function of Extract pH for 

Constituents in Solid Materials using a Parallel Batch Extraction Procedure” 

Appendix B – Method 1314*

 “Liquid-Solid Partitioning as a Function of Liquid-Solid 

Ratio for Constituents in Solid Materials using an Up-flow Percolation Column 

Procedure” 

Appendix C – Method 1315* “Mass Transfer Rates of Constituents in Monolithic or 

Compacted Granular Materials using a Semi-dynamic Tank Leaching Procedure” 

Appendix D – Method 1316*

 “Liquid-Solid Partitioning as a Function of Liquid-Solid 

Ratio for Constituents in Solid Materials using a Parallel Batch Extraction 

Procedure” 

*

 Method identification numbers are subject to change. 

Each test method includes an optional Excel® template for data collection and data transfer 

into LeachXS Lite. 

This report is the first in a series documenting the development, validation and 

implementation of the four LEAF leaching test methods for providing a source term for the 

next generation of environmental assessment methodologies. Subsequent reports will focus 

on (i) the inter-laboratory validation of the LEAF test methods, (ii) the relationship between 

LEAF testing results and field leaching observations, and (iii) applications of the LEAF 

testing approach for evaluating use and disposal options of coal combustion residues. 

2 LEACHING OVERVIEW 

Leaching in an environmental context is the process of constituent transfer from a solid 

material to a contacting liquid or aqueous phase. The release of constituents is governed by a 

combination of chemical processes and mass transfer mechanisms based on the chemical 

composition and physical properties of the solid material along with the pH, redox and 

composition (i.e., dissolved constituents) of the contacting liquid. Constituents of potential 

concern (COPCs) may include major mineral components, highly soluble salts, and 

environmental contaminants. In general, the term “leachability” is used to describe either the 
3 

extent of leaching or time-dependence of release. In environmental applications, leaching 

represents the source term for release of potentially hazardous substances. Additionally, 

leachability also can provide an indication of material durability based on the dissolution and 

transport of the constituents that comprise the solid matrix. 

Figure 1 shows the internal and external factors that influence the extent and rate of leaching 

in a generic release scenario (Garrabrants and Kosson 2005). Transport of constituents 

within the material is controlled by physical parameters such as porosity and permeability as 

well as the mass transport characteristics and equilibrium between the pore solution and solid 

mineral phases. Although Figure 1 depicts the influences on the leaching behavior of a 

monolithic product, the same basic principles apply to finer-grained materials in which 

groundwater contact and leaching occur according to a percolation model. 

Equilibrium in the pore solution is determined by the pH of the pore water (primarily for 

inorganic species), the available content of the constituent in the material, and a series of 

chemical reactions (e.g., sorption/desorption, precipitation/dissolution, complexation) that are 

also influenced by redox potential and ionic strength. For many cases, the kinetics of these 

chemical processes are fast relative to the rate of mass transport (Dijkstra et al. 2006). 

Therefore, the assumption of local equilibrium is a reasonable approximation of leaching in 

granular materials or the pore concentration within the core of a monolithic material. 

Typically, equilibrium, or liquid-solid partitioning (LSP), is determined on the basis of 

constituent concentrations as a function of pH or liquid-to-solid ratio; however, equilibrium 

data may also be reported in terms of the mass of constituent release per unit mass of solid 

material. The mass transport of species through the pore structure to the bulk solid-liquid 

interface often is controlled by a combination of local equilibrium and diffusion properties. 

The rate of mass transport may be reported as mass release per unit surface area of bulk 

interface with respect to time. Characterization of equilibrium and mass transport properties 

as leaching parameters provides a fundamental behavioral pattern of the solid material 

regardless of the release scenario. 
4 

Figure 1. Internal and external factors influencing the leaching process (modified from 

Garrabrants and Kosson, 2005). 

At the material interface, interaction of the solid materials with the surroundings can lead to 

alteration of the material release behavior. In some cases, reactions with components of the 

groundwater or subsurface atmosphere may increase release (e.g., through acid attack, 

erosion, chelation or complexation reactions), while in other cases, release may be reduced 

(e.g., via precipitates which form boundary layers with reduced transport properties). Many 

of these external stresses affect both the leaching properties and durability of the material. 

For example, the composition of the contacting solution, or leachant, has some influence on 

leaching response. Acids and chelants can interact with the inherent chemistry of the solid 

phase and alter the LSP of the resultant leachate. 

In this document, “solid material” is used as a generic reference to the matrix of concern, 

regardless of its nature (e.g., monolithic, granular) in the field. “Leachant” and “leachate” 

are reserved to describe, respectively, the contacting liquid in the natural environment before 

and after contact with the solid. The associated terms for the contacting fluids used in the 

laboratory to characterize the release of constituents from solid materials are referred to as 

“eluent” (before contact) and “eluate” (after contact), respectively. This distinction is made 

to avoid confusion with field samples during lab-to-field comparisons. Thus, eluents are the 

liquid phase specified in leaching tests (e.g., Method 1313 uses dilute acid or base as an 

eluent) while the eluates that result from a leaching test are processed for chemical analysis. 
5 

3 LEACHING ASSESSMENT FRAMEWORK 

The leaching test methods presented under LEAF were developed to be part of a tiered 

assessment methodology that is a more robust, yet flexible, evaluation approach for 

estimating environmental release, particularly in applications where current regulatory tests 

are not required (e.g., beneficial use determinations, waste delisting, treatability evaluations, 

etc.). Under the current regulatory approach, environmental assessment is based on the 

simulation of release in a defined “mismanagement” or near-surface disposal scenario (U.S. 

EPA 1988; U.S. EPA 1999a). The source term used in this assessment is described by 

release estimates for selected metals and organic compounds resulting from single-point 

extraction tests which have been designed to simulate the release conditions for the 

assessment scenario. However, the U.S. EPA Science Advisory Board (U.S. EPA 1991; U.S. 

EPA 1999b; U.S. EPA 2003), the National Academy of Sciences (NRC 2006) and others 

(Sanchez et al. 2006; Thorneloe et al. 2009) have criticized these leaching methods for a lack 

of critical data collection (e.g., final pH is not recorded), overly-broad application for 

materials and scenarios outside the scope of the test design, and limited mechanistic 

understanding due to the single release observation provided by the test. In addition, the 

results of these simulation tests are limited to the pre-determined assessment scenarios and 

are unlikely to address the range of leaching conditions expected occur in actual disposal or 

reuse situations. 

Recognizing the importance of having a robust, mechanistic environmental assessment 

methodology, U.S. EPA conducted a review of available methods, sought Science Advisory 

Board input on the suitability of the available leaching test methods, and ultimately selected 

the tiered assessment published in the literature (Kosson et al. 2002). The series of 

recommended leaching tests published with this manuscript have become the basis for 

development of the methods described in this document. 

The recommended testing increases in detail and complexity depending on the overall 

purpose of the leach testing, the amount of leaching mechanism detail needed, and the 

scenario to be evaluated. In the proposed tiered testing approach, Tier 1 tests provide the 

least amount of information used for screening purposes. Single batch extractions and 

modified versions of the characterization tests shown here may be applicable for screening, 

much as commonly used leach tests provide screening level data. Tier 2 consists of 

equilibrium-based testing of the material in order to characterize the LSP over a broad range 

of plausible management conditions as a function of principle chemical leaching factors of 

pH and liquid-solid ratio (L/S). The pH- and L/S-dependent leaching tests can also be 

adapted for compliance testing between batches of like materials or against the previous full 

detail characterizations, or material specific quality control. Equilibrium tests applicable for 

Tier 2 analysis include Methods 1313, 1314, and 1316. The addition of mass transfer rate 

(monolith or compacted granular materials) testing using Method 1315 completes the 

assessment approach for a third tier of testing for (a) detailed characterization, (b) 
6 

compliance testing, and (c) quality control. The test methods and interpretation protocols 

recommended in LEAF provide an integrated approach for evaluating leaching behavior of 

materials using a tiered approach that considers pH, liquid-to-solid ratio (L/S), and waste 

form properties across a range of plausible field conditions (Kosson et al. 2002; Thorneloe et 

al. 2010). 

3.1 LEACHING TESTS 

Various leaching methodologies applicable to a wide variety of waste forms have been 

reviewed (Garrabrants and Kosson 2005) where it was noted that release from solid materials 

is most often estimated using the results of one or more extraction tests designed to measure 

COPC leaching from materials. Although more than 50 leaching tests have been identified 

for various purposes and materials, only a limited number address a range of test conditions. 

That is, most leach tests currently being used are designed to simulate constituent release 

under a single set of assumptions. Many of these tests are only loosely related to the 

environmental conditions under which leaching of the tested material may actually (or 

plausibly) occur. In addition, many of the tests that do cover a range of conditions differ in 

only minor ways, inferring that a limited set of carefully selected tests can provide 

information on constituent leaching over the expected range of possible exposure conditions 

(van der Sloot et al. 1997). 

In general, leaching test approaches have been designed to simulate release under a specific 

set of experimental conditions (i.e., attempt to mimic field conditions). Another approach is 

to challenge the waste material to a broad range of experimental conditions known to affect 

constituent leaching, with the intent to derive characteristic or fundamental intrinsic 

parameters that control leaching. The latter approach allows one data set to be used to 

evaluate a range of management scenarios for a material, representing different 

environmental conditions (e.g., disposal or beneficial use). This approach is both more 

transparent and flexible for assessing the characteristic leaching behavior from granular and 

monolithic materials (Kosson et al. 2002; van der Sloot 2002b; van der Sloot 2002a; van der 

Sloot and Kosson 2007; van der Sloot et al. 2007). 

Leaching test methods may be categorized by whether the intent of the method is to establish 

equilibrium between the material and the leachant (e.g., “equilibrium-based test”) or to 

measure constituent mass transport as a function of leaching time (e.g., “mass transfer-based 

tests”). Test procedures additionally may be designed as “batch extraction methods” during 

which a solid material is challenged to one or more aliquots of a leaching solution over a 

specified time or as “dynamic leaching methods” where fresh leaching solution is 

continuously supplied and equilibrium between the test material and the leachant is not 

intended to be achieved. 

The methods supported in this document are designed to provide characterization of leaching 

from a solid material under a broad range of conditions with equilibrium leaching determined 
7 

as functions of pH and L/S in addition to mass transport determined as a function of leaching 

time. Of the four methods described in this document, Methods 1313 and 1316 are batch 

leaching procedures, while Method 1314 is a flow-through dynamic (column) leaching 

method. The fourth procedure, Method 1315 is a hybrid of batch and dynamic styles where a 

series of consecutive batch extraction steps are conducted to measure leaching as a function 

of time, often referred to either as a “diffusion” or “tank leaching” method. 

3.1.1 Influence of pH on Equilibrium 

Many of the processes that result in leaching of inorganic constituents (e.g., mineral and 

precipitate dissolution, adsorption/desorption reactions, and aqueous solubility of inorganic 

species) are strongly pH-dependent. Since inorganic constituents in solid materials may be 

(i) incorporated within mineral structures (e.g., strontium or barium substituting for calcium), 

(ii) adsorbed to surfaces of mineral phases such as iron oxy(hydr)oxides or organic matter, 

(iii) precipitated as low-solubility solids within pore spaces, or (iv) dissolved within the 

liquid phase held within the pore structure (Connor 1990), pH is considered a principal 

variable controlling the equilibrium between the liquid and solid phases for many inorganic 

contaminants. The recommended leaching test for determining the pH-dependence on LSP is 

Method 1313. In addition to pH-dependent partitioning, this method also provides an 

acid/base titration curve of the material used to estimate the influence of environmental 

acidity or alkalinity on changes in resulting eluate pH. 

Eluate pH does not directly affect the solubility of most organic contaminants which are 

primarily concentrated in isolated organic phases (e.g., tars and grease) or adsorbed to 

particulate organic matter (van der Sloot 2002a; van der Sloot 2002b). However, pH does 

influence the dissolution of particulate organic matter (POM; i.e., humic substances) which 

may be more soluble at high pH. The measured concentrations of organic contaminants in 

eluates may be greater than theoretical aqueous solubility values due to binding with 

dissolved organic carbon (DOC) or colloidal organic matter. In leachates and eluates, DOC 

is often measured as total organic carbon (TOC) in solution. Method 1313 is useful to assess 

the effect of DOC on the eluate concentration of organic species. For example, when soil 

with high organic content is solidified with Portland cement, an increase in DOC can result in 

an increase in the measured leaching concentrations of some contaminants (e.g., metals, 

polycyclic aromatic hydrocarbons or PAHs). Thus, pH may still be considered a significant 

leaching parameter for organic species. 

3.1.2 Influence of Liquid-to-Solid Ratio on Equilibrium 

As water percolates through a column of granular or high permeability material, highly 

soluble salts (e.g., chloride or nitrate salts of sodium or potassium) are washed out quickly 

and the more soluble mineral phases are dissolved. Changes in pore water chemistry as more 

soluble components are released can alter the dissolution of the more stable mineral phases 

and subsequent pore solutions and leaching of COPCs, as infiltrating water continues to 
8 

percolate. These effects can be examined using either batch or column tests. Column tests 

allow for careful control of water contact and analysis of aqueous (local) equilibrium as a 

function of the amount of fluid passing through the bed mass normalized as an L/S. At low 

L/S, concentrations provide insight into the composition of the initial pore solution; while 

concentrations at an L/S greater than or equal to 5 mL/g-dry indicate the effects of long-term 

exposure on LSP. Method 1314, a column percolation procedure, and Method 1316, a 

parallel batch procedure, may be useful in determining how the liquid-solid partitioning is 

affected by changes in L/S. 

3.1.3 Influence of Mass Transfer Rates 

Release of constituents from larger particles of granular material or other materials of low 

permeability may be controlled by mass transport of the constituents through the pore 

structure to the bulk liquid solid interface. This scenario is the case when a low permeability 

material is surrounded by higher permeability fill. Infiltrating water or groundwater flows 

around the low permeability material and release occurs at the interface between the flowing 

water and the material. 

Mass transport is often characterized in terms of the mass flux (i.e., mass released across an 

exposed surface unit area over a unit time, e.g., mg/m2

yr) or in terms of the cumulated mass 

released as a function of leaching time. Transport parameters (e.g., diffusivity) and physical 

characteristics (e.g., effective surface area, tortuosity) may be estimated from leaching test 

results when certain conditions or assumptions are specified. For example, the observed 

diffusion coefficient of a COPC represents a simple diffusion case applicable only under the 

assumption that large gradients (e.g., pH) internal to the matrix do not exist. Method 1315

includes provisions for integrating the results of the mass transport test with the results of 

equilibrium-based test Method 1313 to evaluate leaching test quality control. These 

provisions also help to approximate the mechanisms that control the release of COPCs from 

monolithic or compacted granular materials under mass transfer conditions. Of course, these 

mechanisms are in force only as long as the low permeability material maintains its physical 

integrity. Equilibrium conditions become more significant as monolithic materials physically 

degrade or if the material is exposed to very low or intermittent flow conditions. 

4 METHOD SUMMARIES AND JUSTIFICATION OF TEST 

PARAMETERS 

In the following sections, each proposed method is briefly summarized followed by the 

rationale supporting the selection of key test conditions specified as part of each method. 

Extensive review of international assessment methodologies and leaching test parameters has 

been presented elsewhere (van der Sloot et al. 2010). Specific test conditions may be 

justified on the basis of the underlying fundamental phenomena, empirical observation 
9 

(results of prior testing), numerical simulation, or practicality for implementation. Test 

specifications for the four methods are provided at the end of Section 4 (see Table 5). 

4.1 PRELIMINARY VERSION OF METHOD 1313 

Method 1313 - “Liquid-Solid Partitioning as a Function of Extract pH for Constituents in 

Solid Materials using a Parallel Batch Extraction Procedure” is a leaching characterization 

method consisting of parallel extractions of a particle-size reduced solid material in dilute 

acid or base. 

4.1.1 Method Summary 

Method 1313 is a batch extraction procedure with parallel extractions designed to provide 

information on the partitioning of constituents between solid and liquid phases under 

specified conditions. A mass of “as tested” solid material equivalent to a specified minimum 

dry mass is added to nine or ten extraction vessels.3

 Solutions of dilute nitric acid or sodium 

hydroxide are added to each vessel according to a schedule of acid and base additions 

formulated from a pre-test titration curve and designed to target specific final pH values 

(eluate pH values) between 2 and 13. Extract bottles are tumbled in an end-over-end fashion 

for a specified contact time that depends on the particle size of the sample. The extract liquid 

is separated from the solid phase via settling or centrifugation, followed by filtration and 

preservation of analytical solutions. 

Recorded data includes equivalents of acid or base added, extract final pH and electrical 

conductivity (EC) with an option for measuring oxidation/reduction potential (ORP) when it 

is expected to influence leaching. The concentration of DOC is often measured in eluates 

and the active fraction for binding of metals and organic contaminants can be determined 

through fractionation of the various organic carbon phases (ISO, 2009). Extract 

concentrations for the constituents of concern are measured and plotted as a function of 

extract pH and compared to quality control and assessment limits. This method provides a 

titration curve of the solid material and the LSP curve for constituents of concern over a 

broad pH range that both represents the range of possible environmental leaching conditions, 

and also illustrates any changes in leaching chemistry that may occur over this range of 

conditions. LSP data as a function of eluate pH may be used with geochemical speciation 

models to infer the speciation of solubility-controlling mineral phases and reactive surfaces 

(e.g., metal oxides, clay and organic matter) for COPCs. 

 

3

 The method requires conducting extractions under natural conditions (i.e., no acid or base addition) as well as 

at nine final target pH values. However, if the natural pH of the material falls within the acceptable tolerance of 

any target pH point, the target pH extraction is not conducted. 
10 

4.1.2 Constituents of Potential Concern 

This method is applicable for inorganic species (e.g., metals, metalloids and ionic salts), nonvolatile organic compounds, and DOC. Given that radionuclides behave chemically as 

inorganic species, the method is also applicable for radionuclides provided that the 

appropriate modifications are taken to ensure adequate worker protection. Although the 

method is capable of providing extracts for evaluation of semi-volatile organic species, the 

premise that pH controls liquid-solid partitioning is not directly applicable to these 

constituents; however, a secondary effect based on association of certain organic species 

(e.g., PAHs) with dissolved organic carbon may be observed. 

4.1.3 Target pH Values 

The specific target pH values are based on environmental or operationally-defined rationale 

as shown in Table 1 (also provided as Table 5 in the method text). Within LEAF, the natural 

pH of the material is defined as the eluate pH of a batch extraction of a <5 mm granular 

sample in regent water at an L/S of 10 mL/g-dry without addition of acid or base. Full 

characterization under Method 1313 requires that a set of eluates be produced with final pH 

values satisfying the nine specified pH targets shown in Table 1. 

If the natural pH of the “as tested” material falls within the range of any target interval (e.g., 

a natural pH of 6.6 falls within the 7.0±0.5 pH range), there is no need to conduct both the 

natural pH extraction and the targeted pH extraction. In this case, the natural pH extraction is 

used to represent that pH range and a total of nine parallel extractions would be conducted 

(i.e., the natural pH extraction plus eight remaining targeted pH extractions). If that natural 

pH falls outside all specified target ranges (e.g., a natural pH of 6.4), the natural pH 

extraction is conducted in addition to the nine specified target conditions shown in Table 1 

(i.e., ten parallel extractions in total). 

These target pH values were selected to standardize the data across the pH profile and to 

provide input on the response of the material to environmental stresses over a broad range of 

pH values. While the extremes of the specified values may not be achieved under anticipated 

field conditions, these values have been selected in order (i) to estimate the fraction of the 

total COPC content available for leaching (absent long-term changes in mineral form), (ii) to 

represent values that may occur as a result of co-management of diverse materials, and/or 

(iii) to facilitate geochemical modeling of the system. 

Table 1. Rationale for Method 1313 Final pH Targets. 

Value pH 

Target

Rationale

1

2

2.0±0.5

4.0±0.5

Estimates total or available content of cationic and amphoteric COPCs

Lower pH limit of typical management scenario
11 

3 5.5±0.5 Typical lower range of industrial waste landfills

4 7.0±0.5 Neutral pH region; high release of oxyanions

5 8.0±0.5 Approximately endpoint pH of carbonated alkaline materials

6 9.0±0.5 Minimum of LSP curve for some cationic and amphoteric COPCs4

7 10.5±0.5 Minimum of LSP curve for some cationic and amphoteric COPCs4

8 12.0±0.5 Maximum in alkaline range for LSP curves of amphoteric COPCs

9 13.0±0.5 Upper bound (field conditions) for amphoteric COPCs

variable Natural pH at L/S 10 mL/g-dry (no acid/base addition)5

The concentration of COPCs over this pH range defines the partitioning curve between 

dissolved species and solid phases as a function of eluate pH and may be used to identify 

how constituent LSP is influenced in environmental scenarios with different characteristic 

pH values (e.g., co-management with other materials) or when eluate pH varies over time in 

response to local environmental conditions (e.g., carbonation of alkali materials, acidification 

processes through oxidation, depletion by leaching of pH controlling constituents from the 

material). In reporting results, the final pH of the extract must be reported so that leachate 

concentrations may be associated with the actual final pH measured in the tests, rather than at 

the target pH value. Leaching at any non-measured pH value can then be estimated by 

interpolation of the resultant concentration versus pH curve. 

4.1.4 Eluent Composition 

Method 1313 requires that the final pH of the extract is controlled by addition of dilute acid 

or base. The intent is that the pH-controlling agent should be completely dissociated under 

test conditions. Thus, organic acids are not recommended for lowering pH below the natural 

pH value. In addition, the acid should not significantly interfere with the chemistry of the 

system. Nitric acid is specified in the method because, although a mild oxidant, it is less 

interfering than other inorganic acids which cause precipitation (e.g., sulfuric or phosphoric 

acids) or form complexes (e.g., chloride from hydrochloric acid). While nitric acid is 

oxidizing and thereby has the potential to provide a biased estimate of leaching for some 

constituents expected to be disposed or utilized in a reducing system, the potential exists in 

many environmental scenarios for reducing systems to become oxidized over time.6

 The 

 

4

 As a whole, the LSP curves for amphoteric and cationic species tend to approach a minimum value in the pH 

range between about 9 (e.g., lead) and 11 (e.g., cadmium); therefore, pH targets of 9.0±0.5 and 10.5±0.5 can be 

useful for estimating the minimum of the LSP curve in most cases. 

5

 Natural pH has also been referred to as “own pH” in other publications, e.g., U.S. EPA, Characterization of 

Coal Combustion Residues from Electric Utilities – Leaching and Characterization Data, EPA-600/R-09/151, 

December 2009. 

6

 In order to address the reverse case where oxidized systems are exposed to reducing conditions, geochemical 

modeling (e.g., using LeachXSTM) may be useful. 
12 

base specified in the method is sodium hydroxide; although potassium hydroxide may also be 

used for cases when sodium is a COPC. 

4.1.5 Minimum Dry Mass Equivalent 

Minimum amounts of material are specified in order to ensure that a representative 

subsample is used in the leaching test. Since heterogeneities are somewhat dependent on 

particle size, the minimum sample amount required to be used varies with the particle size of 

the “as tested” material. The minimum sample mass for each extracted material aliquot is 

specified at 20 g-dry for material < 0.3 mm, 40 g-dry for material < 2 mm, and 80 g-dry for 

material < 5 mm. These specifications are expected to result in a representative sample for 

most materials provided that adequate initial sample mass is sized reduced, if necessary. The 

sample amount used in testing may be increased, with corresponding scale up of leachant 

volumes, if sample heterogeneity is determined to be a problem. 

The L/S used in leaching tests are based on the dry mass of a solid; however, oven drying 

the “as received” material to constant mass prior to testing may be impractical and sometimes 

deleterious to the mineral structure. In such cases where the “as received” material must be 

dried before testing, air-drying or drying over a nitrogen blanket (e.g., in the case of 

oxidation or carbonation sensitive materials) to a moisture content that facilitates material 

handling (e.g., less than 10% wet basis) is recommended. Since the “as tested” material is 

likely to contain some level of moisture, the required mass of solid materials is specified on 

basis of a “dry mass equivalent” (i.e., the mass of an “as tested” sample which, if dried to 

constant mass, would result in the specified dry mass). The dry mass equivalent for a 

specified value can be calculated if the solids content or moisture content (wet basis) is 

known, according to the following equation: 

Equation 1 

where: is the dry mass equivalent of “as tested” solid material [g] 

 is the mass of dry material specified in method [g-dry] 

 is the solids content of “as tested” material [g-dry/g], and 

 is the moisture content (wet basis) of the “as tested” material [gH2O/g] 

The specification for the minimum amount of solid material is based on the homogeneity of 

the sample and the particle size of the test subsample. The minimum dry mass equivalents 

specifications shown in the method assume that, after particle size reduction and sieve 

analysis, the solid material has undergone adequate homogenization. Materials which are 

visually heterogeneous after sample processing may require more mass to achieve an 

adequate representative subsample. 
13 

4.1.6 Particle Size, Liquid-To-Solid Ratio and Contact Time 

In batch testing, the time required to approach equilibrium between the liquid and solid 

phases depends on a relationship that is a function of particle size, liquid-solid ratio and 

contact time.7 Thus, the discussion of one parameter must be conducted in context with the 

others. Since the goal of equilibrium extractions is to achieve a practical approximation of 

equilibrium between the solid materials and the liquid extraction fluid, the specified contact 

time should be long enough to allow for the controlling physical and chemical processes 

(e.g., dissolution and diffusion into the liquid phase) to occur. To reach a practical 

approximation of equilibrium, the contact time may be adjusted based on either the 

maximum particle size of the solid sample or L/S. 

4.1.6.1 Particle Size Reduction and Maximum Particle Size 

Particle size reduction for solid matrices, especially those matrices which are naturally 

monolithic in nature, is often a topic of debate. During batch testing, constituent diffusion 

through larger particles may become the rate-limiting mechanism such that particle size 

reduction of the material prior to testing is necessary. Decreasing the particle size decreases 

the time required to approximate equilibrium by reducing the diffusional distance that a 

solute must traverse to the bulk solution, and increases the surface area for interactions 

between the solid phase and the bulk solution. However, the desire for a prompt response 

from a leach test must be offset by practicality in terms of the effort required for particle size 

reduction. 

The method of particle size reduction should not alter the chemical or mineral composition of 

the material. This means that size reduction operations (e.g., crushing, grind, or milling and 

associated sieving) should not introduce foreign matter to the sample, cause loss of 

constituents, or excessively alter the temperature of the sample. For environmental 

assessment purposes, crushing is less likely to alter the LSP behavior of a material than 

grinding or milling to a fine powder due, in part, to shearing stress and heat development 

(van der Sloot et al. 2001). In addition, the process should be conducted in a timely manner 

in order to minimize the potential for interaction with the atmosphere (e.g., oxidation or 

carbonation). Alternately, particle size reduction may be conducted under a controlled 

atmosphere, such as a nitrogen-purged in a glove box, but this is not always practical. 

Method 1313 allows selection from three specified maximum particle sizes with associated 

minimum sample sizes and minimum contact times. Unless it is impractical to do so, all “as 

received” material to be tested should be size reduced to a maximum of 5 mm diameter. This 

provides an “as tested” sample at the largest allowable particle size. The portion of “as 

received” material that is not readily size reduced to less than 5 mm by crushing is discarded 

 

7

 The contact time to reach equilibrium also is a factor of temperature and the fraction of the total or available 

constituent content in the solid that is soluble at equilibrium (see Contact Time). 
14 

after calculating the mass fraction of the greater than 5 mm and documenting the nature (e.g., 

rocks, sticks, glass, etc.) and approximate particle size of the discarded fraction. Test results 

are not corrected to account for the discarded mass.8 Batch extraction at this level of particle 

size reduction requires 72 hours of contact time; however, shorter contact times may be used 

when further particle size reduction to 2 mm or 0.3 mm is employed. During the particle size 

reduction process, it is likely and unavoidable that a distribution of particle sizes will result 

rather than a single particle size. Thus, the recommended contact time to be used in Method 

1313 should correspond to the particle size for which 85 wt% of the “as tested” sample 

passes the specified sieve size (see Contact Time). 

4.1.6.2 Liquid-To-Solid Ratio 

L/S is defined as the volume of extracting fluid relative to the mass of solid. For batch tests 

designed to approximate equilibrium, lower values of L/S reduce the amount of constituent 

mass that is required to saturate the liquid phase and, thus, decreases the time required to 

reach equilibrium. Although the L/S for fully saturated porous field material (e.g., soils, 

wastes, cementitious materials) can be significantly less than 1.0 mL/g-dry, it is not practical 

to routinely work in the laboratory setting with solid slurries which result from batch 

extraction at very low L/S. At high L/S, differences in eluate concentrations from a similar 

method at a standard L/S of 10 mL/g-dry and a modified L/S of 100 mL/g-dry were 

explained based on either availability or solubility controlled release (Dijkstra et al. 2008). 9 

In order to provide a standardized L/S value for batch testing, Method 1313 specifies an L/S 

of 10 mL/g-dry which provides balance between practicality10 and time required to approach 

equilibrium. In addition, an L/S of 10 mL/g-dry is a reasonable value for extended leaching 

interval in the field, such that observed released masses of COPCs from leaching tests can be 

used to estimate field behavior. 

 

8

 By excluding the mass fraction with particle size greater than 5 mm, some bias may be introduced. However, 

irreducible particles are often not the driver for environmental assessment. In addition, particle size reduction is 

considered to correlate, to some degree, with durability in use. Therefore, it is unlikely that application 

conditions would result in significant particle size reduction to < 5 mm for materials an irreducible mass 

fraction of greater than 20%. For these materials, other leaching tests (e.g., Method 1314 in a large diameter 

column or Method 1315) may be a more appropriate approach to leaching characterization. 

9

 In this context, “availability-controlled” release means that the release is limited to the total amount of a 

constituent in the solid phase that is available for release under the specified conditions. “Solubility-controlled” 

release refers to situations where the release of a constituent is consistent with the solubility as a function of pH 

under the specified conditions. For each constituent, the resultant extract concentration under availabilitycontrolled release is higher than or equal to the solubility-controlled release concentration. 

10 Within the context of L/S ratio, “practicality” refers to reasonable expectations of handling solid-liquid 

slurries such that a minimum amount of eluate can be expected after filtration. 
15 

4.1.6.3 Contact Time 

In equilibrium-based leaching tests, the duration of the extraction is set such that the mass 

transfer rate does not limit release into the liquid phase. The minimum contact time for batch 

testing of particle size reduced material is based on the minimum mass transport time to 

reach a fractional equilibrium concentration in a bath of fixed volume surrounding a 

spherical particle of a particular diameter (Garrabrants 1997). The numerical solution for 

diffusion of a constituent through a spherical particle of diameter 2a into a finite bath as 

(Crank 1975): 

Equation 2 

where is the mass release from a sphere at time t [mg] 

 is the mass release at infinite time (i.e., equilibrium condition) [mg] 

 is the observed diffusion coefficient [m2/s] 

 is the spherical radius [m] 

 is the non-zero roots of the relation; 

Equation 3 

where is the ratio of the volumes of the solution and the sphere [-]. 

The factional solubility (i.e., the fraction of the available mass that is soluble at equilibrium) 

can be expressed as a function of the parameter α as: 

Equation 4 

where is the initial available constituent mass in the sphere [mg]. 

Figure 2 shows a nomagraph of the contact time required to establish 90% of the equilibrium 

(vertical axis) in the fixed bath as functions of particle diameter (horizontal axis) and 

fractional solubility (diagonal axis, not shown). The fractional solubility is defined as the 

fraction of the available content that is soluble at equilibrium. In the figure, the observed 

diffusivity of the transporting species is constant at 10-13 m

2

/s, which is a relatively slow rate 

of diffusion based on past observations (sodium free diffusion in water is on the order of 10-9

m

2

/s while diffusion through concrete may be on the order of 10-12 m

2

/s). 
16 

Figure 2. Contact time required for a species with an observed diffusivity of 10-13 m

2

/s to 

reach 90% of equilibrium ( ) based on mass transport as functions of particle 

diameter and fractional solubility ( ). Figure modified from Garrabrants, 1997. 

The red, short-dashed lines in Figure 2 indicate that spherical particles of 0.3 mm establish 

90% of theoretical equilibrium in less than 24 hours regardless of the fractional solubility 

value. Over a 48-hour period (green, long-dashed lines), 90% of equilibrium can be 

approached for particles of 2 mm if the fractional solubility is less than 0.1 (i.e., less than 

10% of the total or available content is soluble in the fixed bath at infinite time). A 72-hour 

contact time (blue, dot-dash lines) would allow for particles of 5 mm diameters to approach 

90% of equilibrium for fractional solubility values of less than approximately 0.4. 

The above caveats with regard to fraction solubility are reasonable for most inorganic species 

because the more soluble species (e.g., sodium, boron) would likely have higher observed 

diffusion coefficients and, thus, would not be limited by mass transport through the particle 

over the test duration. 

A similar approach can be used in conjunction with Figure 3 to examine the effect of 

diffusivity on the horizontal axis, in this case shown as the negative log of the diffusion 

coefficient (pD), on the time required to reach 90% of equilibrium on the vertical axis as a 

function of fractional solubility on the diagonal axis (not shown) for a spherical particle of 

0.3 mm diameter. The 24-hour test duration specified in Method 1313 would allow 0.3 mm 

diameter particles to approach 90% of equilibrium for fractional solubility less than 0.2 for 

constituents with a mid-range diffusivity of 10-14 m2/s (pD=14; green, long dash line) and for 
17 

fractional solubility less that only 0.01 for constituents with a very low diffusivity of 10-16

m

2

/s (pD=16; blue, dot-dash line). 

Figure 3. Contact time required for a particle of 0.3 mm diameter to reach 90% of 

equilibrium ( ) as function of diffusivity and fractional solubility ( ). 

Figure modified from Garrabrants, 1997. 

Based, in part, on the analysis of mass transport from a spherical particle into a bath of fixed 

volume, the specifications for contact time as a function of particle size shown in 

Table 2 were established. 

Table 2. Extraction parameters as function of maximum particle size. 

Particle Size US Sieve Minimum Contact Suggested 

(85 wt% less than) Size Dry Mass Time Vessel Size 

[mm] [g-dry] [hr] [mL] 

0.3 50 20±0.02 24±2 250 

2.0 10 40±0.02 48±2 500 

5.0 4 80±0.02 72±2 1000 

The above time estimates are based entirely on mass transport considerations assuming that 

(i) the diffusing species is readily available for mass transport (i.e., dissolution is not ratelimiting) and (ii) the solid phase concentration of the species at the center of the particle is 

constant (e.g., the species does not deplete). The latter assumption is most likely valid for 
18 

most solid materials given the relatively low liquid-to-solid ratio. The former assumption 

that dissolution is not kinetically controlled is not valid for all species (e.g., iron oxide 

dissolution) and could result in longer required test durations (Dijkstra et al. 2006). The 

resultant specifications provided in 

Table 2 also consider practicality in striking that balance between test duration and 

increasing effort required for further particle size reduction. 

4.1.7 Temperature 

All test activities are conducted at 21±2 °C which is assumed to be consistent with room 

temperature in most laboratories with environmental control. Deviations in temperature of 

more than approximately 5 °C may result in changes in constituent concentrations such that 

comparison of test results to tests conducted within specification may be misleading. 

4.1.8 Agitation 

Method 1313 specifies “end-over-end” tumbling as the method of agitation. This method 

provides adequate contact between solid and liquid phases as gravity maximizes dispersion 

of particles. Other methods of agitation (e.g., rolling, linear or orbital shaking) allow for 

settling and the formation of a consolidated slurry phase with minimum solid-liquid contact 

area. The rate of agitation is selected to be 30±2 RPM in order to be consistent with 

commercially available tumbling apparatuses and equipment in place for currently 

standardized methods (e.g., TCLP). 

4.1.9 Filtration 

In order to process leaching test solid-liquid mixtures for analysis, the bulk solid and liquid 

phases must be separated. Coarse separation may be accomplished with settling for 10-15 

minutes or centrifugation at an average relative centrifugal force (RCF) of 1,500±100 g for 

10±2 minutes. Fine separation for preparation of analytical solutions typically requires 

filtration. Method 1313 specifies filtration of solutions for inorganic analysis through 0.45-

um polypropylene membranes. The pore size allows for filtration of fine suspended particles 

consistent with the definition of dissolved metals (Csuros and Csuros 2002). Polypropylene 

membranes are specified to minimize adsorption of inorganic species onto the filtration 

membrane. The filtration step can be conducted under vacuum or pressure with an inert gas, 

although pressure filtration is required if mercury is a COPC. 
19 

4.2 PRELIMINARY VERSION OF METHOD 1314 

Method 1314 - “Liquid-Solid Partitioning as a Function of Liquid-Solid Ratio for 

Constituents in Solid Materials Using an Up-Flow Percolation Column Procedure” is a 

leaching characterization test consisting of continuous flow of eluent through a column of 

moderately packed granular material. 

4.2.1 Method Summary 

A solid material is packed11 into a 5 cm diameter by 30 cm long glass column fitted with 

polytetrafloroethylene (PTFE) end caps. Deionized water or 1 mM calcium chloride as an 

eluent is introduced in an up-flow pumping mode and a series of nine sequential eluate 

samples are collected over specific L/S intervals. Up-flow pumping is used to minimize air 

entrainment and flow channeling. The default eluent for most materials is reagent water; 

however, a solution of 1 mM calcium chloride in reagent water is specified when testing 

materials with either a high clay content or high organic matter to prevent deflocculation and 

colloid formation from clay and POM aggregates from depletion of divalent cations. Method 

1314 is intended to characterize the equilibrium between solid and liquid phases as soluble 

species are eluted, so the eluate flow rate is maintained between 0.5-1.0 LS/day to increase 

the likelihood of local equilibrium. An elution rate of 0.75 L/S per day also provides a liquid 

phase mean residence time for flow through the column that is equivalent to the contact time 

for batch testing (i.e., Methods 1313 and 1316). The pH and conductivity of collected eluate 

fractions is recorded and analytical samples are filtered, preserved (as appropriate to specific 

chemical analyses) and chemically analyzed for COPCs. 

Eluate data is plotted as a function of L/S. For the purposes of chemical speciation modeling, 

the entire eluent volume up to 10 mL/g dry sample (g-dry) is analyzed in nine specific 

fractions. Options are included for applications where less detailed leaching information is 

required (see Section 4.2.12). These options include compositing collected eluate fractions 

to form a subset of analytical samples or collected of a limited subset of eluents fractions for 

analysis. 

4.2.2 Particle Size 

Accumulated experience from multiple applications for packed bed flow systems has resulted 

in the generally accepted relationship that the minimum column diameter should be at least 

20 times the nominal material particle size to minimize wall effects and channeling. Using 

this approximation, the calculated maximum particle size for the 4.8-cm inside diameter 

column described in method is 2.4-mm. In order to provide consistency in sample 

 

11 Packing should not inhibit the flow of eluent, but should allow eluent to pass through the packed material. 
20 

preparation between the column test and mid-level particle size reduction in the batch testing, 

the value can be reduced slightly to 2 mm without effecting flow properties. 

Since it is unavoidable that a distribution of particle sizes will result from any particle size 

reduction technique, the criteria for the particle size specification in Method 1314 is based on 

at least 85 wt% of the “as tested” material passing a sieve at the specified particle size. Thus, 

the particle size is specified as 85 wt% less than 2-mm diameter with a maximum particle 

diameter of 5 mm (1/10 the column diameter). 

As described in batch testing, all “as received” material intended for column testing should 

be particle size reduced to 5 mm unless it is impractical to do so. This process provides an 

“as tested” sample at the largest allowable particle size. The portion of “as received” 

material that is not readily size reduced to less than 5 mm by crushing is discarded after 

calculating the mass fraction of the greater than 5 mm and documenting the nature (e.g., 

rocks, sticks, glass, etc.) and approximate particle size of the discarded fraction. Test results 

are not corrected to account for the discarded mass.12 The mass passing the 5 mm sieve is 

further particle size reduced until at least 85 wt% is less than 2 mm to provide the final “as 

tested” material sample. 

The specification for particle size reduction in the Method 1314 column test is a minor 

modification from the 80% less than 1/20 of column diameter suggested after ruggedness 

testing of DIN 19528 column test during the Sickerwasserprognose (leachate forecast) 

program conducted in Germany (Grathwohl and Susset 2009; Susset and Grathwohl 2009; 

Susset et al. 2009), that allows for consistency in material preparation with the batch methods 

(i.e., Method 1313 and Method 1316). 

4.2.3 Constituents of Potential Concern 

Method 1314 is applicable for inorganic species (e.g., metals, metalloids and ionic salts), 

non-volatile organic contaminants and DOC. Given that radionuclides behave chemically as 

inorganic species, the method is also applicable for radionuclides provided that the 

appropriate modifications are taken to ensure adequate worker protection. Although the 

method is capable of providing extracts for evaluation of semi-volatile organic species (e.g., 

PAHs), the materials of construction for the column, seals and tubing must be modified to 

minimize adsorption (i.e., stainless steel and glass are preferable construction materials over 

most plastics, rubber and PTFE). 

 

12 By excluding the mass fraction with particle size greater than 5 mm, some bias may be introduced. However, 

irreducible particles are often not the driver for environmental assessment. In addition, particle size reduction is 

considered to correlate, to some degree, with durability in use. Therefore, it is unlikely that application 

conditions would result in significant particle size reduction to < 5 mm for materials an irreducible mass 

fraction of greater than 20%. 
21 

4.2.4 Eluent Composition 

In general, regent-grade water is used in all characterization tests due to minimal interference 

with the chemistry of the extraction or elution. However, in cases where clayey materials or 

materials with high organic content are tested, a dilute 1 mM solution of calcium chloride is 

specified. Dilute calcium chloride minimizes disaggregation of clays and dissolution of 

organic matter that can lead to colloid formation and either obstruction of column flow via 

plugging in self-filtering materials or washout of very fine particles from the column. The 

use of 1 mM calcium chloride as a leaching solution also is reasonable in the context that 

infiltrating water under most field conditions is likely to contain dilute concentrations of 

divalent cations (Wolt 1994). 

4.2.5 Minimum Column Dimensions 

The minimum column dimensions are specified as 4.8 cm in diameter and 30-cm long. The 

volume contained in a column of these dimensions ensures the use of a minimum subsample 

that is representative of the solid material. In addition, these dimensions and subsample 

amounts provide adequate analytical sample at the lowest L/S of 0.2 mL/g-dry. This volume 

of liquid collected in any fraction i can be calculated using Equation 5. 

Equation 5 

where is the volume collected for fraction i [mL], 

 is the L/S of fraction i [mL/g-dry], 

 is the mass of the “as tested” solid material in the column [g], and 

 is the solid content of the “as tested” material [g-dry/g]. 

4.2.6 Solids Packing 

Method 1314 specifies that granular materials should be packed into the columns in 

approximately 5-cm layers with light tapping or tamping for each layer. This method is 

intended to minimize subsidence or excessive settling in the column while maintaining flow. 

4.2.7 Sand Layers 

Method 1314 specifies a 1-cm layer of clean quartz sand (20-30 mesh) placed at top and 

bottom of the column packing. The top sand layer provides coarse filtration of the eluate and 

the layer thickness should be maintained as specified. The thickness specification for the 

bottom sand layer, which serves as bed support and an eluent distribution layer, may be 

considered a minimum value and the sand layer thickness may be adjusted to modify bed 

volume of the tested material as necessary. The Method 1314 sand layer thickness and grain 

size specifications are approximately consistent with the German Sickerwasserprognose
22 

program which recommends a 1-cm maximum filtration bed of 1-2 mm grain size quartz 

sand (Kalbe et al. 2007). The sand layers in both analyses are expected to provide bed 

support and coarse filtration without significant flow restriction. 

4.2.8 Pre-Equilibration 

Pre-equilibration of a saturated column is required to ensure that the first eluate fraction is in 

equilibrium with the solid material. Ruggedness testing of a European column test, CEN/TS 

14405, indicates that the pre-equilibration of column material should be a minimum of 18 

hours and up to 72 hours (van der Sloot et al. 2010). These specifications were determined 

by the concentrations of constituent in the first eluate fraction with different pre-equilibration 

times. Thus, pre-equilibration for overnight and weekend durations are both technically 

justified and practical. 

4.2.9 Flow Rate 

In Method 1314, a flow rate specification of 0.75±0.25 LS/day is set such that the residence 

time will be between 0.5 and 1 day in the specified column (i.e., 4.8-cm diameter x 30 cm 

bed length) with a solid mass of 500-g-dry material packed at a bed porosity of 40%. An 

estimate of bed porosity for packed columns may be made by weighing the entire column 

apparatus before and after initial saturation with eluent and calculating the volume of water 

retained in the bed as a fraction of the total bed volume. 

Flow rate may be calculated using the formula: 

Equation 6 

Where is the residence time in the column [day], 

 is the bed porosity [volume of pores/volume of bed], 

 is the bed or column diameter [cm] 

 is the bed or column height [cm] 

 is the dry mass of the bed [g-dry], and 

 is the flow rate [LS/day]. 

Assuming a final L/S of 10 mL/g-dry with eluent flowing at 0.75 L/S per day, the total test 

time is approximately 14 days. Ruggedness testing for the Sickerwasserprognose program 

required that eluate flow rate be calculated based on bed properties and average contact or 

residence time. The mean residence time during the testing phases was 16±1 hours (Kalbe et 
23 

al. 2007; Kalbe et al. 2009; Susset and Grathwohl 2009). The flow rate specification in 

Method 1314 should result in a slightly longer residence time than indicated in the German 

ruggedness testing in order to ensure that local equilibrium has been established. Local 

equilibrium may be confirmed by comparing the concentration vs. L/S data between two 

columns prepared in the same manner, but with significantly different flow rates (e.g., 0.5 

and 1.0 L/S per day). An option for a faster flow rate is available if local equilibrium 

conditions during the test can be demonstrated. 

4.2.10 Temperature 

All test activities are conducted at 21±2 °C which is assumed to be consistent with room 

temperature in most laboratories with environmental control. Deviations in temperature of 

more than approximately 5 °C may result in changes in constituent concentrations such that 

comparison of test results to tests conducted within specification may be misleading. 

4.2.11 Filtration and Centrifugation 

While eluates in the column test are filtered to some degree through the sand layer at the top 

of the column, analytical samples with turbidity greater than 100 Formazin Nephelometric 

Units (FNUs) may result in poor analysis. Typically, solutions with high turbidity may be 

clarified through a combination of filtration and centrifugation. Method 1314 specifies 

filtration of solutions for inorganic analysis through 0.45-um polypropylene membranes for 

all eluates, consistent with recommendations stemming from ruggedness testing of a 

proposed German column test DIN 19528 (Susset and Grathwohl 2009). Polypropylene 

membranes are specified in Method 1314 in order to minimize adsorption of inorganic 

species onto the filtration membrane. Eluates prepared for analysis of organic compounds 

should not undergo supplemental membrane filtration. The Sickerwasserprognose program 

noted significant membrane filtration artifacts and recommended that solutions for organics 

analysis not be filtered as there are no suitable membrane materials (Susset and Grathwohl 

2009). In addition, organic solutions were found to display artifacts of centrifugation such 

that centrifugation should be limited to only those cases where turbidity is greater than 100 

FNUs (Susset and Grathwohl 2009). In Method 1314, centrifugation may be required to 

facilitate filtration of high turbidity eluates; however, the use of calcium chloride as an eluent 

is intended to reduce turbidity by minimizing colloid formation. The filtration step can be 

conducted under vacuum or pressure with an inert gas, although pressure filtration is 

specified if mercury is a COPC. 

4.2.12 Eluate Collection and Compositing for Analytical Samples 

Eluates are collected over nine fractions at pre-determined cumulative L/S of 0.2, 0.5, 1.0, 

1.5, 2.0, 4.5, 5.0, 9.5, and 10 mL/g-dry. These intervals have been specified in order to allow 

for three different levels of analysis: complete characterization, limited analysis and index 

testing. The number of chemical analyses for the limited analysis and index testing levels is 

reduced through the creation of eluate composites or combinations of eluate fractions (see 
24 

Method 1314 Section 12.5 and Method 1314, Table 1 for details on compositing). 

Regardless of the level of analysis, all eluate fractions should be collected to facilitate 

uniformity in sample collection and column operation for the method. Having all eluate 

fractions collected also provides a source of analytical solutions should a more detailed 

analytical scheme be warranted following review of limited analysis or index testing 

schemes. 

4.2.12.1 Complete Characterization 

For purposes of developing a comprehensive characterization of the solid material, all eluate 

samples should be processed for analysis. Results may be shown as a function of L/S for 

eluate fraction concentrations (see Method 1314, Figure 4) or cumulative release, i.e., total 

mass released up to an L/S (see Method 1314, Figure 5). No compositing of eluate fractions 

is performed for complete characterization, and all eluate fractions are analyzed (see Method 

1314 Table 1, Option A). Eluate concentrations from complete characterization may be used 

in conjunction with information regarding environmental management scenarios to estimate 

anticipated leaching concentrations, release rates, and extents of release for individual 

material constituents in the management scenarios evaluated. In addition, eluate 

concentrations may be used along with geochemical speciation modeling to infer the mineral 

phases and partitioning processes that control the LSP in the pore structure of the solid 

material (van der Sloot and Kosson 2007; van der Sloot et al. 2008). 

4.2.12.2 Limited Analysis 

Under a limited analysis approach, nine eluate collections and analysis of six analytical 

samples are required. If evaluation is based on eluate concentrations, six discrete eluate 

fractions are chemically analyzed (see Method 1314 Table 1, Option B). If evaluation is 

based on cumulative release, some eluate fractions may be composited by volume-weighted 

averaging to create a set of six analytical samples (see Method 1314 Table 1, Option C). The 

results of Method 1314, Option C cannot be interpreted on the basis of eluate fraction 

concentrations as the LS fraction structure is not preserved upon solution compositing.

4.2.12.3 Index Testing 

For the determination of consistency between the subject material and previously 

characterized materials, nine eluate collections and analysis of three analytical samples are 

required. If consistency is to be determined by eluate concentrations, three discrete eluate 

fractions are chemically analyzed (see Method 1314 Table 1, Option D). If consistency is to 

be determined by cumulative release, some eluate fractions are composited by volumeweighted averaging to create a set of three analytical samples (see Method 1314 Table 1, 

Option E). The results of Method 1314, Option E cannot be interpreted on the basis of eluate 

fraction concentrations as the L/S fraction structure is not preserved upon solution 

compositing. 
25 

4.3 PRELIMINARY VERSION OF METHOD 1315 

Method 1315 - “Mass Transfer Rates of Constituents in Monolithic or Compacted Granular 

Materials Using a Semi-dynamic Tank Leaching Procedure” is a leaching characterization 

procedure consisting of continuous emersion of a monolithic or compacted granular material 

in reagent water at a specified liquid-to-surface area ratio (L/A). 

4.3.1 Method Summary 

This tank leaching method provides information on the rate of mass transport of constituents 

through a monolithic or compacted granular sample. Monolithic samples may be cylinders 

or parallelepipeds, while granular materials are compacted into cylindrical molds at optimum 

moisture content using Proctor compaction effort. The test sample is moved through a series 

of nine eluent-filled tanks of fresh reagent water at L/A ratio of 9±1 mL/cm2

 following a 

schedule of pre-determined test intervals. For each exchange, the sample is freely drained 

and the mass is recorded to monitor the amount of eluent absorbed into the solid matrix. The 

eluate pH and specific conductance is measured for each time interval and analytical samples 

are collected and preserved accordingly based on the subsequent analytical methods. 

The outcome of Method 1315 is nine eluate solutions comprising a set of mass transfer 

leaching data. Eluate pH, conductivity, and analyte concentrations are plotted as a function 

of time and compared to internal and external quality control data (see Method 1315, Figure 

8). Mean interval flux (see Method 1315, Figure 10) and cumulative release (see Method 

1315, Figure 12) are calculated based on eluate concentrations and plotted as a function of 

time. These data may be used to estimate constituent mass transfer parameters (i.e., observed 

diffusivity, tortuosity). 

4.3.2 Constituents of Potential Concern 

This method is applicable for inorganic species (e.g., metals, metalloids and ionic salts), nonvolatile organic compounds and DOC. In that radionuclides behave chemically as inorganic 

species, the method is also applicable for radionuclides given the appropriate modifications 

to provide adequate worker protection. The method also is adequate for characterization of 

mass transport for non-volatile organic species (e.g., dissolved organic carbon). However, 

Method 1315 is not recommended for characterization of leaching for volatile and semivolatile species due to low aqueous solubility of organic compounds and the high probability 

of volatilization losses over the extended leaching intervals. When mercury is a COPC, 

Method 1315 is applicable as long as provisions are taken to ensure a sealed leaching vessel 

with minimal headspace in order to minimize losses due to volatilization. 
26 

4.3.3 Sample Preparation and Geometry 

Monolithic samples are cut or cored from larger samples or molded to size. Compacted 

granular samples are compacted at optimum moisture content using either standard or 

modified Proctor compaction effort depending on the material field density and workability. 

The specimen size is subject to a minimum dimension specified to ensure that depletion of 

COPCs does not occur over the duration of the test. For homogenous monolithic materials 

(e.g., cement mortars), a minimum specimen dimension of 4 cm is adequate; however, up to 

10 or 20 cm might be required in some cases (e.g., concrete containing coarse aggregate) to 

obtain a representative sample. 

Depletion depth may be estimated as a function of observed diffusion coefficient by iteration 

of the equation for mass transport through a semi-infinite media into an infinite bath (Crank, 

1975): 

Equation 7 

where is the time and spatial variant mass concentration in the media [mg/L], 

 is the constant surface mass concentration [mg/L], 

 is the initial mass concentration in the media [mg/L], 

x is the penetration depth into the sample [cm], 

D is the observed diffusion coefficient of a diffusing species [m2/s], and 

t is the leaching time [s]. 

The assumptions of the semi-infinite diffusion model are that (i) the source term is constant 

(i.e., depletion does not occur), (ii) the diffusion coefficient is constant, and (iii) the 

concentration in the leaching fluid is low enough that the driving force for diffusion remains 

high (i.e., infinite bath). While this model has limitations on a practical basis due to the 

above assumptions, it can be used to parameterize the depletion depth as a function of 

diffusion coefficient. 13

The left hand side of Equation 7 provides the ratio of the remaining concentration in the 

media to the initial concentration when the surface concentration is zero ( =0). This ratio 

can be set to 80% such that depletion is defined when 20% of the mass has been removed. 

 

13 The assumption of an infinite bath results in estimated depth of depletion due to leaching that is conservative 

(i.e., biased towards greater depth). The test case specified in the method has a relatively large, but finite, bath 

designed to maintain a dilute, but not zero concentration, boundary condition during test conditions. 
27 

Figure 4 shows the mass fraction remaining, as a function of depth into a semiinfinite media at the end a leaching interval consistent with the 63-day duration of Method 

1315. 

Figure 4. Evaluation of depth of depletion C(x,t)/Co=0.8 as a function of diffusion 

coefficient (pD is the negative logarithm of the diffusion coefficient). 

Four data series are shown spanning the range of diffusivity14 from very quick (pD=10) to 

moderately slow (pD=13) diffusion. The range of diffusivity observed in tank leach tests of 

a broad range of waste materials is 11 < pD < 15; thus pD=11 represents a reasonable case 

for a highly mobile constituent. The red dashed line shows that the maximum depletion 

depth set at is approximately 1.3 cm. Doubling this depletion depth to 

account for three dimensional leaching, 2.6 cm minimum depletion distance is well within 

the minimum sample dimension of 4 cm specified in Method 1315. 

4.3.4 Eluent Composition 

In general, regent-grade water is used in all characterization tests due to minimal interference 

with the chemistry of the extraction or elution. However, in cases where clayey materials or 

materials with high organic content are tested, a dilute 1 mM solution of calcium chloride is 

specified. Dilute calcium chloride will minimize disaggregation of clays and dissolution of 

organic matter that can lead to colloid formation. Use of 1 mM calcium chloride also is 

14 In this report, diffusivities (D) are indicated in units of [m2

/s], and therefore pD values have units of –

log[m2

/s]. 
28 

reasonable in the context that infiltrating water under most field conditions will contain dilute 

concentrations of divalent cations. 

4.3.5 Liquid-To-Surface Area Ratio 

This method specifies a volume of eluent for each step in the tank leaching process based on 

the exposed surface area of the sample. The exposed surface area for compacted granular 

materials is equal to the cross sectional area of the mold. For 3-dimensional (3-D) diffusion 

from monolithic samples, the exposed surface area for cylinders and parallelepipeds may be 

calculated using following expressions: 

Equation 8 

Equation 9 

where Acyl and Ap are exposed surface areas of a cylinder and parallelepiped, 

respectively [cm2], 

r is the radius of the cylinder [cm], 

h is the height of the cylinder or parallelepiped [cm], 

w is the width of a parallelepiped [cm], and 

l is the length of a parallelepiped [cm]. 

A L/A ratio of 9±1 mL/cm2, as specified in Method 1315, ensures a relatively large, but 

finite, bath such that the driving force for diffusion is maintained while allowing for eluate 

concentrations consistent with common analytical methods. 

4.3.6 Tank-Sample Geometry 

The extraction vessel surrounding the sample (i.e., the “tank” of the tank leaching test) 

should be sized such that the bulk of the leaching fluid is in contact with the exposed surface 

area of the sample. There should be at least 2 cm of clearance between the sample surface 

and the tank wall to ensure enough rapid diffusion from the sample surface into the leaching 

fluid and minimize the local concentration gradient of leached species external to the sample 

surface. The geometry of the tank relative to the sample is very important for 1-D mass 

transport cases (e.g., sealed monoliths or compacted granular samples). For these cases, the 

inner diameter of the tank should be sized as close as possible to outer diameter of the sample 

or sample holder such that the bulk of the leaching fluid is in contact with the expose surface 

area when the sample is submerged. 
29 

4.3.7 Temperature 

All test activities are conducted at 21±2 °C which is assumed to be consistent with room 

temperature in most laboratories with environmental control. Deviations in temperature of 

more than approximately 5 °C may result in changes in constituent concentrations such that 

comparison of test results to tests conducted within specification may be misleading. 

The effect of temperature on diffusion coefficients may be evaluated the Stokes-Einstein 

equation (Cussler 1997):

Equation 10

where D is the diffusion coefficient [m2/s],

 is the Boltzmann constant [m2kg/s2K],

 is the absolute temperature [K], 

 is the dynamic viscosity of the solvent [Ns/m2], and 

 is the radius of the diffusing molecule [m]. 

For a constant viscosity and radius, the Stokes-Einstein equation indicates that the 

diffusion coefficient is proportional to temperature, . Thus, when measured at two 

temperatures (T1 < T2), the diffusion coefficient increases in proportion according to: 

 or Equation 11 

4.3.8 Eluent Exchange Sequence 

The pre-determined leaching intervals (see Method 1315, Table 1) were selected to balance 

practicality15 with eluate concentrations that are consistent with analytical methods. If 

leaching intervals are short, eluate concentrations could potentially be below analytical 

detection limits. However, if the duration of leaching intervals is long, the mass accumulated 

in the eluates until equilibrium is established between the solid and liquid phases and the 

driving force for mass transport is reduced to zero. 

The sequence of leaching intervals specified in Method 1315 provides several quality control 

checks to ensure that equilibrium has not been established in eluates during the test duration. 

Eluate concentrations may be compared to LSP data as a function of eluate pH as obtained 

 

15 Practically, in this case, means that eluent exchanges should fall within an 8-hour shift and a 5-day 

workweek. 
30 

from Method 1313 (see Method 1315, Figure 9). Intervals where equilibrium has been 

established will correspond in concentration to LSP data. 

Alternately, a quality control check that equilibrium has not occurred may be conducted by 

looking at the interval mass flux plotted as a function of arithmetic mean of the time square 

root. Since mass flux from a semi-infinite media under the assumption of the simple 

diffusion model is proportional to the square root of time, it is common to compare interval 

mass flux plotted on log-log axes to a line with a slope of -1/2. However, if chemical 

saturation with respect to a precipitated solid phase (i.e., the formation of a saturated aqueous 

phase) has occurred in multiple intervals, the eluate concentrations would be the same since 

all test fractions use the same volume. Thus, at saturation, the internal mass flux would be 

dependent on the cumulative leaching time as shown in Figure 5a for several common tank 

leaching tests. 
31 

Figure 5. Hypothetical internal mass flux assuming the exchange intervals in the tank leach 

test were long enough to results in equilibrium between solid and bulk liquid phases: (a) 

common test methods and (b) Method 1315. 

The initial flux when the eluates are saturated as shown in Figure 5a closely follow the 

square root of time (dashed line) due to the selection of leaching intervals in these tests. 

Therefore, a conclusion that the release is diffusion-controlled based on interpretation of the 

flux data may be inaccurate. The tank leaching intervals of Method 1315 have been selected 

such that intervals of the same duration will display the same internal mass flux if 

equilibrium has occurred over the leaching interval (Figure 5b). Noting this systematic 

pattern in flux data could be used to facilitate interpretation by ensuring that saturation of the 

eluate did not occur during the tank leaching test. 
32 

4.3.9 Filtration 

Unless the integrity of the sample is compromised during the tank leaching methods, bulk 

separation of solids and liquids is not necessary in Method 1315. However, fine separation 

for preparation of analytical solutions is required via filtration. Method 1315 specifies 

filtration of solutions for inorganic analysis through 0.45-um polypropylene membranes. 

Polypropylene membranes are specified to minimize adsorption of inorganic species onto the 

filtration membrane. The filtration step can be conducted under vacuum or pressure with an 

inert gas, although pressure filtration is specified if mercury is a COPC. 
33 

4.4 PRELIMINARY VERSION OF METHOD 1316 

Method 1316 - “Liquid-Solid Partitioning as a Function of Liquid-Solid Ratio for 

Constituents in Solid Materials Using a Parallel Batch Extraction Procedure” is a leaching 

characterization test consisting of five parallel extractions of a particle-size reduced solid 

material in reagent water over a range of L/S. This batch test results in LSP data as a 

function of L/S whereby estimates of initial leachate and pore water composition, as well as 

cumulative release at L/S=10 mL/g-dry, are comparable to the results of Method 1314 (Lopez 

Meza et al. 2008) column test. Whereas the column methods, such as Method 1314, allow 

for collection of eluates at lower L/S than is practical using a batch extraction test, the batch 

test approach described in Method 1316 provides a practical implementation advantage over 

column tests for many materials due to simpler equipment and shorter overall time 

requirements. 

4.4.1 Method Summary 

Method 1316 is a batch extraction procedure with five parallel extractions designed to 

provide information on the liquid-solid partitioning of constituents as a function of L/S. A 

mass of “as tested” solid material equivalent or greater than to a specified minimum dry mass 

is added to five extraction vessels. Reagent water is added such that the final L/S in the five 

extractions is 0.5, 1.0, 2.0, 5.0, and 10.0, respectively. Extracts are tumbled in an end-overend fashion for a specified contact time that depends on the particle size of the sample. The 

extract liquid is separated from the solid phase via settling or centrifugation, followed by 

filtration and preservation of analytical solutions. The pH, conductivity and constituent 

concentrations for each extract are plotted as functions of L/S and compared to quality 

control and assessment limits. 

4.4.2 Constituents of Potential Concern 

This method is applicable for inorganic species (e.g., metals, metalloids and ionic salts), nonvolatile organic compounds and DOC. In that radionuclides behave chemically as inorganic 

species, the method is also applicable for radionuclides given the appropriate modifications 

to provide adequate worker protection. Although the method is capable of providing extracts 

for evaluation of semi-volatile organic species (e.g., PAHs), the materials of construction for 

the extraction vessel must be modified to minimize adsorption. 

4.4.3 Eluent Composition 

In general, regent-grade water is used in all characterization tests due to minimal interference 

with the chemistry of the extraction or elution. However, in cases where clayey materials or 

materials with high organic content are tested, a dilute 1 mM solution of calcium chloride is 

specified. Dilute calcium chloride will minimize disaggregation of clays and dissolution of 
34 

organic matter that can lead to colloid formation. Use of 1 mM calcium chloride also is 

reasonable in the context that infiltrating water under most field conditions will contain dilute 

concentrations of divalent cations. 

4.4.4 Minimum Dry Mass Equivalent 

Minimum amounts of material are specified in order to ensure that a representative 

subsample is used in the leaching test. Since heterogeneities are somewhat dependent on 

particle size, the minimum sample amount varies with the particle size of the “as tested” 

material. The minimum sample mass for each extracted material aliquot is specified at 20 gdry for material < 0.3 mm, 40 g-dry for material < 2 mm, and 80 g-dry for material < 5 mm. 

These specifications are expected to result in a representative sample for most materials 

provided that adequate initial sample mass is sized reduced, if necessary. The sample amount 

used in testing may be increased if sample heterogeneity is determined to be a problem. 

The results of leaching tests are often based on the dry mass of a solid; however, oven drying 

the “as received” material to constant mass prior to testing may be impractical and sometimes 

deleterious to the mineral structure. In such cases where the “as received” material must be 

dried before testing, air-drying or drying over a nitrogen blanket (e.g., in the case of 

oxidation or carbonation sensitive materials) to a moisture content that facilitates material 

handling (e.g., less than 10% wet basis) is recommended. Since the “as tested” material is 

likely to contain some level of moisture, the required mass of solid materials is specified on 

basis of a “dry mass equivalent” (i.e., the mass of an “as tested” sample which, if dried to 

constant mass, would result in the specified dry mass). The dry mass equivalent for a 

specified minimum dry mass can be calculated if the solids content or moisture content (wet 

basis) is known, according to the following equation: 

Equation 1 

where: is the dry mass equivalent of “as tested” solid material [g] 

 is the mass of dry material specified in method [g-dry] 

 is the solids content of “as tested” material [g-dry/g], and 

 is the moisture content (wet basis) of the “as tested” material [gH2O/g] 

The specification for the minimum amount of solid material is based on the homogeneity of 

the sample and the particle size of the test subsample. The minimum dry mass equivalents 

specifications shown in the method assume that, after particle size reduction and sieve 

analysis, the solid material has undergone adequate homogenization. Materials which are 
35 

visually heterogeneous after sample processing may require more mass to achieve an 

adequate representative subsample. 

Since the purpose of Method 1316 is to provide adequate eluate for chemical analysis at low 

L/S, the amount of solid material used in each of the five parallel extractions may exceed, 

and should exceed in practice, the minimum sample specification. The amount of solid 

material may be increased in order to provide adequate solution volume after filtration. For 

example, if 200 mL of eluate is required to complete all analytical methods, the amount of 

solid materials for the five extractions should follow the scheme shown in Table 3. 

Table 3. Suggested Solid Amounts for Method 1316. 

Test Position L/S Desired Eluate Solid Material

[mL/g-dry] [mL] [g-dry]

T01 10 200 20

T02 5 200 40

T03 2 200 100

T04 1 200 200

T05 0.5 200 400

4.4.5 Specified Liquid-To-Solid Ratios 

In order to provide a standardized set of L/S values for batch testing, Method 1316 specifies 

L/S of 10, 5, 2, 1 and 0.5 mL/g-dry. This range covers the range of L/S consistent with 

Method1313 and Method 1314, balanced with the practicality of recovering eluate from 

extracts of granular materials at low L/S. In addition, an L/S of 10 mL/g-dry is a reasonable 

value for extended leaching interval in the field, such that observed released masses of 

COPCs from leaching tests can be used to estimate field behavior. 

4.4.6 Particle Size, Liquid-To-Solid Ratio, and Contact Time 

In batch testing, the time required to approach equilibrium between the liquid and solid 

phases depends on a relationship that is a function of particle size, liquid-solid ratio and 

contact time.16 Thus, the discussion of one parameter must be conducted in context to the 

others. Since the goal of equilibrium extractions is to achieve a practical approximation of 

equilibrium between the solid materials and the liquid extraction fluid, the specified contact 

time should be long enough to allow for the controlling physical and chemical processes 

(e.g., dissolution and diffusion into the liquid phase) to occur. To reach a practical 

approximation of equilibrium, the contact time may be adjusted, to some degree, based on 

either the maximum particle size of the solid sample or L/S. 

 

16 The contact time to reach equilibrium also is a factor of temperature and the fraction of the total or available 

constituent content in the solid that is soluble at equilibrium (see Contact Time). 
36 

4.4.6.1 Particle Size Reduction and Maximum Particle Size 

Particle size reduction for solid matrices, especially those matrices which are naturally 

monolithic in nature, is often a topic of debate. During batch testing, diffusion through larger 

particles may become the rate-limiting mechanism such that particle size reduction of the 

material prior to testing is necessary. Decreasing the particle size decreases the time required 

to approximate equilibrium by reducing the diffusional distance that a solute must traverse to 

the bulk solution and increasing the surface area for interactions between the solid phase and 

the bulk solution. However, the desire for a prompt response from a leach test must be offset 

by practicality in terms of the effort required for particle size reduction. 

The approach for particle size reduction should not alter the chemical or mineral composition 

of the material. This means that size reduction operations (e.g., crushing, grind, or milling 

and associated sieving) should not introduce foreign matter to the sample, cause loss of 

constituents, or alter the temperature the sample excessively. In addition, the process should 

be conducted as quickly as is reasonably possible in order to minimize the potential for 

interaction with the atmosphere (e.g., oxidation or carbonation). Alternately, particle size 

reduction may be conducted under a controlled atmosphere, such as a nitrogen-purged in a 

glove box, but this is not always practical. 

Method 1316 allows selection from three specified maximum particle sizes with associated 

minimum sample sizes and minimum contact times. Unless it is impractical to do so, all “as 

received” material to be tested should be size reduced to a maximum of 5 mm diameter. This 

provides an “as tested” sample at the largest allowable particle size. The portion of “as 

received” material that is not readily size reduced to less than 5 mm by crushing is discarded 

after calculating the mass fraction of the greater than 5 mm and documenting the nature (e.g., 

rocks, sticks, glass, etc.) and approximate particle size of the discarded fraction. Test results 

are not corrected to account for the discarded mass.17 Batch extraction at this level of 

particle size reduction requires 72 hours of contact time; however, shorter contact times may 

be used when further particle size reduction to 2 mm or 0.3 mm is employed. During the 

particle size reduction process, it is likely and unavoidable that a distribution of particle sizes 

will result rather than a single particle size. Thus, the recommended contact time to be used 

in Method 1316 should correspond to the particle size for which 85 wt% of the “as tested” 

sample passes the specified sieve size (see Contact Time). 

 

17 By excluding the mass fraction with particle size greater than 5 mm, some bias may be introduced. However, 

irreducible particles are often not the driver for environmental assessment. In addition, particle size reduction is 

considered to correlate, to some degree, with durability in use. Therefore, it is unlikely that application 

conditions would result in significant particle size reduction to < 5 mm for materials an irreducible mass 

fraction of greater than 20%. For these materials, other leaching tests (e.g., Method 1314 in a large diameter 

column or Method 1315) may be a more appropriate approach to leaching characterization. 
37 

4.4.6.2 Liquid-To-Solid Ratio 

The volume of extracting fluid relative to the mass of solid is the liquid-to-solid (LS) ratio. 

For batch tests designed to approximate equilibrium, lower L/S reduce the amount of 

constituent mass that is required to saturate the liquid phase and, thus, decreases the time 

required to reach equilibrium. Although the L/S of fully saturated porous field material (e.g., 

soils, wastes, cementitious materials) can be significantly less than 1.0 mL/g-dry, it is not 

practical to routinely work in the laboratory setting will solid slurries which result from batch 

extraction at very low L/S. At high L/S, differences in eluate concentrations from a similar 

method at a standard L/S of 10 mL/g-dry and a modified L/S of 100 mL/g-dry were 

explained based on availability or solubility controlled release (Dijkstra et al. 2008). 18 

4.4.6.3 Contact Time 

In equilibrium-based leaching tests, the duration of the extraction is set such that the mass 

transfer rate does not limit release into the liquid phase. The minimum contact time for batch 

testing of particle size reduced material is based on the minimum mass transport time to 

reach a fractional equilibrium concentration in a bath of fixed volume surrounding a 

spherical particle of a particular diameter (Garrabrants 1997). The numerical solution for 

diffusion of a constituent through a spherical particle of diameter 2a into a finite bath as 

(Crank 1975): 

Equation 2 

where is the mass release from a sphere at time t [mg] 

 is the mass release at infinite time (i.e., equilibrium condition) [mg] 

 is the observed diffusion coefficient [m2/s] 

 is the spherical radius [m] 

 is the non-zero roots of the relation; 

Equation 3 

where is the ratio of the volumes of the solution and the sphere [-]. 

 

18 In this context, “availability-controlled” release means that the release is limited to the total amount of a 

constituent in the solid phase that is available for release under the specified conditions. “Solubility-controlled” 

release refers to situations where the release of a constituent is consistent with the solubility as a function of pH 

under the specified conditions. For each constituent, the resultant extract concentration under availabilitycontrolled release is higher than or equal to the solubility-controlled release concentration. 
38 

The factional solubility (i.e., the fraction of the available mass that is soluble at equilibrium) 

can be expressed as a function of the parameter α as: 

Equation 4 

where is the initial available constituent mass in the sphere [mg]. 

Figure 2 shows the contact time required to establish 90% of the equilibrium (vertical axis) in 

the fixed bath as functions of particle diameter (horizontal axis) and fractional solubility 

(diagonal axis, not shown). The fractional solubility is defined as the fraction of the 

available content that is soluble at equilibrium. In the figure, the observed diffusivity of the 

transporting species is constant at 10-13 m

2

/s, which is a relatively slow rate of diffusion 

based on past observations (sodium free diffusion in water is on the order of 10-9 m

2

/s while 

diffusion through concrete may be on the order of 10-12 m

2

/s). 

The red, short dashed lines in Figure 6 indicate that spherical particles of 0.3 mm established 

90% of theoretical equilibrium in less than 24 hours regardless of the fractional solubility 

value. Over a 48-hour period (green, long dash lines), 90% of equilibrium can be approached 

for particles of 2 mm if the fractional solubility is less than 0.1 (i.e., less than 10% of the total 

or available content is soluble in the fixed bath at infinite time). A 72-hour contact time 

(blue, dot-dash lines) would allow for particles of 5 mm diameters to approach 90% of 

equilibrium for fractional solubility values of less than approximately 0.4. These caveats 

with regard to fraction solubility are reasonable for most inorganic species because the more 

highly soluble species (e.g., sodium, boron) would likely have higher observed diffusion 

coefficients and, thus, would not be limited by mass transport through the particle over the 

test duration. 
39 

Figure 6. Contact time required for a species with an observed diffusivity of 10-13 m

2

/s to 

reach 90% of equilibrium ( ) based on mass transport as functions of particle 

diameter and fractional solubility ( ). Figure modified from Garrabrants, 1997. 

A similar approach can be used in conjunction with Figure 7 to examine the effect of 

diffusivity (horizontal axis), in this case shown as pD or the negative log of the diffusion 

coefficient, on the time required to reach 90% of equilibrium (vertical axis) as a function of 

fractional solubility (diagonal axis not shown) for a spherical particle of 0.3 mm diameter. 

The 24-hour test duration specified in Method 1316 would allow 0.3 mm diameter particles 

to approach 90% of equilibrium for fractional solubility less than 0.2 for constituents with a 

mid-range diffusivity of 10-14 m2/s (pD=14; green, long dash line) and for fractional 

solubility less that only 0.01 for constituents with a very low diffusivity of 10-16 m

2

/s 

(pD=16; blue, dot-dash line). 
40 

Figure 7. Contact time required for a particle of 0.3 mm diameter to reach 90% of 

equilibrium ( ) as function of diffusivity and fractional solubility ( ). 

Figure modified from Garrabrants, 1997. 

Based, in part, on the analysis of mass transport from a spherical particle into a bath of fixed 

volume, the specifications for contact time as a function of particle size shown in 

Table 2 were established. The above time estimates are based entirely on mass transport 

considerations assuming that (i) the diffusing species is readily available for mass transport 

(i.e., dissolution is not rate-limiting) and (ii) the solid phase concentration of the species at 

the center of the particle is constant (e.g., the species does not deplete). The latter 

assumption is most likely valid for most solid materials given the relatively low liquid-tosolid ratio. The former assumption that dissolution is not kinetically controlled is not valid 

for all species (e.g., iron oxide dissolution) and could result in longer required test durations 

(Dijkstra et al. 2006). The resultant specifications provided in Table 4 also consider 

practicality in striking that balance between test duration and increasing effort required for 

further particle size reduction. 
41 

Table 4. Extraction Parameters as Function of Maximum Particle Size. 

Particle Size U.S. Sieve Minimum Contact Suggested 

(85 wt% less than) Size Dry Mass Time Vessel Size

[mm] [g-dry] [hr] [mL]

0.3 50 20±0.02 24±2 250

2.0 10 40±0.02 48±2 500

5.0 4 80±0.02 72±2 1000

4.4.7 Temperature 

All test activities are conducted at 21±2 °C which is assumed to be consistent with room 

temperature in most laboratories with environmental control. Deviations in temperature of 

more than approximately 5 °C may result in changes in constituent concentrations such that 

comparison of test results to tests conducted within specification may be misleading. 

4.4.8 Agitation 

Method 1316 specifies “end-over-end” tumbling as the method of agitation. This method 

provides adequate contact between solid and liquid phases as gravity maximizes dispersion 

of particles. Other methods of agitation (e.g., rolling, linear or orbital shaking) allow for 

settling and the formation of a consolidated slurry phase with minimum solid-liquid contact 

area. The rate of agitation is selected to be 30±2 RPM in order to be consistent with 

commercially available tumbling apparatuses and equipment in place for currently 

standardized methods (e.g., TCLP). 

4.4.9 Filtration 

In order to process leaching test solid-liquid mixtures for analysis, the bulk solid and liquid 

phases must be separated. Coarse separation may be accomplished with settling for 10-15 

minutes or centrifugation at an average relative centrifugal force (RCF) of 1,500±100 g for 

10±2 minutes. Fine separation for preparation of analytical solutions typically requires 

filtration. Method 1316 specifies filtration of solutions for inorganic analysis through 0.45-

um polypropylene membranes. Polypropylene membranes are specified to minimize 

adsorption of inorganic species onto the filtration membrane. The filtration step can be 

conducted under vacuum or pressure with an inert gas, although pressure filtration is 

specified if mercury is a COPC. 
42 

Table 5. Comparison of Test Specifications for Preliminary Versions of Methods 1313, 1314, 1315, and 1316. 

Test Name Method 1313 Method 1314 Method 1315 Method 1316

Test Type Equilibrium;

pH-dependence

Equilibrium;

L/S

Mass transfer;

mass transport rates

Equilibrium;

L/S

Test 

Description

Parallel batch extractions 

as function of pH

Column test performed 

in up-flow mode

Tank test with periodic 

eluent renewal

Parallel batch extractions 

as function of L/S

Sample Type 

Dimension

Granular

Particle size of 85% 

(mass/mass) less than 0.3 

mm, 2.0 mm, or 5.0 mm

Granular

Particle size of 85% 

(mass/mass) less than 2 

mm and 100% (m/m) 

less than 5 mm

Monolithic - cylinder or 

cube with 40-mm 

minimum dimension

Granular - compacted 

cylinder with 40-mm 

minimum height

Granular

Particle size of 85% 

(mass/mass) less than 0.3 

mm, 2.0 mm, or 5.0 mm

Target 

Constituents

Inorganic, non-volatile, 

and semi-volatile organic 

species

Inorganic, non-volatile, 

and semi-volatile organic 

species

Inorganic and nonvolatile organic speciesInorganic, non-volatile, 

and semi-volatile organic 

species

Eluent

Composition

Reagent water with 

additions of HNO3 or 

NaOH

Reagent water or 1 mM 

CaCl2

Reagent water or 1 mM 

CaCl2

Reagent water or 1 mM 

CaCl2

pH Range <2 to >12 at specified 

targets

pH dictated by solid 

buffering

pH dictated by solid 

buffering

pH dictated by solid 

buffering

Minimum 

Amount of 

Solid

20 g-dry each extract 300 g 500 g 20 g-dry each extract

Eluent Volume L/S of 10 mL/g-dry L/S varies with 

percolation time

Liquid-surface area ratio 

(L/A) of 10 mL/cm2

L/S of 10, 5.0, 2.0, 1.0 

and 0.5 mL/g-dry

Number of 

Test Fractions

9 (10 if natural pH is not 

within a target range) 9 9 5
43 

Test Name Method 1313 Method 1314 Method 1315 Method 1316

Contact Time Based on particle size: Based on flow rate Eluent renewal at Based on particle size: 

per Test 

Fraction 24 hr (0.3 mm)

48 hr (2 mm)

72 hr (5 mm)

(Total test duration ~10 

days)

specified intervals of 2, 

23 and 23 hr; 5, 7, 14, 7, 

and 14 days

24 hr (0.3 mm)

48 hr (2 mm)

72 hr (5 mm)

Temperature 21±2 oC 21±2 oC 21±2 oC 21±2 oC

Agitation End-over-end rotation at 

30±2 rpm

None None End-over-end rotation at 

30±2 rpm

Assays pH, electrical 

conductivity, redox 

(optional), IC/DOC, 

COPC concentrations

pH, electrical 

conductivity, redox 

(optional), IC/DOC, 

COPC concentrations

pH, electrical 

conductivity, redox 

(optional), IC/DOC, 

COPC concentrations

pH, electrical 

conductivity, redox 

(optional), IC/DOC, 

COPC concentrations

Filtration Settling/ centrifugation; 

filtration at 0.45- m

Settling/ centrifugation; 

filtration at 0.45- m

Settling/ centrifugation; 

filtration at 0.45- m

Settling/ centrifugation; 

filtration at 0.45- m

Comments Extensive QA/QC 

including method blanks 

(maximum acid addition, 

maximum base addition, 

reagent water) and 

analytical quantification/ 

detection limits

Extensive QA/QC 

including method blanks 

(reagent water), 

comparison to Method 

1313, and analytical 

quantification / detection 

limits

Extensive QA/QC 

including method blanks 

(reagent water), 

comparison to Method 

1313, and analytical 

quantification / detection 

limits

Extensive QA/QC 

including method blanks 

(reagent water), 

comparison to Method 

1313, and analytical 

quantification / detection 

limits
44 

5 ESTIMATES OF LABORATORY PROCESSING TIME, MATERIAL 

REQUIREMENTS AND SUPPLY/EQUIPMENT COSTS 

This document provides estimates of time, material and costs for each of the four test methods as 

a means of illustrating the required resources to complete these tests. 

5.1 LABOR/PROCESSING TIME 

Table 6 shows approximate labor time (in hours) and process time (in days) to complete a test 

run and two subsequent test replicates. Process time considers the duration of time from when 

the subject material is received to the completion of the test replicate and includes all preparatory 

steps as specified in the test method. Labor time considers only that time when a technician is 

actively working on a test method which is often a fraction of the total processing time (e.g., the 

technician is free to work elsewhere when batch tests are tumbling or column test are not being 

monitored). 

Table 6. Summary of Estimates for Labor Time and Total Processing Time 

Test (singlet) +1 Replicate +2 Replicates

(duplicate) (triplicate)

Labor Process Labor Process Labor Process

[hr] [d] [hr] [d] [hr] [d]

7a 7a 7a Method 1313 10a-15 -12 15a-20 -14 20a-25 -14

Method 1314 12 21 20 21 28 21

Method 1315 15 64b-69 25 69 35 69

Method 1316 6 7 8 7 10 7

a

 Labor and processing time are reduced if prior knowledge of material behavior is available (e.g., titration curve). 

b

 Processing time is longer for granular materials due to added steps (e.g., optimum density analysis, packing 

samples). 

A step-by-step breakdown of labor time estimates is presented in Table E-1 through Table E-4 

found in Appendix E. Labor time estimates consider that the laboratory technician is familiar 

with the test method, but not significantly experienced. Thus, the labor time required to conduct 

the initial tests when a technician is still learning the test method sequence may be longer than 

provided in the table, whereas significant time reduction may be seen for well-experienced 

laboratory technicians. All labor time estimates account for reduced time based on “economy of 

scale” (e.g., moisture content, drying, particle-size reduction may be conducted for all replicates 

at one time). 
45 

A useful presentation of process time is a Gantt style chart as shown in Figure 8 through Figure 

11. These figures show the method task duration and the critical path relationship between tasks. 

For example, the “as received” moisture content of a subject material is independent of other 

task; whereas, particle size analysis or reduction of “as received” material to produce an “as 

tested” sample is essential for all subsequent tasks for Method 1313, Method 1314, and Method 

1315. Some processing time may be saved if air drying of granular “as received” material is not 

necessary. All task durations estimates are based on previous experience and are considered to 

be conservative (i.e., over-estimate task duration). Schedules for batch extraction procedures 

(Method 1313 and Method 1316) are based on working days, whereas schedules for flowdependent and time-dependent procedures (Method 1314 and Method 1315, respectively) are 

include weekends. 
46 

Figure 8. Gantt Style Chart of A Typical Method 1313 Processing Schedule. 
47 

Notes on Figure 8. 

1) Schedule is based on workdays (i.e., weekends will add time to total). 

2) Particle-size reduction assumes a relatively easy material to reduce (e.g., coal combustion residues, soils) via mechanical grinder or light hand 

grinding with mortar/pestle. 

3) Green case (hatched) – baseline case with air drying and two rounds of pre-test titration (10 pre-test titration points in all). 

4) Red case (solid) – shortened case when air drying is not required for particle-size analysis/reduction. 

5) Blue case (dotted) – shortened case when prior titration knowledge is adequate to complete extractions. 
48 

Figure 9. Gantt Style Chart of a Typical Method 1314 Processing Schedule. 

Notes on Figure 9. 

1) Schedule is based on calendar days (i.e., column/fraction collection continues over weekends). 

2) Particle-size reduction assumes a relatively easy material to reduce (e.g., coal combustion residues, soils) via mechanical grinder or light hand 

grinding with mortar/pestle. 

3) Apparatus set includes sample wetting and equilibration overnight. 

4) Green case (hatched) – baseline case. 

5) Red case (solid) – shortened case when air drying is not required for particle-size analysis/reduction.
49 

Figure 10. Gantt Style Chart of a Typical Method 1315 Processing Schedule. 
50 

Notes on Figure 10. 

1) Schedule is based on calendar days (i.e., tank leaching and refreshes continue over weekends). 

2) Particle-size reduction assumes a relatively easy material to reduce (e.g., coal combustion residues, soils) via mechanical grinder or light hand grinding with 

mortar/pestle. 

3) Green case (hatched) – baseline case for granular materials with air drying. 

4) Red case (solid) – shortened case for granular materials when air drying is not required for particle-size analysis/reduction. 

5) Blue case (dotted) – baseline case for monolithic materials. 
51 

Figure 11. Gantt Style Chart of a Typical Method 1316 Processing Schedule. 

Notes on Figure 11. 

1) Schedule is based on workdays (i.e., weekends will add time to total). 

2) Particle-size reduction assumes a relatively easy material to reduce (e.g., coal 

combustion residues, soils) via mechanical grinder or light hand grinding with 

mortar/pestle. 

3) Green case (hatched) – baseline case with air drying. 

4) Red case (solid) – shortened case when air drying is not necessary for particle-size 

analysis/reduction. 
52 

5.2 MATERIAL REQUIREMENTS 

An estimate of the amount of solid material required to conduct all steps in each test method is 

shown in Table 7 for a single test and two subsequent test replicates. These estimates are based 

on minimum required dry mass for each test with allowance for a 50% safety factor and an 

assumed “as received” moisture content of 20% on a wet basis (i.e., solids content of 80%). 

Thus, the estimates shown in Table 7 may be considered to be conservative for most cases and 

should provide sufficient material to allow for minor mistakes in laboratory procedures. 

Table 7. Summary of Solid Materials Required for Test Methods 

Test

(singlet)

+1 Replicate

(duplicate)

+2 Replicates

(triplicate)

Method 1313 800 g-dry 1,200 g-dry 1,600 g-dry

Method 1314 700 g-dry 1,400 g-dry 2,100 g-dry

Method 1315 (granular) 5,000 g-dry 6,500 g-dry 8,000 g-dry

Method 1316 1,000 g-dry 2,000 g-dry 3,000 g-dry

Subtotal [kg-dry] 7.5 10.0 15.0

w/ 50% safety [kg-dry] 11.0 15.0 22.0

Mass at 80% Solids Content [kg] 15.0 20.0 30.0

The material estimate for Method 1315 is based on testing of a compacted granular sample. In 

this case, material in addition to that required for the test samples must be provided in order to 

determine the optimum moisture/density relationship and determine a target moisture content for 

packing of test samples. Thus, the compact granular case typically requires more sample mass 

than the monolithic material case. When testing monolithic materials, the amount of sample for 

Method 1315 will depend on sample geometry and dimensions as well as material density. For 

example, a 10-cm diameter by 10-cm long cylinder of a monolithic material with a density of 2.0 

g/cm3 would require a sample of approximately 1,600 g. 

5.3 SUPPLIES AND EQUIPMENT 

Total estimated costs of supplies and equipment for the first test run and two subsequent 

replicate tests are shown in Table 8 for each of the four test methods. Supplies costs include 

consumable items which are not reused after the tests (e.g., filter paper, bottles, etc.) whereas 

equipment cost include both capital purchases (e.g., tumblers, pumps, compaction rammers, etc.) 

and supplies which may be cleaned and reused between test replicates (e.g., filter holders). 
53 

Table 8. Summary of Estimated Supply and Equipment Costs (as of July 2010) 

Test (singlet) +1 Replicate 

(duplicate)

+2 Replicates

(triplicate)

Supply Equip. Supply Equip. Supply Equip.

Method 1313 $200 $8,200 $310 $9,100 $430 $10,000

Method 1314 $110 $4,400 $210 $5,800 $310 $7,100

Method 1315a $170 $2,000 $260 $3,000 $350 $4,000

Method 1316 $85 $7,500 $160 $8,000 $230 $8,600

a Method 1315 cost shown for more expensive material type (granular). 

These cost estimates in Table 8 are based on items and costs for supplies and equipment found 

primarily in the Fisher Scientific online catalog as detailed in Appendix G. The items presented 

in the appendix have been selected as examples of items which may be used to complete these 

test methods, but selection does not denote endorsement of vendor, manufacturer or product by 

the authors or U.S. EPA. 

The cost estimates for test replicates account for “economy of scale” within each method (e.g., 

blanks as assumed to be conducted once for all test replicates). However, some savings may 

occur by limiting equipment purchases when a laboratory is preparing the conduct multiple test 

methods (e.g., the same tumbler may be used to conduct both Method 1313 and Method 1314, all 

test may use the same set of filter holders). 
54 

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APPENDIX A 

METHOD 1313 (R2) – 

LIQUID-SOLID PARTITIONING AS A FUNCTION OF EXTRACT pH 

IN SOLID MATERIALS USING A PARALLEL BATCH PROCEDURE 
1313 - 1 Revision 2 

September 2010 

PRELIMINARY VERSION1 OF METHOD 1313 

LIQUID-SOLID PARTITIONING AS A FUNCTION OF EXTRACT pH IN SOLID MATERIALS 

USING A PARALLEL BATCH 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 method use for the analysis 

of method-defined parameters, are intended to be guidance methods which 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. The performance data 

included in this method are for guidance purposes only, and are not intended to be and must not 

be used as absolute quality control (QC) acceptance criteria for purposes of laboratory 

accreditation. 

1.0 SCOPE AND APPLICATION 

 1.1 This method is designed to provide aqueous extracts representing the liquidsolid partitioning (LSP) curve as a function of pH for inorganic constituents (e.g., metals and 

radionuclides), semi-volatile organic constituents (e.g., polycyclic aromatic hydrocarbons or 

PAHs) and non-volatile organic constituents (e.g., dissolved organic carbon) in solid materials. 

The LSP curve is evaluated as a function of final extract pH at a liquid-to-solid ratio (L/S) of 10 

mL extractant/g dry sample (g-dry) and conditions that approach liquid-solid chemical 

equilibrium. This method also yields the acid/base titration and buffering capacity of the tested 

material at an L/S of 10 mL extractant/g-dry sample. The analysis of extracts for dissolved 

organic carbon and the solid phase for total organic carbon allow for the evaluation of the 

impact of organic carbon release and the influence of dissolved organic carbon on the LSP of 

inorganic constituents. 

 1.2 This method is intended to be used as part of an environmental leaching 

assessment for the evaluation of disposal, beneficial use, treatment effectiveness and site 

remediation options. 

 1.3 This method is suitable for a wide range of solid materials. Examples of solid 

materials include: industrial wastes, soils, sludges, combustion residues, sediments, stabilized 

materials, construction materials, and mining wastes. 

 1.4 This method is a leaching characterization method that is used to provide 

values for intrinsic material parameters that control leaching of inorganic and some organic 

 

1

 Preliminary Version denotes that this method has not been endorsed by EPA but is under consideration 

for inclusion into SW-846. This method has been derived from published procedures (Kosson et al, 2002) 

using reviewed and accepted methodologies (U.S. EPA2006, 2008, 2009). The method has been 

submitted to the U.S. EPAOffice of Resource Conservation and Recovery and is currently under review 

for development of interlaboratory validation studies to develop precision and bias information. 
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species under equilibrium conditions. This test method is intended as a means for obtaining a 

series of extracts of a solid material (i.e., the eluates), which may be used to estimate the LSP 

(e.g., solubility and release) of constituents as a function of pH under the laboratory conditions 

described in the method. Eluate constituent concentrations may be used in conjunction with 

information regarding environmental management scenarios to estimate the anticipated 

leaching concentrations, release rate and extent for individual material constituents under the 

management to be evaluated. Eluate constituent concentrations generated by this method may 

also be used along with geochemical speciation modeling to infer the mineral phases that 

control the LSP in the pore structure of the solid material. 

 1.5 This method is not applicable for characterizing the release of volatile organic 

analytes (e.g., benzene, toluene, xylenes). 

 1.6 The relationships between eluate concentrations observed from this method 

and field leachate must be considered in the context of the material being tested and the field 

scenario being evaluated. This method provides solutions considered indicative of eluate under 

field conditions, only where the field leaching pH is the same as the final laboratory extract pH 

and the LSP is controlled by aqueous phase saturation of the constituent of interest. 

 1.7 The maximum mass of constituent released over the range of method pH 

conditions (2 ≤ pH ≤ 13) may be considered an estimate of the maximum mass of the 

constituent leachable under field leaching conditions for intermediate time frames and the 

domain of the laboratory test pHs. 

 1.8 The solvents used in this method include dilute solutions of nitric acid (HNO3) 

and potassium hydroxide (KOH) in reagent water. 

 1.9 Analysts are advised to take reasonable measures to ensure that the sample is 

homogenized to the extent practical, prior to employment of this method. Particle-size reduction 

may provide additional assurance of sample homogenization and also facilitate achievement of 

equilibrium during the test procedure. Table 1 of this standard designates a recommended 

minimum dry mass of sample to be added to each extraction vessel and the associated 

extraction contact time as a function of particle diameter. If the heterogeneity of the sample is 

suspected as the cause of unacceptable precision in replicate test results or is considered 

significant based on professional judgment, the sample mass used in the test procedure may be 

increased to a greater minimum dry mass than that shown in Table 1 with the amount of 

extractant increased proportionately to maintain the designated L/S. 

 1.10 In the preparation of solid materials for use in this method, particle-size 

reduction of samples with a large grain size is performed in order to enhance the approach 

towards equilibrium under the designated contact time interval of the extraction process. The 

extract contact time for samples reduced to a finer maximum particle size will consequently be 

shorter (see Table 1). 

 1.11 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), 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 guidance on the 

intended flexibility in the choice of methods, apparatus, materials, reagents, and supplies, and 

on the responsibilities of the analyst for demonstrating that the techniques employed are 
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appropriate for the analytes of interest, in the matrix of interest, and at the concentration 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 EPA 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. Guidance on defining 

data quality objectives can be obtained at http://www.epa.gov/QUALITY/qs-docs/g4-final.pdf

 1.12 Use of 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 consists of parallel extractions of a particle size-reduced solid material in 

dilute acid or base and reagent water. A flowchart for performing this method is shown in Figure 

1. Particle-size reduction of the material to be tested is performed according to Table 1. A 

schedule of acid and base additions is formulated from a pre-test titration curve or prior 

knowledge indicating the required amount of acid or base (equivalents/g) to be added to a 

series of extraction vessels so as to yield a series of eluates with final pH at nine specified 

target pH values in the range of 2-13. Extraction at natural conditions (e.g., extraction with 

regeant water only at a liquid-solid ratio of 10 mL/g-dry) may be used to substitute for a 

specified target pH if the natural pH falls within the acceptable tolerance for any of the nine 

specified target pH values. If the natural pH does not fall with any acceptable tolerance, an 

additional extraction vessel is required to conduct an extraction at natural pH conditions. In 

addition to the test position extractions, three method blanks without solid sample are carried 

through the procedure in order to verify that analyte interferences are not introduced as a 

consequence of reagent impurities or equipment contamination. The extraction bottles (i.e., 

eight or nine test positions, natural pH, and three method blanks) are tumbled in an end-overend fashion for a specified contact time, which depends on the particle size of the sample (see 

Table 1). At the end of the specified contact interval, the liquid and solid phases are roughly 

separated via settling or centrifugation. Eluate pH and specific conductivity measurements are 

then made on an aliquot of the liquid phase and the remaining bulk of the eluate is clarified by 

either pressure or vacuum filtration. In cases where rough separation is not practical or results 

in grossly incomplete clarification, eluate measurements may be taken immediately following 

filtration. Analytical samples of the filtered eluate are collected and preserved as appropriate for 

the desired chemical analyses. The eluate concentrations of constituents of potential concern 

(COPCs) are determined and reported. In addition, COPC concentrations may be plotted as a 

function of eluate pH and compared to quality control and assessment limits for the 

interpretation of method results. 

3.0 DEFINITIONS 

 3.1 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. 
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 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 LSP — The distribution of COPCs between the solid and liquid phases at the 

conclusion of the extraction. 

 3.4 L/S — The fraction of the total liquid volume (including the moisture contained 

in the “as used” solid sample) to the dry mass equivalent of the solid material. L/S is typically 

expressed in volume units of liquid per dry mass of solid material (mL/g-dry). 

 3.5 “As-tested” sample — The solid sample at the conditions (e.g., moisture content 

and particle-size distribution) present at the time of the start of the test procedure. The “astested” conditions will differ from the "as-received" sample conditions if particle-size reduction 

and drying were necessarily performed. 

 3.6 Dry-mass equivalent — The mass of “as-tested” (i.e., “wet”) sample that 

equates to the mass of dry solids plus associated moisture, based on the moisture content of 

the “as-tested” material. The dry-mass equivalent is typically expressed in mass units of the 

“as-tested” sample (g). 

 3.7 Refer to the SW-846 chapter of terms and acronyms for potentially applicable 

definitions. 

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 allglass systems may be necessary. Refer to each method to be used for specific guidance on 

quality control procedures and to Chapters Three and Four for general guidance on the cleaning 

of laboratory apparatus prior to use. 

 4.2 If potassium is a COPC, the use of KOH as a base reagent will interfere with 

the determination of actual potassium release. In this case, sodium hydroxide (NaOH) of the 

same grade and normality may be used as a substitute. 

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 OSHA regulations regarding the safe handling of the chemicals listed 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 of extracts and processing of extracts, some waste 

materials may generate heat or evolve potentially harmful gases when contacted with acids and 
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bases. Adequate prior knowledge of the material being tested should be used to establish 

appropriate personal protection and workspace ventilation. 

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 setting 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) which nonetheless may be required to perform the method. 

 6.1 Extraction vessels 

 6.1.1 Twelve wide-mouth bottles (i.e., nine for test positions plus three for 

method blanks) constructed of inert material, resistant to high and low pH values and 

interaction with COPCs as described in the following sections. 

NOTE: Depending on the value of the natural pH (determined from prior knowledge or 

the results of the pre-test titration), thirteen extraction bottles may be necessary 

per test replicate. 

 6.1.1.1 For the evaluation of inorganic COPC mobility, bottles 

made of high density polyethylene (HDPE) (e.g., Nalgene #3140-0250 or 

equivalent), polypropylene (PP), or polyvinyl chloride (PVC) are recommended. 

 6.1.1.2 For the evaluation of non-volatile organic and mixed 

organic/inorganic COPC mobility, bottles made of glass or Type 316 stainless 

steel are recommended. Polytetrafluoroethylene (PTFE) is not recommended 

for non-volatile organics due to the sorption of species with high hydrophobicity 

(e.g., PAHs). Borosilicate glass is recommended over other types of glass, 

especially when inorganic analytes are of concern. 

 6.1.2 The extraction vessels must be of sufficient volume to 

accommodate both the solid sample and an extractant volume, based on an L/S of 10 ± 

0.5 mL extractant/g-dry. The head space in the bottle should be minimized to the extent 

possible when semi-volatile organics are COPCs. For example, Table 1 indicates that 

250-mL volume bottles are recommended when the minimum 20 g-dry mass equivalent 

is contacted with 200 mL of extractant. 

 6.1.3 The vessel must have a leak-proof seals that can sustain end-overend tumbling for the duration of the designated contact time. 

 6.1.4 If centrifugation is anticipated to be beneficial for initial phase 

separation, the extraction vessels should be capable of withstanding centrifugation at 

4000 ± 100 rpm for a minimum of 10 ± 2 min. Alternately, samples may be extracted in 

bottles that do not meet this centrifugation specification (e.g., Nalgene I-Chem #311-
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0250 or equivalent) and the solid-liquid slurries transferred into appropriate 

centrifugation vessels for phase separation as needed. 

 6.2 Balance — Capable of 0.01-g resolution for masses less than 500 g. 

 6.3 Rotary tumbler — Capable of rotating the extraction vessels in an end-over-end 

fashion at a constant speed of 28 ± 2 rpm (e.g., Analytical Testing, Werrington, PA or 

equivalent). 

 6.4 Filtration apparatus — Pressure or vacuum filtration apparatus composed of 

appropriate materials so as to maximize the collection of extracts and minimize loss of the 

COPCs (e.g., Nalgene #300-4000 or equivalent) (see Sec. 6.1). 

 6.5 Filtration membranes — Composed of polypropylene or equivalent material with 

an effective pore size of 0.45-μm (e.g., Gelman Sciences GH Polypro #66548 from Fisher 

Scientific 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 Adjustable-volume pipettor — Oxford Benchmate series or equivalent. The 

necessary delivery range will depend on the buffering capacity of the solid material and 

acid/base strength used in the test. 

 6.11 Disposable pipettor tips. 

 6.12 Centrifuge (recommended) — Capable of centrifuging the extraction vessels at 

a rate of 4000 ± 100 rpm for 10 ± 2 min. 

7.0 REAGENTS AND STANDARDS 

 7.1 Reagent-grade chemicals must be used in all tests. Unless otherwise 

indicated, it is intended that all reagents conform to the specifications of the Committee on 

Analytical Reagents of the American Chemical Society, where such specification are available. 

Other grades may be used, provided it is first ascertained that the reagents are of sufficiently 

high purity to permit 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 must be interference free. All references to water in this method 

refer to reagent water unless otherwise specified. 
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 7.3 Nitric acid (2.0 N), HNO3 – Trace-metal grade or better, purchased at strength 

or prepared by diluting concentrated nitric acid with reagent water. Solutions with alternate 

normality may be used as necessary. In such cases, the amounts of HNO3 solution added to 

samples should be adjusted based on the equivalents required in the schedule of acid/base 

additions (see Sec. 11.4). 

 7.4 Potassium hydroxide (1.0 N), KOH – ACS grade, purchased at strength or 

prepared by diluting concentrated potassium hydroxide solution with reagent water, or otherwise 

by dissolving 56.11 g of solid potassium hydroxide in 1 L of reagent water. Solutions with 

alternate normality may be used as necessary. In such cases, the amounts of KOH solution 

added to samples should be adjusted based on the equivalents required in the schedule of 

acid/base additions (see Sec. 11.4). 

 7.5 Consult Methods 9040, 9045 and 9050 for additional information regarding the 

preparation of reagents required for pH and specific conductance measurements. 

8.0 SAMPLE COLLECTION, PRESERVATION, AND STORAGE 

 8.1 See the introductory material to Chapter Three “Inorganic Analytes” and 

Chapter Four “Organic Analytes.” 

 8.2 All samples should be collected using an appropriate sampling plan. 

 8.3 All analytical sample containers should be composed of materials that minimize 

interaction with solution COPCs. For further information, see Chapters Three and Four. 

 8.4 Preservatives should not be added to samples before extraction. 

 8.5 Samples can be refrigerated, unless refrigeration results in an irreversible 

physical change to the sample. 

 8.6 Analytical samples should be preserved according to the guidance given in the 

individual determinative methods for the COPCs. 

 8.7 Extract holding times should be consistent with the aqueous sample holding 

times specified in the determinative methods for the COPCs. 

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 criteria take precedence over both technique-specific criteria and those criteria given in 

Chapter One, and technique-specific QC criteria take precedence over the criteria in Chapter 

One. 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 that will implement the project and assess the results. 

Each laboratory should maintain a formal quality assurance program. The laboratory should 

also maintain records to document the quality of the data generated. All data sheets and quality 

control data should be maintained for reference or inspection. 
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 9.2 In order to demonstrate the purity of reagents and sample contact surfaces, 

method blanks should be tested at the extremes of the acid and base additions, as well as when 

only reagent water (no acid or base addition) is used for extraction. 

 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 quality control 

procedures. 

 9.4 Solid materials should be tested within one month of receipt unless the project 

requires that the "as-received" samples are tested sooner (e.g., the material is part of a timedependent study or the material may change during storage due to oxidation or carbonation). 

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 PREPARATORY PROCEDURES 

 A flowchart for the method procedure is presented in Figure 1. 

 11.1 Particle-size reduction (if required) 

 11.1.1 In this method, particle-size reduction is used for sample 

homogenization and to prepare large-grained samples for extraction so that the 

approach toward liquid-solid equilibrium is enhanced and mass transport through large 

particles is minimized. A longer extract contact time is required for larger maximum 

particle-size designations. This method designates three maximum particle sizes and 

associated contact times (see Table 1). The selection of an appropriate maximum 

particle size from this table should be based on professional judgment regarding the 

practical effort required to size-reduce the solid material. 

 11.1.2 Particle-size reduction of “as received” samples may be achieved 

through crushing, milling or grinding with equipment made from chemically-inert 

materials. During the reduction process, care should be taken to minimize the loss of 

sample and potentially volatile constituents in the sample. 

 11.1.3 If the moisture content of the “as received” material is greater than 

15% (wet basis), air drying or desiccation may be necessary. Oven drying is not 

recommended for the preparation of test samples due to the potential for mineral 
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alteration and volatility loss. In all cases, the moisture content of the “as received” 

material should be recorded. 

NOTE: If the solid material is susceptible to interaction with the atmosphere (e.g., 

carbonation, oxidation), drying should be conducted in an inert environment. 

 11.1.4 When the material appears to be of a relatively uniform particle size, 

calculate the percentage less than the sieve size as follows: 

Where: Msieved = mass of sample passing the sieve (g) 

Mtotal = mass of total sample (g) (e.g., Msieved + mass not passing sieve) 

 11.1.5 The fraction retained by the sieve should be recycled for further 

particle-size reduction until at least 85% of the initial mass has been reduced below the 

designated maximum particle size. Calculate and record the final percentage passing 

the sieve and the designated maximum particle size. For the uncrushable fraction of the 

“as received” material, record the fraction mass and nature (e.g., rock, metal or glass 

shards, etc). 

 11.1.6 Store the size-reduced material in an airtight container in order to 

prevent contamination via gas exchange with the atmosphere. Store the container in a 

cool, dark and dry place prior to use. 

11.2 Determination of solids and moisture content 

 11.2.1 In order to provide the dry mass equivalent of the “as-tested” 

material, the solids content of the subject material should be determined. Often, the 

moisture content of the solid sample is recorded. In this method, the moisture content is 

determined and recorded 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. 

 11.2.2 Place a 5–10-g sample of solid material into a pre-tared dish or 

crucible. Dry the sample to a constant mass at 105 ± 2 °C. Periodically check the 

sample mass after allowing the sample to cool to room temperature (20 ± 2 °C) in a 

desiccator. 

NOTE: The oven-dried sample is not used for the extraction and should be properly 

disposed of once the dry mass is determined. 

 11.2.3 Calculate and report the solids content as follows: 
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 Where: SC = solids content (g-dry/g) 

Mdry = mass of oven-dried sample (g-dry) 

Mtest = mass of “as-tested” sample (g) 

11.2.4 Calculate and report the moisture content (wet basis) as follows: 

 Where: MC(wet) = moisture content on a wet basis (gH2O/g) 

Mdry = mass of oven-dried sample (g-dry) 

Mtest = mass of “as-tested” sample (g) 

 11.3 Pre-test titration (if required) 

 In order to conduct the parallel batch test in Sec. 12.0, a schedule of acid and base 

additions should be formulated from either a pre-test titration or based on prior knowledge of the 

acid/base titration curve of the sample. This section describes the procedure for obtaining a 

titration curve of the test material, when sufficient prior knowledge is unavailable. 

 If the schedule of acid and base additions will be generated from prior knowledge, 

proceed to Sec. 11.4. If the schedule of acid and base additions is already known, proceed to 

Sec. 12.0. 

 Figures 2-4 show example titration curves for a wide variety of solid materials. Table 2 

indicates how these materials may be classified as (a) low alkalinity; (b) moderate alkalinity; or 

(c) high alkalinity in terms of the equivalents of acid required for obtaining final extraction pH 

values in the range of 2-13. 

 11.3.1 Predict the classification of the neutralization behavior of the solid 

material based on professional judgment, preliminary data, or the material examples 

shown in Table 2 and Figures 2-4. 

 11.3.2 Conduct a five-point parallel extraction test using 10-g-dry samples 

of the solid following the pre-test schedule shown in Table 3 for the chosen 

classification. One position in the five-point pre-test must be an extraction under natural 

test conditions (e.g., extraction with reagent water only at liquid-solid ratio of 10 mL/gdry). Perform the extraction following the procedure in Sec. 12.0, omitting the filtration, 

method blanks, and analytical sample collection. 
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 11.3.3 Plot the pre-test titration curve (e.g., the extract pH as a function of 

the equivalents of acid added) considering base equivalents as the negative sign of acid 

equivalents. 

 11.3.4 If a higher resolution in the titration curve is desired in order to 

determine intermediate acid/base additions for all target pH values, reiterate the pre-test 

extraction until the 2-13 pH range can be resolved. 

NOTE: Additional pre-test point(s) interpolating or extrapolating from the pre-test 

schedule may be necessary to provide adequate resolution in the titration curve. 

 11.3.5 Pre-test titration using provided Microsoft® Excel template 

 The “Pre-Test” worksheet in the provided Excel template may be used to 

calculate pre-test extraction formulations and plot the pre-test titration curve. Mandatory 

input data for the template includes: 

a) particle size of the “as tested” material (see Sec. 11.1); 

b) solids content of the “as tested” material (see Sec. 11.2); and 

c) five acid/base additions based on the predicted response classification of the 

solid material (see Sec. 11.3). 

Enter the eluate pH and plot the pre-test titration curve. Compare the resulting titration 

curve to the target pH values as designated in Table 4. 

 11.4 Formulation of acid and base additions schedule 

 A schedule of acid and base additions is used in the main extraction procedure (Sec. 

12.0) to set up nine extractions of the test material plus three method blanks. Based on either 

prior knowledge of the acid/base titration curve of the sample or the results of the pre-test 

titration procedure in Sec. 11.3, formulate a schedule of test extractions using the example in 

Table 4 and the following steps. 

 11.4.1 Using the extraction parameters in Table 1, identify the 

recommended minimum dry-mass equivalent associated with the particle size of the “astested” sample. Calculate and record the amount of “as tested” material equivalent to 

the dry-material mass from Table 1 as follows: 

Where: Mtest = mass of “as-tested” solid equivalent to the dry-material mass (g) 

 Mdry = mass of dry material specified in the method (g-dry) 

 SC = solids content of “as-tested” material (g-dry/g) 

 11.4.2 Label Column A of the schedule table with consecutive numbers for 

the nine test positions (shown in Table 4 as “TXX” labels) and three method blanks 

(shown in Table 4 as “BXX” labels). 
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 11.4.3 Copy the nine target pH points as shown in Table 5 and enter this 

data into Column B of the schedule table. The natural pH value (e.g., pH resulting from 

extraction with reagent water only at L/S 10) may be used as a substitute for a test 

position pH value if it falls within the tolerance of the specified target pH. For example, if 

the natural pH is 11.8 and would satisfy the target pH of 12.0 ± 0.5, the extraction at 

natural conditions would be conducted and the specified target point of 12.5 ± 0.5 would 

be removed from Table 5. 

 11.4.4 For each test position, determine the equivalents of acid or base 

required to meet the target pH from the pre-test titration curve (see Sec. 11.3). Enter 

this data into Column C of the schedule table. Interpolate intermediate acid additions on 

the pre-test titration curve using linear interpolation or other regression techniques. 

NOTE: Linear interpolation will have some inherent error, which may result in an extract 

pH that falls outside of the target pH tolerance. Additional pre-test points 

interpolating or extrapolating from the pre-test schedule in Table 3 may be 

necessary to provide adequate resolution of the titration curve. 

 11.4.5 Enter the acid volumes in Column D and base volumes in Column E 

of the schedule after converting the equivalents of acid and base to volume as follows: 

 Where: Va/b = volume of acid or base to be entered in the schedule table (mL) 

Eqa/b = equivalents of acid or base selected for the target pH as 

 determined from the pre-test titration curve (meq/g) 

Na/b = normality of the acid or base solution (meq/mL) 

 11.4.6 In Column F of the schedule table, calculate the volume of moisture 

contained in the “as tested” sample as follows: 

Where: VW,sample = volume of water in the “as tested” sample (mL) 

Mtest = mass of the “as tested” sample (g) 

SC = solids content of the “as tested” sample (g-dry/g) 

ρw = density of water (1.0 g/mL at room temperature) 

 11.4.7 In Column G of the schedule table, calculate the volume of reagent 

water required to bring each extraction to an L/S of 10 mL/g-dry solid as follows: 
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Where: VRW = volume of reagent water required to complete L/S (mL) 

Mdry = dry mass equivalent of solid sample (g) 

L/S= liquid-to-dry-solid ratio (10 mL/g) 

VW,sample = volume of water in “as used” sample (mL) 

Va/b = volume of acid or base for the extraction recipe (mL) 

 11.4.8 Method Blanks 

 In the schedule table, include three additional extractions for processing 

method blanks. Method blanks extractions are performed using the same equipment, 

reagents, and extraction process as the test positions, but without solid sample. The 

three method blanks should include: 

a) reagent water (B01 in Table 4); 

b) reagent water + maximum volume of acid in the schedule (B02 in Table 4); 

and 

c) reagent water + maximum volume of base in the schedule (B03 in Table 4). 

NOTE: If multiple materials or replicate tests are carried out in parallel, only one set of 

method blanks is necessary. 

 11.4.9 Schedule formulation using Excel template 

 The “Test Data” worksheet in the provided Excel template may be used to 

automatically calculate a schedule of acid and base additions, as well as to plot the 

response eluate pH and conductivity as a function of acid addition. Mandatory input 

data for the template includes: 

a) particle size of the “as tested” material (see Sec. 11.1); 

b) solid content of the “as tested” material (see Sec. 11.2); and 

c) nine acid/base additions determined from the pre-test titration curve with 

respect to target pH values designated in Table 5. 

 Subsequent to the extraction procedure, eluate pH, conductivity, and oxidation/reduction 

potential (optional) for up to three replicates may be entered and plotted as a function of acid 

added. 

12.0 EXTRACTION PROCEDURE 

 Use the schedule of acid and base additions (Sec. 11.4) as a guide to set up nine test 

extractions and three method blanks as follows: 

 12.1 Label bottles with test position and method blank numbers according to the 

schedule of acid and base additions (see Column A in Table 4). 
1313 - 14 Revision 2 

September 2010 

 12.2 Use the extraction parameters in Table 1 to identify the recommended drymass equivalent associated with the particle size of the “as tested” sample. Calculate and 

record the amount of “as tested” material equivalent to the identified dry mass from Table 1 as 

follows: 

Where: Mtest = mass of “as tested” solid equivalent to g of dry material (g) 

Mdry = mass of dry material specified in method (g) 

SC = solids content of “as tested” material (g/g) 

 12.3 Place the dry equivalent mass (± 0.1 g) of the “as tested” sample, calculated 

above, into each of the test position extraction vessels. 

NOTE: Do NOT put solid material in the method blank extraction vessels. 

 12.4 Add the appropriate volume of reagent water (± 5% of target value) to both the 

test position and method blank extraction vessels, as specified in the schedule for the L/S 

makeup (see Column G in Table 4). 

 12.5 Add the appropriate volume of acid or base (± 1% of target value) to each 

vessel, using a continuously adjustable pipettor, as designated in the schedule for acid/base 

addition (see Column D and Column E in Table 4). 

 12.6 Tighten the leak-proof lid on each bottle and tumble all extractions 

(i.e., test positions and method blanks) in an end-over-end fashion at a speed of 28 ± 2 

rpm at room temperature (20 ± 2 °C). The contact time for this method will vary depending on 

the sample particle size as shown in Table 1. 

NOTE: The length of the contact time is designed to enhance the approach toward liquid-solid 

equilibrium. Longer contact times are required for larger particles to compensate for the 

effects of intra-particle diffusion. See Table 1 for recommended contact times based on 

particle size. 

 12.7 Remove the extraction vessels from the rotary tumbler and clarify the 

extractants by allowing the bottles to stand for 15 ± 5 min. Alternately, centrifuge the extraction 

vessels at 4000 ± 100 rpm for 10 ± 2 min. 

NOTE: If clarification is significantly incomplete after settling or centrifugation, eluate 

measurements for pH, conductivity, and oxidization-reduction potential (ORP) may be 

taken on filtered samples. In this case, perform the filtration in 12.9 prior to eluate 

measurement in 12.8 and note the deviation from the written procedure. 

CAUTION: Following separation from the solid phase, eluate samples lack the buffering 

provided by the solid phase and therefore may be susceptible to pH change 

resulting from interaction with air. 
1313 - 15 Revision 2 

September 2010 

 12.8 For each extract vessel, decant a minimum volume (~ 5 mL) of clear, 

unpreserved supernatant into a clean container. Measure and record the pH, specific 

conductivity, and oxidation-reduction potential (optional, but strongly recommended) of the 

extracts (see Methods 9040, 9045, and 9050). 

NOTE: Eluate measurements for pH, conductivity, and ORP should be taken as soon as 

possible after the settling and preferably within 1 hour after completion of tumbling 

(12.6). 

12.9 Separate the solid from the remaining liquid in each extraction vessel by 

pressure or vacuum filtration through a clean 0.45-μm pore size membrane (Sec. 6.5). The 

filtration apparatus may be exchanged for a clean apparatus as often as necessary until all 

liquid has been filtered. 

NOTE: If it is suspected that COPCs (e.g., mercury) might be lost under vacuum, the samples 

may be pressure-filtered using an inert gas (e.g., nitrogen or argon). 

 12.10 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. 

13.0 DATA ANALYSIS AND CALCULATIONS (EXCEL TEMPLATE PROVIDED) 

 13.1 Data reporting 

 13.1.1 Figure 5 shows an example of a data sheet that may be used to 

report the concentration results of this method. This example is included in the Excel 

template. At a minimum, the basic test report should include: 

 a) Name of the laboratory 

 b) Laboratory technical contact information 

 c) Date at the start of the test 

 d) Name or code of the solid material 

 e) Particle size (85 wt% less than) 

 f) Type of acid and/or base used in test 

 g) Extraction contact time (h) 

 h) Ambient temperature during extraction (°C) 

 i) Eluate specific information (see Sec. 13.1.2 below) 
1313 - 16 Revision 2 

September 2010 

 13.1.2 The minimum set of data that should be reported for each eluate 

includes: 

 a) Eluate sample ID 

 b) Mass of “as tested” solid material used (g) 

 c) Moisture content of material used (gH O2 /g) 

 d) Volume (mL) and normality (N) of acid and/or base used 

 e) Volume of water added (mL) 

 f) Target pH 

 g) Measured final eluate pH 

 h) Measured eluate conductivity (mS/cm) 

 I) Measured ORP (mV) (optional) 

 j) Concentrations of all COPCs 

 k) Analytical QC qualifiers as appropriate 

13.2 Data interpretation (optional) 

 13.2.1 Acid/base neutralization curve 

 Plot the pH of each extract as a function of the equivalents of acid or base 

added per dry gram of material to generate an acid/base neutralization curve. 

NOTE: For materials in which both acid and base were used, equivalents of base can 

be presented as the opposite sign of acid equivalents (i.e., 5 meq/g-dry of base 

would correspond to -5 meq/g-dry of acid). 

 The titration curve can be interpreted as showing the amount of acid or base 

that is needed to shift the pH of the subject material. This is helpful when evaluating 

field scenarios where the pH of leachates is not buffered by the acidity or alkalinity of the 

solid material. 

 13.2.2 LSP curve 

 An LSP curve can be generated for each COPC following chemical analyses of 

all extracts by plotting the target analyte concentration in the liquid phase as a function 

of the measured extract pH for each extract. As an example, Figure 6 illustrates the LSP 

curves for arsenic and selenium from a coal combustion fly ash and indicates the limits 

of quantitation (shown as ML and MDL) and the natural concentration response. 

 13.2.2.1 The lower limit of quantitation (LLOQ) of the 

determinative method for each COPC may be shown as a horizontal line. 

COPC concentrations below this line indicate negligible or non-quantitative 

concentrations. 

NOTE: The lower limit of quantitation is highly matrix dependent and should be 

determined as part of a QA/QC plan. 
1313 - 17 Revision 2 

September 2010 

 13.2.2.2 Natural response is defined as the eluate pH and 

COPC concentration measured when the solid material is extracted with 

reagent water at an L/S of 10 mL/g-dry. The natural response values can be 

shown on the LSP curve as a vertical line from the x-axis (at the replicate 

average natural pH) intersected with a horizontal line (at the replicate average 

COPC concentration). Alternatively, the natural response can be indicated in 

results using a different symbol from other results. 

 13.2.2.3 The values on the curve indicate the eluate 

concentration of the constituent of interest at an L/S of 10 mL/g-dry over a pH 

range. The shape of the LSP curve is indicative of the speciation of the COPC 

in the solid phase with four characteristic LSP curve shapes (i.e., relative 

locations of maxima and minima) presented schematically in Figure 7. 

 Cationic Species (e.g., Cd) — The LSP curve of cationic species 

typically has a maximum concentration in the acidic pH range that decreases to 

lower values at alkaline pH. 

 Amphoteric Species (e.g., Pb, Cr(III), Cu.) — The LSP curves tend 

to be similar in shape to cationic LSP curves with greater concentrations in the 

acidic pH range. However, the concentrations pass through a minimum in the 

near neutral to slightly acid pH range only to increase again for alkaline pH 

values. Typically, the increase at high pH is due to the solubility of hydroxide 

complexes (e.g., [Pb(OH3)]-

). 

 Oxyanionic Species (e.g. [AsO - - 4] , [SeO4] , [MnO ]- 4 ) — The LSP 

curves often show maxima in the neutral to slightly alkaline range. 

 Highly Soluble Species (e.g., Na+

, K+, Cl-) — The LSP curve is only 

a weak function of pH. 

 The idealized LSP curves in Figure 7 can be compared with the 

general shape of the test data to infer the speciation of the COPC in the solid 

matrix. Concentration results from this method may be simulated with 

geochemical speciation models to infer the mineral phases, adsorption 

reactions, and soluble complexes that control the release of the COPC (see 

Ref. 1). 

14.0 METHOD PERFORMANCE 

 14.1 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. These performance data are not intended to be and must not be used as 

absolute QC acceptance criteria for purposes of laboratory accreditation. 

 14.2 Refs. 2 and 3 may provide additional guidance and insight on the use, 

performance and application of this method. 
1313 - 18 Revision 2 

September 2010 

15.0 POLLUTION PREVENTION 

 15.1 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 U.S. EPA recommends recycling as the next best option as long as the 

management option if protective of human health and the environment. 

 15.2 For information about pollution prevention that may be applicable to 

laboratories and research institutions consult Less is Better: Laboratory Chemical Management 

for Waste Reduction available from the American Chemical Society's Department of 

Government Relations and Science Policy, 1155 16th St., N.W. Washington, D.C. 20036, 

http://www.acs.org. 

16.0 WASTE MANAGEMENT 

 The Environmental Protection Agency requires that laboratory waste management 

practices be conducted consistent with all applicable rules and regulations. The Agency urges 

laboratories to protect the 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 American Chemical Society at the address listed in Sec. 14.2. 

17.0 REFERENCES 

1. H. A. van der Sloot, P.F.A.B. Seignette, J.C.L. Meeussen, O. Hjelmar and D.S. Kosson, 

(2008), “A Database, Speciation Modeling and Decision Support Tool for Soil, Sludge, 

Sediments, Wastes and Construction Products: LeachXSTM-ORCHESTRA,” in Venice 

2008: Second International Symposium on Energy from Biomass and Waste, Venice, 

Italy, 17-20 November 2008 (also see www.leaching.com). 

2. D.S. Kosson, H.A. van der Sloot, F. Sanchez and A.C. Garrabrants, (2002), “An 

Integrated Framework for Evaluating Leaching in Waste Management and Utilization of 

Secondary Materials,” Environmental Engineering Science, 19(3) 159-204. 

3. D.S. Kosson, A.C. Garrabrants, H.A. van der Sloot (2009) “Background Information for 

the Development of Leaching Test Draft Methods 1313 through Method 1316”, (in 

preparation). 
1313 - 19 Revision 2 

September 2010 

4. U.S. EPA(2006) Characterization of Mercury-Enriched Coal Combustion Residues from 

Electric Utilities Using Enhanced Sorbents for Mercury Control, EPA-600/R-06/008, 

February 2006. 

5. U.S. EPA(2008) Characterization of Coal Combustion Residues from Electric Utilities 

Using Wet Scrubbers for Multi-Pollutant Control, EPA-600/R-08/077, July 2008. 

6. U.S. EPA(2009) Characterization of Coal Combustion Residues from Electric Utilities – 

Leaching and Characterization Data, EPA-600/R-09/151, December 2009. 

18.0 TABLES, DIAGRAMS, FLOW CHARTS, AND VALIDATION DATA 

 The following pages contain the tables and figures referenced by this method. 
1313 - 20 Revision 2 

September 2010 

TABLE 1 

EXTRACTION PARAMETERS AS FUNCTION OF MAXIMUM PARTICLE SIZE 

Particle Size 

(85 wt% less than)

(mm)

US Sieve 

Size 

Minimum Dry 

Mass

(g-dry)

Contact 

(h)

Time Suggested 

Vessel Size

(mL)

0.3 50 20 ± 0.02 24 ± 2 250 

2.0 10 40 ± 0.02 48 ± 2 500 

5.0 4 80 ± 0.02 72 ± 2 1000 

TABLE 2 

MATERIAL NEUTRALIZATION CLASSIFICATIONS 

Neutralization 

Classification 

Material Types 

Low Alkalinity soils; sediments; CCR fly ash; CCR bottom ash; coal milling rejects; 

MSWI fly ash, MSWI bottom ash; sewage sludge amended soil 

Moderate Alkalinity soils; wood 

arc furnace 

mortar 

preserving waste; MSWI bottom ash; steel slag; electric 

dust; MSW compost; nickel sludge; Portland cement 

High Alkalinity Portland 

(fly ash, 

cement clinker; steel blast furnace slag, 

blast furnace slag, Portland cement) 

solidified waste 

NOTE: CCR = Coal combustion residue 

MSWI = Municipal solid waste incinerator 
1313 - 21 Revision 2 

September 2010 

TABLE 3 

PRE-TEST TITRATION: ACID EQUIVALENT SCHEDULE 

Neutralization 

Classification 

Equivalents of Acid (meq/g-dry)

Bottle 1 Bottle 2 Bottle 3 Bottle 4 Bottle 5 

Low Alkalinity -2.0 -1.0 0 1.0 2.0 

Moderate Alkalinity -2.0 0 2.0 5.0 10.0 

High Alkalinity 0 5.0 10.0 15.0 25.0 

NOTE: 1) 

2) 

 

Base additions shown as opposite sign of acid equivalents. 

Additional pre-test point(s) interpolating or extrapolating from the pre-test 

may be necessary to provide adequate resolution in the titration curve. 

schedule 

TABLE 4 

EXAMPLE SCHEDULE OF ACID AND BASE ADDITIONS 

A B C D E F G 

Test 

position 

Target 

extract 

pH 

Equivalents 

of Acid

Volume of 

2N HNO3

Volume of 

1N KOH 

Volume of 

moisture in 

sample 

Volume of 

reagent water

(meq/g-dry) (mL) (mL) (mL) (mL)

T01 13.0 -1.10 - 22.0 2.22 176

T02 12.0 -0.75 - 15.0 2.22 183

T03 10.5 -0.38 - 7.60 2.22 190

T04 9.0 -0.15 - 3.0 2.22 195

T05 8.0 -0.05 - 1.0 2.22 197

T06 Natural 0 - - 2.22 198

T07 5.5 0.12 1.20 - 2.22 197

T08 4.0 0.90 9.00 - 2.22 189

T09 2.0 3.10 31.0 - 2.22 167

B01 QA/QC 0 - - - 200

B02 QA/QC 3.10 31.0 - - 169

B03 QA/QC -1.10 - 22.0 - 178

NOTE: 1) This schedule is based on “as tested” sample mass of 22.2±0.1 g (i.e., equivalent 

 “as tested” mass for a 20.0 g-dry sample at a solids content of 0.90 g-dry/g). 

2) In this example, the natural pH is assumed to be 7.0±0.5. 

3) Test positions marked B01, B02, and B03 are method blanks of reagent water, 

 reagent water + maximum acid addition, and reagent water + maximum base 

 addition, respectively. 

Data modified from Ref. 2. 
1313 - 22 Revision 2 

September 2010 

TABLE 5 

FINAL EXTRACT PH TARGETS 

pH Target Rationale 

2.0±0.5 Provides estimates of total or available COPC content 

4.0±0.5 Lower pH limit of typical management scenario 

5.5±0.5 Typical lower range of industrial waste landfills 

7.0±0.5 Neutral pH region; high release of oxyanions 

8.0±0.5 Endpoint pH of carbonated alkaline materials 

9.0±0.5 Minimum of LSP curve for some cationic and amphoteric COPCs 

10.5±0.5 Minimum of LSP curve for some cationic and amphoteric COPCs

12.0±0.5 Maximum in alkaline range for LSP curves of amphoteric COPCs 

13.0±0.5 Upper bound (field conditions) for amphoteric COPCs 

variable Natural pH at L/S 10 ml/g-dry (no acid/base addition)
1313 - 23 Revision 2

September 2010

FIGURE 1 

METHOD FLOWCHART 
1313 - 24 Revision 1.1 

April 2010 

FIGURE 2 

EXAMPLE TITRATION CURVES FOR SELECTED “LOW ALKALINITY” WASTES 

Some data taken LeachXS database (Ref. 1). 
1313 - 25 Revision 1.1 

April 2010 

FIGURE 3 

EXAMPLE TITRATION CURVES FOR SELECTED “MODERATE ALKALINITY” WASTES 

Some data taken from LeachXS database (Ref. 1). 
1313 - 26 Revision 1.1 

April 2010 

FIGURE 4 

EXAMPLE TITRATION CURVES FOR SELECTED “HIGH ALKALINITY” WASTES 

Some data taken from LeachXS database (Ref. 1).
1313 - 27 Revision 1.1 

April 2010 

FIGURE 5 

EXAMPLE DATA REPORT FORMAT 

EPA METHOD 1313

ABC Laboratories Report of Analysis

123 Main Street

Anytown, USA

 Contact: John Smith

 (555) 111-1111

Client Contact: Susan Jones

 (555) 222-2222

Material Code: XYZ Particle Size: 88% passing 2-mm sieve

Material Type: Coal Combustion Fly Ash Contact Time: 48 hours

Date Received: 10/1/20xx Lab Temperature: 21 ± 2 °C

Test Date: 11/1/20xx Acid Used: Nitric acid

Report Date: 12/1/20xx Base Used: Sodium hydroxide

Test

Position Replicate Value Units Method Note

T01 A

Eluate Sample ID XYZ-1313-T01-A

Solid Material 40.0 g

Moisture Content 0.01 g

Water Added 386.0 gH2O/g

Acid Added 14.0 mL

Acid Strength 2.0 mL

Base Added - N

Base Strength 1.0 mL

Target pH 2.0 ± 0.5 -

Eluate pH 1.89 - EPA 9040

Eluate Conductivity 12.6 mS/c

m 

EPA 9050

Eluate ORP 203 mv

QC Dilution

Chemical Analysis Value Units Flag Method Date Factor

Al 216.0 mg/L EPA 6020 11/7/20xx 1000

As 0.64 mg/L EPA 6020 11/7/20xx 10

Cl < 4.13 mg/L U EPA 9056 11/9/20xx 1

Test

Position Replicate Value Units Method Note

T02 A

Eluate Sample ID XYZ-1313-T02-A

Solid Material 40.0 g

Moisture Content 0.01 g

Water Added 400.0 gH2O/g

Acid Added 14.0 mL

Acid Strength 2.0 mL

Base Added - N

Base Strength 1.0 mL

Target pH 4.0 ± 0.5 -

Eluate pH 3.86 - EPA 9040 Natural pH

Eluate Conductivity 0.99 mS/c

m 

EPA 9050

Eluate ORP 180 mv

QC Dilution

Chemical Analysis Value Units Flag Method Date Factor

Al 449.0 mg/L EPA 6020 11/7/20xx 1000

As 0.979 mg/L EPA 6020 11/7/20xx 10

Cl < 4.13 mg/L U EPA 9056 11/7/20xx 1

QC Flag Key: U Value below lower limit of quantitation as reported (< "LLOQ")
1313 - 28 Revision 1.1 

April 2010 

FIGURE 6 

EXAMPLE LSP CURVES FROM A COAL COMBUSTION FLY ASH SHOWING ASSESSMENT 

ZONES FOR A LANDFILL SCENARIO 

Figure taken from Ref. 4. 
1313 - 29 Revision 1.1 

April 2010 

FIGURE 7 

SCHEMATIC LSP CURVES OF CATIONIC, AMPHOTERIC, 

AND OXYANIONIC SPECIES 

Figure taken from Ref. 2. 
APPENDIX B 

METHOD 1314 – 

ULIQUID-SOLID PARTITIONING AS A FUNCTION OF 

LIQUID-SOLID RATIO FOR CONSTITUENTS IN SOLID MATERIALS 

USING AN UP-FLOW PERCOLATION COLUMN PROCEDURE 
1314 - 1 Revision 1 

December 2009 

PRELIMINARY VERSION1 OF METHOD 1314 

ULIQUID-SOLID PARTITIONING AS A FUNCTION OF LIQUID-SOLID RATIO FOR 

CONSTITUENTS IN SOLID MATERIALS USING AN UP-FLOW PERCOLATION COLUMN 

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 method use for the analysis 

of method-defined parameters, are intended to be guidance methods which 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. The performance data 

included in this method are for guidance purposes only, and are not intended to be and must not 

be used as absolute QC acceptance criteria for purposes of laboratory accreditation. 

1.0 SCOPE AND APPLICATION 

 1.1 This method is designed to provide the liquid-solid partitioning (LSP) of 

inorganic constituents (e.g., metals, radionuclides) and non-volatile organic constituents (e.g., 

polycyclic aromatic hydrocarbons (PAHs), dissolved organic carbon) in a granular solid material 

as a function of liquid-to-solid (LS) ratio under percolation conditions. The first eluates of the 

column test provide insight into pore solution composition either in a granular bed (e.g., soil 

column) or in the pore space of low-permeability material (e.g., solidified monolithic or 

compacted granular fill). Analyses of eluates for dissolved organic carbon and of the solid 

phase for total organic carbon afford evaluation of the impact of organic carbon release and the 

influence of dissolved organic carbon on the LSP of inorganic constituents. 

 1.2 This method is intended to be used as part of environmental leaching 

assessment for the evaluation of disposal, beneficial use, treatment effectiveness and site 

remediation. 

 1.3 This method is suitable to a wide range of granular solid materials. Example 

materials include industrial wastes, soils, sludges, combustion residues, sediments, construction 

materials, and mining wastes. This method is not suitable to monolithic materials (e.g., cementbased and stabilized materials) without particle-size reduction prior to testing. 

 1.4 This test method is intended as a means for obtaining a series of extracts (i.e., 

the eluates) of a granular solid material which may be used to show eluate concentrations 

 

1 Preliminary Version denotes that this method has not been endorsed by EPA but is under consideration 

for inclusion into SW-846. This method has been derived from published procedures (Kosson et al, 

2002). The method has been submitted to the U.S. EPAOffice of Resource Conservation and Recovery 

and is currently under review for development of interlaboratory validation studies to develop precision 

and bias information.
1314 - 2 Revision 1 

December 2009 

and/or cumulative release as a function of LS ratio which can be related to a time scale when 

data on mean infiltration rate, density and height of application are available. 

 1.5 This method provides options for the preparation of analytical samples that 

provide flexibility based on the level of detail required. For example, when the purpose of 

characterization is for comparison to previous testing, compositing of eluates may be possible to 

create a reduced set of analytical samples. Table 1 outlines the eluate fractions and collection 

options, based on whether concentration or cumulative release is to be reported. The collection 

schemes are described below. 

 1.5.1 Complete characterization 

 For complete characterization of eluate concentration and cumulative release 

as a function of LS ratio, nine discrete eluate collections and analyses are required (see 

Table 1, Option A). No compositing of eluate fractions is performed for complete 

characterization, and all eluate fractions are analyzed. 

 Eluate concentrations from complete characterization may be used in 

conjunction with information regarding environmental management scenarios to 

estimate anticipated leaching concentrations, release rates, and extents of release for 

individual material constituents in the management scenarios evaluated. Eluate 

concentrations may also be used along with geochemical speciation modeling to infer 

the mineral phases that control the LSP in the pore structure of the solid material. 

 1.5.2 Limited analysis 

 Under a limited analysis approach, nine eluate collections and analysis of six 

analytical samples are required. If evaluation is based on eluate concentrations, six 

discrete eluate fractions are chemically analyzed (see 

Table 1, Option B). If evaluation is based on cumulative release, some eluate fractions 

are composited by volume-weighted averaging to create a set of six analytical samples 

(see Table 1, Option C). The concentrations of composite analytical samples cannot be 

interpreted along with eluate fractions on the basis of concentration. 

 1.5.3 Index testing

 For the determination of consistency between the subject material and 

previously characterized materials, nine eluate collections and analysis of three 

analytical samples are required. If consistency is to be determined by eluate 

concentrations, three discrete eluate fractions are chemically analyzed (see Table 1, 

Option D). If consistency is to be determined by cumulative release, some eluate 

fractions are composited by volume-weighted averaging to create a set of three 

analytical samples (see Table 1, Option E). The concentrations of composited 

analytical samples cannot be interpreted along with eluate fractions on the basis of 

concentration. 

 1.6 This method is not applicable to characterize the release of volatile organic 

analytes. 

 1.7 This method provides eluate solutions considered indicative of leachate under 

field conditions only where the field leaching pH is controlled by the alkalinity or acidity of the 
1314 - 3 Revision 1 

December 2009 

solid material and the field leachate is not subject to dilution or other attenuation mechanisms. 

The cumulative mass of constituent released over a LS ratio range may be considered an 

estimate of the maximum mass of that constituent to be leached under field leaching over 

intermediate time frames (e.g., up to 100 years) and the domain of laboratory test pH. 

 1.8 Prior to employing this method, analysts are advised to take reasonable 

measures to ensure that the granular sample is homogenized to the extent practical. Particlesize reduction may provide additional assurance of sample homogenization. 

 1.9 In preparation of solid materials for use in this method, particle-size reduction or 

exclusion of samples with large grain size is used to enhance the approach towards liquid-solid 

equilibrium over the residence time of eluant in the column. 

 1.10 The structure and use of this method is similar to that of NEN 7343 (see Ref. 1) 

and CEN TS 14405 (see Ref. 2). 

 1.11 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), quality control 

(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 guidance 

on the intended flexibility in the choice of methods, apparatus, materials, reagents, and 

supplies, and on 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 

concentration 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 EPA 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. Guidance on defining 

data quality objectives can be obtained at HUhttp://www.epa.gov/QUALITY/qs-docs/g4-final.pdf

 1.12 Use of 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 

 Eluant is introduced into a column of moderately-packed granular material in an up-flow 

pumping mode, with eluate collection performed as a function of the cumulative LS ratio. Upflow pumping is used to minimize air entrainment and flow channeling. The default eluant for 

most materials is reagent water. However, a solution of 1.0 mM calcium chloride in reagent 

water is used when testing materials with either a high clay content (i.e., to prevent 

deflocculation of clay layers) or high organic matter (i.e., to moderate mobilization of dissolved 

organic carbon). The flow rate is maintained between 0.5-1.0 LS/day to increase the likelihood 

of local equilibrium between the solid and liquid phases, due to residence times longer than 1 

day. Eluate volumes are chemically analyzed for a combination of inorganic and non-volatile 

organic analytes depending on the constituents of potential concern (COPC). For the purposes 

of chemical speciation modeling, the entire eluant volume up to 10 mL/g dry sample (g-dry) is 
1314 - 4 Revision 1 

December 2009 

collected in nine specific aliquots of varying volume. A limited subset of eluants volumes within 

the same LS ratio range may be collected and analyzed for regulatory and compliance 

purposes. A flowchart for performing this method is shown in Figure 1. 

3.0 DEFINITIONS 

 3.1 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 LSP — The distribution of COPCs between the solid and liquid phases at the 

conclusion of the extraction. 

 3.4 LS ratio — the fraction of the total liquid volume (including the moisture 

contained in the “as used” solid sample) to the dry mass equivalent of the solid material. LS

ratio is typically expressed in volume units of liquid per dry mass of solid material (mL/g-dry). 

 3.5 “As-tested” sample — The solid sample at the conditions (e.g., moisture content 

and particle-size distribution) present at the time of the start of the test procedure. The “astested” conditions will differ from the "as-received" sample conditions if particle-size reduction 

and drying were necessarily performed. 

 3.6 Dry-mass equivalent — The mass of “as-tested” (i.e., “wet”) sample that 

equates to the mass of dry solids plus associated moisture, based on the moisture content of 

the “as-tested” material. The dry-mass equivalent is typically expressed in mass units of the 

“as-tested” sample (g). 

 3.7 Refer to the SW-846 chapter of terms and acronyms for potentially applicable 

definitions. 

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 allglass systems may be necessary. Refer to each method to be used for specific guidance on 

quality control procedures and to Chapters Three and Four for general guidance on the cleaning 

of laboratory apparatus prior to use. 

 4.2 When the test method is applied to solid materials with a clay content greater 

than 10% or an organic matter content greater than 1%, a solution of 1.0 mM calcium chloride in 

reagent water is recommended to minimize deflocculation of clay minerals. However, the use of 

calcium chloride solution will interfere with the determination of actual calcium and chloride 

release. 
1314 - 5 Revision 1 

December 2009 

UNOTEU: The critical values of clay and organic matter content are verified during ruggedness 

testing. 

 4.3 When this method is applied to fine-grained, granular materials, tamping during 

column preparation may result in flow problems due to a low-permeability sample bed. This 

problem can be resolved by incorporating 20-50% inert material (e.g., 20–30-mesh normal sand 

or 2-mm borosilicate glass beads) into the solid sample. Alternatively, mass release from lowpermeability materials may be measured using Method 1315. 

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 OSHA regulations regarding the safe handling of the chemicals listed in this method. A 

reference file of material safety data sheets (MSDSs) should be available to all personnel 

involved in these analyses. 

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 setting 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). 

 6.1 Column apparatus 

 This method recommends the use of a specific column apparatus (see Figure 2). 

Equipment with equivalent specifications may be substituted. The apparatus should have 

valves and quick connectors (e.g., Luer lock fittings) such that the column with end caps can be 

removed for packing with test material and mass measurements. 

 6.1.2 A 30-cm, straight cylindrical column with an inner diameter (ID) of 5-

cm and constructed of inert material, resistant to high- and low-pH conditions and 

interaction with constituents of interest. 

 6.1.2.1 For the evaluation of inorganic COPC mobility, 

equipment composed of borosilicate glass (e.g., Kimble-Kontes CHROMAFLEX 

#420830-3020 or equivalent), polytetra-fluoroethylene (PTFE), high density 

polyethylene (HDPE), polypropylene (PP), or polyvinyl chloride (PVC) is 

recommended. 

 6.1.2.2 For the evaluation of non-volatile organic and mixed 

organic/inorganic COPCs, equipment composed of glass or Type 316 stainless 

steel is recommended. PTFE is not recommended for 
1314 - 6 Revision 1 

December 2009 

non-volatile organics, due sorption of species with high hydrophobicity (e.g., 

PAHs). Borosilicate glass is recommended over other types of glass, especially 

when inorganic analytes are of concern. 

 6.1.3 The column must be of sufficient volume to accommodate a 

minimum of a 300–g-dry material plus a 1-cm layer of silica sand (20-30 mesh) used at 

the bottom of the column to distribute eluant flow and at the top of the column to form a 

coarse filter for eluate particulates. 

 6.1.4 The column must have end cap materials that form a leak-proof seal 

and that can withstand pressures, such as encountered when pumping eluant through 

the column. 

 6.2 Eluant feed stock container — Resealable bottle or other container, constructed 

of inert material, capable of withstanding extreme pH conditions and interaction with any 

constituents of interest (see guidance in Sec. 6.1.2.). 

 6.3 Eluant feed tubing — 2-mm or similarly small ID tubing composed of 

chemically-inert material such as polyvinyl chloride or equivalent. 

UNOTEU: Larger ID tubing may be required if a single eluent stock container is used to feed 

multiple column set-ups. 

 6.4 Eluate collection bottles — capable of assembly with column apparatus using 

simple water locks in order to prevent the intrusion of air (see Figure 2). 

 6.5 20–30-mesh normal washed quartz sand 

6.6 Balance — Capable of 0.01-g resolution for masses less than 500 g. 

6.7 Filtration apparatus — Pressure or vacuum filtration apparatus composed of 

appropriate materials so as to maximize the collection of extracts and minimize loss of the 

COPCs (e.g., Nalgene #300-4000 or equivalent) (see Sec. 6.1). 

6.8 Filtration membranes — Composed of PP or equivalent material with an 

effective pore size of 0.45-μm (e.g., Gelman Sciences GH Polypro #66548 from Fisher Scientific 

or equivalent). 

6.9 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. 

6.10 pH combination electrode — Composed of chemically-resistant materials. 

6.11 Conductivity meter — Laboratory model (e.g., Accumet 20, Fisher Scientific or 

equivalent), with a minimum resolution of 5% of the measured value. 

6.12 Conductivity electrodes — Composed of chemically-resistant materials. 

7.0 REAGENTS AND STANDARDS 
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December 2009 

 7.1 Reagent-grade chemical must be used in all tests. Unless otherwise indicated, 

it is intended that all reagents conform to the specifications of the Committee on Analytical 

Reagents of the American Chemical Society, where such specification are available. Other 

grade may be used, provided it is first ascertained that 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 must be interference free. All references to water in this method 

refer to reagent water unless otherwise specified. 

 7.3 Calcium chloride (1.0 mM), CaCl2 — Prepared by dissolving 0.11 g of ACS 

grade or better solid calcium chloride in 1 L of reagent water. 

8.0 SAMPLE COLLECTION, PRESERVATION, AND STORAGE 

 8.1 See the introductory material to Chapter Three “Inorganic Analytes” and 

Chapter Four “Organic Analytes.” 

 8.2 All samples should be collected using an appropriate sampling plan. 

 8.3 All analytical sample containers should be composed of materials that minimize 

interaction with solution COPCs. For further information, see Chapters Three and Four. 

 8.4 Preservatives should not be added to samples before extraction. 

 8.5 Samples can be refrigerated, unless refrigeration results in an irreversible 

physical change to the sample. 

 8.6 Extracts should be preserved according to the guidance given in the individual 

determinative methods for the COPCs. 

 8.7 Extract holding times should be consistent with the aqueous sample holding 

times specified in the determinative methods for the COPCs. 

9.0 QUALITY CONTROL 

 9.1 Refer to Chapter One for guidance on quality assurance (QA) and QC 

protocols. When inconsistencies exist between QC guidelines, method-specific QC criteria take 

precedence over both technique-specific criteria and those criteria given in Chapter One, and 

technique-specific QC criteria take precedence over the criteria in Chapter One. 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 that will implement the project and assess the results. Each laboratory should 

maintain a formal quality assurance program. The laboratory should also maintain records to 

document the quality of the data generated. All data sheets and quality control data should be 

maintained for reference or inspection. 
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December 2009 

 9.2 In order to demonstrate the purity of reagents, at least one eluant blank should 

be tested. If multiple batches of eluant are employed, one eluant blank from each batch should 

be analyzed. 

 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 quality control 

procedures. 

 9.4 Unless the "as-received" samples are part of a time-dependent (e.g., aging) 

study, solid materials should be processed and tested within one month of their receipt. 

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 PREPARATORY PROCEDURES 

 11.1 Particle-size reduction (if required) 

 11.1.1 In this method, particle-size reduction is used to prepare largegrained samples for the column test so that the approach toward liquid-solid equilibrium 

is enhanced and fluid channeling along column walls is minimized. The maximum 

particle size of the solid should ≤ 1/20 of the column diameter. For the column 

recommended in this method, a maximum particle size of 2.5 mm is acceptable. 

Therefore, 85% of the test material should pass through a 2.38-mm (U.S. No. 8) sieve. 

If less than 15% of the solid material is larger than the maximum acceptable particle 

size, this fraction of the solid may be excluded from the material tested, rather than 

particle size-reduced. The mass and nature of the discarded fraction should be 

documented. 

 11.1.2 Particle-size reduction of “as received” sample may be achieved 

through crushing, milling or grinding with equipment made from chemically-inert 

materials. During the reduction process, care should be taken to minimize the loss of 

sample and potentially volatile constituents in the sample. 

 11.1.3 If the moisture content of the “as received” material is greater than 

15% (wet basis), air drying or desiccation may be necessary. Oven drying is not 

recommended for the preparation of test samples due to the potential for mineral 

alteration and volatility loss. In all cases, the moisture content of the “as received” 

material should be recorded. 
1314 - 9 Revision 1 

December 2009 

UNOTEU: If the solid material is susceptible to interaction with the atmosphere (e.g., 

carbonation, oxidation), drying should be conducted in an inert environment. 

 11.1.4 When the material seems to be of a somewhat uniform particle size, 

calculate the percentage less than the sieve size as follows: 

Where: Msieved = mass of sample passing the sieve (g) 

Mtotal = mass of total sample (g) (e.g., Msieved + mass not passing sieve) 

 11.1.5 The fraction retained by the sieve should be recycled for further 

particle-size reduction until at least 85% of the initial mass has been reduced below the 

designated maximum particle size. Calculate and record the final percentage passing 

the sieve and the designated maximum particle size. For the uncrushable fraction of the 

“as received” material, record the fraction mass and nature (e.g., rock, metal or glass 

shards, etc). 

 11.1.6 Store the size-reduced material in an airtight container in order to 

prevent contamination via gas exchange with the atmosphere. Store the container in a 

cool, dark and dry place prior to use. 

11.2 Determination of solids and moisture content 

 11.2.1 In order to calculate eluate collection as a function of the dry-mass 

equivalent of “as tested” sample material, the solids content of the solid sample material 

should be determined and recorded. In this method, the moisture content is determined 

and recorded on the basis of the “wet” or “as-tested” sample. 

UWARNINGU: 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. 

 11.2.2 Place a 5–10-g sample of solid material into a clean, pre-tared dish 

or crucible. Dry the sample to a constant mass at 105 ± 2 °C. Periodically check the 

sample mass after allowing the sample to cool to room temperature (20 ± 2 °C) in a 

desiccator. 

UNOTEU: The oven-dried sample is not used for the extraction and should be properly 

disposed of once the dry mass is determined. 

 11.2.3 Calculate and report the solids content as follows: 
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December 2009 

 Where: SC = solids content (g-dry/g) 

Mdry = mass of oven-dried sample (g-dry) 

Mtest = mass of “as-tested” sample (g) 

11.2.4 Calculate and report the moisture content (wet basis) as follows: 

 Where: MC(wet) = moisture content on a wet basis (gH2O/g) 

Mdry = mass of oven-dried sample (g-dry) 

Mtest = mass of “as-tested” sample (g) 

11.3 Column preparation 

 11.3.1 Prepare the column test apparatus as depicted in Figure 2. Eluant 

feed should be directed through the lower end cap and upwards into the column, in order 

to minimize air retention in the packed bed and fluid channeling along the column walls. 

UNOTEU: When solid samples may be affected by dissolved oxygen in the feed stock, an 

inert gas (e.g., nitrogen or argon) may be bubbled through the feed solution to 

displace oxygen or used to purge the headspace above the feed solution. 

UNOTEU: When alkaline or other air-sensitive eluates are expected, the vapor space of 

empty collections bottles may be purged with an inert gas 

(e.g., nitrogen or argon) prior to eluate collection. 

 11.3.2 Record the mass of the empty column with end caps and any tubing 

leads that are needed to separate the column from the entire apparatus. 

11.3.3 Place an approximately 1-cm thick layer of quartz sand (Sec. 6.5) 

on the bottom of the column using a small scoop or spoon. Record the mass of the 

column and sand layer. Level the sand layer by tapping the sides of the column. 

11.3.4 Pack the main body of the column with a minimum 300-g dry-mass 

equivalent of “as tested” sample in approximately five layers with light tamping with a 

glass rod to level the material between layers. The top of the packed sample should be 

approximately 1 cm from the level of the column interface with the top end cap. Record 

the mass of the column, lower sand layer, and “as tested” sample. 
1314 - 11 Revision 1 

December 2009 

11.3.5 Place a layer of sand to fill the approximate 1-cm gap between the 

top of the sample packing and the interface between the column and top-end cap. 

Record the total mass of the completely-packed column. 

11.3.6 Determine the “as tested” mass of the sample packing by 

subtracting the mass of the column and lower sand layer (Sec. 11.3.3) from the mass of 

the column, sand layer and packing (Sec. 11.3.4). 

11.3.7 Calculate the dry-mass equivalent packed of “as tested” sample into 

the column using the solids content as follows: 

 Where: Mdry = dry-mass equivalent of sample in column (g-dry) 

SC = solids content (g-dry/g) 

Mtest = mass of “as tested” sample in column (g) 

11.4 Pump setup 

 11.4.1 Prior to the start of the test, set the flow rate of the pump to a value 

that will provide an eluate production rate of 0.75 ± 0.25 LS/day. For example, given a 

dry-mass equivalent of 350 g-dry, an LS ratio of 0.5 would translate to 175 mL/g-dry, in 

which case the pump should be set to a flow rate of 175 mL/day. 

11.4.2 Prime the tubing with eluant 

11.4.2.1 Detach the inlet tubing from the bottom of the column 

and place the open end into a waste container. 

11.4.2.2 Turn on the pump and allow the inlet tubing to fill with 

eluent. Remove any air bubbles trapped in the inlet tubing. 

11.4.2.3 When the inlet tubing is full with eluant, stop the pump 

and reconnect the tubing to the bottom of the column. 

11.5 Eluant collection schedule 

11.5.1 Table 2 provides a schedule of fraction end-point LS ratios, interval 

LS ratios, and eluate fraction volumes for collection, assuming a 

dry-mass equivalent of 300 g-dry. The minimum volume of each collection bottle should 

be sized so as to capture the entire eluate fraction. 

11.5.2 Using the assumed pump rate and the dry-mass equivalent of the 

sample, calculate the durations of column testing required to reach the target eluate 

collection LS ratios shown in Table 2 as follows: 
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December 2009 

Where: Ti = target time from start for collection of eluant fraction i (day) 

Mdry = dry-mass equivalent of sample in column (g-dry) 

= target cumulative LS ratio for interval i from Table 1 (mL/g-dry) 

Ri = pump rate assumed for interval i (mL/day) 

 Alternatively, use the provided Microsoft® Excel spreadsheet template to 

develop the schedule of target collection times. 

UNOTEU: The schedule of predicted collection times is for reference purposes only. 

Typically, the eluate collection rate is slower that predicted initially, due in part to 

pump inefficiencies, back pressure and dead-volume lag times. The decision to 

switch collection bottles should be made based on the volume of eluate 

collected with time. The schedule may be revised with each eluate fraction 

collected, so that the prediction of future collections may be more accurate. 

Pump flow-rate adjustment may be necessary. 

12.0 COLUMN TEST PROCEDURE 

 12.1 Column/eluant equilibration 

 12.1.1 Turn on the pump and allow the column to fill with eluant, thus 

wetting the column packing. 

 12.1.2 When the column packing is completely wetted and the eluant level 

is even with the top of the column (or just beginning to be seen through the effluent 

tubing at the top of the column apparatus), stop the pump and allow the column to 

equilibrate for 24 hours. 

 12.2 Column test 

 12.2.1 Following equilibration, begin the column test by starting the pump 

and recording the date and time. 

UNOTEU: The eluate production rate should be monitored frequently during the column 

test and the pump rate adjusted, such that the eluate production rate is 

maintained at approximately 0.75 ± 0.25 LS/day. 

 12.2.2 When the eluate fraction has reached the target volume according 

to the predicted collection schedule, release the Luer lock connecting the active 

collection bottle and attach the eluant tubing to a new collection bottle. 

 12.3. Eluate processing 

 12.3.1 Decant a minimum volume (~ 5 mL) of the eluate fraction from the 

collection vessel in order to measure the solution characteristics. 
1314 - 13 Revision 1 

December 2009 

 12.3.2 Measure and record the pH, specific conductivity, and oxidationreduction potential (ORP) (optional, but strongly recommended) of the eluate (see 

Methods 9040, 9045, and 9050). 

 12.3.3 Separate any suspended particulates from the remaining liquid in 

the collection bottle by pressure or vacuum filtration through a 0.45-μm filtration 

membrane (Sec.6.8). 

UNOTEU: If either low-volatility organic species or mercury is a COPC, pressure filtration is 

recommended over vacuum filtration in order to minimize volatility losses. 

 12.3.4 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. 

 12.4 Reiterate Secs. 12.2.2-12.3.4 until nine eluate fractions are collected up to an 

LS ratio of 10 ± 0.2 mL/g-dry. 

UNOTEU: In order to complete this method, all nine eluate fractions must be collected from 

the column. However, for purposes of limited analysis or index testing with 

interpretation based on cumulative release, fractions may be composited by 

volume-weighted averaging to create a single analytical sample from multiple 

eluate fractions. 

 12.5. Analytical sample preparation options 

 This method allows for options in the preparation of analytical samples based on the 

detail of characterization required (e.g., complete, limited or index) and the basis for data 

reporting (e.g., concentration or cumulative release). However, the complete set of nine eluate 

fractions must be collected in all cases. 

 12.5.1 Table 1 shows the analytical preparation scheme for Options A-E 

described in the following sections. Each composite sample may be created either by 

combining the total eluate volumes and preserving the total sample for analysis; or 

combining aliquots of two eluate fractions using volume-weighted averages. However, it 

is recommended that composite analytical samples be prepared using aliquots of eluate 

fractions whenever possible, rather than whole eluate fractions as this approach allows 

for potential analysis of discrete eluate fractions if desired at a later date. 

 12.5.1.1 UOption AU — This sample preparation option is used for complete 

characterization and includes analysis of all eluate fractions. Since the entire cumulative 

release curve is captured in nine discrete fractions, reported data may be based on 

either eluate concentrations or cumulative release. 

 12.5.1.2 UOption BU — This sample preparation option is used only for limited 

analyses based on eluate concentration. Six discrete eluate fractions are analyzed. 

Data obtained using this option cannot be used for cumulative release since there 

are sections of the cumulative release curve not analyzed. 
1314 - 14 Revision 1 

December 2009 

 12.5.1.3 UOption CU — This sample preparation option is used only for limited 

analysis based on cumulative release. Six analytical samples are created from 

three discrete eluate fractions and three composite samples. In the scheme shown 

in Table 1, the following fractions are composited: 

• T04 and T05 

• T06 and T07 

• T08 and T09 

 12.5.1.4 UOption DU — This sample preparation option is used only for index 

testing based on eluate concentration. Three discrete eluate fractions are analyzed. 

Data obtained using this option cannot be used for cumulative release since there are 

sections of the cumulative release curve not analyzed. 

 12.5.1.5 UOption EU — This sample preparation option is used only for index 

testing based on cumulative release. Three analytical samples are created from 

one discrete eluate fraction and two composite samples. In the scheme shown in 

Table 1, the following fractions are composited: 

• T02, T03, T04, and T05 

• T06, T07, T08, and T09 

 12.5.2 Volume-weighted composites 

 12.5.2.1 The volume of aliquots of eluate fractions for composite analytical 

samples may be calculated using the Excel template provided or the following 

formula: 

 Where: Vi = the volume of an aliquot from eluate fraction i (mL) 

Fi = the collected volume of eluate fraction i (mL) 

Vsample = the total volume of the analytical sample (mL) 

n = total number of eluate fractions to be composited 

 As an illustration of volume-weighted averaging, eluate fraction aliquots are 

calculated as required to create an analytical sample by compositing eluate fractions 

T06 through T09 for index testing based on cumulative release. The calculation 

follows the example volumes shown in Table 2 and assumes that an analytical 

sample volume of 100 mL is required. 
1314 - 15 Revision 1 

December 2009 

UNOTEU: The above illustration uses example eluate fraction volumes based on 

interval LS ratios and an assumed test material mass. When calculating the 

aliquots of collected eluates fractions for composite samples, the actual collected 

fraction volumes should be used. 

13.0 DATA ANALYSIS AND CALCULATIONS (EXCEL TEMPLATE PROVIDED) 

 13.1 Data reporting 

 Figure 3 presents an example of a data sheet that may be used to report the 

concentration results of this method. This example is included in the Excel template. At 

a minimum, the basic test report should include the following: 

 a) Name of the laboratory 

 b) Laboratory contact information 

 c) Date and time at the start of eluate flow (start of test) 

 d) Name or code of the solid material tested 

 e) Particle size (85 wt% less than) 

 f) Packed bed dimensions (column ID and bed depth (cm)) 

 g) Mass of solid material in column packing 

 h) Moisture content of solid material packed in column (gH O2 /g) 

 i) Eluate specific information (see below) 

 The minimum set of data that should be reported for each eluate includes: 

 a) Eluate sample ID 

 b) Eluate collection date and time 

 c) Amount of eluate collected (mass or volume) 

 d) Measured eluate pH 
1314 - 16 Revision 1 

December 2009 

 e) Measured eluate conductivity (mS/cm) 

 f) Measured ORP (mV) (optional) 

 g) Concentration of all COPCs 

 h) Analytical QC qualifiers as appropriate 

13.2 Data Interpretation (optional) 

 13.2.1 Concentration as a function of LS ratio 

 13.2.1.1 A curve of the eluate concentration as a function of LS ratio can be 

generated for each COPC after chemical analysis of all extracts by plotting the 

constituent concentration in the liquid phase as a function of the cumulative collected LS 

ratio. The curve indicates the nominal equilibrium concentration of the constituent of 

interest as a function of LS ratio from 0 to 10 mL/g-dry at natural pH. An example such 

curve is provided in Figure 4. 

 13.2.1.2 The lower limit of quantitation (LLOQ) of the determinative method 

for each COPC may be shown as a horizontal line. COPC concentrations below this line 

indicate negligible or non-quantitative concentrations. 

UNOTEU: The lower limit of quantitation is highly matrix dependent and should be 

determined as part of a QA/QC plan. 

 13.3 Cumulative release as a function of LS ratio 

 13.4.1 The cumulative mass release of a COPC per unit solid material may 

be calculated as follows: 

ΣMi = Σ[Ci (ΣLSi – ΣLSi–1)]

 Where: ΣMi = the cumulative mass release through interval i (mg/kg-dry]) 

Ci = the concentration of the COPC in the eluant collected during 

 interval i (mg/L) 

ΣLSi = the cumulative LS ratio of eluate collected through 

 interval i (L/kg-dry) 

ΣLSi-1 = the cumulative LS ratio of eluate collected through 

 interval i-1 (L/kg-dry) 

i 

 13.4.2 Prepare a curve of the cumulative mass release generated for each 

COPC by plotting the cumulative mass release calculated in Sec. 13.4.1 as a function of 

the cumulative collected LS ratio. This curve provides an interpretation of the cumulative 

mass expected to be leached from a column of material as a function of LS ratio 

percolating through the column. 

 13.4.3 A comparison of the slope of the mass release curve to a unity 

slope, which is indicative of solubility-controlled release, may be made by plotting the 

cumulative mass release calculated in Sec. 13.4.1 versus the logarithm of the 

cumulative collected LS ratio. An example is provided in Figure 5. 
1314 - 17 Revision 1 

December 2009 

14.0 METHOD PERFORMANCE 

 14.1 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. UThese performance data are not intended to be and must not be used as 

absolute QC acceptance criteria for purposes of laboratory accreditation U. 

 14.2 Refs. 3 and 4 may provide additional guidance and insight on the use, 

performance and application of this method. 

15.0 POLLUTION PREVENTION 

 15.1 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. 

 15.2 For information about pollution prevention that may be applicable to 

laboratories and research institutions consult Less is Better: Laboratory Chemical Management 

for Waste Reduction available from the American Chemical Society's Department of 

Government Relations and Science Policy, 1155 16th St., N.W. Washington, D.C. 20036, 

http://www.acs.org. 

16.0 WASTE MANAGEMENT 

 The Environmental Protection Agency requires that laboratory waste management 

practices be conducted consistent with all applicable rules and regulations. The Agency urges 

laboratories to protect the 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 1314 - 18 Rev 0 January 2009 Pre-release DRAFT for comment waste 

identification rules and land disposal restrictions. For further information on waste 

management, consult The Waste Management Manual for Laboratory Personnel available from 

the American Chemical Society at the address listed in Sec. 15.2. 

17.0 REFERENCES 

1. NEN 7343, (1995), “Leaching Characteristics of Solid Earth and Stony 

Materials – Leaching Tests – Determination of the leaching of Inorganic Constituents 

from Powdery and Granular Materials with the Percolation Test,” Dutch Standardization 

Institute, Delft, The Netherlands. 
1314 - 18 Revision 1 

December 2009 

2. CEN TS/14405, (2004), “Characterization of Waste – Leaching Behaviour Tests – Upflow Percolation Test (Under Specified Conditions),” European Committee for 

Standardization (CEN), Brussels, Belgium. 

3. D.S. Kosson, H.A. van der Sloot, F. Sanchez and A.C. Garrabrants, (2002), “An 

Integrated Framework for Evaluating Leaching in Waste Management and Utilization of 

Secondary Materials,” Environmental Engineering Science, 19(3) 159-204. 

4. D.S. Kosson, A.C. Garrabrants, H.A. van der Sloot, (2009), “Background Information for 

the Development of Leaching Test Draft Methods 1313 through Method 1316,” (in 

preparation). 

18.0 TABLES, DIAGRAMS, FLOW CHARTS, AND VALIDATION DATA 

The following pages contain the tables and figures referenced by this method. 
1314 - 19 Revision 1 

December 2009 

TABLE 1 

SCHEDULE OF FRACTION COLLECTIONS AND ANALYTICAL SAMPLES 

Option A B C D E

Characterization Limited Analysis Index Testing Fraction ΣLS Ratio 

Label (mL/g-dry) Conc. ΣRel Conc. ΣRel Conc. ΣRel

T01 0.2 ± 0.1      

T02 0.5 ± 0.1     ↓

T03 1.0 ± 0.1     ↓

↓ T04 1.5 ± 0.2   ↓ T05c

T05 T05c 2.0 ± 0.2    

T06 4.5 ± 0.2   ↓ ↓

T07 T07c 5.0 ± 0.2    ↓

↓ T08 9.5 ± 0.2   ↓ T09c

T09 T09c 10.0 ± 0.2    

UNOTEU: ΣRel = Cumulative release. 

 = Collect eluate fraction (or pool of fractions) as analytical sample. 

↓ = composite eluate fraction with next fraction to create analytical sample. 

TABLE 2 

SCHEDULE OF ELUATE FRACTIONS FOR COLLECTION 

WITH EXAMPLE VOLUMES 

Interval End Point Fraction Example

Label ΣLS Ratio ΣLS Ratio Fraction

Volume

(mL/g-dry) (mL/g-dry) (mL)

T01 0.2 ± 0.1 0.2 60

T02 0.5 ± 0.1 0.3 90

T03 1.0 ± 0.1 0.5 150

T04 1.5 ± 0.2 0.5 150

T05 2.0 ± 0.2 0.5 150

T06 4.5 ± 0.2 1.5 450

T07 5.0 ± 0.2 0.5 150

T08 9.5 ± 0.2 4.5 1350

T09 10.0 ± 0.2 0.5 150

B01 Eluant 100

UNOTEU: Example fraction volumes based on assumed packing mass of 300 g-dry.
1314 - 20 Revision 1 

December 2009 

FIGURE 1 

EXAMPLE DATA REPORT FORMAT 

EPA METHOD 1314

ABC Laboratories Report of Analysis

123 Main Street

Anytown, USA

 Contact: John Smith

 (555) 111-1111

Client Contact: Susan Jones

 (555) 222-2222

Material Code: XYZ Particle Size: 88% passing 2-mm sieve

Material Type: Coal Combustion Fly Ash Mass used in Column: 360 g

Date Received: 10/1/20xx Moisture Content: 0.002 gH2O/g

Test Date: 11/1/20xx Column ID: 4.8 cm

Report Date: 12/1/20xx Packing Bed Depth: 28 cm

Eluant: ASTM Type II Water

Lab Temperature: 21 ± 2 °C

Test

Position Replicate Value Units Method Note

T01 A

Eluate Sample ID XYZ-1314-T01-A

Collection Date 11/1/20xx

Collection Time 12:35 PM

Eluate Mass 70.4 g

Eluate pH 8.82 - EPA 9040

Eluate Conductivity 5.4 mS/c

m 

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

Cl 5.42 mg/L EPA 9056 11/9/20xx 1

Test

Position Replicate Value Units Method Note

T02 A

Eluate Sample ID XYZ-1314-T02-A

Collection Date 11/1/20xx

Collection Time 9:15 AM

Eluate Mass 105.1 g

Eluate pH 9.15 -

Eluate Conductivity 2.3 mS/c

Eluate ORP NA mvm 

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

Cl 4.20 mg/L U EPA 9056 11/7/20xx 1

QC Flag Key: U Value below lower limit of quantitation as reported (< "LLOQ")
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December 2009 

FIGURE 2 

METHOD 1314 FLOWCHART 
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December 2009 

FIGURE 3 

SCHEMATIC OF COLUMN TEST APPARATUS 

UNOTEU: Figure not drawn to scale 
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December 2009 

FIGURE 4 

EXAMPLE ELUATE CONCENTRATION CURVES FOR COMPLETE CHARACTERIZATION 

OF A COAL COMBUSTION FLY ASH 
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December 2009 

FIGURE 5 

EXAMPLE CUMULATIVE RELEASE CURVES FOR COMPLETE CHARACTERIZATION OF A 

COAL COMBUSTION FLY ASH 

UNOTEU: Dashed line represents solubility control (slope = 1). 
APPENDIX C 

METHOD 1315 – 

U MASS TRANSFER RATES OF CONSTITIUENTS IN MONOLITHIC 

OR COMPACTED GRANULAR MATERIALS USING 

A SEMI-DYNAMIC TANK LEACHING PROCEDURE 
1315 - 1 Revision 1 

December 2009 

PRELIMINARY VERSION1 OF METHOD 1315 

MASS TRANSFER RATES OF CONSTITIUENTS 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 method use for the analysis 

of method-defined parameters, are intended to be guidance methods which 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. The performance data 

included in this method are for guidance purposes only, and are not intended to be and must not 

be used as absolute quality control (QC) acceptance criteria for purposes of laboratory 

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 diffusioncontrolled 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, 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. 

 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 eluants which may be used to estimate 

the diffusivity of constituents and physical retention parameter of the solid material under 

specified laboratory conditions. 

 1.4 This method is not applicable to characterize the release of volatile or semivolatile organic analytes. 

 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. 

 

1 Preliminary Version denotes that this method has not been endorsed by EPA but is under consideration 

for inclusion into SW-846. This method has been derived from published procedures (Kosson et al, 

2002). The method has been submitted to the U.S. EPAU.S. EPA Office of Resource Conservation and 

Recovery and is currently under review for development of interlaboratory validation studies to develop 

precision and bias information. 
1315 - 2 Revision 1 

December 2009 

2), ANSI/ANS 16.1 (see Ref. 3), and ASTM C1308 (see Ref. 4). However, this method differs 

from previous methods in that: (a) leaching intervals are modified to improve quality control, (b) 

sample preparation accounts for mass transfer from compacted granular samples, and (c) mass 

transfer may be interpreted by more complex release models that account for physical retention 

of the porous medium and chemical retention at the pore wall through geochemical speciation 

modeling 

 1.7 The geometry of monolithic samples may be rectangular (e.g., bricks, tiles), 

cubes, wafers, cylinders. Samples may also have a variety of faces exposed to eluant 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 (LSa) ratio 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 eluant and the bulk of the eluant (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. 

 1.8 Compacted granular materials are granular solids, screened to pass 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 LSa ratio 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 eluant volume is on top of the 

sample. Figure 2 shows an example of a holder and leaching configuration for a compacted 

granular sample. 

 1.9 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 eluant and the solid matrix may result in precipitation and pore blocking, which may interfere 

with characterization or complicate data interpretation. 

 1.10 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) 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 guidance on the 

intended flexibility in the choice of methods, apparatus, materials, reagents, and supplies, and 

on 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 
1315 - 3 Revision 1 

December 2009 

requirements. The information contained in this method is provided by EPA 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. 

 1.11 Use of 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 eluant-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 eluant is recommended. Samples are contacted with reagent water at a specified 

LSa ratio. 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 eluant 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 

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 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 LSa ratio — The ratio representing the total liquid volume used in the leaching 

interval to the external geometric surface area of the solid material. LSa ratio 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. 
1315 - 4 Revision 1 

December 2009 

 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). 

 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 Refer to the SW-846 chapter of terms and acronyms for potentially applicable 

definitions. 

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 allglass 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 the cleaning of 

laboratory apparatus prior to use. 

 4.2 The reaction of atmospheric gases can influence the measured concentrations 

of constituents in eluates. For example, reaction of carbon dioxide with eluants 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 air-tight 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 

 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 OSHA 

regulations regarding the safe handling of the chemicals listed in this method. A reference file 

of material safety data sheets (MSDSs) should be available to all personnel involved in these 

analyses. 
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December 2009 

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 setting used during the method development or subsequently evaluated by the Agency. 

Glassware, reagents, supplies, equipment, and setting 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). 

 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 pHs is recommended. 

 6.1.1.2 The holder should be designed such that at least 98% 

of the sample external surface area may be exposed to eluant. 

 6.1.1.3 The holder should be designed to match the geometry 

of the mass transfer such that the bulk of the eluant 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 eluant 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 11.3.5) 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 eluant 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. 
1315 - 6 Revision 1 

December 2009 

 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 air-tight 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 eluant volume based on an LSa ratio of 9 ± 1 mL eluant/cm2

sample surface area. Ideally, the vessel should be sized such that the headspace is 

minimized within the tolerance of the LSa ratio. 

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 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. 
1315 - 7 Revision 1 

December 2009 

 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 

6.4 Filtration apparatus — Pressure- or vacuum-filtering apparatus made 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 PP or similar material with an 

effective pore size of 0.45-μm (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 must be used in all tests. Unless otherwise 

indicated, it is intended that all reagents conform to the specifications of the Committee on 

Analytical Reagents of the American Chemical Society, where such specification are available. 

Other grade may be used, provided it is first ascertained that the reagent is of sufficiently high 

purity to permit its use without lessening the accuracy of the determination. 

 7.2 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 the introductory material to Chapter Three "Inorganic Analytes." 

 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. 
1315 - 8 Revision 1 

December 2009 

9.0 QUALITY CONTROL 

 9.1 Refer to Chapter One for guidance on quality assurance (QA) and QC 

protocols. When inconsistencies exist between QC guidelines, method-specific QC criteria take 

precedence over both technique-specific criteria and those criteria given in Chapter One, and 

technique-specific QC criteria take precedence over the criteria in Chapter One. 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 that will implement the project and assess the results. Each laboratory should 

maintain a formal quality assurance program. The laboratory should also maintain records to 

document the quality of the data generated. All data sheets and quality control data should be 

maintained for reference or inspection. 

 9.2 Method blanks – In order to demonstrate the purity of reagents and container 

surfaces, a method blank 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 quality control 

procedures. 

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 PREPARATORY PROCEDURES 

 A flowchart of this method, including preparatory and leaching procedures, is shown in 

Figure 3. 

 11.1 Determination of solids and moisture content 

 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. 
1315 - 9 Revision 1 

December 2009 

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 a 5–10-g sample of solid material into a clean, pre-weighed 

dish or crucible. Dry the sample to a constant mass at 105 ± 2 °C. Periodically check 

the sample mass after allowing the sample to cool to room temperature (20 ± 2 °C) in a 

desiccator. 

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: 

 Where: SC = solids content (g-dry/g) 

Mdry = mass of oven-dried sample (g-dry) 

Mtest = mass of "as-tested" sample (g) 

11.1.3 Calculate and report the moisture content (wet basis) as follows: 

Where: MC(wet) = moisture content on a wet basis (gH2O/g) 

Mdry = mass of oven-dried sample (g-dry) 

Mtest = mass of "as-tested" sample (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. 
1315 - 10 Revision 1 

December 2009 

 11.2.3 The geometry of monolithic samples may be rectangular (e.g., 

bricks, tiles), cubes, wafers, cylinders. Samples may also have a variety of faces 

exposed to eluant forming 1-, 2-, or 3-D mass-transfer cases. Example monolithic 

sample leaching setups are shown in Figure 1. 

 11.2.4 A minimum sample size of 5 cm in the direction of mass transfer 

must be employed and the LSa ratio 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. 12.0. 

 11.3 Preparation of compacted granular samples 

 Compacted granular materials, for 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 LSa ratio 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 compacted 

in three layers (rather than the five layers specified in Ref. 5) to maintain the total compaction 

effort. The granular sample should be compacted at optimum moisture content in order to 

obtain packing densities that approximate field conditions. Optimum moisture content refers to 

the amount of moisture or fractional mass of water (gH O2 /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 

pretest measuring 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 thirdorder polynomial fit through the graph of dry-packing density as a function of moisture 

content (wet basis). 

 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 alternate to hand mixing, a 

mechanical paddle mixer may used. 

NOTE: The pretest 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. 
1315 - 11 Revision 1 

December 2009 

 1.3.1.2 Mix a known amount of tap water with the bulk materi

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 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 moisture content curve. 

 11.3.1.3 Calculate the new moisture content for the trial as 

follows: 

al 

Where: = moisture content (wet basis) of the pre-test trial (gH2O/g) 

Mtest = mass of "as-tested" material used in the trial (g) 

MC(wet) = moisture content (wet basis) of the "as-tested" 

 material (gH2O/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 pretared 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: 

Where: ρpack = packing density (dry basis) (g-dry/cm3) 

m = mass of the compacted sample (g) 

SC = solids content of the "as -received" granular material (gdry/g) 

d = measured diameter of the compacted sample (cm) 

h = measured height of the compacted sample (cm) 

 11.3.1.7 Repeat Secs. 11.3.1.1-11.3.1.6 for four subsequent 

trials until the value of the calculated packing density decreases. 
1315 - 12 Revision 1 

December 2009 

 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 provided 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" sample (g) 

ρopt = optimal packing density (dry basis) (g-dry/cm3

) 

 determined in Sec. 11.3.1.9. 

SC = solids content of the "as received" granular material (g-dry/g) 

d = measured diameter of the sample mold (cm) 

h = measured height 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 mono-layer 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. 

12.0 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 eluant 

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. 
1315 - 13 Revision 1 

December 2009 

12.1 Pre-test measurements 

 12.1.1 For the surface area calculation, measure and record the 

dimensions of the test specimen (i.e., diameter and height for a cylinder; length, 

width and depth for a parallelepiped; or diameter of exposed surface for a 

compacted granular sample). 

 12.1.2 Measure and record the mass of the specimen. This value should 

be monitored for each eluant exchange. 

 12.1.3 If a holder is used, place the specimen in the monolith holder. 

 12.1.4 Measure and record the mass of the specimen and holder, if 

applicable. 

 12.1.5 The recommended temperature for conducting this method is room 

temperature (20 ± 2 °C). When conducted at temperatures readings or variations other 

than those recommended, record the ambient temperature at each eluant renewal. 

12.2 Eluant exchange 

 12.2.1 Fill a clean leaching vessel with the required volume of reagent 

water based on an LSa ratio of 9 ± 1 mL/cm2

. Record the amount of eluant used. 

 12.2.2 Carefully place the specimen or the specimen and holder in the 

leaching vessel (Figure 6a) so that the sample is centered in the eluant (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. 

 12.2.3 Cover the leaching vessel with the air-tight 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. 

 12.2.4 Prior to the end of the leaching interval, repeat Sec. 12.2.1 in order 

to prepare a vessel for the next leaching interval. 

 12.2.5 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. 

 12.2.6 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 eluant 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 intervals and sample absorption may not be evident. 

CAUTION: Mass gain may also be indicative of carbonate precipitation if the vessel is 

not tightly sealed and carbon dioxide is absorbed from the atmosphere. 
1315 - 14 Revision 1 

December 2009 

 12.2.7 Place the specimen or the specimen and holder into the clean 

leaching vessel filled with new eluant as prepared in Sec. 12.2.4. 

 12.2.8 Cover the new leaching vessel with the air-tight lid and place in a 

safe location until the end of the leaching interval. 

 12.3 Eluate processing 

 12.3.1 Measure and record the pH, specific conductivity, and oxidationreduction potential (ORP) (optional, but strongly recommended) of the eluate of the 

decanted eluate from the previous leaching interval (see Methods 9040, 9045, and 

9050). 

 12.3.2 Filter the remaining eluate through a 0.45-μm membrane (Sec. 6.5). 

 12.3.3 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. 

 12.3.4 Collect all subsequent eluate by repeating the eluant exchange and 

eluate processing procedures in Secs. 12.2 and 12.3. 

13.0 DATA ANALYSIS AND CALCULATIONS 

 13.1 Data reporting 

 Figure 7 shows an example of a data sheet which may be used to report the 

concentrations results of this method. This example is included in the Excel template. At a 

minimum, the basic test report should include the following: 

 a) Name of the laboratory 

 b) Laboratory 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 (gH O2 /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 below) 

 The minimum set of data that should be reported for each eluate includes: 

 a) Eluate sample ID 

 b) Target eluant exchange date and time 

 c) Actual eluant exchange date and time 

 d) Volume of eluant used (mL) 

 e) Mass of sample and holder (g) 

 f) Measured eluate pH 
1315 - 15 Revision 1 

December 2009 

g) Measured eluate conductivity (mS/cm) 

h) Measured ORP (mV) (optional) 

i) Concentration of all COPCs 

j) Analytical QC qualifiers as appropriate 

13.2 Data presentation 

 13.2.1 Interval concentrations 

 13.2.1.1 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. 

 13.2.1.2 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 if 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. 

 13.2.2 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: 

Where: = 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 eluant (m2

) 

 13.2.3 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 ( ). 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). 
1315 - 16 Revision 1 

December 2009 

 13.2.3.1 The flux across the exposed surface of the sample can 

be calculated by dividing the interval mass release by the interval duration as 

follows: 

Where Fi = flux for interval, i (mg/m2·s) 

Mi= mass released during the current leaching interval i (mg/m2) 

ti = cumulative time at the end of the current leaching interval i (s) 

ti-1 = cumulative time at the end of the previous leaching 

 interval i-1 (s) 

 13.2.3.2 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, ti, and the cumulative time at the 

end of the previous interval, ti-1. 

Where : = generalized mean leaching time for the current interval, i (s) 

t i = cumulative time at the end of the current leaching interval, i (s) 

t i-1 = 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. 

 13.2.4 Cumulative release 

 13.2.4.1 The interval release calculated in 13.2.2 can be 

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. 

 13.2.4.2 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). 
1315 - 17 Revision 1 

December 2009 

Where: Mt = cumulative mass released during leaching interval, i (mg/m2) 

ρ = density of the "as-tested" sample (kg/m3

) 

Co = 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 becomes linear with the square root of time. 

 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. 

 Other models 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). 

 13.2.5 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 diffusioncontrolled 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 

0.5 ± 0.15 (see Refs. 10 and 11) by the following: 
1315 - 18 Revision 1 

December 2009 

Where: = observed diffusivity of a COPC for leaching 

 interval, i (m2

/s) 

= mass released during leaching interval, i (mg/m2) 

ti = cumulative contact time after leaching interval, i (s) 

ti-1 = cumulative contact time after leaching interval, i - 1 (s) 

Co = initial leachable content (i.e., available release 

 potential) (mg/kg) 

ρ = sample density (kg-dry/m3

) 

 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. 

 13.3 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 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). 

14.0 METHOD PERFORMANCE 

 14.1 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. These performance data are not intended to be and must not be used as 

absolute QC acceptance criteria for purposes of laboratory accreditation. 

 14.2 Refs. 1 and 7 may provide additional guidance and insight on the use, 

performance and application of this method. 

15.0 POLLUTION PREVENTION 

 15.1 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 
1315 - 19 Revision 1 

December 2009 

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. 

 15.2 For information about pollution prevention that may be applicable to 

laboratories and research institutions consult Less is Better: Laboratory Chemical Management 

for Waste Reduction available from the American Chemical Society's Department of 

Government Relations and Science Policy, 1155 16th St., N.W. Washington, D.C. 20036, 

http://www.acs.org. 

16.0 WASTE MANAGEMENT 

 The Environmental Protection Agency requires that laboratory waste management 

practices be conducted consistent with all applicable rules and regulations. The Agency urges 

laboratories to protect the 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 American Chemical Society at the address listed in Sec. 15.2. 

REFERENCES 

1. D.S. Kosson, H.A. van der Sloot, F. Sanchez and A.C. Garrabrants (2002) "An 

Integrated Framework for Evaluating Leaching in Waste Management and Utilization of 

Secondary Materials," Environmental Engineering Science, 19(3) 159-204. 

2. NEN 7345 (1995) "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. 

3. ANSI/ANS 16.1 (1986) "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. 

4. ASTM D1308-95 (2001) "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. 

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 (1991) "Long-term Processes in a Stabilized CoalWaste Block Exposed to Seawater," Environmental Science and Technology, 25(8), 

1408-1414. 
1315 - 20 Revision 1 

December 2009 

7. D.S. Kosson, A.C. Garrabrants, H.A. van der Sloot (2009) "Background Information for 

the Development of Leaching Test," Draft Methods 1313 through Method 1316, (in 

preparation). 

8. Crank (1986) Mathematics of Diffusion, Oxford University Press, London. 

9. Hinsenveld, and P.L. Bishop (1996) "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. 

10. Sanchez (1996) "Étude de la lixiviation de milieux poreux contenant des espèces 

solubles: Application au cas des déchets solidifiés par liants hydrauliques," doctoral 

thesis, Institut National des Sciences Appliquées de Lyon, Lyon, France. 

11. IAWG (1997) Municipal Solid Waste Incinerator Residues, International Ash Working 

Group, Elsevier Science Publishers, Amsterdam, the Netherlands. 

12. J. de Groot, and H. A. van der Sloot (1992) "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. 

13. A.C. Garrabrants and D.S. Kosson (2005) "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. 

18.0 

TABLES, DIAGRAMS, FLOW CHARTS, AND VALIDATION DATA 

 The following pages contain the tables and figures referenced by this method 
1315 - 21 Revision 1 

December 2009 

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 

intervals to provide 

release. 

be extended for additional 14-day contact 

more information regarding longer-term 
1315 - 22 Revision 1 

December 2009 

FIGURE 1 

EXAMPLES OF MONOLITHIC SAMPLE HOLDERS 

a)

b)
1315 - 23 Revision 1 

December 2009 

FIGURE 2 

EXAMPLE COMPACTED GRANULAR SAMPLE HOLDER AND SETUP 
1315 - 24 Revision 1 

December 2009 

FIGURE 3 

METHOD 1315 FLOWCHART 
1315 - 25 Revision 1 

December 2009 

FIGURE 4 

EXAMPLE CURVE OF PACKING DENSITY AS A FUNCTION OF MOISTURE CONTENT 

y = 55.975x3

 – 65.036x2 + 1.8352 

r

2

 = 0.983 
1315 - 26 Revision 1 

December 2009 

 

FIGURE 5 

SCHEMATIC OF SEMI-DYNAMIC MASS TRANSFER TEST PROCESS 

Figure obtained and modified from Ref. 11. 
1315 - 27 Revision 1 

December 2009 

FIGURE 6 

EXAMPLE LEACHING PROCEDURE STEPS 
1315 - 28 Revision 1 

December 2009 

FIGURE 7 

EXAMPLE DATA REPORTING SHEET 

EPA METHOD 1315

ABC Laboratories Report of Analysis

123 Main Street

Anytown, USA

 Contact: John Smith

 (555) 111-1111

Client Contact: Susan Jones

 (555) 222-2222

Material Code: XYZ 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 Start 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

Eluant: 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 11/1/20xx

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

m 

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

Cl 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 11/1/20xx

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

m 

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

Cl 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 - 29 Revision 1 

December 2009 

FIGURE 8 

EXAMPLE INTERVAL CONCENTRATION GRAPHS 

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 - 30 Revision 1 

December 2009 

FIGURE 9 

EXAMPLE OF SATURATION CHECK BETWEEN INTERVAL CONCENTRATIONS 

AND METHOD 1313 DATA 

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 - 31 Revision 1 

December 2009 

FIGURE 10

EXAMPLE INTERVAL FLUX GRAPHS 

NOTE: Orange data represent cumulative release if all eluate extracts were at the quantitation limit 

(dashes) and detection limit (solid line). 
1315 - 32 Revision 1 

December 2009 

FIGURE 11 

INTERVAL FLUX AT ELUATE SATURATION 

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 - 33 Revision 1 

December 2009 

FIGURE 12 

EXAMPLE CUMULATIVE RELEASE GRAPHS 

NOTE: Orange data represent cumulative release if all eluate extracts were at the quantitation limit 

(dashes) and detection limit (solid line). 
1315 - 34 Revision 1 

December 2009 

FIGURE 13 

DATA REPRESENTATION BY CONSTITUENT (QUAD FORMAT) 

NOTE: Orange data represent cumulative release if all eluate extracts were at the quantitation limit 

(dashes) and detection limit (solid line). 
APPENDIX D 

METHOD 1316 – 

LIQUID-SOLID PARTITIONING AS A FUNCTION OF 

LIQUID-TO-SOLID RATIO IN SOLID MATERIALS 

USING A PARALLEL BATCH PROCEDURE 
1316 - 1 Revision 1.1 

April 2010

PRELIMINARY VERSION1 OF METHOD 1316 

LIQUID-SOLID PARTITIONING AS A FUNCTION OF LIQUID-TO-SOLID RATIO IN SOLID 

MATERIALS USING A PARALLEL BATCH 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 method use for the analysis 

of method-defined parameters, are intended to be guidance methods which 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. The performance data 

included in this method are for guidance purposes only, and are not intended to be and must not 

be used as absolute QC acceptance criteria for purposes of laboratory accreditation. 

1.0 SCOPE AND APPLICATION 

 1.1 This method is designed to provide the liquid-solid partitioning (LSP) of 

inorganic constituents (e.g., metals, radionuclides) and non-volatile organic constituents (e.g., 

polycyclic aromatic hydrocarbons (PAHs), dissolved organic carbon) at the natural pH of the 

solid material as a function of liquid-to-solid ratio (L/S) under conditions that approach liquidsolid chemical equilibrium. Table 1 shows the range of target L/S values tested under this 

method. 

 1.2 The eluate concentrations at a low L/S provide insight into pore solution 

composition either in a granular bed (e.g., soil column) or in the pore space of low-permeability 

material (e.g., solidified monolithic or compacted granular fill). In addition, analysis of eluates 

for dissolved organic carbon and of the solid phase for total organic carbon allow for evaluation 

of the impact of organic carbon release and the influence of dissolved organic carbon on the 

LSP of inorganic constituents. 

 1.3 This method is intended to be used as part of environmental leaching 

assessment for the evaluation of disposal, beneficial use, treatment effectiveness and site 

remediation. 

 1.4 This method is suitable to a wide range of solid materials. Example solid 

materials include industrial wastes, soils, sludges, combustion residues, sediments, stabilized 

materials, construction materials, and mining wastes. 

 

1 Preliminary Version denotes that this method has not been endorsed by EPA but is under consideration 

for inclusion into SW-846. This method has been derived from published procedures (Kosson et al, 2002) 

using reviewed and accepted methodologies (USEPA 2006, 2008, 2009). The method has been 

submitted to the USEPA Office of Resource Conservation and Recovery and is currently under review for 

development of interlaboratory validation studies to develop precision and bias information. 
1316 - 2 Revision 1.1 

April 2010

 1.5 This method is a leaching characterization method used to provide intrinsic 

material parameters that control leaching of inorganic species under equilibrium conditions. 

This test method is intended as a means for obtaining an extract (i.e., the eluate) of a solid 

material which may be used to estimate the solubility and release of inorganic constituents 

under the laboratory conditions described in this method. Extract concentrations may be used 

in conjunction with information regarding environmental management scenarios to estimate 

anticipated leaching concentrations, release rate and extent for individual material constituents 

in the management scenarios evaluated. Extract concentrations may also be used along with 

geochemical speciation modeling to infer the mineral phases that control the LSP in the pore 

structure of the solid material. 

 1.6 This method is not applicable to characterize the release of volatile organic 

analytes. 

 1.7 This method provides solutions that are considered to be indicative of eluate 

under field conditions only where the field leaching pH and L/S is the same as the laboratory 

extract final conditions and the LSP is controlled by aqueous-phase saturation of the constituent 

of interest. 

 1.8 The solvent used in this method is reagent water 

 1.9 Analysts are advised to take reasonable measures to ensure that the sample is 

homogenized to the extent practical prior to employment of this method. Particle-size reduction 

may provide additional assurance of sample homogenization. Table 2 designates a minimum 

dry equivalent mass of sample to be added to each extraction vessel and the associated 

extraction contact time as a function maximum particle diameter. If the heterogeneity of the 

sample is suspected as the cause of unacceptable levels of precision in replicate test results or 

is considered significant based on professional judgment, the sample mass used in the test 

procedure may be increased to a greater minimum dry equivalent mass than shown in Table 1 

with the amount of extractant increased proportionately to maintain the designated L/S. 

 1.10 In the preparation of solid materials for use in this method, particle-size 

reduction of samples with large grain size is used to enhance the approach towards liquid-solid 

equilibrium under the designated contact time interval of the extract process. The extract 

contact time for samples reduced to a finer maximum particle size will be shorter. 

 1.11 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), quality control (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 guidance on the intended flexibility in the choice of methods, 

apparatus, materials, reagents, and supplies, and on 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 EPA 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. 
1316 - 3 Revision 1.1 

April 2010

 1.12 Use of 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 consists of five parallel extractions of a particle-size reduced solid material 

in reagent water over a range of L/S values from 0.5 to 10 mL eluant/g dry material (see Table 

1). In addition to the five test extractions, a method blank without solid sample is carried 

through the procedure in order to verify that analyte interferences are not introduced as a 

consequence of reagent impurities or equipment contamination (If multiple materials or replicate 

tests are carried out in parallel, only one set of method blanks is necessary). In total, six bottles 

(i.e., five test positions and one method blank) are tumbled in an end-over-end fashion for a 

specified contact time based on the maximum particle size of the solid (see Table 2). At the end 

of the contact interval, the liquid and solid phases are roughly separated via settling or 

centrifugation. Extract pH and specific conductance measurements are then taken on an 

aliquot of the liquid phase. The bulk of the eluate is clarified by pressure or vacuum filtration in 

preparation for constituent analysis. Analytical aliquots of the extracts are collected and 

preserved accordingly based on the determinative methods to be performed. The eluate 

constituent concentrations are plotted as a function of L/S and compared to QC and 

assessment limits. 

3.0 DEFINITIONS 

 3.1 Release — The dissolution or partitioning of a constituent of potential concern 

(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. 

 3.2 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. 

 3.3 LSP — The distribution of COPCs between the solid and liquid phases at the 

conclusion of the extraction. 

 3.4 L/S — the fraction of the total liquid volume (including the moisture contained in 

the “as used” solid sample) to the dry mass equivalent of the solid material. L/S is typically 

expressed in volume units of liquid per dry mass of solid material (mL/g-dry). 

 3.5 “As-tested” sample — The solid sample at the conditions (e.g., moisture content 

and particle-size distribution) present at the time of the start of the test procedure. The “astested” conditions will differ from the "as-received" sample conditions if particle-size reduction 

and drying were necessarily performed. 

 3.6 Dry-mass equivalent — The mass of “as-tested” (i.e., “wet”) sample that 

equates to the mass of dry solids plus associated moisture, based on the moisture content of 

the “as-tested” material. The dry-mass equivalent is typically expressed in mass units of the 

“as-tested” sample (g). 
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April 2010

 3.7 Refer to the SW-846 chapter of terms and acronyms for potentially applicable 

definitions. 

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 allglass systems may be necessary. Refer to each method to be used for specific guidance on 

quality control procedures and to Chapters Three and Four for general guidance on the cleaning 

of laboratory apparatus prior to use. 

 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 OSHA regulations regarding the safe handling of the chemicals listed in this method. A 

reference file of material safety data sheets (MSDSs) should be available to all personnel 

involved in these analyses. 

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 setting used during the method development or subsequently evaluated by the Agency. 

Glassware, reagents, supplies, equipment, and setting 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). 

 6.1 Extraction vessels 

 6.1.1 Six wide-mouth bottles (i.e., five for test positions plus one for a 

method blank) constructed of an inert material resistant to high and low pH conditions or 

interaction with the constituents of interest. 

 6.1.1.1 For the evaluation of inorganic COPC mobility, bottles 

composed of high density polyethylene (HDPE) (e.g., Nalgene #3140-0250 or 

equivalent), polypropylene (PP), or polyvinyl chloride (PVC) are recommended. 

 6.1.1.2 For the evaluation of non-volatile organic and mixed 

organic/inorganic COPCs, equipment composed of glass or Type 316 stainless 

steel is recommended. PTFE is not recommended for non-volatile organics, 

due sorption of species with high hydrophobicity (e.g., PAHs). Borosilicate 
1316 - 5 Revision 1.1 

April 2010

glass is recommended over other types of glass, especially when inorganic 

analytes are of concern. 

 6.1.2. The extraction vessels must be of sufficient volume to 

accommodate both the solid sample and an extractant volume based on the schedule of 

L/S values shown in Table 1. For example, a 500-mL bottle is recommended when 100 

g dry equivalent mass is contacted with 200 mL of eluant (see T03 in Table 1). 

 6.1.3 The vessels must have a leak-proof seals that can sustain end-overend tumbling for the duration of the designated contact time. 

 6.1.4 If centrifugation is anticipated to be beneficial for initial phase 

separation, the extraction vessels should be capable of withstanding centrifugation at 

4000 ± 100 rpm for a minimum of 10 ± 2 min. Alternately, samples may be extracted in 

bottles that do not meet this centrifugation specification (e.g., Nalgene I-Chem #311-

0250 or equivalent) and the solid-liquid slurries transferred into appropriate 

centrifugation vessels for phase separation as needed. 

 6.2 Balance — Capable of 0.01-g resolution for masses less than 500 g. 

 6.3 Rotary tumbler — Capable of rotating the extraction vessels in an end-over-end 

fashion at a constant speed of 28 ± 2 rpm (e.g., Analytical Testing, Werrington, PA or 

equivalent). 

 6.4 Filtration apparatus — Pressure or vacuum filtration apparatus composed of 

appropriate materials so as to maximize the collection of extracts and minimize loss of the 

COPCs (e.g., Nalgene #300-4000 or equivalent) (see Sec. 6.1). 

 6.5 Filtration membranes — Composed of polypropylene or equivalent material with 

an effective pore size of 0.45-μm (e.g., Gelman Sciences GH Polypro #66548 from Fisher 

Scientific 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 Adjustable-volume pipettor — Oxford Benchmate series or equivalent The 

necessary delivery range will depend on the buffering capacity of the solid material and 

acid/base strength used in the test. 

 6.11 Disposable pipettor tips. 

 6.12 Centrifuge (recommended) — Capable of centrifuging the extraction vessels at 

a rate of 4000 ± 100 rpm for 10 ± 2 min. 
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April 2010

7.0 REAGENTS AND STANDARDS 

 7.1 Reagent-grade chemicals must be used in all tests. Unless otherwise 

indicated, it is intended that all reagents conform to the specifications of the Committee on 

Analytical Reagents of the American Chemical Society, where such specification are available. 

Other grades may be used, provided it is first ascertained that the reagents are of sufficiently 

high purity to permit 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 must be interference free. All references to water in this method 

refer to reagent water unless otherwise specified. 

 7.3 Consult Methods 9040 and 9050 for additional information regarding the 

preparation of reagents required for pH and specific conductance measurements. 

8.0 SAMPLE COLLECTION, PRESERVATION, AND STORAGE 

 8.1 See the introductory material to Chapter Three “Inorganic Analytes” and 

Chapter Four “Organic Analytes.” 

 8.2 All samples should be collected using an appropriate sampling plan. 

 8.3 All analytical sample containers should be composed of materials that minimize 

interaction with solution COPCs. For further information, see Chapters Three and Four. 

 8.4 Preservatives should not be added to samples before extraction. 

 8.5 Samples can be refrigerated, unless refrigeration results in an irreversible 

physical change to the sample. 

 8.6 Analytical samples should be preserved according to the guidance given in the 

individual determinative methods for the COPCs. 

 8.7 Extract holding times should be consistent with the aqueous sample holding 

times specified in the determinative methods for the COPCs. 

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 criteria take precedence over both technique-specific criteria and those criteria given in 

Chapter One, and technique-specific QC criteria take precedence over the criteria in Chapter 

One. 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 that will implement the project and assess the results. 

Each laboratory should maintain a formal quality assurance program. The laboratory should 
1316 - 7 Revision 1.1 

April 2010

also maintain records to document the quality of the data generated. All data sheets and quality 

control data should be maintained for reference or inspection. 

 9.2 In order to demonstrate the purity of reagents and sample contact surfaces, a 

method blank (e.g., a bottle without solid material but with eluant carried through the extraction, 

filtration and analytical sample preparation process) should be tested. 

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 quality control 

procedures. 

 9.4 Solid materials should be tested within one month of receipt unless the project 

requires that the "as-received" samples are tested sooner (e.g., the material is part of a timedependent study or the material may change during storage due to oxidation or carbonation). 

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 PREPARATORY PROCEDURES 

 A flowchart of the method is presented in Figure 1. 

 11.1 Particle-size reduction (if required) 

 11.1.1 In this method, particle-size reduction is used to prepare largegrained samples for extraction so that the approach toward liquid-solid equilibrium is 

enhanced and mass transport through large particles is minimized. A longer extract 

contact time is required for larger maximum particle-size designations. This method 

designates three maximum particle sizes and associated contact times (see Table 2). 

The selection of an appropriate maximum particle size from this table should be based 

on professional judgment regarding the practical effort required to size reduce the solid 

material. 

 11.1.2 Particle-size reduction of “as received” sample may be achieved 

through crushing, milling or grinding with equipment made from chemically inert 

materials. During the reduction process, care should be taken to minimize loss of 

sample and potentially volatile constituents in the sample. 
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April 2010

 11.1.3 If the moisture content of the “as-received” material is greater than 

15% (wet basis), air drying or desiccation may be necessary. Oven drying is not 

recommended for preparation of test samples due to the potential for mineral alteration. 

In all cases, the moisture content of the “as received” material should be recorded. 

NOTE: If the solid material is susceptible to interaction with the atmosphere (e.g., 

carbonation, oxidation), drying should be conducted in an inert environment. 

 11.1.4 When the material seems to be of a relatively uniform particle size, 

calculate the percentage less than the sieve size as follows: 

Where: Msieved = mass of sample passing the sieve (g) 

Mtotal = mass of total sample (g) (e.g., Msieved + mass not passing sieve) 

 11.1.5 The fraction retained by the sieve should be recycled for further 

particle-size reduction until at least 85% of the initial mass has been reduced below the 

designated maximum particle size. Calculate and record the final percentage passing 

the sieve and the designated maximum particle size. For the uncrushable fraction of the 

“as received” material, record the fraction mass and nature (e.g., rock, metal or glass 

shards, etc). 

 11.1.6 Store the size-reduced material in an airtight container in order to 

prevent contamination via gas exchange with the atmosphere. Store the container in a 

cool, dark and dry place prior to use. 

11.2 Determination of solids and moisture content 

 11.2.1 In order to provide the dry mass equivalent of the “as-tested” 

material, the solids content of the subject material should be determined. Often, the 

moisture content of the solid sample is recorded. In this method, the moisture content is 

determined and recorded 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. 

 11.2.2 Place a 5–10-g sample of solid material into a pre-tared dish or 

crucible. Dry the sample to a constant mass at 105 ± 2 °C. Periodically check the 

sample mass after allowing the sample to cool to room temperature 

(20 ± 2 °C) in a desiccator. 
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April 2010

NOTE: The oven-dried sample is not used for the extraction and should be properly 

disposed of once the dry mass is determined. 

 11.2.3 Calculate and report the solids content as follows: 

 Where: SC = solids content (g-dry/g) 

Mdry = mass of oven-dried sample (g-dry) 

Mtest = mass of “as-tested” sample (g) 

11.2.4 Calculate and report the moisture content (wet basis) as follows: 

 Where: MC(wet) = moisture content on a wet basis (gH2O/g) 

Mdry = mass of oven-dried sample (g-dry) 

Mtest = mass of “as-tested” sample (g) 

11.3 Extraction setup schedule (Microsoft® Excel template provided) 

 This method provides an Excel template which may be used to set up the 

extraction schedule. If using the provided template, disregard Sec. 11.3 and proceed to 

the extraction procedure Sec. 11.4. 

 11.3.1 Using the schedule shown in Table 1 as a guide, set up five test 

extractions and one method blank. The mass of solids in an extraction may be scaled to 

minimize headspace in each extraction vessel. However, the volume of eluant should 

always be based on the target L/S in Column B of Table 1. 

 11.3.2 Calculate and record the amount of “as-tested” material equivalent 

to the dry mass in Column D of Table 1 as follows: 

 Where: Mtest = mass of “as-tested” solid equivalent to the dry-material mass (g) 

Mdry = mass of dry material specified in the method (g-dry) 

SC = solids content of “as-tested” material (g-dry/g) 
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April 2010

 11.3.3 Calculate and record the volume of moisture contained in the “astested” sample in Column E of Table 1 as follows: 

 Where: VW,sample = volume of water in the “as tested” sample (mL) 

Mtest = mass of the “as tested” sample (g) 

SC = solids content of the “as tested” sample (g-dry/g) 

ρw = density of water (1.0 g/mL at room temperature) 

 11.3.4 Calculate and record the volume of reagent water required to bring 

each extraction to the target L/S in Column F of Table 1 as follows: 

 Where: VRW = volume of reagent water required to complete L/S (mL) 

Mdry = dry mass equivalent of solid sample (g) 

LS = liquid-to-dry-solid ratio (10 mL/g) 

VW,sample = volume of water in “as used” sample (mL) 

 The size of the extraction bottle should be sufficient to contain the combined 

volume of solid material and eluant, ideally with a minimum amount of headspace. 

12.0 EXTRACTION PROCEDURE 

 12.1 Label five bottles with test position numbers and an additional bottle as a 

method blank according to Column A in Table 1. 

 12.2 Place the dry-mass equivalent (± 0.1 g) of “as-tested” sample as shown in 

Column D in Table 1 into each of the five test position extraction vessels. 

NOTE: Do not put solid material in the method blank extraction vessel 

 12.3 Add the appropriate volume ( ± 0.5 mL) of reagent water to both the test 

position and method blank extraction vessels as specified in Column F of Table 1. 

 12.4 Tighten the leak-proof lid on each bottle and tumble all extractions (i.e., test 

positions and method blanks) in an end-over-end fashion at a speed of 28 ± 2 rpm at room 

temperature (20 ± 2 °C). The contact time for this method will vary depending on the maximum 

particle size as shown in Table 2. 

NOTE: The length of the contact time is designed to enhance the approach toward liquid-solid 

equilibrium. Longer contact times are required for larger particles to compensate for the 
1316 - 11 Revision 1.1 

April 2010

effects of intra-particle diffusion. See Table 2 for required contact times based on the 

maximum particle size. 

 12.5 Remove the extraction vessels from the rotary tumbler and clarify the 

extractants by allowing the bottles to stand for 15 ± 5 min. Alternately, centrifuge the extraction 

vessels at 4000 ± 100 rpm for 10 ± 2 min. 

NOTE: If clarification is significantly incomplete after settling or centrifugation, eluate 

measurements for pH, conductivity, and oxidization-reduction potential (ORP) may be 

taken on filtered samples. In this case, perform the filtration in 12.7 prior to eluate 

measurement in 12.6 and note the deviation from the written procedure. 

CAUTION: Following separation from the solid phase, eluate samples lack the buffering 

provided by the solid phase and therefore may be susceptible to pH change 

resulting from interaction with air. 

 12.6 For each extraction vessel, decant a minimum volume (~ 5 mL) of clear, 

unpreserved supernatant into a clean container. Measure and record the pH, specific 

conductivity, and oxidation-reduction potential (ORP) (optional, but strongly recommended) of 

the extracts (see Methods 9040, 9045, and 9050). 

12.7 Separate the solid from the remaining liquid in each extraction vessel by 

pressure or vacuum filtration through a clean 0.45-μm pore size membrane (Sec. 6.5). The 

filtration apparatus may be exchanged for a clean apparatus as often as necessary until all 

liquid has been filtered. 

NOTE: Eluate measurements for pH, conductivity, and ORP should be taken as soon as 

possible after the settling and preferably within 1 hour after completion of tumbling 

(12.6). 

12.8 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. 

13.0 DATA ANALYSIS AND CALCULATIONS (EXCEL TEMPLATE PROVIDED) 

 13.1 Data reporting 

 13.1.1 Figure 2 shows an example of a data sheet that may be used to 

report the concentration results of this method. This example is included in the Excel 

template. At a minimum, the basic test report should include: 

 a) Name of the laboratory 

 b) Laboratory contact information 

 c) Date at the start of the test 

 d) Name or code of the solid material 

 e) Particle size (85 wt% less than) 

 f) Ambient temperature during extraction (°C) 

 g) Extraction contact time (h) 

 h) Eluate specific information (see Sec. 13.1.2 below) 
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April 2010

 13.1.2 The minimum set of data that should be reported for each eluate 

includes: 

 a) Eluate sample ID 

 b) Target L/S (mL/g-dry) 

 c) Mass of “as tested” solid material used (g) 

 d) Moisture content of material used (gH O2 /g) 

 e) Volume of eluant used (mL) 

 f) Measured final eluate pH 

 g) Measured eluate conductivity (mS/cm) 

 h) Measured ORP (mV) (optional) 

 i) Concentrations of all COPCs 

 j) Analytical QC qualifiers as appropriate 

 13.2 Data interpretation and presentation (optional) 

 13.2.1 LSP curve 

 13.2.1.1 A constituent LSP curve can be generated for each 

COPC after chemical analysis of all extracts by plotting the constituent 

concentration in the liquid phase as a function of L/S used for each extraction. 

The curve indicates the equilibrium concentration of the COPC as a function of 

L/S at the natural pH. 

 13.2.1.2 The lower limit of quantitation (LLOQ) for the analytical 

technique for each COPC may be shown as a horizontal line. COPC 

concentrations below this line indicate negligible or non-quantitative 

concentrations. 

NOTE: The LLOQ is highly matrix dependent and should be determined as 

part of a QA/QC plan. 

 13.2.1.3 Figure 3 provides example LSP curves as a function of 

L/S for a coal combustion fly ash and a coal combustion flue gas desulfurization 

filter cake. 

14.0 METHOD PERFORMANCE 

 14.1 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. These performance data are not intended to be and must not be used as 

absolute QC acceptance criteria for purposes of laboratory accreditation. 

 14.2 Refs. 1 and 2 may provide additional guidance and insight on the use, 

performance and application of this method. 
1316 - 13 Revision 1.1 

April 2010

15.0 

POLLUTION PREVENTION 

 15.1 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. 

 15.2 For information about pollution prevention that may be applicable to 

laboratories and research institutions consult Less is Better: Laboratory Chemical Management 

for Waste Reduction available from the American Chemical Society's Department of 

Government Relations and Science Policy, 1155 16th St., N.W. Washington, D.C. 20036, 

http://www.acs.org. 

16.0 WASTE MANAGEMENT 

 The Environmental Protection Agency requires that laboratory waste management 

practices be conducted consistent with all applicable rules and regulations. The Agency urges 

laboratories to protect the 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 American Chemical Society at the address listed in Sec. 15.2. 

17.0 REFERENCES 

1. D.S. Kosson, H.A. van der Sloot, F. Sanchez and A.C. Garrabrants (2002) “An 

Integrated Framework for Evaluating Leaching in Waste Management and Utilization of 

Secondary Materials,” Environmental Engineering Science, 19(3) 159-204. 

2. D.S. Kosson, A.C. Garrabrants, H.A. van der Sloot (2009) “Background Information for 

the Development of Leaching Test Draft Methods 1313 through Method 1316,” (in 

preparation). 

3. USEPA (2006) Characterization of Mercury-Enriched Coal Combustion Residues from 

Electric Utilities Using Enhanced Sorbents for Mercury Control, EPA-600/R-06/008, 

February 2006. 

4. USEPA (2008) Characterization of Coal Combustion Residues from Electric Utilities 

Using Wet Scrubbers for Multi-Pollutant Control, EPA-600/R-08/077, July 2008. 

5. USEPA (2009) Characterization of Coal Combustion Residues from Electric Utilities – 

Leaching and Characterization Data, EPA-600/R-09/151, December 2009. 
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April 2010

18.0 TABLES, DIAGRAMS, FLOW CHARTS, AND VALIDATION DATA 

The following pages contain the tables and figures referenced by this method 
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April 2010

EXAMPLE 

TABLE 

SCHEDULE FOR 

1 

EXTRACTION SETUP 

A B C D E F G

Test

Position

Target

LS

Minimum Dry 

Mass 

(g-dry)

Mass of

"As-Tested"

Sample

(g)

Moisture in

"As-Tested"

Sample

(mL)

Volume of 

Reagent

Water

(mL)

Recommended

Bottle Size

(mL)

T01 10.0 20 22.2 2.2 198 250

T02 5.0 40 44.4 4.4 196 250

T03 2.0 100 111.1 11.1 189 500

T04 1.0 200 222.2 22.2 178 500

T05 0.5 400 444.4 44.4 156 1000

B03 QC – 200 250

Total – 844.4 1120

NOTE: 1) 

2) 

3) 

Table data 

This schedule assumes a target liquid 

This schedule is based on “as tested” 

Test position marked B01 is a method 

modified from Ref. 1. 

volume of 200 mL. 

solids content of 0.90 g-dry/g. 

blank of reagent water. 

TABLE 2 

EXTRACTION PARAMETERS AS FUNCTION OF MAXIMUM PARTICLE SIZE 

Particle Size US Sieve Minimum Recommended

(85% less than) Size Dry Mass Contact Time Vessel size

(mm) (g-dry) (h) (mL)

0.3 50 20 ± 0.05 24 ± 2 250

2.0 10 40 ± 0.1 48 ± 2 500

5.0 4 80 ± 0.1 72 ± 2 1000
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April 2010

FIGURE 1 

METHOD FLOWCHART 
1316 - 17 Revision 1.1 

April 2010

FIGURE 2 

EXAMPLE DATA REPORTING SHEET 

EPA METHOD 1316

ABC Laboratories Report of Analysis

123 Main Street

Anytown, USA

Contact: John Smith

 (555) 111-1111

Client Contact: Susan Jones

 (555) 222-2222

Material Code: FAX Particle Size: 88% passing 2-mm sieve

Material Type: Coal Combustion Fly Ash Contact Time: 860 g

Date Received: 10/1/20xx Lab Temperature: 21 ± 2 °C

Test Start Date: 11/1/20xx Eluant Used: ASTM Type II Water

Report Date: 12/1/20xx

Test

Position Replicate Value Units Method Note

T01 A

Eluate Sample ID XYZ-1316-T01-A

Solid Material 40.0 g

Moisture Content 0.01 gH2O/g

Water Added 386.0 mL

Target L/S 10.0 mL/g-dry

Eluate pH 1.89 – EPA 9040

Eluate Conductivity 12.6 mS/cm EPA 9050

Eluate ORP 203 mv

QC Dilution

Chemical Analysis Value Units Flag Method Date Factor

Al 216.0 mg/L EPA 6020 11/7/20xx 1000

As 7.64 mg/L EPA 6020 11/7/20xx 10

Cl < 4.13 mg/L U EPA 9056 11/9/20xx 1

Test

Position Replicate Value Units Method Note

T02 A

Eluate Sample ID XYZ-1316-T02-A

Solid Material 20.0 g

Moisture Content 0.01 gH2O/g

Water Added 400.0 mL

Target L/S 5.0 mL/gEluate pH dry 3.86 – EPA 9040

Eluate Conductivity 0.99 mS/cm EPA 9050

Eluate ORP 180 mv

QC Dilution

Chemical Analysis Value Units Flag Method Date Factor

Al 449.0 mg/L EPA 6020 11/7/20xx 1000

As 97.9 mg/L EPA 6020 11/7/20xx 10

Cl < 4.13 mg/L U EPA 9056 11/7/20xx 1

QC Flag Key: U Value below lower limit of quantitation as reported (< "LLOQ")
1316 - 18 Revision 1.1 

April 2010
1316 - 19 Revision 1.1 

April 2010

FIGURE 3 

EXAMPLE CONCENTRATON RESULTS FROM A COAL COMBUSTION FLY ASH AND 

FLUE-GAS DESULFURIZATION FILTER CAKE 
E - 1 

APPENDIX E. DETAILS OF TIME, MATERIALS, AND COST 

ESTIMATES BY METHOD 

Table E-1. Detailed Labor Time Estimates for Method 1313. 

Task

Subtask

Units per 

Test

Subtask 

Time [min]

Task Time 

[h]

Moisture Content (“as received”) 2 0.5

Air Drying (1-2 days assumed) 1 0.5

Particle-size Analysis/Reduction 1 1.5

Sieving

Grinding

1

1

30

60

Moisture Content (“as tested”) 2 0.5

Pre-Test Titration (2 x 5 extracts) 10 2.5

Labeling bottles

Solids-filling, weighing & recording

Liquid-filling, weighing & recording

Acid/base addition

pH measurement & recording

Data template management

10

10

10

10

10

2

10

20

20

20

50

30

Extraction Procedure (9 extracts + 3 QC) 12 6.2

Labeling bottles

Solids-filling, weighing & recording

Liquid-filling, weighing & recording

Acid/base addition

pH/EC/Eh measurement & recording

Eluate filtration

12

9

12

11

12

12

12

18

24

22

60

60

Sample preservation

Data template management

Clean Up (12 filter holders)

24

3

3

24

60

90

Total Labor Time 11.7

Notes: 

1) Particle-size reduction assumes a relatively easy material to reduce (e.g., coal combustion residues, 

soils) via mechanical grinder or light hand grinding with mortar and pestle. 

2) Pre-test titration step assumes two rounds of five extractions are required to adequately define the 

titration curve (10 pre-test extractions in all). 
E - 2 

Table E-2. Detailed Labor Time Estimates for Method 1314. 

Task

Subtask

Units per 

Test

Subtask 

Time [min]

Task Time 

[h]

Moisture Content (“as received”) 2 0.5

Air Drying (1-2 days assumed) 1 0.5

Particle-size 

Sieving

Grinding

Analysis/Reduction 1

1

1

30

60

1.5

Moisture Content (“as tested”) 2 0.5

Column Setup 

Column packing, weighing 

Eluant preparation

Pump adjustment

& recording

1

1

1

1

30

15

60

1.8

Column Test Procedure (9 eluates + 1 QC)

Checking system & flowrate (daily)

Bottle exchange (9 eluates – 8 changes)

pH/EC/Eh measurement & recording

Eluate filtration

10

15

8

9

10

75

40

30

30

6.9

Sample preservation

Data template management (daily)

Clean up (1 filter holders per exchange)

20

15

8

60

75

100

Clean up (column) 1 1.0

Total Labor Time 12.7

Notes: 

1) Particle-size reduction assumes a relatively easy material to reduce (e.g., coal 

soils) via mechanical grinder or light hand grinding with mortar and pestle. 

2) Column operation assumes light to moderate daily systems maintenance (e.g., 

rate measurement & recording). 

combustion residues, 

pump adjustment, flow 
E - 3 

Table E-3. Detailed Labor Time Estimates for Method 1315 (Granular Material). 

Task

Subtask

Units per 

Test

Subtask 

Time [min]

Task Time 

[h]

Moisture Content (“as received”) 2 0.5

Air Drying (1-2 days assumed) 1 0.5

Particle-size 

Sieving

Grinding

Analysis/Reduction 1

1

1

30

60

1.5

Moisture Content (“as tested”) 2 0.5

Optimum Moisture/Density ( 5 trials)

Moisture adjustment

Sample packing

Dimension measurement & recording

Mass measurement & recording

Data template management

5

5

5

5

5

1

50

80

25

25

30

3.5

Compacted Granular Sample Preparation 1 1.0

Moisture Content (“as packed”) 2 0.5

Test Procedure (9 fractions + 9 QC)

Eluant-filling, weighing & recording

Sample exchange, weighing & recording

pH/EC/Eh measurement & recording

Eluate filtration

Sample preservation

Data template management

Clean Up (2 vessels + 2 filter holders)

18

9

9

18

18

10

36

9

18

18

54

36

50

108

180

7.8

Total Labor Time 15.8

Notes: 

1) Particle-size reduction assumes a relatively easy material to reduce (e.g., coal combustion residues, 

soils) via mechanical grinder or light hand grinding with mortar and pestle. 

2) Monolithic samples are assumed to be provided at an appropriate size such that no cutting or coring is 

necessary. 

3) In most cases, testing of a monolithic sample would require only “as received” moisture content and 

the test procedure steps, totaling approximately 8.5 labor hours. 
E - 4 

Table E-4. Detailed Labor Time Estimates for Method 1316. 

Task

Subtask

Units per 

Test

Subtask 

Time [min]

Task Time 

[h]

Moisture Content (“as received”) 2 0.5

Air Drying (1-2 days assumed) 1 0.5

Particle-size Analysis/Reduction 1 1.5

Sieving

Grinding

1

1

30

60

Moisture Content (“as tested”) 2 0.5

Extraction Procedure (5 extracts + 1 QC) 6 3.6

Labeling bottles

Solids-filling, weighing & recording

Liquid-filling, weighing & recording

pH/EC/Eh measurement & recording

Eluate filtration

6

5

6

6

6

6

12

12

30

30

Sample preservation

Data template management

Clean Up (12 filter holders)

12

1

1

36

30

60

Total Labor Time 6.6

Notes: 

1) Particle-size reduction assumes 

soils) via mechanical grinder or 

a relatively easy material to reduce (e.g., coal 

light hand grinding with mortar and pestle. 

combustion residues, 

Table E-5. Minimum Solid Material Required for Method 1313. 

Method 1313 Number of Solid Samples Sample Mass 

[g-dry]

Mass Required 

[g-dry]

Moisture Content (MC) 2 analyses x 2 replicates 10 40

Pre-Test Titration 2 trials x 5 extracts 40 400

Batch Test Extracts 9 extracts 40 360

Mass Required for Method 1313 800
E - 5 

Table E-6. Minimum Solid Material Required for Method 1314. 

Method 1314 Number of Solid Samples Sample Mass Mass Required 

[g-dry] [g-dry]

MC 2 analyses x 2 replicates 10 40

Column Test 1 column 660

Mass Required for Method 1314 700

a

 Mass estimate assumes cylindrical column (5-cm dia. x 30 cm) and packing density of 1.2 3 g-dry/cm .

Table E-7. Minimum Solid Material Required for Method 1315. 

Method 1313 Number of Solid Samples Sample Mass Mass Required 

[g-dry] [g-dry]

MC – monolith 3 analyses x 2 replicates 10 60

MC – granular 2 analysis x 2 replicates 10 20

Optimum a Density 5 samples 700 3500

Tank Testb 1 sample 1400 1400

Mass Required for Method 1315 (granular)c 4960

Mass Required for Method 1315 (monolithic) 1420

a

 

b

 

c

 

Estimate assumes packing 1⁄2 volume of test sample per optimum density trial. 

Mass estimate assumes cylindrical sample (10-cm dia. x 10 cm) and packed density 

1st Optimum density assessment is conducted only for test. 

of 1.7 3 g-dry/cm .

Table E-8. Minimum Solid Material Required for Method 1316. 

Method 1313 Number of Solid Samples Sample Mass 

[g-dry]

Mass Required 

[g-dry]

MC 2 analyses x 2 replicates 10 40

Batch Test Extracts 5 extracts @ different LS 950

LS=10 mL/g-dry

LS=5 mL/g-dry

LS=2 mL/g-dry

LS=1 mL/g-dry

LS=0.5 mL/g-dry

25

50

125

250

500

Mass Required for Method 1316 990
E - 6 

Table E-9. Estimate of Supply Costs for Batch Method 1313.(1)

Item Description Fisher 

Scientific 

Catalog #

Required 

for 3

Test

Reps

Unit 

(2) Price

Cost 

Test

for 3

Reps

Moisture Content

Aluminum weighing dish, 2.3 fl. oz., Fisherbrand 08-732-103 12 $0.57 $6.84 

Granular Material Storage

I-Chem HDPE wide-mouth bottle, 1000 mL 05-719-357 3 $5.23 $15.69 

Pre-Test Titration

I-Chem HDPE wide-mouth bottle, 250 mL 05-719-353 10 $2.95 $29.50 

Nitric Acid, tracemetal grade, Fisher Chemical A509-212 50 mL $0.05 $2.50 

Sodium Hydroxide solution, 2N, Fisher Chemical SS264-1 50 mL $0.06 $3.00 

BD Falcon 15 mL conical centrifuge tube 14-959-49B 10 $0.42 $4.20 

Extraction Setup

I-Chem HDPE wide-mouth bottle, 250 mL 05-719-353 30 $2.95 $88.50 

Nitric Acid, tracemetal grade, Fisher Chemical A509-212 ~150 mL $0.05 $7.50 

Sodium Hydroxide solution, 2N, Fisher Chemical SS264-1 ~150 mL $0.06 $9.00 

Eluate Processing

BD Falcon 15 mL conical centrifuge tube 14-959-49B 30 $0.42 $12.60 

GH Polypro filter, 0.45-μm pore, Andwin Scientific NC9035907 30 $2.47 $74.10 

I-Chem HDPE wide-mouth bottle, 125 mL 05-719-351 60(3) $2.39 $143.40 

Nitric acid, optima grade, Fisher Chemical A467-500 30 mL $0.75 $22.50 

Total Supplies Cost per Test $419.33 

Equipment and Durable Items

12-port tumbler, LE-1002, Environmental Express 09-732-79 1 $6,880.00 $6,880.00 

Polycarbonate filter holder, 250 mL, Nalgene 09-740-23A 12(4) $104.52 $1,254.24

Total Equipment Cost per Test $8,134.24

Notes: 

(1) Supply and equipment costs are shown as example costs associated with conducting the method and do not 

denote any endorsement by the authors or USEPA of a specific vendor, manufacturer or product. 

(2) Prices based on Fisher Scientific online catalog (www.fishersci.com) as of 3/25/10 unless otherwise noted. 

(3) Assumes two analytical samples per test position with one preserved using optima nitric acid. 

(4) Filtration holders may be soap-water washed, rinsed with 10% nitric acid, and triple reagent water rinsed 

between uses. Thirty (30) filter holders are recommended if washing between replicates is not anticipated. 
E - 7 

Table E-10. Estimate of Supply and Equipment Costs for Column Method 1314.(1)

Item Description Fisher Required Unit Cost for 

(2) Scientific for 3 Test Price 3 Test

Catalog # Reps Reps

Moisture Content

Aluminum weighing dish, 2.3 fl. oz., Fisherbrand 08-732-103 12 $0.57 $6.84 

Granular Material Storage

I-Chem HDPE wide-mouth bottle, 1000 mL 05-719-357 3 $5.23 $15.69 

Column Setup

PTFE column bed support, 4.8-cm, Kimble-Kontes K420809-2040 6 $6.51 $39.06 

Tygon R-3603 tubing, 1/16” ID, St. Gobain 14-169-1B 30 ft $0.28 $8.40 

Calcium chloride dihydrate, ACS, Fisher Chemical C79-500 1.5 g/10L $0.05 $0.50 

Eluate Processing

BD Falcon 15 mL conical centrifuge tube 14-959-49B 28 $0.42 $11.76 

GH Polypro filter, 0.45-μm, Andwin Scientific NC9035907 28 $2.47 $69.16 

I-Chem HDPE wide-mouth bottle, 125 mL 05-719-351 56(3) $2.39 $133.84 

Nitric acid, optima grade, Fisher Chemical A467-500 ~30 mL $0.75 $22.50 

Total Supplies Cost per Test $307.75 

Equipment and Durable Items

Chromaflex column, 4.8-cm ID, Kimble-Kontes K420830-3020 3 $318.95 $956.85 

Nalgene filter holder, 250 mL, Thermo Scientific 09-740-23A 28(4) $104.52 $2,926.56 

Manostat “Carter” pump, 12/6, Thermo Scientific 13-875-249 1 $2,818.82 $2,818.82 

Pump link, pharmed, 0.89 mm, Thermo Scientific 13-875-296 3 $7.52 $22.56 

LDPE Carboy, 20 L, Nalgene 02-961-60E 1 $124.83 $124.83 

Polycarbonate straight-side jar, 250 mL, Nalgene 11-815-10D 18 $3.77 $67.86 

Polypropylene mason jar, 2000 mL, Nalgene 11-825C 3 $16.79 $50.37 

Polypropylene mason jar, 3000 mL, Nalgene 11-825D 3 $21.58 $64.74 

Total Equipment Cost per Test $7,032.59 

Notes: 

(1) Supply and equipment costs are shown as example costs associated with conducting the method and do not 

denote any endorsement by the authors or USEPA of a specific vendor. 

(2) Estimates based on Fisher Scientific online catalog (www.fishersci.com) as of 3/25/10 unless otherwise noted. 

(3) Assumes two analytical samples per test position with one preserved using optima nitric acid. 

(4) Filtration holders may be soap-water washed, rinsed with 10% nitric acid, and triple reagent water rinsed 

between uses such that less than 28 holders are required. 
E - 8 

Table E-11. Estimate of Supply and Equipment Costs for Mass Transport Method 1315.(1)

Item Description Fisher Required Catalog Cost for 3

(2) Scientific for 3 Test Price Test Reps

Catalog # Reps

Moisture Content

Aluminum weighing dish, 2.3 fl. oz., Fisherbrand 08-732-103 12 $0.57 $6.84 

Granular Material Storage (Granular Only)

I-Chem HDPE wide-mouth bottle, 1000 mL 05-719-357 3 $5.23 $15.69 

Optimum Density Analysis (Granular Only)

Concrete cylinder molds, 4” ID x 8” (cut to 3”) NA(a) 5 $0.98 $4.90 

Sample Preparation (Granular Only)

Concrete cylinder molds, 4” ID x 8” (cut to 3”) NA(a) 3 $0.98 $2.94 

Eluate Processing

BD Falcon 15 mL conical centrifuge tube 14-959-49B 36 $0.42 $15.12 

GH Polypro filter disc, 0.45-μm, Andwin Scientific NC9035907 36 $2.47 $88.92 

I-Chem HDPE wide-mouth bottle, 125 mL 05-719-351 72 $2.39 $172.08 

Nitric acid, Optima grade, Fisher Chemical A467-500 36 mL $0.75 $27.00 

Total Supplies Cost per Test (Granular Material) $333.49 

Total Supplies Cost per Test (Monolithic Material) $309.96 

Equipment and Durable Items

Compaction rammer (granular) NA(b) 1 $100.00 $100.00 

Polycarbonate straight-side jar, 1000 mL (granular) 11-815-10F 8 $8.07 $64.56 

LDPE 170 oz container (monolithic), Nalge Nunc 12-566-113 8 $4.00 $32.00 

Polycarbonate filter holder, 250 mL, Nalgene 09-740-23A 36(3) $104.52 $3,762.72 

Total Equipment Cost per Test (Granular Material) $2,013.64 

Total Equipment Cost per Test (Monolithic Material) $1,897.36 

Notes: 

(1) Supply and equipment costs are shown as example costs associated with conducting the method and do not 

denote any endorsement by the authors or USEPA of a specific vendor. 

(2) Estimates based on Fisher Scientific online catalog (www.fishersci.com) as of 3/25/10 unless otherwise noted. a

 available as item #004-873 through MA Industries, Peachtree City, GA at www.maind.com. 

b

 available as item #EL24-0963 through ELE International at www.ele.com/usa (cost approximated). 

(3) Filtration holders may be soap-water washed, rinsed with 10% nitric acid, and triple reagent water rinsed 

between uses such that less than 36 holders are required. 
E - 9 

Table E-12. Estimate of Supply Costs for Batch Method 1316.(1)

Item Description Fisher Required Catalog Cost for 3 

(2) Catalog # for 3 Test Price Test Reps

Reps

Moisture Content

Fisherbrand aluminum weighing dish, 2.3 fl. oz. 08-732-103 12 $0.57 $6.84 

Granular Material Storage

I-Chem HDPE wide-mouth bottle, 1000 mL 05-719-357 3 $5.23 $15.69 

Extraction Setup

I-Chem HDPE wide-mouth bottle, 500 mL 05-719-349 16 $4.24 $67.84 

Eluate Processing

BD Falcon 15 mL conical centrifuge tube 14-959-49B 16 $0.42 $6.72 

Andwin Scientific GH Polypro filter, 0.45-μm NC9035907 16 $2.47 $39.52 

I-Chem HDPE wide-mouth bottle, 125 mL 05-719-351 32 $2.39 $76.48 

Fisher Chemical Nitric acid (optima grade) A467-500 ~16 mL $0.75 $12.00 

Total Supply Cost per Test $225.09 

Durable Supplies

Environmental Express LE-1002 tumbler, 12 port 09-732-79 1 6,880.00 $6,880.00 

Nalgene polycarb filter holder, 250 mL 09-740-23A 16(3) $104.52 $1,672.32 

Total Durables Cost per Test $8,552.32 

Notes: 

(1) Supply and equipment costs are shown as example costs associated with conducting the method and do not 

denote any endorsement by the authors or USEPA of a specific vendor. 

2) Estimates based on Fisher Scientific online catalog (www.fishersci.com) as of 2/01/10 unless otherwise noted. 

3) Filtration holders may be soap-water washed, rinsed with 10% nitric acid, and triple reagent water rinsed 

between uses such that less that 30 holders are required.