v>EPA
United States
Environmental Protection
Agency
Office of Solid Waste
and Emergency Response
Washington DC 20460
EPA/530-SW-84-015
December 1984
Solid Waste
Draft
Permit Guidance Manual on
Hazardous Waste
Land Treatment
Demonstrations
For Public Comment
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DISCLAIMER
This is a draft manual that is being released by EPA for public
comment on the accuracy and usefulness of the information it contains.
Since the Agency's peer and administrative review of this document has not
yet been completed, it does not necessarily reflect the views and policies
of the Agency. Mention of trade names or commercial products does not
constitute endorsement or recommendation for use.
ii
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PREFACE
Subtitle C of the Resource Conservation and Recovery Act (RCRA) re-
quires the Environmental Protection Agency (EPA) to establish a Federal
hazardous waste management program. This program must ensure that hazar-
dous wastes are handled safely from generation to final disposition. EPA
issued a series of hazardous waste regul ations under Subtitle C of RCRA,
published in 40 Code of Federal Regulations (CFR) Parts 260 through 265,
270 and 124.
Part 264 and 265 of 40 CFR contain standards applicable to owners and
operators of all facilities that treat, store, or dispose of hazardous
wastes. Wastes are identified or listed as hazardous under 40 CRF Part
261. The Part 264 standards are implemented through permits issued by
authorized States or the EPA in accordance with 40 CFR Part 124 and Part
270 regulations. Land treatment, storage, and disposal (LTSD) regulations
in 40 CFR Part 264 issued on July 26, 1982, establish performance standards
for hazardous waste landfills, surface impoundments, land treatment units,
and waste piles.
This draft manual provides guidance on treatment demonstrations, which
are required under §264.272 for all owners/operators of hazardous waste
land treatment units. The manual delineates specific laboratory and field
test methods that may be used to complete the demonstration and describes
the applicability of alternative technical approaches to and permitting
procedures (e.g., short-term permits, two-phase permits, etc.) for various
situations. The manual addresses numerous technical and policy questions
regarding the overall approach to the demonstration, the extensiveness of
the demonstration, and the permitting of land treatment units to accom-
modate the treatment demonstration.
This manual and other EPA guidance documents do not supersede the
regul ations promul gated under RCRA and publ ished in the Code of Federal
Regulations. Instead, they provide guidance, interpretations, suggestions,
and references to additional information. This guidance is not intended to
suggest that other designs might not also satisfy the regulatory standards.
EPA intends to revise this manual as soon as possible based on com-
ments received. Comments on this manual should be addressed to Docket
Clerk, Office of Solid Waste (WH-562), U. S. EPA, 401 M Street SW, Wash-
ington, DC 20460. Because this draft manual was developed before the
passage of the RCRA amendments of 1984, certain aspects of the document may
be modified once EPA implements this legislation.
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EXECUTIVE SUMMARY
Successful performance of the land treatment demonstration (LTD) is
the key step in obtaining a final permit under 40 CFR Parts 264 and 270 for
a hazardous waste land treatment unit. In consideration of the complexity
of the demonstration requirements, this document was prepared both to give
the applicant guidance on the preliminary information needed and to help in
choosing and implementing an LTD approach.
Permit options for land treatment differ from those of other land
disposal technologies. The LTD, much like the trial burn for
incinerators, requires permit alternatives to allow for trial performance.
Thus, the alternatives are the short-term treatment demonstration permit,
the two phase permit, and the full scale facility permit. The applicable
permit alternative depends on a number of factors, including but not
limited to 1) whether the unit is new or existing, 2) the condition of site
records, 3) past, present, and planned operations, 4) data from waste
analyses and p«"el iminary site investigations.
While much of the information preliminary to the LTD should have been
supplied via other permit application requirements, this document
nevertheless provides supplementary guidance on some aspects of these
application requirements. Of particular importance for existing units is
guidance on reconnaissance-level soil sampling and analysis. Data from
this investigation play a key role in formulating the permit and treatment
demonstration approach by generally defining the spatial distribution of
hazardous constituents across the HWLT unit.
The logic and flow of decision-making in choosing the permit approach
and the technical elements to be performed in the LTD involve answering a
series of questions. In brief, the questions ask 1) whether the unit is
new or existing, 2) whether major design and operation changes are planned,
3) whether the unit is operating effectively to treat wastes, and 4)
whether the operator has adequate documentation of past activities. The
answers to these questions and, to some extent, the judgement or preference
of the applicant and the permit writer determine which of four LTD
scenarios will be employed.
Technical methods for performing each step of the LTD are presented in
the latter chapters. By first choosing the LTD permit scenario the appli-
cant defines the technical elements to be carried out and may then assemble
a treatment demonstration plan using the chapters that describe these
technical elements. Test methods include intensive site sampling and
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EXECUTIVE SUMMARY - Continued
analysis, acute toxicity testing, barrel lysimeter and field plot studies,
and follow-up, full scale field monitoring; these methods are not neces-
sarily listed In order of performance nor are they all required in any
given case. In addition to the above information, this manual provides
guidance on how to analyze samples, interpret data, and draw design conclu-
sions.
Finally, appendices cover numerous soil analytical procedures and
methods for collection and installation of barrel lysimeters and answer
some commonly asked questions about land treatment.
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TABLE OF CONTENTS
Page
DISCLAIMER 11
PREFACE 111
EXECUTIVE SUMMARY 1v
LIST OF FIGURES x
LIST OF TABLES xi
LIST OF ABBREVIATIONS xii
ACKNOWLEDGMENTS xiii
1.0 BACKGROUND AND GENERAL INFORMATION 1
1.1 Introduction 1
1.2 Overview of Manual 2
1.3 Approaches to the LTD 3
1.3.1 Administrative Approaches 5
1.3.2 Technical Approaches 8
1.4 Other Sources of Information 10
2.0 PRELIMINARY INFORMATION NEEDS 11
2.1 Soil Characterization 11
2.1.1 Soil Survey 12
2.1.1.1 Conducting the Soil Survey 12
2.1.1.2 Analysis of Samples Obtained in the Soil
Survey 13
2.1.1.2.1 Soil Physical Properties. . . 13
2.1.1.2.2 Soil Chemical Properties. . . 13
2.1.1.2.3 Soil Biological Properties. . 14
2.1.2 Reconnaissance Characterization of Waste Con-
stituent Distribution in Soil 14
2.1.2.1 Soil Cores 14
2.1.2.1.1 Depth 15
2.1.2.1.2 Areal Distribution 15
2.1.2.1.3 Number of Samples 15
—continued—
vi
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TABLE OF CONTENTS - Continued
Page
2.1.2.1 Soil Cores - Continued
2.1.2.1.4 Analysis of Soil Core Samples 15
2.1.2.1.5 Interpretation of Soil Core
Sample Data 17
2.1.2.2 Soil-Pore Liquid 17
2.2 Waste Characterization 18
2.2.1 Sampling 19
2.2.2 Sample Collection 19
2.2.3 Sample Handling and Storage 20
2.2.4 Sample Analysis 20
2.2.5 Appendix VIII Constituents 21
3.0 TREATMENT DEMONSTRATION SCENARIOS AND DECISION-MAKING .... 26
3.1 Criteria for Choosing a Land Treatment Demonstration
Scenario • 26
3.1.1 Are Major Design and Operation Changes Planned? . 28
3.1.1.1 Planned Unit Processes 28
3.1.1.2 Planned Waste Application Rates 29
3.1.1.3 Planned Use of Soils 29
3.1.1.4 Guidance on Planned Design and Operation 30
3.1.2 Is the Performance of the Existing HWLT Unit
Acceptable? 31
3.1.2.1 Monitoring System Design 31
3.1.2.2 Performance Evaluation 32
3.1.3 Are the Waste Management Records Complete?. ... 32
3.2 Treatment Demonstration Permitting Scenarios 33
3.2.1 Scenario 1 35
3.2.2 Scenario 2 37
3.2.3 Scenario 3 38
3.2.4 Scenario 4 39
4.0 INTENSIVE SITE DATA COLLECTION 40
4.1 Soil Core Sampling and Analysis 40
4.2 Soil-Pore Liquid 40
4.3 Analysis of Samples 41
4.4 Interpretation of Data 41
5.0 TOXICITY TEST PROCEDURE 43
5.1 Test System Description 44
—continued--
vii
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TABLE OF CONTENTS - Continued
5.2 General Experimental Procedures
5.2.1 Water Soluble Fractions ^
5.2.2 Test System Operation j5
5.3 Toxicity Test Applications and Procedures 46
5.3.1 Application Rate Determination 46
5.3.2 Maximum Residual Concentration 4#
5.4 Data Interpretations 49
5.5 Maximum Acceptable Initial Loading Rate 50
5.5.1 MAIL Rate Window Determination 50
6.0 BARREL LYSIMETER STUDY 52
6.1 Experimental Design 52
6.1.1 Collection and Installation of Lysimeters .... 53
6.1.2 Preparation of Lysimeters for Study 55
6.2 Experimental Methods 55
6.2.1 Waste Application 55
6.2.2 Water Management 55
6.2.3 Soil Sample Collection and Analysis 56
6.2.4 Soil-pore Liquid Sample Collection and Analysis . 57
6.3 Data Reduction and Interpretation 57
6.3.1 Degradation Rate and Half-Life Determination. . . 57
6.3.2 Immobilization 58
7.0 FIELD PLOT STUDY 60
7.1 Experimental Design 60
7.1.1 Plot Preparaton 62
7.1.1.1 Size 62
7.1.1.2 Slope 62
7.1.1.3 Plot Isolation 62
7.1.1.4 Run-off Collection 62
7.1.2 Number, Location, and Installation of Soil-Pore
Liquid Samplers 63
7.2 Experimental Methods 63
7.2.1 Waste Application 63
7.2.2 Plot Management 69
7.2.3 Sample Collection and Analysis 69
7.2.4 Soil-Pore Liquid Sample Collection and Analysis . 70
7.3 Data Reduction and Interpretation 70
7.3.1 Degradation Rate and Half Life Determination. . . 70
7.3.2 Immobi 1 i zati on 72
8.0 DATA INTERPRETATIONS 73
8.1 Waste Application Limit 73
8.2 Annual Waste Loading Rate 73
—continued--
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TABLE OF CONTENTS - Continued
Page
8.3 Required Unit Area 75
8.4 Unit Life 76
9.0 TWO YEAR FOLLOW-UP STUDY 79
9.1 Soil Core Samples 79
9.2 Soil-Pore Liquid Monitoring 80
9.3 Soil Core and Soil-Pore Liquid Sample Analysis 80
9.4 Interpretation 80
10.0 TIERED SAMPLE ANALYSIS 81
10.1 Tier 1 81
10.2 Tier II 81
10.3 Tier III 82
10.4 Quality Assurance/Quality Control 83
APPENDIX A SOIL SAMPLING AND ANALYSIS
A.I Soil Sampling 85
A.2 Analytical Methods for Soils 90
A.2.1 Physical Methods 90
A.2.1.1 Particle Size Analysis 90
A.2.1.2 Bulk Density 92
A.2.1.3 Moisture Retention 94
A.2.2 Soil Chemical Methods 98
A.2.2.1 Paste pH 98
A.2.2.2 Lime Requirements by SMP Buffer .... 100
A.2.2.3 Double Acid Extractable Phosphorus, Pot-
assium, Calcium, and Magnesium 102
A.2.2.4 Total Nitrogen by Kjeldahl Method ... 108
A.2.2.5 Sodium Saturated Cation Exchange
Capacity Ill
A.2.2.6 Electrical Conductance of Soil Extract. 114
A.2.2.7 Organic Carbon by Low Temperature
Ignition 117
APPENDIX 8 DETAILED PROCEDURE FOR COLLECTING BARREL SIZED UN-
DISTURBED
B.I Scope and Applicaton 119
B.2 Lysimeter Installation 119
APPENDIX C QUESTIONS AND ANSWERS 123
IX
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LIST OF FIGURES
Number Page
1.1 Treatment demonstration decision flow chart 4a
3.1 Treatment demonstration decision flow chart 27a
7.1 Porous cup soil-pore liquid sampler and pressure vacuum
pump used to collect sample 64
7.2 Glass brick soil pore liquid sampler (pore type). ...... 65
7.3 Soil-pore liquid sample locations 66
7.4 Installation of samplers in pits . 67
7.5 Soil-pore liquid sampling station 68
B.I Support frame design for barrel lysimeter collection. . . . 120
B.2 Lifting harness for removing and rotating barrel lysimeter. 122
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LIST OF TABLES
Number
1.1 Land Treatment Permit Elements 6
1.2 Permit Application Content for Each Permit Element. ... 7
1.3 Selected References on Land Treatment 10
2.1 Physical and Chemical Anaylsis of Wastes 21
2.2 Hazardous Constituents Suspected to be Present in
Refinery Wastes 23
3.1 Planned Operations Information Needs 30
3.2 Criteria for Deciding the Completeness of Waste Management
Data and Records 34
6.1 Waste Application Soil Sampling Schedule for Barrel
Lysimeter Study * 54
7.1 Waste Application Soil Sampling Schedule for Barrel
Lysimeter Study . 61
lO.f Components of Analyitical Tiers Used in the Land Treat-
ment Demonstration 82
A.I Soil-SMP Buffer pH and Corresponding Lime Requirment
to Bring Materials to pH 6.5 102
A.2 Phosphorus Standards 105
A.3 Calcium Standards 107
A.4 Magnesium Standards 107
xi
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LIST OF ABBREVIATIONS
ALC Application Limiting Constituent
CLC Capacity Limiting Constituents
EPA U. S. Environmental Protection Agency
GRW Groundwater Monitoring
HWLT Hazardous Waste Land Treatment
ISS Interim Status Standards
LTD Land Treatment Demonstration
MAIL Maximum Acceptable Initial Loading Rate
PAGM Permit Applicants Guidance Manual
RCRA Resource Conservation and Recovery Act
SCS U. S. Soil Conservation Service
UZM Unsaturated Zone Monitoring
WSF Water Soluble Fraction
ZOI Zone of Incorporation
xii
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ACKNOWLEDGMENTS
This document was prepared by Gordon B. Evans, Jr., William Hornby,
and K.C. Donnelly with the firm of K.W. Brown & Associates, Inc. (6A
Graham Road, College Station, Texas) under subcontract to GCA Corporation
(Bedford, Massachusetts; EPA Contract No. 68-01-6871, Work Assignment No.
14).
The authors wish to express their appreciation to Michael P. Flynn,
EPA Project Officer, whose understanding of the technical and regulatory
aspects of land treatment technology enabled him to make significant con-
tributions to the final organization and content of this document. Like-
wise, we wish to acknowledge the contribution of John Matthews of EPA's
Robert S. Kerr Laboratory, who drafted one of the foundation documents used
as a resource in preparation of this document and provided invaluable imput
into the toxicity testing protocol. We would also like to thank Charles
Young, who served as GCA Work Assignment Manager, for his assistance and
good demeanor through the many iterations in the drafting of the document.
Special praises also go to Beth D. Frentrup and Debra Hower for hours of
capable editorial labors under the pressure of deadlines and to Beth
Rutkowski for her patient and accurate typing of the document.
xi i i
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Chapter 1
BACKGROUND AND GENERAL INFORMATION
1.1 INTRODUCTION
Under the Authority of Subtitle C of the Resource Conservation and
Recovery Act (RCRA), EPA promulgated regulations for the treatment, stor-
age, and disposal of hazardous waste in land treatment units (40 CFR 264).
These regulations require a permit for the operation of a hazardous waste
land treatment (HWLT) unit. Section 264.272 stipulates that the first step
in obtaining such a permit is to complete a land treatment demonstration
(LTD).
The land treatment demonstration is used by the permitting authority
to define two elements of the land treatment program. First, the demon-
stration establishes what wastes may be managed at the unit. Wastes that
will be applied must be subject to degradation, transformation, and/or
immobilization processes in the soil such that hazardous constituents are
not expected to emerge from the defined treatment zone. Second, results of
the treatment demonstration will be used to define the initial set of waste
management practices, including loading rates, that will be incorporated
into the facility permit.
The treatment demonstration can be completed using information derived
from published literature, laboratory studies, field studies, and/or actual
facility operating experience. However, the Agency generally believes that
an inadequate data base exists in the published literature to predict unit-
specific waste-soil interactions. Consequently, most land treatment permit
applicants must use laboratory studies, field studies, actual facility
operating experience, or a combination of these approaches to complete the
treatment demonstration.
The purpose of this manual is to provide guidance on specific labora-
tory and field test methods that may be used to complete the treatment
demonstration as required under §264.272 for all owners and operators of
hazardous waste land treatment units. The manual also addresses numerous
questions on policy and technical aspects of the demonstration and de-
scribes alternative permitting approaches and their applicability to
various facility "scenarios".
In this manual, which is designed to encourage an information and
decision-making flow, care is taken to maintain a logical progression from
the beginning to the end of the treatment demonstration. Two primary
tenets used to select tests for the experimental portion of the protocol
are:
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1) avoidance of unnecessary test redundancy (e.g., It is un-
necessary to determine degradation rates by both soil res-
pi rometry and bench scale degradation experiments); and
2) performance of only those tests that yield definitive infor-
mation leading to clear decisions on issues pertinent to the
LTD (§264.272) (i.e., treatability, waste loading rates, and
monitoring parameters).
This manual clarifies and elaborates on the general guidance on treat-
ment demonstrations already provided in the following documents:
o Permit Applicants' Guidance Manual for Hazardous Waste Land
Treatment, Storage, and Disposal Facilities (EPA, 1984A);
o Hazardous Waste Land Treatment (SW-874); EPA, 1983); and
o RCRA Guidance Document: Land Treatment Units (Draft, EPA,
1983B).
EPA wishes to emphasize that the methods described in this manual are
guidance, not regulations; an applicant may use alternative methods,
provided that these methods are equivalent to or more comprehensive than
those described herein. While the Agency believes that the specifications
provided for each of the described test methods are a reasonable estimate
for a complete treatment demonstration in compliance with §264.272, the
permit writer may modify these specifications as necessary.
1.2 OVERVIEW OF MANUAL
The planning of a treatment demonstration involves a decision-making
process in which various general technical approaches (e.g., operating
data, lab tests, field tests) are evaluated, and in which regulatory,
technical, administrative, and practical constraints are considered. Once
the general technical approach is determined, the appropriate permitting
procedure (e.g., short-term permit, two-phase permit) is selected in con-
sultation with the permitting authority. Finally, detailed experimental
methods must be developed and the test completed.
This manual is organized to assist the permit applicant in planning
and implementing a treatment demonstration in compliance with §264.272.
Thus, the manual focuses on the decision-making process (illustrated in
Figure 1.1) and emphasizes a logical flow for the treatment demonstration,
beginning with site and waste characterization and ending with submittal of
the demonstration results.
Section 1.3 of this chapter, a brief description of the general tech-
nical and administrative approaches to the demonstration, lays the founda-
tion for a more detailed discussion in Chapter 3 of various permitting
"scenarios" which incorporate certain technical and administrative
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approaches.
Chapter 2 describes the preliminary waste and site information (much
of which should already have been generated to meet the permit application
requirements of 40 CFR Part 270) that is necessary in selecting the appro-
priate treatment demonstration "scenario" and details preliminary data
needs in the following categories:
1) waste characterization, both general and specific to the
batches of waste to be used in the LTD; and
2) soil characterization, including a) a soil survey and chemical and
physical analyses and b) for existing sites, reconnaissance-level
sampling of the entire soil profile from the surface to six meters
(or the water table) and analysis to determine if degradation and
immobilization have been occurring effectively.
Once the preliminary information has been collected, the applicant
begins the decision-making process in coordination with the permitting
authority; the elements of this process are described in Chapter 3. The
specific LTD approach subsequently adopted by the applicant will be a
function of 1) how the facility conditions and records fit the possible
permitting scenarios; and 2) the applicant's preference among the various
technical options within each scenario.
Chapters 4 through 9 describe how to execute the various components of
the technical approaches and outline not only experimental methods, but
analysis and evaluation of the results as well. For example, as Figure 1.1
notes, the toxicity test is described in Chapter 5.
Chapter 10 describes a tiered sample analysis scheme. The objective
of this scheme is to minimize analytical costs during the demonstration by
providing for three levels of analysis depending on the particular data
needs. The scheme also specifies the minimum data requirements for each
tier.
Appendix A describes analytical methods for the chemical analysis of
soil (discussed in Chapter 2). Appendix B details installation methods
for barrel lysimeters. Appendix C provides guidance on frequently asked
questions on policy and technical aspects of the treatment demonstration.
1.3 APPROACHES TO THE LTD
The decision-making flow chart (Figure 1.1) described in Section 1.2
leads to four possible permitting scenarios which incorporate various
administrative permitting procedures and technical approaches. These ele-
ments are briefly introduced below.
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d
PRELIMINARY
INFORMATION
NEEDS
SELECTION AND
DESCRIPTION OF
TREATMENT
DEMONSTRATION
SCENARIOS
DESIGN
NO OPERA
CHANGES
NNE
FIG. I.I. TREATMENT DEMONSTRATION DECISION FLOW CHART.
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r
r
SCENARIO I
SCENARIO 2
SCENARIO 3
SCENARIO 4
ALTERNATIVE /
INTENSIVE
SITE DATA
COLLECTION
X^
1PPROACH
ISSUED PHASE 1
OF A TWO
PHASE PERMIT
A
7
s
LEFT UNDER
INTERIM
STATUS
STANDARDS
TEMPORARILY
SH
Tl
OEM
PEF
SHORT TERM
TREATMENT
IMONSTRATON
PERMIT ISSUED
TOXICITY
TEST
BARREL
LrSIMETER
STUDY
TOXICITY
TEST
FIELD
PLOT
STUDY
LYSIMETER
STUDY
TOXICITY
TEST
BARREL
LYSIMETER
STUDY
PERMIT ISSUED
TOXICITY
TEST
TWO YEAR
FOLLOW-UP
STUDY
TWO YEAR
FOLLOW- UP
STUDY
FIG. |.l. TREATMENT DEMONSTRATION DECISION FLOW CHART. (CONTINUED)
(NUMBERS IN BOXES REFER TO CHAPTERS)
4b
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1.3.1 Administrative Approaches
Land treatment differs from other hazardous waste management technolo-
gies in that, among other things, all land treatment units are required to
complete a treatment demonstration prior to obtaining a full-scale permit.
If, as the regulations allow, the applicant intends to use field or labora-
tory tests to make the LTD, these tests, which involve the treatment and
disposal of hazardous waste, can only be performed under a permit. Special
administrative procedures allow applicants to choose one of three permit
approaches, depending upon their circumstances:
1) an immediate full-scale facility permit;
2) a short-term treatment demonstration permit followed by a
full-scale facility permit; or
3) a two-phase permit.
Short-term and two-phase permits are described in 40 CFR 270.63. Table 1.1
outlines the essential elements of these permit approaches, and Table 1.2
briefly covers the content of applications for each of these types of
permits.
The full-scale facility permit is the "normal" permit used when com-
plete data is available to satisfy the treatment demonstration. In the
application for a full-scale facility permit, the applicant submits both
the treatment demonstration plan and its results and the other information
described in Table 1.2.
The short-term treatment demonstration permit, which authorizes small-
scale laboratory or field tests, contains only provisions necessary to meet
the general performance standards in §264.272(c) (See Table 1.2). An
applicant should apply for this permit when insufficient treatment informa-
tion exists to 1) fully satisfy the treatment demonstration for a full-
scale permit, or 2) establish preliminary permit conditions for the full-
scale facility in a two-phase permit. Normal permitting procedures, in-
cluding public comment and hearing, must be followed. After the lab or
field tests are complete, the applicant must apply for a full-scale
facility permit.
The two-phase permit is a combination of the short-term permit and
full-scale facility permit; Phase I of the permit includes conditions for
the treatment demonstration, and Phase 2 includes provisions for the full-
scale facility design and operation. This permit should be used in the
following circumstances: when substantial but incomplete treatment data
exist to satisfy the treatment demonstration, and when sufficient data are
available to determine the preliminary set of full-scale facility
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Table 1.1. Land Treatment Permit Elements
Full-Scale Facility Permit
- Used when complete data have been collected to satisfy the treatment
demonstration requirement (i.e., using available literature data,
operating data, and/or lab or field test results).
- Must contain provisions necessary to meet all the Subpart M, Part 264
requirements and all other applicable Part 264 standards.
- Requires public comment and hearing.
Short-Tern Treatment Demonstration Permit
- involves smai I-scale lab or field experiment to demonstrate that hazar-
dous constituents in waste can be treated in the land treatment unit.
- Used when insufficient "treatment" information exists to satisfy treat-
ment demonstration requirement for full-scale facility permits or to
establish preliminary Phase 2 (full-scale) conditions for two-phase
permit.
- Must contain only provisions necessary to meet the general performance
standards in §264.272(c).
- Requires public comment and hearing.
Two-Phase Permit
- Combination of above two permits when Phase 1 is for the treatment
demonstration and Phase 2 is for the full-scale facility design and
operation.
- Used when substantial but incomplete "treatment" data exists and when
sufficient data are not available to completely satisfy treatment demon-
stration but are avai 1 abl e to determine the prel iminary set of ful 1 -
scale facility permit conditions.
- Used when Phase 1 and 2 permits are based on substantial but incomplete
information; Phase 2 permit is modified to the incorporate results of
Phase 1.
- Avoids the burden of two separate permitting procedures (e.g., only one
public comment and hearing is necessary rather than two).
- Contains provisions necessary to meet treatment demonstration (Phase 1);
contains provisions to meet all applicable Part 264 standards (Phase 2).
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Table 1.2 Permit Application Content for Each Permit Element
Full-Scale Facility Permit
- Information addressing the general standards applicable to all facili-
ties - §270.14, "General Information Requirements" (see Permit Appli-
cant's Guidance Manual for General Facility Standards).
- Information requirements of §270.20 addressing the Subpart M, Part 264
requirements
— Treatment Demonstration Plan and Results
— Land Treatment Program
— Design and Operating Requirements
— Food Chain Crops
-- Closure and Post-Closure Care
— Ignitable and Reactive Waste
-- Incompatible Wastes
- Information addressing the groundwater protection requirements in
Subpart F, Part 264.
Short-Term Treatment Demonstration Permit
- Treatment demonstration plan including provisions to meet the
§264.272(c) performance standard.
- Results submitted to the Regional Administrator at end of study and as
part of full-scale facility permit application.
Two-Phase Permit
- Same as full-scale facility permit except that the results of the treat-
ment demonstration are submitted after completion (Phase 1).
conditions. For the two phase permit, the applicant submits the same
information as for the full-scale facility permit, except that the results
of the treatment demonstration (Phase 1) are submitted at a later date.
Thus, the permitting official first writes a draft permit for Phases 1 and
2 and then, after the treatment demonstration results are submitted,
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modifies the Phase 2 Permit. The primary advantage of the two-phase permit
is that it eliminates the need for two separate permitting procedures, one
for the treatment demonstration and one for the full-scale facility permit.
For existing land treatment units with interim status, a final ap-
proach for completing treatment demonstration field tests under a permit is
available. Because permittees' interim status facilities are "treated as
though they have been issued permits" (while awaiting completion of the
Part 264 permitting process), field tests on hazardous wastes currently
handl ed at the faci 1 i ty may be conducted at these uni ts. However, these
tests must not be carried out in a manner that will lead to a to violation
of the Part 265 interim status standards. If the tests are likely to
violate the interim status standards, one of the special permits described
above (short-term or two-phase) must be obtained.
In summary, an applicant who can complete the treatment demonstration
based on available literature data or operating data from an existing
interim status 1 and treatment unit may apply directly for a ful 1 -seal e
facility permit. An applicant who must use laboratory or field studies to
complete the treatment demonstration, however, has two options depending
upon the amount of data al ready avai 1 abl e. He may 1) apply for a short-
term treatment demonstration permit and then a full-scale facility permit;
or 2) apply for a two-phase permit. In addition, field studies in com-
pliance with the Part 265 standards may be completed at an interim-status
land treatment unit.
The four permitting scenarios briefly described in Section 1.2 incor-
porate one or more of these administrative approaches. However, the choice
of which permitting scenario to use depends on a relatively complex set of
criteria which, along with the practical implementation of the chosen
permitting scenarios, is the subject of Chapter 3.
1.3.2 Technical Approaches
While three general technical approaches to performing a land treat-
ment demonstration are explained in this document, the approach which is
chosen and how it fits into the various permitting scenarios will vary
depending upon the applicant's circumstances (see Chapter 3). These tech-
nical approaches are as follows:
1) Use of existing operating data, supplemented with intensive
site data collection.
2) A one year field plot or "barrel lysimeter" study, followed
by a short-term laboratory toxicity test.
3) A short-term laboratory toxicity test with a one year field
plot or "barrel lysimeter" study, followed by the laboratory
toxicity and a two-year follow-up field study.
Although the Part 264 regulations allow the use of existing literature
data to complete the demonstration, this approach is not considered as a
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viable option at this time because of the lack of detailed site-specific
data available in literature. To be useful, literature data must have been
generated under conditions similar to those at the proposed unit and must
include information on the fate of specific hazardous constituents (i.e.,
Appendix VIII compounds) present in the waste. Although it may assist in
the design of laboratory and field tests, literature data alone rarely
satisfies the treatment demonstration fully. In the future as the data
base improves, literature data may be more useful.
The first technical approach, the use of existing operating data
supplemented with intensive site data collection, is the most straightfor-
ward and economical method for the demonstration. Further, comprehensive
field data from the operational HWLT unit is considered to be the best
approximation of reality (i.e., the best demonstration of treatment). This
approach consists of both tabulation and evaluation of existing operating
data and high density soil core sampling and analysis from the surface to
six meters (about 20 ft) to confirm treatment of hazardous constituents.
The use of waste analysis data and past records in conjunction with soil
core data should demonstrate that degradation of organics has been occur-
ring with no unacceptable leaching or build-up of hazardous constituents.
The major limitations of this method, which may be used in select cases and
only for existing units, are the requirements for several years of operat-
ing data and records and relatively consistent past and projected opera-
tions. Criteria for deciding if an HWLT unit qualifies for this technical
approach are discussed in Section 3.1.
Except for those well run and documented existing HWLT units that
qualify for the above approach, all new or existing units must adopt one of
the other two technical approaches; the criteria for determining which HWLT
units qualify for these approaches are also discussed in Section 3.1. The
second general approach consists of a one year field plot study or a
"barrel lysimeter" study. Technically, since these two options are
parallel in design and in the information obtained, the applicant may
select either option. The field plot study, which follows the traditional
agricultural type study, involves several small scale plots, subject to the
variability of soils and climate and to concerns such as plot fringe ef-
fects. The second option in the approach is the "barrel lysimeter" study,
which is conducted on large undisturbed soil monoliths or columns collected
(e.g., in 55 gallon drums) from the field. All degradation, transforma-
tion, and immobilization testing takes place in these barrel sized "lysi-
meters". (NOTE: In this document, "lysimeter" refers to the large undis-
turbed soil monoliths; the porous ceramic or pan devices used to collect
soil-pore liquid are called "soil-pore liquid samplers". This is consis-
tent with the use of the term "lysimeter" in soil physics terminology.)
Field plots and, in most cases, lysimeter studies must continue for no less
than one year. Acute toxicity testing is then used as a follow-up to help
set final waste loading rates.
The third general approach includes a laboratory acute toxicity test,
followed by a one year field plot or barrel lysimeter study, a repeated
laboratory toxicity test, and a two-year follow-up study. This approach,
using a short-term test to determine initial waste application limits for
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the demonstration, is employed in instances where little information exists
on the treatability of a waste (see Chapter 3). After the one-year field
plot or barrel lysimeter study has been conducted, further acute toxicity
testing to determine tentative design criteria leads to a final two-year
follow-up field study, usually on the full-scale operational unit, to
confirm the findings of the laboratory and small scale testing.
The choice of the specific technical approach and the particulars
involved are a function of many factors, including the facility's operating
record under interim status regulations, technical factors, and, to some
degree, applicant preference. The criteria involved and all of the pos-
sible LTD permitting scenarios (which incorporate both administrative and
technical approaches) are described in Chapter 3.
Chapter 2 specifies the preliminary information for the demonstration
that is necessary for all applicants. Chapter 3 then assists the applicant
through the LTD decision-making process.
1.4 OTHER SOURCES OF INFORMATION
Whenever possible, this document avoids lengthy commentary and techni-
cal explanations and attempts to provide the applicant with a clear set of
usable instructions. In some sections, however, the reader is referred to
one or more of the available treatises on land treatment (Table 1.3) for
additional explanation.
Table 1.3 Selected References on Land Treatment
Hazardous Waste Land Treatment SW-874 (EPA, 1983) or
Brown et al., 1983
RCRA Part 264 Guidance Document: EPA, Draft, May, 1983B
Land Treatment
Permit Applicants' Guidance Manual EPA, 1984B
for Hazardous Waste Land Treatment,
Storage, and Disposal Facilities
Unsaturated Zone Monitoring for Haz- EPA, 1984A
ardous Waste Land Treatment Units
Design of Land Treatment Systems for Overcash and Pal, 1979
Industrial Wastes-Theory and Practice
10
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Chapter 2
PRELIMINARY INFORMATION NEEDS
Before the land treatment demonstration can begin on either an exist-
ing or a new treatment unit, detailed information about the waste and site
must be generated. This information should already have been gathered to
fulfill the Part 270 requirements for the Part B permit application. In
particular, an in-depth soil characterization and mapping should have been
conducted. Waste analyses should have characterized the waste streams
(both hazardous and nonhazarous) to be land treated and to be used in the
treatment demonstration. For existing units, the preliminary information
should also include chemical characterization of both the waste/soil mix-
ture in the active area of the unit and the soil below the treatment zone.
This chapter summarizes the Part 270 data requirements applicable to
treatment demonstration planning and provides additional guidance to the
applicant where necessary. This discussion supplements the guidance pro-
vided in the Permit Applicants Guidance Manual for HWLTSD Facilities (PAGM)
(EPA, 1984A) with some specifics on how to gather the information suggested
by the PAGM.
2.1 SOIL CHARACTERIZATION
A basic understanding of the potential for successful degradation,
transformation, or immobilization of a waste involves an understanding of
the site's physical, chemical, and biological properties. Much of this
information (e.g., hydrogeology, topography, and climate) should have al-
ready been determined to fulfill the Part 270 information requirements for
Part B of the permit application. Critical to the treatment demonstration
is a thorough understanding of the soil that will be the treatment medium
for the waste. Therefore, an in-depth study of the soil as outlined in
this section is necessary.
Since soil is the treatment medium for the HWLT, a thorough analysis
of the soil is necessary to develop a data base for any of the technical
approaches to the LTD outlined in this protocol. This analysis will iden-
tify any limiting conditions that may restrict the use of the site as an
HWLT unit and will provide an indication of whether waste constituents are
building up to undesirable concentrations or leaching out of the treatment
zone. The major components of interest are the variations in physical,
chemical, and biological properties of the soil (EPA, 1982) and the area!
and vertical distribution of waste constituents in the soil.
Information on soils in the treatment zone is an important element of
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the Part 270 information requirements for HWLT units. Section 270.20(a)(3)
requires that the Part B permit application for land treatment units out-
line the treatment demonstration plan. This plan must provide, among other
things, a description of the characteristics of the unit that will be
simulated in the demonstration, including treatment zone characteristics,
climatic conditions, and operating practices. Also, §270.20(b)(5) requires
that the land treatment program identify the proposed dimensions of the
treatment zone. Finally, §270.20(c) requires a description of how the unit
is or will be designed, constructed, operated, and maintained in order to
meet the requirements of §264.273. Guidance on these information require-
ments is provided in Section 7.4.3.7 of the PAGM. The following discussion
offers more detailed guidance on the type of soils information that should
be gathered.
2.1.1 Soil Survey
A soil survey, commonly done for soil characterization, should already
have been conducted for the permit application according to PAGM guidance.
Many areas have already been broadly surveyed by the Soil Conservation
Service (SCS). If such a survey exists for a given site, it may be used as
a guide. However, an existing SCS survey, unless done specifically for the
site, cannot be used as a substitute for a detailed site-specific survey
and sampling program because the scale used to conduct the SCS surveys is
too large, analyses are too few, and often they do not include all of the
pertinent parameters. If an acceptable soil survey conducted by a quali-
fied soil scientist has not been done, a soil scientist should be retained
to conduct the soil survey.
2.1.1.1 Conducting the Soil Survey--
In a soil survey, the soil series present at a given site are identi-
fied and sampled. Samples obtained for the soil survey should be collected
at random at a rate of at least four per acre for the HWLT site. Sampling
depth will vary depending upon the soils present at the site. Charac-
terization of waste distribution in soils requires a more detailed and
carefully controlled sampling program than is needed for the soil survey
(Section 2.1.1). Soil series, generally varied from one location to
another, are differentiated on the basis of both physical and chemical
characteristics. The soil survey should include soil profile descriptions,
mineralogy, use and vegetation, and estimated soil properties: perme-
ability, flood frequency and duration, and frost action potential. The
following information, which is included in SCS surveys, should also be
included in surveys of HWLT units: 1) estimates of credibility of the
soil, which are used to calculate terrace spacings and other erosion con-
trol structures, 2) information on the depth and texture of surface hori-
zons and subsoils, which is used to determine if the soil is suitable for
contaminant attenuation and for constructing berms and lined run-off reten-
tion ponds, and 3) depths to seasonal high water table and zones such as a
fragipans that limit vertical water movement.
Surveying the soils of a proposed or even an existing site will help
define "uniform areas" of the treatment unit as well as identify any poten-
12
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tial problem areas such as small inclusions of sandy materials with high
permeability. Uniform area is defined as an area of the active portion of
a HWLT unit composed of soils of the same soil series to which similar
wastes are applied at similar rates. Two different soil series may be
included in a given uniform area if a qualified soil scientist certifies
that the characteristics that differentiate the soil series will not have
any affect on success of land treatment (see Question #11 in Appendix C).
For new units, the soil within the confines of the proposed land
treatment unit (i.e., within the boundaries defined by the run-on/run-off
control structures) should be surveyed along with background soils (i.e.,
untreated soils outside the boundaries). While the same process should be
followed for existing units, difficulties are often encountered as the
result of waste additions and drastic disturbances that may have signifi-
cantly altered active area soil properties. If a definable native soil
still exists, the soil survey must emphasize deeper sampling and a greater
use of test pits to identify the soil series present, their boundaries, and
their continuity with background areas. In some cases, no native soil will
be present or identifiable. Nevertheless, the soil survey should be con-
ducted according to the guidance in this manual and in the PAGM. The soil
scientist should use this information to assist the owner/operator in
determining "uniform areas."
2.1.1.2 Analysis of Samples Obtained in the Soil Survey--
Numerous samples should be obtained during the course of the soil
survey. Regardless of whether these soil samples are background or from
active areas, a number of analyses are needed to characterize their chemi-
cal and physical properties. The following sections list the parameters of
concern, and Appendix A includes analytical procedures that may not be
widely employed by typical water, waste, and sediment laboratories. Such
methods are, however, standard soil procedures used by soils laboratories
and are suggested to ensure reliable results. Initially, only enough
samples should be analyzed to determine sample variance. If the variance
is large, all samples may need to be analyzed to establish the spatial
variability of the soils.
2.1.1.2.1 Soil Physical Properties—Soil physical properties, defined
as those characteristics, processes, or reactions of a soil caused by
physical forces, are described by physical terms or equations. Measure-
ments of physical properties should include particle size distribution,
bulk density, and moisture retention (i.e., available water capacity). For
an in-depth discussion of these properties the applicant should refer to
Hazardous Waste Land Treatment (EPA, 1983A). Specific analytical proce-
dures for measuring these parameters are listed in Appendix A of this
protocol.
2.1.1.2.2 Soil Chemical Properties—Chemical reactions that occur
between waste constituents and the soil must be considered in land treat-
ment demonstrations. Large numbers of complex chemical reactions and
transformations, including exchange reactions, sorption, precipitation, and
complexing, occur in the soil. Understanding the fundamentals of soil
13
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chemistry and the soil components that control these reactions makes it
possible to predict the fate of a particular waste in the soil. Chemical
properties that need to be evaluated are cation exchange capacity, total
organic carbon, nutrients (pertinent non hazardous constituents that may
affect treatment), electrical conductivity, pH, and buffering capacity.
Each of these soil chemical parameters is discussed in detail in EPA (1983)
and in Methods of Soil Analysis (Black, 1965). Analytical procedures for
each of these parameters are included in Appendix A.
2.1.1.2.3 Soil Biological Properties—The soil provides a suitable
habitat for a diverse range of organisms that may help render a waste less
hazardous. The types and numbers of decomposer organisms present in a
waste-amended soil depend on soil moisture content, available oxygen, and
nutrient composition.
Following the land application of a waste, the population establish-
ment of decomposer organisms begins with bacteria, actinomycetes, fungi,
and algae (Dindal, 1978), organisms which have diverse enzymatic capabili-
ties and can withstand extremes in environmental conditions. While enum-
eration of species and numbers of microbes is not necessary in site char-
acterization, a recognition of the importance of these organisms and their
role in the waste treatment process is critical. Indeed, management of the
unit should be designed to manipulate environmental factors to enhance the
activity of these decomposer organisms. A more in-depth discussion of
soil organisms is given in Hazardous Waste Land Treatment (EPA, 1983A) and
Introduction to Soil Microbiology (Alexander, 1977).
2.1.2 Reconnaissance Characterization of Waste Constituent Distribution in
Soil(Existing or previously contaminated sites only)
Regardless of the LTD approach for existing units, reconnaissance data
collection is required to determine: 1) if hazardous constituents have
moved below the defined treatment zone; 2) if so, how far they have moved;
and 3) if degradation, immobilization, and/or transformation are occurring
within the treatment zone. If hazardous constituents have leached below the
bottom of the treatment zone, secondary information on soil drainage class
and HWLT site topographic location (e.g., toe of slope versus top of slope)
will assist in decision-making. These data are collected through analysis
of soil cores and soil-pore liquid samples from both the HWLT unit and
background soil.
2.1.2.1 Soil Cores-
Waste constituents may move slowly through the soil profile for a
number of reasons, a few of which are: 1) lack of sufficient soil moisture
to leach rapidly through the system, 2) a natural or artificial layer or
horizon of low hydraulic conductivity, or 3) waste constituents that ex-
hibit only low to moderate mobility relative to soil water. Soil core
monitoring can identify any one or a combination of these effects, and deep
coring can determine if long-term movement of contaminants is occurring.
The intent of such monitoring is to demonstrate whether significantly
higher concentrations of hazardous constituents are present and moving in
14
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the material below the treatment zone than in background soils. The
applicant should refer to the guidance on soil sampling procedures and
equipment provided in EPA (1984A) but should be aware that if a shelby tube
or spl it spoon sampler is used, at least 75% sample recovery per push is
expected. Should unacceptable recovery occur, the depth increment per push
should be reduced.
2.1.2.1.1 Depth—The soil core should reach a depth of six meters or
just into the top of the first aquifer (not merely perched water), which-
ever distance is less. After samples of the zone of incorporation are
taken, that zone should be removed to avoid contamination of lower hori-
zons. Within the following zones, each boring may be composited with
depth: 0-15 cm, 15-45 cm, 45-90 cm, 90-150 cm, 150-200 cm, 200-250 cm,
250-400 cm, and 400-600 cm.
2.1.2.1.2 Area! Distribution--Whi le the soil series delineates the
domain of each set of soil samples, the location of each sample point
within the domain of each soil series is determined randomly. In addition
to the random sampling points, locations which represent "hot spots"
within an HWLT unit should also be sampled and should possibly be analyzed
separately. These "hot spots", which may include but are not limited to
toe slope positions, are important for soils with an hydraulical ly restric-
tive lower horizon that may cause primarily lateral movement of soil-pore
liquid with subsequent accumulation at the base of the slope. Other pos-
sible hot spots include swales on the treatment plots or waste dumping
locations adjacent to roadways, areas where greater than average amounts of
waste could accumulate. This soil series-specific sampling approach as-
sumes that only one waste is being treated at the site. If more than one
waste is being treated, the domain of each randomly selected sample set
will be the "uniform area", defined as an area of the active portion of an
HWLT unit composed of soils of the same soil series to which similar wastes
or waste mixtures are applied at similar rates.
2.1.2.1.3 Number of Samples--There should be a minimum of six soil
cores per uniform area of active treatment zone at a density of one soil
core per two acres. Background soil cores must be collected at a density
of four for each soil series that occurs on the HWLT unit. Background
should be considered the area just outside of the HWLT unit, not necessari-
ly an undisturbed, pristine area. Samples should represent the conditions
of this background area and not be selected in a biased fashion that would
lead to unreal istical ly low or high concentrations of hazardous consti-
tuents. If high concentrations of hazardous constituents in the background
are found, the fact should be reported to the permitting official.
2.1.2.1.4 Analysis of Soil Core Samples—At this point in the site
characterization, samples must be analyzed rigorously (Tier III, Chap-
ter 10). Such rigorous analysis, necessary to provide information about
all Appendix VIII constituents that may be present and therefore must be
monitored throughout the life of the HWLT unit. The hazardous constituents
may be those present at the time of waste application or other degradation
products not originally in the waste. Because this level of analysis is
not required under interim status standards (40 CFR 265), the applicant
15
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does not usually possess data about all possible hazardous constituents.
Data acquired by soil core sampling could also help to determine the degra-
dation rate of applied waste.
following stepwise approach to selecting and compositing samples
'sis should be followed to conserve analytical costs while main-
The
for analysi
taining the integrity of the data:
1) After splitting each sample increment and reserving a portion
for possible later use, composite the 0-15 cm zone with the
15-45 cm zone for each core. Do likewise with the 45-90 cm,
and 90-150 cm zones, and the 200-250 cm, 250-400 cm, and 400-
600 cm zones. Four depth increments wi11 resul t: 0-45, 45-
150, 150-200, and 200-600 cm. Next, composite all four
background cores for each soil series to form one sample set
per series. In the active area, compositing should be done
to yield three composite sets per uniform area. (For ex-
ample, if there is only one uniform area at the land treat-
ment unit, the compositing will yield three active area
sample sets and one background sample set, with each set
consisting of four depth increments.) Next, analyze these
samples at the Tier III level.
2) If any or all of the background sample increments are free of
hazardous organic constituents (i.e., below detection
limits), corresponding active area depth increments that are
similarly free of hazardous organics may be eliminated from
further consideration. If any background depth increment
does indicate the presence of hazardous organics, al 1 four
background cores per soil series at that depth should be
analyzed separately at the Tier II level for only those
constituents that were identified in the initial analysis.
This approach is necessary to determine the variability and
distribution of the hazardous constituents across the back-
ground area. Once the background samples show no hazardous
organics or analyses are begun to determine the mean and
variance in background samples, appropriate active area sam-
ples can be selected for analysis. For only those depth
increments on the active area that yiel d concentrations of
hazardous constituents greater than background, samples from
every core should be analyzed at the Tier II level and should
include those constituents that were present at greater than
background concentrations.
3) Finally, if greater than background concentrations of hazar-
dous constituents are found at a given depth, the depth
increments that were composited to form the increment ana-
lyzed should now be analyzed separately at Tier II. Simi-
larly, any "hot spot" should be analyzed by individual sam-
pling depths. In some cases, resampling and Tier II analysis
of "hot spots" may be needed (a) to confirm that the initial
core samples were not subject to cross contamination from
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other depths and/or (b) to determine the extent of the "hot
spot".
2.1.2.1.5 Interpretation of Soil Core Sample Data-in the analysis of
the data collected under this section, sound statistical principles should
be used. A land treatment unit should be designed and operated such that
no vertical movement of significant quantities of hazardous constituents
occurs below the treatment zone. Thus, the following null hypothesis
should be tested: the population means are equal (H: i = 2» A: 1 2^*
The key to valid comparison between these populations is the choice of
sample size (number of replications) and the use of random sampling. The
reconnaissance sampling program indicated here meets the requirements for a
good statistical design and is therefore well suited to interpretation
using the "t" statistic. A step-by-step procedure for statistical inter-
pretation of the data is presented in UZM Manual (EPA, 1984A).
The results of the statistical interpretation will help to provide the
basis for a decision on the appropriate LTD permitting approach (described
in Chapter 3). Specifical ly, this data assists the permit writer in an-
swering the question: "Is the design and operation acceptable?" (see
Figure 3.1). Also, if 1) a hazardous constituent has been found below the
treatment zone or 2) an unacceptable degree of degradation of the waste
organics fraction or specific hazardous organic constituents or an unac-
ceptable build-up of conservative constituents (e.g., metals) has occurred
in the zone of incorporation, the permit writer and applicant will need to
address the following questions:
1) Is the site permittable? That is, does an environmentally
damaging situation exist for which no remedial action can be
taken other than site closure?
2) If the site is not permittable, what are the waste management
alternatives?
3) If the site is permittable, what is the plan for remedial
action to clean up the contaminated area?
Acceptable "degradation" (loss by some means) is defined as at least 80%
loss of the total (organic fraction or constituent) waste applied over the
facility life and no more than twice the concentration of an organic con-
stituent in the ZOI (0-15 cm) than the concentration applied annually to
the soil. For inorganics criteria, consult EPA (1983A). It should be
noted that because all of these decisions involve contact with the EPA or
the State, they are beyond the scope of this document.
2.1.2.2 Soil-Pore Liquid-
Percolating water added to the soil by precipitation, irrigation, or
waste applications may pass through the treatment zone and rapidly tran-
sport some mobile waste constituents or degradation products through the
unsaturated zone to the groundwater. Soil-pore liquid monitoring is in-
tended to detect these rapid pulses of contaminants that occur immediately
17
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after heavy precipitation and that are not likely to be observed through
the analysis of shallow soil core samples. Therefore, the timing (sea-
sonal ity) of soil-pore liquid sampling is essential to the usefulness of
this technique (i.e., scheduled sampling cannot be planned on a preset
date, but must be coordinated with precipitation). Soil-pore liquid sam-
pling in the reconnaissance site evaluation is used to determine if any
mobile hazardous constituents are leaving the treatment zone. However,
existing monitoring data may suffice if samples have already been analyzed
at the Tier III level (to include Appendix VIII constituents).
Since interim status standards require the installation and use of
soil-pore liquid sampling equipment, data concerning the status of soil-
pore liquid below the treatment zone may already exist. However, if these
data do not include all of the parameters of concern in the LTD and in
future management and monitoring, an applicant with presently operational
soil-pore liquid samplers should collect current samples and analyze them
at the Tier III level (See Chapter 10). For sites without soil-pore liquid
samplers or with samplers that are not functioning, the reconnaissance site
evaluation will be based on soil core data only. If soil-pore liquid
samplers have been installed but are not functioning effectively, possible
reasons for their failure (e.g., improper installation, mechanical
failures, installation in a soil horizon which has a low hydraulic conduc-
tivity, such as a fragipan) should be investigated. The applicant should
note that lack of compliance with Part 265 soil-pore liquid monitoring may
affect the allowable permitting scenario (see Section 3.1.2) as well as
expose the operator to possible enforcement action. For more detailed
discussion of soil-pore liquid samplers see Chapter 7 and EPA (1984A).
2.2 WASTE CHARACTERIZATION
A demonstration of the land treatability of a given waste must na-
turally begin with waste characterization. Only after the thorough charac-
terization of a waste has been completed can an appropriate LTD can be
conducted, since comprehensive waste analytical data are needed to identify
and quantify the hazardous constituents contained in the waste. If signi-
ficant concentrations of hazardous and organic constituents are present,
the analytical procedures throughout the course of the LTD must necessarily
be more extensive (i.e., analyses for many of the 40 CFR 261, Appendix VIII
compounds versus gross parameters such as total oil and grease). The
converse also may be true: thorough characterization may allow the elimi-
nation of certain analytical procedures throughout the course of the LTD
(see Chapter 10).
The general Part B information requirements specified under §270.14(b)
require the submittal of 1) chemical and physical analysis data on the
hazardous wastes to be handled at the facil ity, including al 1 data that
must be known to treat, store, or dispose of wastes properly in accordance
with Part 264, and 2) a copy of the waste analysis plan. In addition, the
specific information requirements under §270.20 require an owner/operator
of any facility that includes a land treatment unit to submit "a 1 ist of
hazardous constituents reasonably expected to be in, or derived from, the
18
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wastes to be land treated based on waste analyses performed pursuant to
§264.13. Finally, §270.20{a) stipulates that the description of the
treatment demonstration plan must include a list of potential hazardous
constituents in the waste.
Although the PAGM provides general guidance on waste analyses for land
treatment permit applications, information presented in this manual may
further aid the applicant in determining what is expected of the waste
characterization. One key point is that the program of routine, broad
scale waste characterization done for the Part B only partially fulfills
the LTD data needs. More importantly for the LTD, representative waste
batches must be obtained and characterized in detail if an experimental
(i.e., lysimeter or field plot) demonstration is planned. If the waste for
the LTD can be conveniently obtained at the time of sampling for general
waste characterization, one set of analyses may suffice for both purposes.
Although a treatment demonstration is not required for land treatment
of a nonhazardous waste, the presence of nonhazardous waste within the same
treatment zone as the hazardous waste will affect the treatment of the
hazardous waste. Therefore, in instances where nonhazardous wastes are
disposed/treated within the same treatment zone as the hazardous waste, a
detailed characterization of the nonhazardous waste (including Appendix
VIII hazardous constituents) must also be provided. Of course, the appli-
cant has the option of segregating the hazardous and nonhazardous wastes at
the land treatment unit, and thus avoid being subject to the nonhazardous
waste characterization.
The characterization phase is also important in identifying possible
capacity limiting constituents (CLC), often metals, and application limit-
ing constituents (ALC). These constituents will be positively confirmed
according to data subsequently obtained from the LTD. The limiting levels
for the CLCs will depend partially on the closure method employed at the
HWLT unit. For a thorough discussion on CLCs and ALCs, the applicant
should refer to Chapter 7 of Hazardous Waste Land Treatment (EPA, 1983A).
2.2.1 Sampling
Sampling of waste is to be conducted in accordance with good scienti-
fic methods to ensure that accurate, representative samples of the waste
are obtained. Specific amounts needed for analysis and use in the field
plot study or lysimeter study depend on the treatment demonstration chosen
and on whether an existing site is being used for demonstration of a
waste's treatability. The applicant should refer to the appropriate sec-
tions of this document when estimating amounts of wastes required to carry
out the respective treatment demonstration approaches.
2.2.2 Sample Collection
A representative sample of the waste to be applied must be collected
for characterization and use in the LTD. Because waste uniformity and
variability always present a problem in treatment demonstrations, all
samples should be collected using sampling and compositing procedures
19
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prescribed by EPA (1982). In some complex waste generating situations,
sampling may need to be carried out over a period of months to produce a
representative set of samples (e.g., due to intermittent waste generation
or seasonal variability). To decrease the analytical burden, the quantity
of waste to be used in the treatment demonstration could in some cases be
collected and stored at the time of sampling for overall waste stream
characteri zati on.
2.2.3 Sample Handling and Storage
Al 1 sampl ing equipment should be thoroughly clean and free of con-
tamination both prior to use and between samples; storage containers should
be similarly free of contamination. While only plastic or Teflon" may be
used for samples intended for inorganic analysis, glass, Teflon1" or stain-
less steel may be used for samples intended for organic analysis. Care
should be taken that both the samples and storage container materials are
not reactive with the waste. Also, if the sample is to be frozen in
storage, ample room for expansion must be provided in the sample container.
Following sampling operations, all samples should be tightly sealed
and preserved at 4°C, unless known characteristics require other preserva-
tion methods. Although other methods should be avoided for wastes col-
lected for the LTD to prevent bias in the LTD results, freezing may be
required when organic constituents are expected to be lost through volati-
lization; this may be easily accomplished by packaging all sealed sample
containers in dry ice directly after collection if other refrigeration
methods are not immediately available. The applicant should make prior
arrangements with the receiving laboratory to ensure sample integrity until
the time of analysis. Since storage of large waste volumes for the LTD may
present problems in terms of qualitative and quantitative waste integrity,
the applicant should strive to minimize storage time.
2.2.4 Sample Analysis
Necessary physical and chemical analyses of waste are listed in the
following table. The procedures used to determine these waste properties
should be those approved by EPA. These methods are described in EPA
(1983A) and Test Methods for Evaluating Solid Waste (SW-846) (EPA, 1982).
20
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Table 2.1 Physical and Chemical Analyses of Wastes
Water Content
Solids Content
Ash Content
Soluble Salts*
Nitrogen Series*
Phosphorus Series*
pH .
Metals (total concentration and not EP toxicity data)'
Total Organic Carbon
Total Oil and Grease
Volatile Organics (by purge and trap)
* Pertinent nonhazardous constituents that may affect treatment.
t Includes hazardous and important nonhazardous metals beyond merely those
for which a waste is listed as hazardous.
2.2.5 Appendix VIII Constituents
In addition to the general parameters outlined above, Appendix VIII
(40 CFR 261) constituents present must be identified and quantified accord-
ing to procedures approved by the EPA (1982). Where wastes handled at a
facility are from an identified process (e.g., petroleum refinery
processes), EPA may accept analysis performed on a subset of Appendix VIII
compounds which are "reasonably expected to be in or derived from the
wastes to be land treated" (see §270.20). Such a subset, developed by EPA
for wastes from petroleum refineries, is included in Table 2.2.
The list of hazardous constituents suspected to be present in refinery
wastes (Table 2.2) was derived from a review of data on petroleum refinery
wastewater and sludge characteristics from the following sources: 1)
literature, particularly EPA research reports; 2) in-house waste analyses
completed by EPA research laboratories; 3) preliminary data from the Office
of Solid Waste (EPA) refinery waste study; and 4) an evaluation of petro-
leum refinery processes. Although the above sources were used, the data
base on specific hazardous organic constituents in sludges was still
limited. Considerable emphasis was placed on wastewater data as indicators
of sludge characteristics (e.g, API separator sludge).
Table 2.2 is a generic list developed by combining waste analysis data
on all five listed refinery wastes (K048-K052). Due to the lack of exten-
sive data, however, no attempt was made to differentiate between the char-
acteristics of these five refinery wastes. Until sufficient information is
available to allow development of separate lists for each waste, the
attached list should be considered applicable only to dissolved air flota-
21
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tion float (K048), slop oil emulsion solids (K049), heat exchanger bundle
cleaning sludge (K050), API separator sludge (K051), and leaded tank bot-
toms (K052).
To compensate for the limited data base and variability among re-
fineries, the attached list is purposely comprehensive; it includes a total
of 89 hazardous constituents or groups of constituents (e.g., trichloro-
benzenes), all of which have been identified as possibly present in the
above-referenced wastes. Many of the compounds on the list may be present
at low concentrations, and others may not be present at all in certain
wastes at some refineries.
Permit writers use the attached list as a guide to the Appendix VIII
constituents that should be addressed in the preliminary waste analyses and
waste analysis plans for Part B applications that propose land treatment of
petroleum refinery wastes. A permit applicant may further refine this list
by providing detailed evidence that certain hazardous constituents cannot
be present in the listed wastes at that particular refinery. In most
cases, however, waste analysis data on the constituents listed in Table 2.2
is necessary to demonstrate such a claim. [An interpretative note about
volatiles: Although current regulations and guidance do not include moni-
toring or interpretations of air emissions, waste analysis calls for data
on the waste volatiles fraction. The major point to be emphasized about
this data is that wastes containing large concentrations of volatile hazar-
dous constituents (e.g..greater than 0.5%) may not be amenable to land
treatment unless applied at very low concentrations, by the correct method,
and under favorable soil conditions. Since the atmosphere could be the sink
for such constituents if they are not applied and managed properly in the
soil, LTD studies should be specifically designed to show that degradation
rather than volatilization is the primary loss mechanism.]
22
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Table 2.2 Hazardous Constituents Suspected to be Present in Refinery
Wastes
Acetonitrile' (Ethanenitrile)
Acroleiiy (2-Propenal)
Acrylonitri1e' (2-Propenenitri1e)
Aniline (Benzenaraine)
Antimony
Arsenic
Barium
Benz (c) acridine (3,4-Benzacridine)
Benz (ai anthracene (1,2-Benzanthracene)
Benzene" (Cyclohexatriene)
Benzenethiol (Thiophenol)
Benzidine {l,l-Biphenyl-4,4 diamine)
Benzo(b)fluoranthene (2,3-Benzofluoranthene)
Benzo (j) Fluoranthene (7,8-Benzofluoranthene)
Benzo(a)pyrene (3,4-Benzopyrene)
Benzyl chloride* (Benzene, (chloromethyl)-)
Beryl1i urn
Bis (2-chloroethyl) ether (Ethane, 1,1-oxybis (2-chloro-)
Bis (2-chloroisoprqpyl) ether (Propane, 2,2-oxybis (2-chloro-))
**
Bis (2-ethylhexyl) phthalate (1,2-Benzenedicarboxylic acid, bis (2-
ethylhexylJester
Butyl benzyl phthalate (1,2-Benzenedicarboxylic acid, butyl phenylmethyl
ester)
Cadmium
Carbon disulfide (Carbon bisulfide)
p-Chloro-m-cresol
Chlorobenzene (Benzene, chloro-)
Chloroform* (Methane, trichloro-)
Chloromethane* (Methyl chloride)
2-Chloronaphthalene (Naphthalene, beta-chloro-)
2-Chlorophenol (Phenol, o-chloro-)
Chromium
Chrysene (1,2-Benzphenanthrene)
Cresols (Cresylic acid) (Phenol, methyl-)
Crotonaldehyde* (2-Butenal)
Cyanide
Dibenz(a,h)acridine (1,2,5,6-Dibenzacridine)
Dibenz(a,j)acridine (1,2,7,8-Dibenzacridine)
Dibenz(a,h)anthracene (1,2,5,6-Dibenzanthracene)
7H-Dibenzo(c,g)carbazole (3,4,5,6-Dibenzcarbazole)
Dibenzo(a,e)pyrene (1,2,4,5-Dibenzpyrene)
Dibenzo(a,h)pyrene (1,2,5,6-Dibenzpyrene)
--continued--
23
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Table 2.2 Continued
•«WM-WBW—MMW^^H^^WHWWWall-"M*MWH-W--W---M---W»^H*IWMIWWaMW>-
Dibenzo(a,i)pyrene (1,2,7,8-Dibenzpyrene)
1,2-Dibromoethane* (Ethylene dibromide)
Di-n-butyl phthalate (1,2-Benzenedicarboxylic acid, dibutyl ester)
Dichlorobenzenes*
1,2-Dichloroethane (Ethylene dichloride)
trans-l,2-Dichloroethane" (Ethylene dichloride)
1,1-Dichloroethylen' (1,2-Dichlorethylene)
Dichloromethanej (Methylene chloride)
Dichloropropane*
Dichloropropanol
Diethyl phthalate (1,2-Benzenedicarboxylic acid, diethyl ester)
7,12-Dimethyl-benz(a)anthracene
2,4-Dimethylphenol (Phenol, 2,4-dimethyl-)
Dimethyl phthalate (1,2-Benzenedicarboxylic acid, dimethyl ester)
4,6-Dini tro-o-cresol
2,4-Dinitrophenol (phenol, 2,4-nitro-)
2,4-Dinitrotoluene (Benzene, l-methyl-2,4-dinitro~)
Di-n-octyl phthalate (1,2-Benzenedicarboxylic acid, dioctyl ester)
1,4-Dioxane* (1,4-Diethylene oxide)
1,2-Diphenylhydrazine (Hydrazine, 1,2-diphenyl-)
EthyleneimineT (Azridine)
Ethylene oxide* (Oxirane)
Fluoranthene (Benzo (j,k) fluorene)
Formaldehyde*
Hydrogen sulfide (Sulfur hydride)
Indeno (l,2,3-cd)pyrene (1 10(l,2-phenylene)pyrene)
Lead
Mercury
Methanethiol (Thiomethanol)
3-Methy1chlolanthrene (Benz(j)aceanthry1ene, 1,2-dihydro-3-methy1 -)
Methyl ethyl ketone1" (MEK) (2-Butanone)
Naphthalene
Nickel
p-Nitroaniline (Benzenamine, 4-nitro-)
Nitrobenzene (Benzene, nitro-)
4-Nitrophenol (Phenol, pentachloro-)
Pentachlorophenol (Phenol, pentachloro-)
Phenol (Benzene, hydroxy-)
Pyridine
Selenium
Tetrachl oroethanes*!!
Tetrachloroethylene* (Ethene, 1,1,2,2-tetra chloro-)
Toluene* (Benzene, methyl-)
Tri chlorobenzenes*
—continued—
24
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Table 2.2 Continued
Trichloroethanes**
Trichloroethene (Trichloroethylene)
Trichlorophenols*
Vanadium
* If any of these groups of compounds are found, the specific isomers
listed in Appendix VIII should be identified.
t Use Test Method 8240 for these volatile compounds.
# Use Test Method 3050 in SW-846 for al1 metal s; see Skinner (1984) for
semi-volatile organic compounds.
** Bis(Chloromethyl) ether deleted because it is unstable in water
25
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Chapter 3
TREATMENT DEMONSTRATION SCENARIOS AND DECISION-MAKING
Thus far, this document has introduced the nature and intent of the
land treatment demonstration and has described the information required
prior to the choice and implementation of an LTD approach. This chapter
states the available regulatory/technical LTD options and provides clear
criteria to enable the applicant, in consultation with the permitting
authority, to choose the appropriate scenario. The flow chart (Figure 3.1)
which was introduced in Chapter 1 can be used as a guide to the LTD
scenarios and as the basis for further discussion and decisions. The
reader is encouraged to refer to this chart often since it presents the
scenarios that are the focus of this document in capsule form. Once a
scenario is selected, the individual technical activities that are required
(see Figure 3.1) for the chosen scenario can be assembled from among those
described in Chapters 4 through 10.
Briefly, the flow chart consists of two major sections. The top
portion of the chart shows the decision flow leading the applicant to one
of four permitting scenarios; the criteria to guide the applicant at each
decision point (diamond-shaped box) are provided in detail in Section 3.1.
Once the appropriate land treatment permitting scenario has been deter-
mined, the applicant should refer to the bottom portion of the chart, which
outl ines the steps invol ved in each scenario; Section 3.2 explores the
logic behind each scenario more thoroughly. It should be noted that while
Scenario 4 represents the case generally available to most applicants, only
in the most restricted circumstances can an applicant qualify for Sce-
nario 1. Of course, any applicant may opt for a more comprehensive
scenario than the one he is qualified for (see dashed "alternatives" arrows
in Figure 3.1).
3.1 CRITERIA FOR CHOOSING A LAND TREATMENT DEMONSTRATION SCENARIO
The choice of an LTD scenario involves organizing information and
answering four questions, the first of which is easy: "Is the land treat-
ment unit new or existing?" As noted in the regulations (40 CFR 270.2), an
existing unit is one that was in operation or for which construction had
commenced on or before November 19, 1980. For the purposes of this
document, the unit is considered "new" only if does not fit this defini-
tion; a complete definition appears in the regulation cited above. For
existing units, the following sections address the next three questions in
sequence.
26
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SELECTION AND
DESCRIPTION OF
TREATMENT
DEMONSTRATION
SCENARIOS
PRELIMINARY
INFORMATION
NEEDS
DESIGN
NO OPERAT
CHANGES
PLANNE
IS
EXISTING
HWLT UNIT
PERMIT
WRITER
DECIDES
SCENARIO
WASTE
4AGEMI
RECORDS
FIG. 3.1. TREATMENT DEMONSTRATION DECISION FLOW CHART.
27a
-------
r
r
SCENARIO I
SCENARIO 2
SCENARIO 3
SCENARIO 4
INTENSIVE
SITE DATA
COLLECTION
FULL SCALE
.PART 264
FACILITY
PERMIT
ISSUED
ALTERNATIVE /
IVE
VTA
riON
x
tPPROACH
ISSUED PHASE 1
OF A TWO
PHASE PERMIT
A
7
s
LEFT UNDER
INTERIM
STATUS
STANDARDS
TEMPORARILY
*
SH
Tl
OEM
PEF
SHORT TERM
TREATMENT
iMONSTRATWN
PERMIT ISSUED
BARREL
LYSIMETER
STUDY
FIELD
PLOT
STUDY
FIELD
PLOT
STUDY
TOXICITY
TEST
LYSIMETER
STUDY
BARREL
LYSIMETER
STUDY
PHASE I OF A
TWO PHASE
PERMIT ISSUED
TWO YEAR
FOLLOW-UP
STUDY
TWO YEAR
FOLLOW-UP
STUDY
FULL SCALE
PART 264
FACILITY
PERMIT
ISSUED
FIG. 3.1. TREATMENT DEMONSTRATION DECISION FLOW CHART. (CONTINUED)
(NUMBERS IN BOXES REFER TO CHAPTERS)
27b
-------
While permitting Scenario 4 is generally required for new units (see
Figure 3.1), one special case may al low the use of one of the other three
scenarios. The regulations allow existing operating data (from another HWLT
unit that is very similar to the proposed unit) or literature data to
satisfy the demonstration if strict criteria are met. Since experimental
evidence and practical experience has shown that a single waste or similar
wastes behave differently when placed in a different setting (i.e., dif-
ferent climate, soil, management, etc.), the following criteria must be met
for data from another HWLT unit to satisfy the LTD:
1) Wastes must be qualitatively and quantitatively similar
(i.e., the same set or a subset of hazardous or pertinent
nonhazardous constituents);
2) This same previously demonstrated waste must have been tested
in the same climatic regime;
3) Soils and shallow hydrogeology of the two sites must be
practically the same according to accepted classification
methods and supporting analyses;
4) Anticipated waste application rates at the applicant's unit
must be the same or less than those at the demonstrated
site; and
5) Management techniques should be essentially comparable in
their ability to achieve the desired results.
In the above sense, the concept of a regional LTD might be feasible for
several operators who share these common features.
3.1.1 Are Major Design and Operation Changes Planned?
For an existing HWLT unit to be permitted on the basis of current
design and management, the planned future activities under a Part 264
permit must involve a generally similar waste application rate and method
which both maintains similar waste(s) quality and management practices and
continues to use the same soil as the treatment medium. If current and
future activities are not the same, the planned changes must lead to more
conservative application rates, better waste quality (i.e., lower concen-
trations of hazardous or pertinent nonhazardous constituents), or better
management practices or design. In addition, the soils presently used
cannot be replaced by others. To demonstrate future consistency of opera-
tion, three areas - planned unit processes, waste application rates, and
use of soil - must be accounted for.
3.1.1.1 Planned Unit Processes--
No changes should be planned in the unit processes generating the
wastes because such changes would result in substantial qualitative dif-
ferences in the waste streams to be land treated. Substantial differences
are primarily considered to be the introduction of measurable amounts of
28
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hazardous or pertinent nonhazardous compounds not previously found in the
wastes. Because these substances would not have been tested in the treat-
ment demonstration, their behavior in the HWLT unit would not be known.
This is not meant to imply that later refinements in unit process design
and/or operation or the addition of new production units will necessarily
warrant a new LTD. However, if qualitative waste changes occur, another
LTD may be necessary. It is also recognized that the relative abundance of
the various waste constituents in even a single waste stream will vary due
not only to seasonal effects but also to such influences as fluctuations in
feed stocks, relative market demand for the various products of the waste
generator, and the intermittent batch generation of certain wastes. These
variations should already be taken into account in the waste characteriza-
tion. In any case, the ongoing waste monitoring program must be capable of
detecting substantial long-term changes in waste quality. For the LTD, the
best that can be done is to identify anticipated changes that could affect
waste quality.
3.1.1.2 Planned Waste Application Rates--
The applicant may anticipate a significant increase in the waste
application rates due to a decrease in the usable land area available for
HWLT or increases in the rate of production for one or several waste
streams; in either case, this significant increase in application rate must
be taken into account in the LTD. Anticipated increases on the order of 20%
or less would be considered acceptable. Should greater increases that are
not accounted for in the LTD be anticipated, or should such increases occur
at anytime in the future, additional LTD work would be warranted. De-
creased application rates present no problem.
Planned application rates should be expressed in terms of the concen-
trations and application rates of limiting constituents or constituents
that are nearly limiting but not in terms of gross parameters such as oil
content. This way of expressing application rates prevents not only misin-
terpretation of the artificial effects of dilution but also the false
impression that no change in a gross parameter such as oil or water content
has occurred and, thus, that no application rate change has occurred. For
example, increases in hazardous constituent production rates that are
merely offset by dewatering still constitute an increased application rate.
3.1.1.3 Planned Use of Soils—
The use of soil other than that already in place significantly affects
the behavior and fate of waste constituents. Due to inherent differences
among the physical, chemical, and biological properties of soils, treat-
ability of waste likewise varies (Brown et al., 1983); thus, planned
operations should include the continued use of present soils. An expansion
of the HWLT unit onto a different soil series would be considered a change
in treatment medium and would thus require a separate LTD. Likewise,
removal of soil present on an existing active area or replacement with soil
from a different series, also regarded as a change of treatment medium,
would require a separate LTD. Finally, a major disruption of the treatment
29
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zone would significantly alter conditions as well. While normal operations
are expected to disrupt surface soils in the zone of incorporation, major
disruption involves one of the following: deep tillage (an activity which
mixes the lower portion of the soil profile that should normally remain
undisturbed during HWLT operations) or the artificial drainage and lowering
of a seasonal high water table that had previously encroached into the
treatment zone in order to meet the separation requirements of 40 CFR
264.271 (c)(2)
3.1.1.4 Guidance on Planned Design and Operation--
Management personnel should be consulted to determine possible near-
term modifications to the waste streams or land treatment unit. Table 3.1
shows the categories of information needed and summarizes the previous
discussions to aid in interpreting this information. Long term changes
become a question of assessing whether it is more effective to do the LTD
for the revised unit now or later. If it is determined that design and
operation changes will occur, HWLT permitting Scenario 4 is required
(Figure 3.1). If it is determined that no changes in design and operation
are planned, the applicant should proceed to the third question (and deci-
sion point on the chart), discussed in the next section.
Table 3.1 Planned Operations Information Needs
Confirmation of No Design
Category and Operation Changes
Unit Processes No anticipated measurable quantities
of additional hazardous or pertinent
nonhazardous constituents that are not
presently in the land treated wastes.
Waste Application Rates No greater than a 20% increase in the
quantities of hazardous or pertinent
nonhazardous constituents applied per
unit area per unit time (kg/ha/yr).
Soil No expansion onto new soil series;
no importation of different soils for
use as the treatment medium; no major
disruption of existing soils.
30
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3.1.2 Is the Performance of the Existing HWLT Unit Acceptable?
The third question to be answered in the flow of decisions (Figure
3.1) is whether the performance of the existing HWLT unit is acceptable.
EPA will address this question by evaluating the results of:
1) Unsaturated zone monitoring (UZM) performed and recorded by
the owner or operator in accordance with 40 CFR §§265.278
and 265.73:
2) Groundwater monitoring (GWM) performed and recorded by the
owner or operator in accordance with 40 CFR §§265.90 -265.94
(Subpart F) and §265.73; and
3) Reconnaissance sampling conducted as part of the preliminary
assessment of the site (see Chapter 2, Section 2.1.2).
The discussion below regarding UZM and GWM pertains only to informa-
tion needs for permitting HWLT units; it does not relieve the owner/
operator of possible enforcement action for inadequate compliance with
interim status monitoring requirements.
3.1.2.1 Monitoring System Design--
To provide reliable and useful data, the unsaturated zone and ground-
water monitoring systems must be properly designed and implemented. Major
deficiencies in these monitoring systems significantly limit the usefulness
of any data and automatically trigger a more comprehensive approach to the
treatment demonstration (i.e., Scenario 3 or 4).
EPA uses the following minimum criteria to detemine whether the moni-
toring systems provide useful and reliable data for the treatment demon-
stration:
1) The UZM program must have included, since the date that the
HWLT unit was granted interim status (usually November 19,
1980), at least semi-annual sampling analysis of soil cores
and soil-pore liquid from at least three locations within the
active portion of the HWLT unit. Also, background data from
at least one location outside of the active poriton should
have been collected for both soil core and soil pore liquid.
In addition, the monitoring program must have met the gen-
eral monitoring objectives defined in §265.278.
2) The groundwater monitoring program must have met, since the
effective date of the interim status groundwater monitoring
requirements, the minimum requirements specified in Subpart
F of Part 265.
The applicant must use the information required in the facility operating
record for monitoring (§265.73(b)(6)) to document that the above criteria
31
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have been met.
3.1.2.2 Performance Evaluation--
Using the criteria below, EPA evaluates the performance of the HWLT
unit according to the results of unsaturated zone and groundwater monitor-
ing during interim status and recent reconnaissance sampling (for all
Appendix VIII hazardous constituents) of the site.
1) The unsaturated zone monitoring data (including soil core
and soil-pore liquid data) collected during interim status
and included in the operating record as required under
§265.73 must show no significant migration of hazardous
waste constituents below the proposed treatment zone. Also,
the GWM data must not indicate the presence of contamination
as defined in Subpart F of Part 265; and
2) The reconnaissance sampling data (including soil core and
soil-pore liquid data) must show:
a. no significant increase of hazardous constituents (Ap-
pendix VIII) below the proposed treatment zone within
the active portion compared to background; and
b. no unacceptable build-up of hazardous organic consti-
tuents within the zone of incorporation (ZOI) (e.g., 0-
30 cm). The concentration of hazardous organic consti-
tuents in the ZOI are acceptable if they are 1) no
greater than two times the annual loading rate of that
constituent when the ZOI is sampled after waste is
incorporated and dried, or 2) no greater than the annual
loading rate of that constituent when the ZOI is sampled
immediatley prior to a scheduled waste application.
For HWLT units that satisfy the criteria in sections 3.1.2.1 and
3.1.2.2, the next and final step is to determine whether their waste
management records are complete (see Section 3.1.3). This last step also
determines if the HWLT unit falls into Scenario 1 or 2.
HWLT units that do not meet the criteria in Sections 3.1.2.1 and
3.1.2.2 fall into Scenario 3 or 4. After considering the unit's current
design and operation, the permit writer decides whether the unit should
follow Scenario 3 or 4. If possible interim status violation becomes
apparent to the permit writer, he will inform the EPA or State enforcement
officials for possible enforcement action.
3.1.3 Are the Waste Management Records Complete?
The final question in the decison-making process is whether the waste
management records are complete. If the land treatment demonstration is to
rely primarily on past operating data to satisfy the treatment demonstra-
tion (i.e., Scenario 1), this operating data must include detailed waste
32
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management records that clearly document the set of conditions that pre-
viously allowed successful treatment of hazardous waste at the site. This
documentation provides the necessary background and support for the permit-
ting official to establish specific permit conditions for future operation.
Table 3.2 lists what constitutes complete the waste management data
and records. These records, which must include the history of waste appli-
cation (i.e., application rates, timing, and location) and the history of
waste quality (i.e., waste analysis and unit process data), are more com-
prehensive than those required under interim status but are necessary to
provide adequate data for the demonstration.
The records described in Table 3.2 include data from recent and past
operations. Since wastes are continually being treated in the system, the
recent years are most important to the historical construction. As one
looks further into the past, each preceding year has a diminishing impact
on current treatment zone characteristics. The completeness of the records
can thus be judged against two frames of reference:
1) recent activities that are most influential and require rela-
tively detailed records of waste application rates, distribu-
tion, timing, and quality; and
2) older operations that are usually less influential and re-
quire only general estimates of past activities.
Based on half-lives of less than one to two years for most land treatable
organic constituents in soils (Brown et al., 1983), four years of good
records should suffice for the first frame of reference. With regard to
the longer time frame, only estimates of the waste application rates are
needed beyond four years.
If the waste management records are complete (as documented by the
operating record required under §265.73) and the HWLT unit has satisfied
the other criteria described in Sections 3.1.1 and 3.1.2, the owner or
operator may qualify for the Scenario 1 demonstration approach. Section
3.2.1 describes the technical approach taken in Scenario 1. Those HWLT
units that have incomplete records yet have satisfied the other decision
criteria in Sections 3.1.1 and 3.1.2 fall into Scenario 2.
3.2 TREATMENT DEMONSTRATION PERMITTING SCENARIOS
At this point, with the guidance for choosing an LTD permitting scena-
rio presented, applicants should be able to identify the proper scenario
for their conditions. Before proceeding, however, the applicant should
obtain approval of the chosen scenario by EPA or the State in a pre-LTD
meeting or review. As noted in the previous section, the choice of one of
four scenarios is possible. This section describes the content of and
justification for each of the four scenarios.
Using Figure 3.1 and the following descriptions, each of which notes
33
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Table 3.2 Criteria for Deciding the Completeness of Waste Management Data
and Records
Category
Item
Minimum Degree of Completeness Needed
History of Waste
Application
History of Waste
Quality
Years in service
and annual quan-
tity of wastes
land treated
Placement of
wastes on land
treatment plots
Estimated annual
quantity of was-
tes land treated
Approximate
placement of
wastes
Waste analyses
Unit Processes
Records of measured annual waste
quantity (dry weight) treated over the
life of the HWLT unit or for four
years, whichever is less. Must in-
clude al 1 wastes, both hazardous and
nonhazardous, that are managed on the
same unit.
Records of quantity (dry weight),
date, and location of each waste
application for each land-treated
waste over the 1 ife of the LT unit or
for four years, whichever is less.
Estimated annual waste quantity (dry
weight) treated during the life of the
unit excluding the most recent four
years.
Approximate quantity (dry weight),
timing, and location of each waste
application during the life of the
unit excluding the most recent four
years.
Semi-annual analyses of each land-
treated hazardous waste during the
last four years. (Nonhazardous waste
analyses are also necessary if these
wastes are land treated in same plot
as hazardous wastes.) Parameters must
include bulk organics (e.g., TOC, oil
& grease, solvent extractable, etc.),
key metals (totals on a dry weight
basis and NOT EP toxicity test re-
sults) and some measure of residual
solids (i.e., after loss of water and
organics).
History of unit processes employed in
the generation and treatment of the
land treated wastes (i.e., wastewater
treatment) for the entire unit life.
Processes must have been relatively
constant during this period, with
little change in waste quality.
34
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what is expected technically, the applicant should be able to assemble a
land treatment demonstration. The technical elements of the LTD are de-
scribed in Chapters 4 through 10. The information in this section is de-
signed to be used as the basis for a written LTD plan, as required by
§270.20(a), and to guide the applicant in the performance of the LTD.
3.2.1 Scenario 1
Owners/operators of HWLT units who have gathered the preliminary
information described in Chapter 2 and have met the decision-making cri-
teria described earlier in this chapter may satisfy the LTD with the,Scen-
ario 1 approach. Scenario 1, which involves the use of past operating data
along with a one-time intensive soil characterization, is based on the
assumption that for well documented, designed, and operated HWLT units an
approximate mass balance can be estimated between the hazardous consti-
tuents applied and those remaining. As described below, this approximate
mass balance is estimated according to a combination of complete historical
data from past operation and more detailed, current intensive soil and
waste characterization data. If proper data is available, the Scenario 1
approach should confirm that hazardous constituents are being degraded,
transformed, or immobilized at the HWLT unit.
The first step in determining the approximate mass balance is compila-
tion of the past history of the HWLT unit performance, temporal and areal
distribution of the land treated wastes, and waste characteristics. Three
types of information are needed to construct this past history:
/
1) documentation of acceptable performance of the existing HWLT
unit (as defined in Section 3.1.2);
2) history of waste application (Section 3.1.3); and
3) history of waste quality (Section 3.1.3).
This historical data collected during interim status will have certain
limitations because the ISS waste analysis and UZM standards required the
owner or operator to address only those "hazardous waste constituents" that
1) are in 40 CFR 261 Appendix VII for listed wastes, or 2) cause a waste to
exhibit the EP toxicity characteristic for characteristic wastes (see Table
1 of §261.24). The land treatment demonstration standard, however, re-
quires data on al 1 hazardous constituents in Appendix VIII of 40 CFR 261
present in the waste. Thus, the historical record must be supplemented
with more comprehensive data addressing all hazardous constituents in the
waste. This may be accomplished by first collecting detailed, intensive
data on current waste quality and site conditions and then correlating this
data to the general waste and site data included in the historical record
(i.e., making a retrospective extrapolation). For example, the applicant
may be able to establish a correlation between the concentration of waste
constituents analyzed during interim status and the concentration of Appen-
dix VIII constituents identified in the current comprehensive waste ana-
lyses for the Part B appl ication (see Chapter 2). It may be assumed that
35
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the comprehensive waste analyses represents the mean of the waste stream
population. Records from past analyses should be used to support the
assumptions. This correlation can then be used along with the data on
waste application rates in the historical record to roughly estimate the
loading rate of individual hazardous constituents.
Therefore, in addition to the historical records, the applicant must
gather and include the following information in his analysis for Scen-
ario 1:
1) current complete characterization of soils (i.e., reconnais-
sance sampling) and representative waste streams for all
hazardous and pertinent nonhazardous constituents (as de-
scribed in Chapter 2); and
2) recent intensive site characterization for hazardous consti-
tuents (as described in Chapter 4).
The intensive site-data collection (Chapter 4) provides data on pre-
sent site conditions such as concentrations of hazardous constituents in
and migration below the treatment zone. Although the sampling prescribed
in Chapter 4 is much more comprehensive than reconnaissance sampling de-
scribed in Chapter 2, some or all of the data obtained from reconnaissance
sampling may nevertheless be applicable. The intensive site sampling
involves coring and subsampling from the surface to 200 cm. Analyses should
be performed for all hazardous constituents known or suspected to be in the
waste or waste degradation by-products. Background site information can
be used as a basis for judging the contribution from naturally occurring
constituents (e.g., metals). (Note: Chapter 4 also describes the inter-
pretation of all data from the Scenario 1 analysis. Once information
gathering and presentation are complete and acceptable, the applicant may
apply for a full-scale Part 264 facility permit.)
In considering the Scenario 1 option, the applicant should recognize
the limitations of this approach. First, the approach requires documented
historical records and intensive soil and waste characterization data that
must allow one to make reliable retrospective extrapolations and conclu-
sions regarding the treatment of individual hazardous constituents.
Second, the applicant is limited to the waste application rates and fre-
quencies used during the past operations (i.e., the applicant does not have
the opportunity to evaluate higher loadings or frequencies). Third,
because Scenario 1 is a retrospective analysis, it is unlikely that
sufficient information on the relative mobility and degradation of
hazardous constituents will be available to determine the "principle
hazardous constituents" that may serve as indicators for UZM during full-
scale operation. In most cases, prospective studies (as presented for
Scenarios 2-4) are needed to provide sufficient data to make selection of
PHCs possible.
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3.2.2 Scenario 2
Scenario 2 is generally designed for existing HWLT units which demon-
strate relatively good design and operation (i.e., comply with ISS, have
waste application rates at or below optimum for good degradation of
organics, and show no significant hazardous constituents leaching below the
treatment zone) but which lack adequate long-term records to establish a
reliable mass balance of waste application and constituent fate. From a
permitting perspective, this scenario involves a two-phase permit
(described in Chapter 1); technically, it requires the applicant to choose
and carry out either a barrel lysimeter study (Chapter 6) or a field plot
study (Chapter 7) to be followed by acute toxicity testing (Chapter 5).
An applicant who has determined in consultation with the permitting
official that his HWLT unit qualifies for Scenario 2 should submit a Part B
permit application for a two-phase permit. As required under §270.20(a),
this application should outline a treatment demonstration plan, which
should include the barrel lysimeter study, field plot study, or an equiva-
lent study design. The applicant should identify his preference in the
pre-application meeting with the permit writer to allow a discussion of any
questions or issues early in the permit process.
Under this scenario, the permit writer writes a two-phase permit:
Phase 1 outlines conditions necessary to meet §264.272(c) for the treatment
demonstration, and Phase 2 outlines provisions for the full-scale facility
design and operation (including all Subpart M and other general require-
ments). All the administrative steps (except permit modifications) for the
two-phase permit, including public hearings, occur at this point.
After the two-phase permit is issued, Phase 1 is effective during the
period of the treatment demonstration (i.e., approximately one year in this
case). It should be noted that Phase 1 of the permit is only applicable to
the barrel lysimeters or the portions of the HWLT unit on which field plot
demonstration tests are being done; these portions may be the size recom-
mended in Chapter 7 of this document or some larger area designated by the
permit writer. Since the interim status of the remainder of the HWLT unit
is unaffected during Phase 1, the owner/operator may continue to operate
under interim status on this remaining area during the demonstration.
Nevertheless, the owner/operator is subject to enforcement action if in-
terim status violations occur in this remaining area.
The owner/operator must submit the following to the permitting
authority within 90 days of completion of the tests: 1) a certification
that the LTD tests have been carried out in accordance with Phase 1 of the
permit and 2) all the data collected during the LTU along with interpreta-
tions and final design adjustments.
The permitting authority then evaluates the results and modifies the
second phase of the permit (usually a minor modification under §270.42) to
incorporate these results. Phase 2 of the permit (i.e., full scale opera-
tion) becomes effective after the modifications are completed.
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Technically, Scenario 2 allows the applicant a choice between barrel
lysimeter (Chapter 6) or field plot studies (Chapter 7). It is assumed
that enough is known about the site to limit the LTD work to a single test
system without prior toxicity testing or other bench scale work. Depending
on findings and climatic conditions (e.g., unseasonably dry weather or poor
degradation rates may lead to an extended time frame), the barrel lysimeter
study and the field plots should run for one year or more. In the mean-
time, routine monitoring of the HWLT unit according to the monitoring plan
and analysis for all hazardous and pertinent nonhazardous constituents
should continue in conjunction with the barrel or field plot testing.
Finally, acute toxicity testing must be performed as described in Section
5.3.2, Maximum Residual Concentration.
3.2.3 Scenario 3
If an owner or operator of an existing HWLT unit plans to continue the
same or a more conservative design and operation but the design and opera-
tion are unacceptable according to the criteria in Section 3.1.2, Scenario
3 or 4 are the available options for the LTD. The permit writer will
determine which option should be followed. The deficiencies in such HWLT
units require that a greater amount of information be collected in this
scenario than in Scenarios 1 or 2. Additionally, the permit approach is
significantly different from Scenario 2 in terms of when a two-phase permit
is issued.
Lack of information to allow a satisfactory two-phase permit to be
written prevents such a permit from being issued until considerable LTD
work is al ready complete. Under §270.63(a)(l), a two-phase permit may be
issued only if the Part B application includes substantial, although incom-
plete or inconclusive, information upon which to base the issuance. Since
owners or operators subject to Scenario 3 do not immediately satisfy this
requirement, the first portion of testing in Scenario 3 is designed to
generate "substantial, although incomplete or inconclusive, information" so
that the facility may qualify for a two-phase permit. This first portion
of testing, which includes a laboratory toxicity test and a barrel lysi-
meter or field plot study, may be done while ISS remain in force for the
HWLT unit. Upon completion of the first portion of testing, Phase 1 of a
two-phase permit is issued to cover a non-intensive, two year follow-up
study on a large scale. Finally, Phase 2 of the two-phase permit becomes
effective pending satisfactory completion of the follow-up work.
The above approach is the most expeditious route to completion of the
LTD and to final permitting of HWLT units falling into Scenario 3. As
discussed in Chapter 1, owners/operators may conduct treatment demonstra-
tion studies at an interim status unit, provided the ISS are not violated;
such an approach is taken in the first portion of this scenario. As an
alternative, however, the applicant may choose Scenario 4 and may apply for
a short-term permit.
The technical requirements for Scenario 3 involve several steps.
First, the laboratory-level acute toxicity test (Chapter 5) determines the
concentration of fresh waste in soil that would be acutely toxic to
38
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decomposer organisms and helps set waste application rates for the second
step, either barrel lysimeter studies (Chapter 6) or a field plot study
(Chapter 7). Findings of the first two steps along with results of follow-
up acute toxicity testing (Section 5.3.2) may lead to lower or even higher
annual waste loading rates than applied previously at the HWLT unit. The
revised loading rate and any other necessary improvements in design and
operation are then verified in a large scale two year follow-up study
(Chapter 9), done under Phase 1 of a two-phase permit, that may encompass
the entire HWLT unit. Satisfactory completion and documentation of the
Phase 1 follow-up study would lead to modifications to Phase 2 of the
permit. Phase 2, which applies to the full-scale operation, becomes effec-
tive after the modifications are made. Thus, Scenario 3 requires approxi-
mately 3 years from initiation of the LTD to the final decision on Phase 2.
3.2.4 Scenario 4
Any new or redesigned existing land treatment unit, including cases of
al tered waste qual ity (i.e., different hazardous constituents to be 1 and
treated), significantly increased waste loading rates, or drastic changes
in the soils used, requires that the applicant follow Scenario 4 to obtain
a permit. Likewise, units having significant ISS violations may also be
required to follow Scenario 4. While its technical requirements are the
same as those of Scenario 3, Scenario 4 is unique in its use of the short-
term permit option (described in Chapter 1).
Prior to beginning the LTD, the applicant must obtain a short-term
treatment demonstration permit which should incorporate only those provi-
sions necessary to meet the general performance standards in §264.272(c).
Public comment and hearing are required. Once this permit is obtained, the
LTD may begin. If the facility is existing and if the unit is in com-
pliance with the ISS requirements, continuance of present operations under
interim status may be permitted during LTD performance. Once the technical
effort for the LTD is complete, a final Part B application incorporating
the LTD results should be submitted. A full scale Part 264 facility permit
is issued after appropriate administrative steps, including a second manda-
tory period for public comment and hearing, are taken.
The technical steps involved are identical to the Scenario 3 approach.
First, acute toxicity testing (Chapter 5) is done as a preliminary screen-
ing measure to hel p set waste appl ication rates prior to either a barrel
lysimeter (Chapter 6) or field plot study (Chapter 7). Follow-up acute
toxicity testing (Section 5.3.2) is then done to help set annual waste
application rates. Finally, information from this intensive study on the
degradation, transformation, and immobilization of the waste(s) guides the
design to be tested in a non-intensive two year follow-up study
(Chapter 9).
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Chapter 4
INTENSIVE SITE DATA COLLECTION
For those sites with good records of waste analysis, waste
application, unsaturated zone and groundwater monitoring, and operating
acceptably, on intensive soil sampling of the facility to confirm treatment
of hazardous constituents may be undertaken. (See Chapter 3 to confirm
whether this technical approach is acceptable for a given site.) The
intensive soil sampling data described in this chapter may be supplemented
by data collected in the reconnaissance soil sampling (Chapter 2).
Together, these two sets of data (along with the historical record) satisfy
the Scenario 1 demonstration approach. The following describes the
intensive soil sampling that is needed as a component of Scenario 1.
4.1 SOIL CORE SAMPLING AND ANALYSIS
With some exceptions, the soil core sampling approach should follow
that described in Chapter 2, reconnaissance site data collection. Within a
uniform area, twelve soil cores should be collected randomly, unless the
uniform area is greater than 12 acres, in which case a minimum of one soil
core per acre should be collected. If reconnaissance sampling was done at
half this density, as recommended in Chapter 2, only one additional core
per two acres is needed to complete the requirement. Unless widespread
contamination was found outside the HWLT unit, no further background sam-
pling is necessary. Additional soil core samples should be collected at
select locations (i.e., "hot spots") within the HWLT unit where wastes are
most likely to build up or migrate. Except for well run units (where
attention is placed on uniformity of waste applications and management) few
sites can avoid at least some sampling of select locations in addition to
the random sampling.
The depth of sampling should be as follows: 0-15, 15-45, 45-90, 90-
150, and 150-200 cm. Depending on the number of samples analyzed and the
type of analyses performed, the analytical data obtained from the recon-
naissance investigation may be used to partially fulfill the data require-
ments of this investigation.
4.2 SOIL-PORE LIQUID
The applicant should collect samples from the existing soil-pore liquid
samplers as soon as possible for analysis. These devices should be
randomly located at a rate of one per two acres, with a minimum of six per
uniform area. Additional samplers may be needed at select "hot spot" loca-
tions, as determined by soil, topography, waste distribution, and
40
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operational features.
4.3 ANALYSIS OF SAMPLES
For purposes of the intensive site data collection described herein,
analysis should be at Tier II, as outlined in Chapter 10, for all soil
samples collected between 0 and 2 meters and for all soil-pore liquid
samples.
4.4 INTERPRETATION OF DATA
Because the intensive site data collection approach is a mass balance
method, the applicant should present his analytical data from waste, soil
cores, and soil survey samples, along with records of past activities, to
meet two objectives:
1) To assess contaminant immobilization, statistical analysis of
soil core and soil-pore liquid data should be done by compar-
ing the concentrations of hazardous constituents in soil and
soil-pore liquid below the treatment zone with background
values. A significant difference would indicate hazardous
constituent mobility unless other circumstances account for
any such differences (e.g., pockets of buried materials not
associated with the land treatment operation).
2) To assess degradation and transformation, treatment zone
waste application data and waste and soil analyses should be
used to determine the quantity of organic hazardous
constituents (OHCs) degraded and the conserved species built
up. Apparent degradation, which may in fact include other
losses such as volatilization or leaching, can be expressed
as:
OHCs Applied - OHCs Remaining = OHCs "degraded"
This relationship should be determined for all nonconserva-
tive hazardous constituents (e.g., organics).
In the latter evaluation, the "zone of incorporation" (typically 30 cm or
less, but a maximum of 60 cm) should be considered separately from the
remainder of the treatment zone. This is because active degradation pri-
marily occurs in the zone of incorporation, while any materials that have
penetrated deeper or have been covered by successive waste applications are
effectively buried. Although some degradation may occur at depth, only the
soil's capacity to immobilize these deeper materials should be considered
to achieve treatment in most cases. Within the zone of incorporation
(ZOI), the mass balance for each hazardous organic constituent should show
that:
41
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1) Less than 2Q% of the total amount of each hazardous organic
constituent applied over the life of the unit remains in the
zone of incorporation (as measured at or adjusted to the
beginning or end of the degradation season) (API, 1983); and
2) The concentration of each hazardous organic constituent in
the top portion of the ZOI is less than two times the annual
concentration of that constituent applied (EPA, 1983A).
The top portion of the treatment zone is chosen to avoid artificial dilu-
tion due to the transition to deeper, "cleaner" soils. Below the transi-
tion from the ZOI but still within the treatment zone (e.g., 45-90 and 90-
150 cm), concentrations of hazardous constituents should decrease with
depth to practically background levels near the lower treatment zone boun-
dary. If great depths of undegraded organics are present (e.g., the land
surface is one or more meters above the original level due to organics and
solids build-up), the issue must be addressed appropriately in the closure
plan. More importantly, this condition eliminates Scenario 1 as the appro-
priate permitting/LTO option.
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Chapter 5
TOXICITY TEST PROCEDURE
The acute toxicity assay should provide two groups of data. First, an
evaluation of the toxicity of the soil, waste, and four soil-waste mixtures
is made to estimate the initial waste application rates {mass/area/applica-
tion) for use in the barrel lysimeter or field plot studies (Chapters 6 and
7). Second, the analytical data from the barrel lysimeter field plot
studies are used to refine the waste application rate prior to the follow-
up field study (Chapter 9) or final permit issuance. Refinements in the
application rates are based upon the data from acute toxicity testing of
the most resistant specific hazardous organic constituents found in the
lysimeter or field plot studies. A revised waste loading rate may be deter-
mined by estimating the maximum allowable residual concentration in soil
of each hazardous organic constituent at the land treatment unit and calcu-
lating the degradation rate of that constituent found in the lysimeter or
field plot work.
The toxicity test procedure selected should employ a single species,
acute toxicity test to estimate the acute impact of waste application or
waste fractions on the soil biota responsible for waste treatment.
For any toxicity test to be practical for environmental monitoring, it
must be validated extensively. The Microtox System™ suggested below is a
rapid and simple toxicity test which has been validated with a large number
of pure compounds and complex industrial waste waters and sludges. This
procedure, as any other bioassay which could be recommended, offers poten-
tial disadvantages. First, the Microtox™ test organism is a photolum-
inescent bacteria of marine origin, which may not accurately represent the
response of soil microbes. In addition, this test measures the toxicity of
water soluble constituents and may therefore underestimate the toxicity of
hydrophobic compounds. Extensive developmental work and evaluation that
involves a variety of waste-soil mixtures tend to discount either disad-
vantage as a hinderance for the purposes of the test.
Alternate procedures of measuring acute toxicity include the follow-
ing: tests that use aquatic organisms such as the Daphnia and fathead
minnow (Peltier, 1978), phototoxicity tests that measure root elongation
(Edwards and Ross-Todd, 1980), a terrestrial toxicity test that uses earth-
worms (Neuhauser et al., 1983), and a plate count assay that uses soil
bacteria (Brown et al., 1983). Each of these alternate procedures offers a
separate set of potential advantages and problems. In addition, none
approaches the rapidity and simplicity of the Microtex™ test.
No single bioassay can provide a comprehensive view of toxicity. Only
through a battery of acute and chronic toxicity tests can a comprehensive
43
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T
view of toxicity be obtained. However, almost any validated toxicity test
can produce the information required in this chapter for a treatment demon-
stration, since the primary objective of such a procedure, within the
context of a land treatment demonstration, is to use a rapid, single
species toxicity test to indicate the optimum initial application rate for
a specific hazardous waste.
5.1 TEST SYSTEM DESCRIPTION
Since the test system used as an acute toxicity bioassay should be
rapid and simple and should have been validated with a large number of
samples, the Microtox System™ (registered trademark, Beckman Instruments,
Inc.) is suggested as the primary toxicity bioassay. Numerous evaluations
have revealed that Microtox is sensitive to a wide spectrum of toxicants,
with results correlating with other procedures (Qureshi et al., 1982;
Casseri et al., 1983; Burks et al., 1982). The Microtox System™, which
utilizes a suspension of the marine luminescent bacterium (Photobacterium
phosphoreum) as a bioassay organism for measuring acute toxicity in aqueous
samples, is an instrumental approach in which bioassay organisms are han-
dled like chemical reagents. Suspensions containing approximately
1,000,000 bioluminescent organisms are "challenged" by the addition of
several concentrations/dilutions of an unknown sample. A temperature con-
trolled photometric device with attached recorder quantitatively measures
and records the light output of the organisms in each suspension before and
after they are challenged; a reduction of light output reflects a deterior-
ation in the state of health of the organisms, thereby indicating the
presence of toxicants in the sample. A comprehensive discussion of the
Microtox System™, including its benefits and limitations, principles of
operation, operating procedure, and basic data reduction schemes, has been
prepared for distribution by Beckman Instruments, Inc. (1982).
Two major pieces of experimental apparatus are required to conduct the
toxicity test procedures. First, a tumbler shaker, a wrist-action shaker,
or a platform shaker is used to extract the water soluble fraction from
each sample, and then the Microtox™ system is used to test this extract.
5.2 GENERAL EXPERIMENTAL PROCEDURES
The Microtox1" test is conducted on the water soluble fractions from
two groups of samples. The following sections outline the methods used to
obtain these samples and provide a brief description of the Microtox™
procedure.
5.2.1 Water Soluble Fractions
The following procedure is used to obtain the water soluble fraction
(WSF):
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a. Place a 100 g (dry wt) sample of soil, waste, or soil-waste
mixture into the extraction vessel. If the waste has a high
water content, a thoroughly mixed sample can be centrifuged
to obtain the WSF for toxicity testing, thus eliminating-the
need for the extraction step.
b. Add 400 ml of distilled, deionized water (4:1 vol/wt ratio)
to the vessel and cap tightly.
c. The tumbler shaker is the method of choice. However, if a
wrist action shaker is used, place the vessel on the shaker
at a 180° angle; if a platform shaker is used, place the
vessel on its side. In all cases, be certain the cap is on
tightly.
d. Allow the flasks or bottles to shake for 22 ±2 hr at approxi-
mately 30 rpm in the tumbler shaker or 60 rpm on the wrist-
action or platform shaker.
e. Following the specified mixing period; remove flasks from the
shaker and al low them to sit for one hour. Pour the decant
into high-speed centrifuge tubes, adding 0.49 of NaCl for
each 20 ml of sample, shaking, and then centrifuging at 2,500
rpm for 10 minutes.
f. Prepare a sample from each test unit for Microtox™ testing by
carefully pipetting 20 ml of centrifugate from each centri-
fuge tube into a clean graduated cylinder and storing at 4°C.
Care must be taken to ensure that any floating material is
not transferred. As soon as all samples are prepared, begin
Microtox™ testing; conduct all tests the same day that they
are prepared.
g. Follow the test procedure outlined in the Microtox System
Operation Manual (Beckman Instruments, 1982).
5.2.2 Test System Operation
While detailed instructions, reagents, and the instrument can be
obtained from Beckman Instruments, Inc. (Carlsbad, CA), the following is a
brief outline of the procedure:
a. Adjust the instrument to the desired temperature (15°C for
most applications).
b. Rehydrate the cell suspension.
c. Place 5-7 pairs of cuvettes in incubation block.
d. Add 0.5 ml diluent followed by 0.01 ml of cell suspension to
one member of each pair of cuvettes.
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e. Add 1.0 ml of appropriate sample dilution (or sample to be
compared) to the other member of each pair of cuvettes. One
cuvette receives diluent only and serves as a blank.
f. Allow 10 minutes for cuvettes to reach test temperature.
g. Take an initial reading of light output (relative to blank)
for each cell suspension.
h. Transfer 0.5 ml from blank and sample cuvettes to appropriate
cell suspension.
i. After the desired reaction time (5 minutes for most
applications) take final reading of light output for each
cuvette.
j. Use blank to correct sample for time-dependent drift in light
output.
5.3 TOXICITY TEST APPLICATIONS AND PROCEDURES
It was stated earlier that the acute toxicity test is used for two
purposes. The following sections describe the methods for the two determi-
nations and provide a rationale for each.
5.3.1 Application Rate Determination
Where some question exists about the acceptable annual waste applica-
tion rate influenced by degradation (due to current site overloading, a
desired increase in application rate over past practices, or a new site) a
method must be employed to select a reasonable rate(s) for testing out of
the universe of possibilities. A well designed acute toxicity test pro-
vides a reasonable starting point by defining the amount of waste that may
be applied in a single dose to avoid undesirable impact on soil microbial
populations essential to organics degradation. The specified single
application limit in a barrel lysimeter or field plot study that employs
varying application frequencies (Chapters 6 and 7) can then be used to
determine the frequency of application and annual waste loading rates. The
following method is designed to determine the single application rate
(mass/area/application):
a. Obtain a 5 kg sample of soil and a 500 g sample of the waste
to be tested. Be certain that the characteristics of the
samples of soil and waste are representative of the char-
acteristics anticipated at the site.
b. Conduct Microtox™ test on waste WSF. If the waste has a
significant water content, obtain a sample for toxicity
testing as described in section 5.2.1.3. Add 0.45 Nad to 20
ml of contrifugate and conduct Microtox™ test as described in
Section 5.2.2. For other waste samples, obtain the WSF for
46
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Microtox™ testing as described in Section 5.2.1. If the
waste WSF has an EC50 of greater than 33, no additional tests
are required since acute toxicity will not be a significant
problem.
c. Choose four loading rates for waste-soil Microtox"1 testing
according to the following criteria:
1) the highest loading rate to be used is equivalent to
the lower limit of the 95% confidence interval for the
waste WSF EC50;
2) calculate waste WSF EC50 and 95% confidence interval;
and
3) the remaining three loading rates represent 1/4, 1/2,
and 3/4 of the high rate selected.
d. Weigh out two 100 g samples of air-dried soil which has been
crushed and sieved to 2 mm. Extract the WSF as described in
Section 5.2.1 and conduct Microtox™ tests on each sample.
e. If the soil WSF is non-toxic {i.e., no significant light
reduction is effected in the 100% WSF dilution), normal
dilution water can be used to conduct the remaining tests.
If the soil WSF effects 'a significant light reduction (i.e.,
the soil has some residual toxicity), the soil extract should
be used as diluent to determine ECso's for each loading rate
tested.
f. Weigh out four 300 g samples of soil. Add waste to the soil
samples at loading rates (wt/wt) determined by the criteria
described above.
)
g. From each of the four samples, remove two 100 g (dry wt) sub-
samples and place in a flask or bottle for extraction. Dis-
card the remainder of the sample.
h. Extract each of the eight subsamples with distilled, de-
ionized water according to the procedure described in Section
5.2.1 and conduct Microtox™ test on the water soluble
fraction.
i. Calculate the EC50 for each waste-soil WSF. The EC50 is the
effective concentration of the WSF which causes a 50%
decrease in light output by the test organisms. Transpose
each EC50 value to toxicity units in soil using the following
equation:
Soil Toxicity = 42°- x 4
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Prepare a log-log plot of loading rates versus toxicity
units. The interception point for 20 toxicity units is the
predicted maximum acceptable initial loading rate (MAIL).
The three rates for subsequent tests are the MAIL rate +25%.
5.3.2 Maximum Residual Concentration
In order for the specific organic degradation rate data obtained from
the barrel lysimeter or field plot study to be of any use, that rate of
degradation must somehow be related to an upper limit of accumulation in
soil for each important constituent. The upper limit is characteristically
the concentration at which soil microorganisms succumb to the compound's
toxic characteristics. If degradation rates of all hazardous organic
constituents are more rapid than the bulk organic fraction (e.g., oil and
grease), annual waste application rates may be based merely on the bulk
fraction or other limiting factor (e.g., leaching hazard); however, more
resistant hazardous organics, especially those present in relatively large
concentrations, may be the waste constituents that ultimately limit degra-
dation. The following method should be used as a follow-up to barrel
lysimeter or field plot testing and the results used to help establish
final permit conditions or conditions for a two year follow-up study.
a. Using the results from the lysimeter or field plot study,
determine the most resistant specific hazardous organic con-
stituents.
b. Obtain a 2 kg sample of soil and chroraatographic grade sam-
ples of each resistant hazardous organic constituent to be
tested. Be certain that the characteristics of the soil
sample are representative of the characteristics anticipated
at the site. If the HWLT unit is currently operating, the
soil should come from active areas to which waste has not
recently been applied (i.e., the area is considered to be
ready for reapplication of waste).
c. Weigh out five 300 g samples of soil per chemical to be
tested. Add each chemical to four of the soil samples at
four loading rates, leaving the fifth soil sample as an
unamended control. Prepare a sixth sample with an aqueous
solution of the chemical at its solubility limit.
d. From each of the five soil samples for each chemical tested,
remove two 100 g (dry wt) subsamples and place in a flask or
bottle for extraction. Discard the remainder of the sample.
Split the aqueous solutions into duplicates.
e. Extract each of the ten soil subsamples with distilled,
deionized water according to the procedure described in Sec-
tion 5.2 and conduct the Microtox™ test on the water soluble
fraction. Using soil extract rather than diluent as blank,
determine the concentration of each waste constituent (wt/wt)
required to give 80 percent reduction in light output
48
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If the chosen chemical additions to the soil are not enough
to induce a toxic response (EC8D) to the water soluble ex-
tract, greater amounts of chemical should be added to and
extracted from additional soil samples for analysis unless
even the saturated aqueous solution induces no toxic
response.
The concentration in soil (wt/wt, dry) of each specific
hazardous constituent producing an 80 percent light reduction
(EC80) in the water soluble extract is considered the thres-
hold or critical (Ccn-t) concentration at which unacceptable
microbial toxicity occurs (Brown et al., 1983). In some
cases, a given constituent may not be capable of inducing
such toxicity, thus releasing it from concern as a limiting
constituent from the standpoint of degradation.
5.4 DATA INTERPRETATIONS
Data from the Microtox™ test are used to determine both the percent of
fresh waste in soil (wt/wt) required to give a WSF EC50 value of 20 percent
and the concentration (mg/kg) of each specific hazardous constituent in
soil required to give an 80 percent reduction in light output (ECop).
These calculations define the initial waste loading rate for later pilot
scale testing (based on overall waste toxicity effects) and the maximum
allowable residual concentration in soil for specific hazardous consti-
tuents, respectively. The maximum residual concentration, considered in
conjunction with the compound degradation rate (i.e., half-life in soil)
found in the lysimeter or lab study and desired land treatment unit life,
can provide an acceptable waste loading rate to be used in either the
follow-up field study or a full scale facility permit.
a. Determine mean chart readings for three blank cuvettes (cell
diluent) and two cuvettes for each sample concentration at 5
minutes (t5) after adding sample to reconstituted cell sus-
pension.
b. Calculate the gamma 1 ight decrease (ratio of 1 ight lost to
light remaining) for each waste-soil WSF or compound concen-
tration in soil using the following formula:
where: = gamma light decrease;
= mean chart reading for blank at time t; and
= mean chart reading for sample.
Calculations for the remaining WSF dilutions or soil concentrations
are as fol lows:
49
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= corrected 0 time Tight level
5 minute light level for sample
corrected 0 time light level = (0 time light level) x (blank ratio)
Blank ratio = (5 minute blank light level)
(0 time blank light level)
c. Plot gamma light decrease vs. concentration of waste WSF or
compound in soil on log-log paper. This should convert the
dose-response curve to a straight line and allow the estima-
tion of the waste-soil WSF EC50 or the EC80 concentration of
potential residual toxicants in soil.
d. Profit analysis provides an attempt method for determining
EC5Q values and a 95% confidence interval.
e. Average duplicate test unit ECgQ or ECgQ values for each
sample.
f. Complete calculations as desribed in Section 5.3.Hi) to
determine the MAIL rate.
5.5 MAXIMUM ACCEPTABLE INITIAL LOADING RATE
Detoxification of a hazardous waste in soil can be achieved only if
the waste is applied at such a rate that the matrix of toxic constituents
contained in the waste does not significantly impact soil bacteria. The
Microtox01 acute toxicity test described in this chapter provides one method
of determining a MAIL rate window which is acceptable to the soil microbes.
5.5.1 MAIL Rate Window Determination
The following steps are used to establish the MAIL rate window for
subsequent demonstration studies:
a. Calculate an ECcQ and the 95% confidence interval for the raw
wast WSF. The Tower ECtjQ limit for the confidence interval
provides the upper loading rate for waste-soil toxicity test-
ing. Additional rates for testing are 1/4, 1/2, and 3/4 of
this rate.
b. Calculate an ECg0 for each waste-soil loading rate WSF.
c. Transpose ECcg values for each loading rate to toxicity units
using the following formula:
50
-------
Toxicity Units = ° x 4
d. Prepare a log-log plot of the WSF toxiclty unit values versus
the waste-soil loading rates extracted. Find the
interception point for 20 toxicity units.
e. Determine the loading rate window (waste weight %) according
to the waste-soil loading at this interception point +25%.
This loading rate can be transposed as desired if the water,
solids, oil , etc. of the waste and the bulb density of the
soil are known (i.e., oil content per m , etc.).
51
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Chapter 6
BARREL LYSIMETER STUDY
Design and operating requirements for a land treatment unit are
focused on maximizing soil treatment of hazardous constituents via degrada-
tion, transformation, and/or immobilization processes within the treatment
zone and on minimizing the escape of these constituents to groundwater,
surface water, and air. The potential for transport of hazardous consti-
tuents from the treatment zone via vertical migration depends on the con-
centration of water soluble constituents in the waste, the absorptive
potential and capacity of the soil, the kinetics of soil water movement,
and the degradation potential of mobile waste constituents and intermediate
degradation products (EPA, 1983A; Kaufman, 1983).
The barrel sized lysimeter provides a test apparatus that can be used
to interpret the various interactions influencing land treatment. A barrel
lysimeter is a large, undisturbed soil monolith enclosed by a watertight,
waste compatible casing and equipped with leachate collection devices.
Twelve such units are typically required to conduct most treatment demon-
strations. Although the barrel lysimeter is of limited size compared to
field plots, both degradation and mobility can be measured with this ap-
paratus, with test conditions closely approximating those anticipated in
the field. The barrel size suggested here (55 gallon drum) is large enough
to encompass most soil macrofeatures and soil-water relations. However,
alternative designs which use an approximate diameter to depth ratio of
1:1.5 may also be acceptable.
6.1 EXPERIMENTAL DESIGN
The experimental design suggested for the barrel lysimeter study is a
randomized complete block design, with three replications of each treatment
per soil series to receive waste in the actual HWLT unit. Previous ex-
perience with a well operated HWLT unit (see permitting Scenario 2 in
Chapter 3) or the results of acute toxicity testing (see Scenario 3 or 4)
as described in Chapter 5 should determine the waste application rate to be
studied. Unless no change in current waste loading rate is desired or
anticipated, this study should typically test three annual waste loading
rates and a control and should yield 12 barrel lysimeters per soil series
(uniform area) tested.
For Scenarios 3 and 4, where acute toxicity testing is employed to set
waste application rates, the concentration of waste in soil corresponding
to the LD50 is used to determine the rates. The LD50 waste concentration
is the amount of waste to be applied in a single application (kg/ha/appli-
cation); all treatments that receive waste should have this amount applied
initially. The frequency of waste reapplication will then determine the
52
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annual waste loading rate (kg/ha/year). For barrel lysimeter testing,
waste application is recommended on three schedules (Table 6.1) resulting
in the suggested three waste application rates.
The schedule shown is for a 12 month study. Group numbers correspond
to treatments receiving various respective waste application frequencies.
As the table demonstrates, the ideal application frequencies for the test
are semiannual, quarterly, and bi-monthly. In relatively harsh climates
such as cold northern locales, applications may need to be limited to the
warm season; however, if the local climate is suitable for year round
biological activity, the applications may be spaced evenly throughout the
year.
Under Scenario 2, the current annual loading rate (kg/ha/yr) should be
divided into four equal applications at appropriate intervals through the
year. These same single application amounts (kg/ha/application) should be
applied to the other treatments at different intervals (i.e., every two
months and six months) to yield three annual loading rates. As for the
above scenarios, Table 6.1 may be used as a guide to waste application and
soil sample scheduling.
6.1.1 Collection and Installation of Barrel Lysimeters
Because the use of lysimeters for demonstrating waste treatability may
be a relatively unfamiliar subject to the applicant, the following discus-
sion of general installation techniques is provided.
The experimental apparatus, a barrel sized monol ith of undisturbed
soil, should be collected in a straight-walled cylindrical casing 57 cm OD
and 85.7 cm tall or in an equivalently configured container. (A white
painted exterior is recommended to help control the absorption of radiation
that may increase soil temperature.) The casing is placed in a support
device and gently pushed into the soil with a backhoe. With the backhoe
and a lifting harness, the monolith is then lifted from the soil and
rotated to permit installation of soil-pore liquid samplers and leachate
removal devices. Following installation of these devices, the casing lid
can be sealed with silicon caulk or an appropriate waste-compatible sealant
or gasket and can be clamped into place. After the barrels are righted,
they may be transported as desired for performing tests. Soil should then
be backfil led into the trench, particularly if the lysimeters were col-
lected from within the active land treatment area. To reproduce thermal
gradients similar to normal soil, lysimeters should be insulated or par-
tially buried. The procedures for collection and installation of lysi-
meters, described in detail by Brown et al. (1974) and Brown et al. (1984),
may be found in Appendix B of this document.
53
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Table fa.l. Waste Application Soil Sampling Schedule for Barrel Lysimeter Study
en
Waste
Appl ication
Treatment Frequency
Groups (months)
A 0
B 6
C 3
0 2
Sampling Schedule*
0 30
Z2 Zl
Z2 Zl
Z2 Zl
Z2 Zl
Day
60 90
Zl Z2
Zl Z2
Zl Z2f
Zl
Z21" Zl
Zl
120 150 180
Zl Zl Z3
C3
Zl Zl Z31"
C3
Zl Zl Z3
C3
Z2f Zl Z3
Zl C3
240
Zl
Zl
Zl
Z2t
Zl
270
Z2
Z2
ZZ*
Zl
Zl
300
Zl
Zl
Zl
Z2f
Zl
3bO
Z2
C2
Z2
C2
Z2
C2
Z2
C2
* Sampling schedule: Z = zone of incorporation (0-15 cm); C = core samples (15-45 cm; 45-90 cm).
Levels of analysis: 1 = Tier I; 2 = Tier II; and 3=TierIIL
t Waste reapplication date. Analyze zone of incorporation at Tier II prior to application; collect
sample after application for Tier I analysis.
-------
6.1.2 Preparation of Lysimeters for Study
Using the general installation techniques from Section 6.1.1, the
applicant may assemble the lysimeter study as follows:
a. Collect twelve undisturbed soil monoliths (lysimeters) from
the site of the land treatment unit. Fewer lysimeters may be
collected by applicants for facilities at which the design
and operating requirements (e.g., expected waste loading
rate) have already been more clearly defined. The applicant
may want to reduce experimental protocol and investigate only
one application rate and frequency, which would require only
three barrels.
b. Transport soil monoliths to experimental site and install the
leachate collection system. Collect 200 g soil from the zone
of incorporation (deeper for soils already containing wastes
from an active unit) of each lysimeter. These samples will
be used to define the background of each lysimeter. Simi-
larly, leachate samples representing approximately 0.2 pore
volumes (about 20 liters) should be collected for baseline
characterization. Leachate should also be generated for a
second purpose: with 100 ppm bromide as a tracer, 0.2 pore
volume increments of leachate should be collected and tested
for bromide to determine the Br breakthrough curve. This
procedure confirms that sidewall flow will not shortcircuit
the system and bias the subsequent soil-pore liquid quality
data.
6.2 EXPERIMENTAL METHODS
Performance of the barrel lysimeter study (described below) involves
application of waste, management of the water budget, and sampling of soils
and soil-pore liquid.
6.2.1 Waste Application
Waste application and reapplications should be done according to the
schedule given in Table 6.1. To apply waste, remove the zone of incorpora-
tion (e.g., 15 cm) from a given lysimeter and mix the waste with the soil
at the chosen application rate(s) (see Section 5.3.1) until the mixture is
homogeneous. Lay a plastic barrier around the edge of each casing to
prevent side channel flow, as described in Appendix B. Replace the soil-
waste mixture into the lysimeter in 5 cm lifts, tamping each successive
layer if necessary, to achieve field bulk density.
6.2.2 Water Management
Lysimeters should be sheltered from normal precipitation (e.g., with
an open-sided pole barn), and instead, water should be applied in specified
amounts and timed to simulate the moisture distribution of a wetter-than-
55
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normal degradation season. The site water budget developed earlier may be
useful in terms of water added via other sources (e.g., irrigation). How-
ever, it is most suitable to choose a specific wet year from the climatic
record. After calculated losses due to run-off have been subtracted,
appropriate amounts of water may be applied according to the precipitation
record (and planned irrigation schedule, if irrigation is to be used). The
rationale of this approach is that climatically induced wet/dry cycles may
cause the waste constituents to behave differently than they would if, for
example, regularly scheduled water applications were to keep the soil
continuously moist.
6.2.3 Soil Sample Collection and Analysis
Soil samples should be collected according to the schedule described
in Table 6.1. The Tier III analysis of soil core samples collected on-site
at the time of lysimeter collection can serve as baseline samples for the
lysimeters if the two are taken from adjacent locations. If 12 lysimeters
are used, they are divided into four groups of three replications. The
first group, which receives no waste application, serves as a control; the
second group receives one waste application on day 0; the third group
receives two waste appl ications, on days 0 and 90; and the fourth group
receives three waste applications, on days 0, 60, and 120. Immediately
after the first waste application, a 200 g soil sample should be collected
from the zone of incorporation of each lysimeter; these samples should be
evaluated using Tier II analyses (Chapter 10). Thirty days following waste
application, a second 200 g soil sample is collected from the zone of
incorporation of each lysimeter for Tier I analysis. On day 60, a 200 g
soil sample is collected from each lysimeter in Group IV (Table 6.1) prior
to a second waste application, and the three samples are analyzed using a
Tier II analysis. Finally, after the waste is reapplied to the three
lysimeters in Group IV, zone of incorporation samples are collected from
all lysimeters for Tier I analysis and the sampling and waste application
routine is repeated (see Table 6.1).
On day 180, zone of incorporation and soil core samples are collected
from all lysimeters and analyzed at Tier III instead of Tier II in order to
identify possible degradation products. The three replicate soil core
samples from the respective treatments should form one core, partitioned
into 15 cm depth increments. Subsamples of the composite cores are com-
bined into 0-15, 15-45, and 45-90 cm increments and used for the initial
analysis. The remaining 15 cm core increments should be stored as reserve
samples in case a more refined estimate of hazardous constituent penetra-
tion is needed. The sampling and waste application schedule should be
continued for the next 180 days according to Table 6.1.
The experiment may be terminated when the results of soil core and
soil-pore liquid analysis are adequate to characterize degradation/immobi-
lization. In some cases, termination may occur as soon as the 180 day
analytical results are complete, assuming adequate amounts of leachate have
been generated, as discussed below.
56
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6.2.4 Soil -Pore Liquid Sample Collection and Analysis
Soil -pore liquid samples should be collected according to a schedule
based on the pore volume of the lysimeter. If the simulated water budget
is relatively "arid," or if "tight" soils limit leachate production,
leachate sampling may have to be modified to coincide with leachate produc-
tion rather than be conducted on a set schedule. In addition to the
determination of the bromide breakthrough curve described earlier, a back-
ground leachate sample equal to 0.2 pore volumes (approximately 20 liters)
should be collected from each lysimeter prior to waste application. Fol-
lowing waste application, leachate should be collected via continuous
suction until a total of 2.0 pore volumes have been gathered from each
lysimeter. Two pore volumes is considered adequate to yield usable hazar-
dous constituent mobility results. A total of five composite leachate
samples, each representing 0.4 pore volumes, should be collected, and a 2-
liter subsample of each composite leachate sample should be extracted and
subjected to a Tier II analysis. One exception is that the first sampling
of treatment group C should be analyzed at Tier III. As noted above, water
is added to the lysimeters according to a schedule based on the water
budget at the land treatment unit. Collection should continue, and the
leachate samples should be stored until the degradation study is complete
and two pore volumes have been collected. (NOTE: In arid regions or
"tight" soils, this approach may need to be modified).
6.3 DATA REDUCTION AND INTERPRETATION
The data provided by the barrel lysimeter study is used to evaluate
the potential of a waste to be adequately treated in the land treatment
system and to determine the half-life (or degradation rate) of the organic
fraction or specific hazardous organic constituents of the waste. Half-
life is defined as the time required for a 50 percent disappearance of
applied carbon (EPA, 1983A). The degradation rate of the sludge is also an
important parameter for evaluating the frequency of application of the
waste and the time required between the last application of the waste and
closure. Soil core and soil -pore liquid analyses further confirm whether
or not hazardous constituents (or pertinent nonhazardous constituents) are
being immobilized by the soil.
6.3.1 Degradation Rate and Half-Life Determination
The method used to determine degradation rate, outlined in Section
7.2.1.2 of Hazardous Waste Land Treatment (EPA, 1983), involves the ex-
traction of the organic fraction from the soil. Calculations are done
f ol 1 ows :
Oto
57
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where: Dto = fraction of organic carbon degraded over time;
Cao = the amount of carbon applied in the organic fraction of
the waste;
Cro = the amount of residual carbon in the organic fraction of
waste amended soil; and
Cs = the amount of organic carbon which can be extracted from
unamended soil .
The following equation is used to determine the degradation rate of indivi-
dual organic subfractions:
Dt1 = (6.2)
where: D = fraction of carbon degraded in subfraction i;
cai = cart>on applied from subfraction i in the waste;
Cr-j = carbon residual in subfraction i in waste amend
Csl- = the amount of carbon present in an unamended soil from
subfraction i.
The clarity of separation of all subfractions should be verified for ex-
ample by gas chromatography.
Once the degradation rates are determined, half-life of the waste or
constituents thereof may be calculated as follows (EPA, 1983):
1/2 {6.3)
where: t = time in days that the waste was degraded to generate the
data used in equations 6.1 and 6.2;
tj/2 = half-life of waste organics in soil (days); and
D^ = fraction of carbon or specific hazardous constituent
degraded in t days.
An optional method that may be used to calculate half-lives is to plot
cumulative percent carbon or specific hazardous constituent degraded as a
function of time on a semi-log scale graph. The point in time when 50
percent of the waste has been degraded may be read directly. The more
resistant compounds should be identified as possible candidates for limit-
ing constituent, and the results may be used in the follow-up acute toxi-
city testing (Chapter 5).
6.3.2 Immobilization
Immobilization is determined by data from the analysis of soil core
and soil-pore liquid samples. For the gross parameters (total organic
carbon and total extractable hydrocarbons), the data from waste amended and
control lysimeters are compared. If the quantity of either gross parameter
is significantly greater in the waste-amended lysimeters than in the con-
58
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trol lysimeters, the waste has failed the immobilization test. The waste
has also failed the immobilization test if any Appendix VIII constituent is
detected in a soil-pore liquid or lower portion of a soil core. If a
hazardous constituent is detected in one of the composite soil cores (15-45
or 45-90 cm), the core should be subsampled in 15 cm increments and re-
analyzed for the mobile constituent to further define the concentration and
rate at which the compound is moving through the soil.
59
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Chapter 7
FIELD PLOT STUDY
The treatment demonstration required under 264.272(a) can be partially
accomplished using information derived from the following field plot study.
As in the case of the barrel lysimeter study (Chapter 6), the primary
objectives of the field plot study are to demonstrate whether or not a
particular waste will be degraded, transformed, or immobilized within the
defined treatment zone. Accomplishing these objectives in the field in-
volves intensive (high sampling density) monitoring of the unsaturated zone
and the treatment zone of experimental field plots. The following field
plot design and procedure should be followed unless an alternative method
can be justified to the EPA. The duration of testing should be a minimum
of one year.
7.1 EXPERIMENTAL DESIGN
The experimental design suggested for the field plot study is a ran-
domized complete block design, with three replications of each treatment
per soil series to receive waste in the HWLT unit. Previous experience
with a well operated HWLT unit (see permitting Scenario 2 in Chapter 3) or
the results of acute toxicity testing (see Scenario 3 or 4 in Chapter 5)
should determine the waste application rate to be studied. Unless no
change in current waste loading rate is desired or anticipated, this study
should typically test three waste loading rates and should yield nine field
plots per soil series tested.
For Scenarios 3 and 4, where acute toxicity testing is employed to set
waste application rates, the concentration of waste in soil corresponding
to the LD50 is used to determine the rates. The LD50 waste concentration
is the amount of waste to be applied in a single application (kg/ha/appli-
cation). All treatments that receive waste should have this amount of
waste applied initially. The frequency of waste reapplication will then
determine the annual waste loading rate (kg/ha/year). For these two
scenarios, waste application is recommended on three schedules (Table 7.1)
resulting in the suggested three waste application rates. Treatment groups
correspond to the three replications of each treatment and their respective
waste loading rates and frequencies. As the table demonstrates, the ideal
application frequencies are semiannual, quarterly, and bi-monthly. In
relatively harsh climates such as cold northern locales, applications may
need to be limited to the warm season; however, if the local climate is
suitable for year round biological activity, the applications may be spaced
evenly throughout the year.
60
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Table 7.1. Waste Application Soil Sampling Schedule for Field Plot Study
Waste
Application
Treatment Frequency
Groups (months)
A 0
B 6
C 3
D 2
Sampling Schedule*
0 30
12 Zl
Z2 Zl
Z2 Zl
Z2 Zl
60
Zl
Zl
Zl
Z2t
Zl
Day
90
Z2
Z2
Z2t
Zl
Zl
120
Zl
Zl
Zl
Z2f
Zl
150
Zl
Zl
Zl
Zl
180
Z3
C3
Z3t
C3
Z3
C3
Z3
C3
240
Zl
Zl
Zl
Z2t
Zl
270 300
Z2 Zl
Z2 Zl
Z2f Zl
Zl
Zl Z2f
Zl
360
Z2
C2
Z2
C2
Z2
C2
Z2
C2
* Sampling schedule: Z = zone of incorporation (0-15 cm); C = core samples (0-200 cm). Levels of
analysis: 1 - Tier I; 2 = Tier II; and 3 = Tier III.
t Waste reapplication date. Analyze zone of incorporation at Tier II prior to application; collect
sample after application for Tier I analysis.
-------
Under Scenario 2, the current annual loading rate (kg/ha/yr) should be
divided into four equal applications at appropriate intervals (see above
discussion) through the year. These same single application amounts
(kg/ha/application) should be applied to the other treatments at different
intervals (i.e., every two months and six months) to yield three annual
loading rates. As for the above scenarios, Table 7.1 may be used as a
guide to waste application and soil sample scheduling.
7.1.1 Plot Preparation
While the location of experimental plots on the HWLT unit is deter-
mined to some extent by the location of representative soils, ease of
access and isolation from existing waste treatment must also be considered.
Plots should be located so that al 1 si ope positions are represented. A
scale drawing depicting the location of the plots on the facility and
indicating treatments to be applied to each plot should be included in the
treatment demonstration plan required under §270.20(a).
7.1.1.1 Size-
Each experimental field plot should be 12 feet (3.6 meters) wide by 48
feet (14.4 meters) long with a defined treatment zone up to 1.5 meters
deep. Larger plots may be used if application techniques require a larger
area. However, with larger plots, more monitoring samples are necessary to
maintain the same density of sampling.
7.1.1.2 Slope—
The slope on which a field plot is established should be representa-
tive of the HWLT unit as a whole (e.g., if the unit is in a rol 1 ing nil 1
setting, field plots should not be placed on level ground alone). In all
cases, plots should run up and down the slope to include variability due
to slope in the data analysis.
7.1.1.3 Plot Isolation—
The experimental field plots should be isolated from existing waste
treatment areas using berms around and between plots to eliminate the
possibility of cross contamination from existing waste. The berms, which
can usually be constructed from on-site materials, need to be high enough
and wide enough to contain stormwater flow. Additionally, they must meet
40 CFR 264.273(c) and (d) requirements for run-on control and run-off
containment from a 24 hr/25 yr storm.
7.1.1.4 Run-off Collection-
Small sumps or impoundments at the low slope position of each plot are
needed to contain run-off in order to prevent off-site contamination. The
size of the collection area is calculated based on the water balance com-
puted for the site. Run-off collection ponds should be designed to contain
run-off from the 24 hr/25 yr storm for the treatment demonstration site or
individual plots.
62
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7.1.2 Number, Location, and Installation of Soil-pore Liquid Samplers
Each plot normally should have two each of two sampler types, the
pressure-vacuum porous ceramic cup (Figure 7.1) and the pan design (Figure
7.2), with the samplers located as shown in Figure 7.3. Up to three of
each sampler per plot may be needed or desired in some cases, so Figure 7.3
reflects this arrangement. The outline below should be followed during the
installation of the sampler.
1. Cut trenches for sample collection tube using a ditching
machine or other piece of equipment.
2. Dig installation pits 5.5 ft x 6 ft (approximately) as lo-
cated on Figure 7.3. As it is removed, segregate soil by
horizons for later replacement.
3. Install soil-pore liquid samplers (Figure 7.4).
4- Install sample col lection stations (Figure 7.5 and Figure
7.3).
5. Back-fill pits and trenches, replacing soil horizons in
proper sequence and compacting the soil to field bulk density
in lifts. Some settling may occur if trenches have not been
backfi11 ed properly.
6. Grade site to desired slope.
Locate trenches and pits as indicated in Figure 7.3 to minimize the area of
disturbance on the plots. After the site is graded, the plots are ready to
receive waste. More detailed descriptions of the sampler types may be
found in Section 7.2.2 and in EPA (1984). The latter reference also in-
cludes detailed instructions for sampler installation and operation.
7.2 EXPERIMENTAL METHODS
The performance of the field plot study involves application of waste,
site management, and sampling of soils and soil-pore liquid.
7.2.1 Waste Application
Application of waste onto experimental plots should duplicate the
procedures to be used on the land treatment unit. Even distribution of the
waste over the plots is very important. Incorporation of waste into the
soil should, if possilbe, be accomplished with the same type of equipment
that will be used on the HWLT unit.
63
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cr>
POROUS -
CERAMIC
CUP
SAMPLE DISCHARGE
HOSE
PRESSURE/VACUUM
HOSE
VACUUM
I— PRESSURE
FIGURE 7.1 POROUS CUP SOIL-PORE LIQUID SAMPLER AND PRESSURE
VACUUM PUMP USED TO COLLECT SAMPLE.
-------
en
tn
12
GEOTEXTILE
FIBER
HOLLOW SAMPLE
STORAGE AREA
X
TO SAMPLE
COLLECTION
EQUIPMENT
FIGURE 72 GLASS BRICK SOIL-PORE-LIQUID SAMPLER (PAN TYPE)
-------
O1
TRENCH
6"wld«x30"dt«p
SOIL PORE LIQUID SAMPLERS
D GLASS BRICK (FIGURE 7.2)
Q PRESSURE/VACUUM-
POROUS CERAMIC CUP
(FIGURE 7.6)
INSTALLATION PITS
66" x 72" (opprox.)
SAMPLING STATION
FIGURE 7.3. SOIL PORE LIQUID SAMPLE LOCATIONS IN FIELD PLOTS
-------
PIT SIDE WALL
•TO SAMPLE STATION
PAN TYPE SAMPLER
PIT SIDE WALL
TO SAMPLE STATION
PRESSURE/VACUUM SAMPLER
FIGURE 7.4. INSTALLATION OF SAMPLERS IN PITS
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4 PVC CAP
3/8 PLEXIGLASS PLATE
4" PVC
1/4" 1.0. LATEX TUBING
I/4"O.D. POLYTUBING
FIGURE 7.5. SOIL-PORE LIQUID SAMPLING STATION
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7.2.2 Plot Management
Management of field plots, which should simulate conditions that will
occur under ful 1-scale operation of the HWLT unit, requires 1) tillage,
which must be practiced in the field plot study, 2) irrigation/drainage,
and 3) soil amendment. Soil amendments should include liming of soil as
necessary to maintain a near neutral pH and adding nitrogen fertilizer to
reduce the carbon:nitrogen ratio of waste/soil mixture to at least 100:1.
More guidance on unit management practices may be found in EPA (1983A).
7.2.3 Sample Collection and Analysis
Monitoring of experimental plots, designed to ensure accurate assess-
ment of waste treatability, involves both soil core and soil-pore liquid
sampling and analysis. Analysis of soil cores is necessary to monitor the
behavior of hazardous constituents present in the treatment zone, to
identify any possible degradation products, and to detect slowly migrating
hazardous constituents below the treatment zone.
The monitoring schedule shown in Table 7.1 is designed to sample soil
at frequent enough intervals to determine whether a waste is being de-
graded, immobilized, or transformed and whether hazardous constituents are
passing below the treatment zone. To set a zero time for degradation and
half-life determinations, ZOI soil samples must be taken immediately after
the initial waste application and incorporation. Note that soil core
samples need only be taken at the same frequency as soil-pore liquid sam-
ples (Table 7.1).
Zone of incorporation soil samples and soil cores should be collected
at random on each plot with an appropriate device (e.g., Shelby tube sam-
pler). EPA (1984A) provides guidance on the appropriate sampling device
for specific soils. Scheduled ZOI samples should be collected to a depth
of 15 cm, and soil core samples should be collected to a depth of two
meters for a 1.5 m treatment zone, with analysis of each 15 cm section. At
a minimum, six sample locations per plot are required for both zone of
incorporation and soil core samples. Samples may be composited within
plots to provide one composite sample (or set of samples) for analysis per
plot for each sampling date.
During waste characterization (Chapter 2), a subset of Appendix VIII
constituents may have been identified. This does not, however, eliminate
the need to analyze at Tier III some time during the first year of the
field plot demonstration, since degradation products which were not present
in the waste initially may appear or a constituent may build up to above
detection limits after successive waste applications. Therefore, Tier III
analysis should be performed on ZOI samples obtained from plots in treat-
ment group C (i.e., the highest waste loading rate tested) at 180 days. In
this case, Tier III should include the list of compounds for which the
potential hazardous degradation products based on an assessment of degrada-
tion pathways for the parent compounds. All other samples should be ana-
lyzed at Tier I or Tier II as indicated in Table 7.1.
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7.2.4 Soil-Pore Liquid Sample Collection and Analysis
Percolating water added to the soil by precipitation, irrigation,
snow-melt, or waste applications may pass through the treatment zone and
rapidly transport some mobile waste constituents or degradation products
through the unsaturated zone to the groundwater. Soil-pore liquid monitor-
ing is intended to detect these rapid pulses of contaminants since they may
not be observed through the analysis of soil cores. For this reason, the
timing of soil-pore liquid sampling is a key to the usefulness of this
technique. Seasonality is the rule with soil-pore 1iquid sample timing
(i.e., scheduled sampling cannot be done on a preset date in many areas,
but must be geared instead to major leachate generating events). Soil-pore
liquid sampling in the field plot demonstration is used to determine if any
mobile hazardous constituents are leaving the treatment zone.
As previously indicated, two types of soil-pore liquid samplers are
needed for the field plot study: the pan-type soil-pore liquid sampler
(Figure 7.2) and the pressure-vacuum, porous cup soil-pore liquid sampler
(Figure 7.3). These two types of soil-pore liquid samplers are described in
detail in EPA (1984A). While each sampler has advantages and disad-
vantages, one major reason for using pan lysimeters is to confirm whether
large quantities of leachate are flowing through structural macropores and
possibly bypassing much of the soil's treatment capacity. In highly struc-
tured soils which allow a high flux of liquid (e.g., after precipitation or
irrigation), the pan type sampler collects a sample very efficiently be-
cause it acts as a textural discontinuity in the soil profile, forming a
perched water table above the pan surface. Water then flows through the
holes in the top surface to be collected and stored in the collection area
(Figure 7.2). The sample must be removed soon (e.g., within 24 hours)
after a rapid influx of liquid to prevent sample quality changes within in
the pan type sampler.
Under moist conditions with a low flux of moisture and little macro-
pore flow, the pressure-vacuum soil-pore liquid samplers may more effi-
ciently collect a soil-pore liquid sample. However, proper operation of
the pressure-vacuum sampler is essential (see EPA, 1984B). Timing the
removal of the sample for analysis is determined by soil moisture condi-
tions, and once the amount of time required to fill the storage capacity of
the sampler is determined, samples should be collected within 24 hours to
assure good quality. Both types of samplers must be checked frequently to
monitor the accumulation of the sample (with pan-type) or to see if the
sample can be obtained (with pressure-vacuum type).
If one of the two sampler types performs decisively better after 90
days, the other may be eliminated for the remainder of the study. Finally,
soil-pore liquid samples should be collected using the one sampler type
every 90 days or as liquid is available. For each sampling date, all
liquid obtained from samplers of the same type within each plot should be
composited, resulting in three replicate liquid samples per treatment per
quarter.
While analysis of soil-pore liquid samples should be at Tier III for
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the first sampling date for treatment group C, Tier II analysis will suf-
fice for all other sample sets.
7.3 DATA REDUCTION AND INTERPRETATION
The data provided by the field plot study is used to evaluate the
potential of a waste to be adequately treated in the land treatment system
and to determine the half-life (or degradation rate) of the organic frac-
tion or specific hazardous organic constituents of the waste. Half-life is
defined as the time required for a 50 percent disappearance of applied
carbon (EPA, 1983A). The degradation rate of the sludge is also an impor-
tant parameter for evaluating the frequency of application of the waste and
the time required between the last appl ication of the waste and closure.
Soil core and soil-pore liquid analyses further confirm whether or not
hazardous constituents (or pertinent nonhazardous constituents) are being
immobilized by the soil.
7.3.1 Degradation Rate and Half-Life Determination
The method used to determine degradation rate, outlined in Section
5.3.2.3.2 of Hazardous Waste Land Treatment (EPA, 1983), involves the ex-
traction of the organic fraction from the soil. Calculations are done
fol1ows:
where: Dto = fraction of organic carbon degraded over time;
Cao = the amount of carbon applied in the organic fraction of
the waste;
CrQ = the amount of residual carbon in the organic fraction of
waste amended soil; and
C. = the amount of organic carbon which can be extracted from
unamended soil.
The following equation is used to determine the degradation rate of indivi-
dual organic subfractions:
Dti = (7.2)
where: Dtl- = fraction of carbon degraded in subfraction i;
C^! = carbon applied from subfraction i in the waste;
C*] = carbon residual in subfraction i in waste amended soil; and
C ] = the amount of carbon present in an unamended soil from
subfraction i.
The clarity of separation of all subfractions should be verified for ex-
ample by gas chromatography.
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Once the degradation rates are determined, half-life of the waste or
constituents thereof may be calculated as follows (EPA, 1983):
(7.3)
where: t = time in days that the waste was degraded to generate the
data used in equations 7.1 and 7.2;
= half-life of waste organics in soil (days); and
* = fraction of carbon or specific hazardous constituent
degraded in t days.
An optional method that may be used to calculate half-lives is to plot
cumulative percent carbon or specific hazardous constituent degraded as a
function of time on a semi-log scale graph. The point in time when 50
percent of the waste has been degraded may be read directly. The more
resistant compounds should be identified as possible candidates for limit-
ing constituent, and the results may be used in the follow-up acute toxi-
city testing (Chapter 5).
7.3.2 Immobilization
Data from sampling for hazardous constituent leaching should be com-
pared statistically with background concentrations. If either soil core or
soil-pore liquid data indicate a leaching hazard at the waste loading rates
tested, a reduced waste loading rate is in order. The optimum treatment
within the field plot study is the treatment that allows for the largest
application rate at the greatest frequency without migration of hazardous
constituents below the treatment zone.
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Chapter 8
DATA INTERPRETATIONS
Following completion of the field plot or lysimeter study, the data
which has been accumulated from on-site field studies, barrel lysimeter or
field plot tests, and the Microtox™ test may be interpreted to form the
basis for the treatment demonstration. The interpretation of these data
will be used to determine 1) the maximum residual concentration of specific
hazardous organic constituents (Chapter 5), 2) the waste degradation rate
(Chapters 6 and 7), 3) the waste application rate and frequency, 4) the re-
quired unit area, and 5) the anticipated unit life. While interpretations
of items (1) and (2) are found in the appropriate sections of Chapters 5,
6, and 7, the remainding information, some of which has been modified from
Hazardous Waste Land Treatment (Brown et al., 1983), is presented in this
chapter.
8.1 WASTE APPLICATION LIMIT
The first parameter that should be determined is the amount of waste
that can safely be applied in a single application (mass/area/application).
Although this parameter can be determined by the LD50 (calculated from the
Microtox™ test, Section 5.4), acute toxicity may not always be the most
restrictive factor influencing waste application rate. For example, the
waste application rate may have to be reduced in situations where leaching
of undesirable constituents occurs at the optimum application rate for
degradation. In these situations, the application limiting constituent
(the constituent that limits the amount of waste that may be applied in a
single dose) may be determined through leaching observations conducted as
part of the barrel lysimeter (Section 6.2.4) or field plot (Section 7.2.4)
studies. Thus, the amount of waste on a given area per application is
limited by either the acute toxicity or the mobility of waste constituents.
The ALC is typically lost very rapidly from the soil; however, overloading
in a single application may present a hazard to human health or to the
environment or may drastically inhibit soil biological activity.
8.2 ANNUAL WASTE LOADING RATE
The limit of how much waste may be applied in a single application
(based on the ALC) combined with the frequency of application yields the
first estimate of the annual waste loading rate (mass/area/year). The
experimental designs suggested for the barrel lysimeter study (Chapter 6)
and the field plot study (Chapter 7) include testing this ALC-determined
application limit at several frequencies and monitoring the tests' yielded
data on degradation rates and mobility for the specific hazardous con-
73
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stituents found in the waste. Further, acute toxlcity testing of three or
more of the most resistant organic constituents identifies the constituents
of greatest concern according to their potential toxicity to soil biota
(LC8o). The following guidelines permit the appropriate application rate
and frequency to be chosen.
1) For each resistant organic compound tested, choose the
frequency of application at which the compound exhibits the
shortest half life (T1/2);
2) Depending upon the concentration of each compound in the
waste and the choice of frequency from step 1, calculate the
respective annual loading rate for each compound as follows:
4)
x C,
w
where:
uyr
LR
= the rate of application of the compound or frac-
tion of interest to soil (kg/ha/yr);
= annual waste loading rate tentatively estimated
using the application limit and frequency for
the compound of interest (kg/ha/yr);
Cw = concentration of the compound or fraction of
interest in the bulk waste (kg/kg) from waste
analysis.
3) Calculate the macimum accumulation that will occur for each
compound:
where:
'max
cmax = 2 x Cyr x T1/2
maximum accumulation that will occur during the
unit life under th given conditions (kg/ha);
Tl/2 = half
life of
Chapter 6 or 7
the compound
(yr).
as calculated in
Compare compounds using the ratio of the Cmax to the critical
concentration in soil (Ccr1t) at which toxicity occurs, as
measured by the LD8Q in the acute toxicity test (Chapter 5).
Among those constituents that exhibit a ratio of greater than
1, the constituent having the largest ratio is termed the
rate limiting constituent (RLC). If no constituent has a
ratio greater than 1, there is effectively no RLC in the
degradable organics fraction.
5) Calculate an adjusted annual waste loading rate with the
equations below and the derived values for the parameters:
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and
LRRLC
where:
LRmr = the adjusted annual waste loading rate based on
the RLC (kg/ha/yr).
The above procedure leads the applicant to a loading rate that may be
incorporated into the final facility permit (permit Scenario 2) or that may
be managed on the unit during the two year follow-up study (Scenarios 3 and
4). If, however, a Teachable constituent constrains waste applications to
lower rates due to potential groundwater hazards, this more restrictive
condition supersedes waste degradation as the limiting factor. Mobility
results and the associated calculations are discussed in the interpretation
sections of Chapters 6 and 7.
8.3 REQUIRED UNIT AREA
After the most limiting constituents are identified, the final deci-
sions on the required land area and the minimum number of applications per
year are made using the following calculations:
A =
where:
A = required treatment area (ha);
PR = waste (wet weight) production rate (kg/yr); and
LRRLC = waste loading rate based on the RLC (kg/ha/yr).
If the value calculated for A is greater than the area available for
treatment, 1 and treatment cannot accommodate al1 of the waste produced.
NA =
where:
NA = number of applications per year and is equal to
the smallest integer greater than or equal to
the actual value calculated;
LRRLC = waste loading rate based on the RLC (kg/ha/yr);
and
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AL = application limit based on the ALC
(kg/ha/applicaton).
8.4 UNIT LIFE
The land treatment unit life and concomitant choice of a capacity
limiting constituent (CLC) are predicted in a relatively straightforward
manner. The choice may be based purely on a calculation approach rather
than on any particular piece of data from the LTD. Three classes of
potentially conservative constituents have been identified: 1) metals, 2)
phosphorus, and 3) inorganic acids, bases, and salts. Calculating a unit
life based on each allows the design unit life and CLC to be chosen as that
constituent which is the most restrictive. Phosphorus is redistributed
throughout the treatment zone while salts (if conserved, such as in cli-
mates or soil drainage conditions where they usually accumulate and do not
leach) tend to accumlate near the surface and thus can be described by the
following equation:
UL =
where:
UL = unit life (yr);
LCAPpS = waste loading capacity beyond which the CLC will
exceed allowable accumulations (kg/ha); and
LRRLC = waste loading rate based on the RLC (kg/ha/yr).
Since metals, by contrast, are practically immobile and are mixed in
the waste with a heterogeneous matirx of water, degradable organics, mobile
consituents, and nondegradable residual solids, waste application is not
merely the addition of a pure element to soil. Because residual solids
fraction (RS) adds to the original soil mass, wastes containing high RS
concentrations can significantly raise the level of the land treatment unit
as well as limit the amount of soil which can be used to dilute the waste.
If the concentration of a given metal in the RS of a waste is less than the
maximum allowable concentration in soil, the given metal cannot limit waste
application. The metal with the largest ratio greater than one is the
possible CLC, and unit life is determined as follows:
1) determine the concentration (ca) of the metal in the waste
residual solids (mg/kg);
2) calculate the residual solids loading rate from the equation;
LRRLC x (wei9nt fraction of residual
solids in waste)
z. = x 1(T5
3 BRS
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where:
za = volumetric waste loading rate on a residual
solids basis (cm/yr);
BRS = bulk density of residual solids, assumed to be
the same as that of the soil after tillage and
settling (kg/1); and
10~5 = conversion factor from 1/ha to cm;
3) choose a tillage or waste-soil mixing method and determine
the "plow" depth (zp) in cm;
4) from the background soil analysis, obtain the background
concentration (mg/kg) of the given metal (cpo);
5) from reference to the specific metal in Chapter 6 of
Hazardous Waste Land Treatment (EPA, 1983) of that metal
(mg/kg);
6) using these quantities, solve for n in the following equation
(Chapra, unpublished paper) where n is the number of
applications which result in the concentration of the surface
layer being cpn:
n =
7) determine the corresponding unit life as:
UL = nt.
a
where: ta = time between applications.
The equation idealizes the process of application and plowing as a
continuous process. To do this, the following assumptions must be made:
1) that sludge is applied at equal intervals, ta in length.
2) that the sludge always has the same concentration ca.
3) that the sludge is always applied at a thickness of za.
4) that there is complete mixing of the surface layer to depth
Zp due to plowing.
5) that the plowed soil and the sludge have equal porosity.
6) that the annually applied waste degrades and dries approxi-
mately down to residual solids.
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Finally, a design unit life (years) is chosen from among salts, phos-
phorus, and metals, with the shortest life of the three the desired value.
For many waste constituents, inadequate information is available to pro-
perly assess loading rates. Pilot experiments and basic research are
needed in this area to begin to develop an understanding of the fate of
various constituents in soil; however, such research is beyond the scope of
this document. When land treatment is proposed for a waste constituent
about which only scant knowledge is available and for which no pilot
studies have been conducted, the loading rate chosen for such a constituent
should be conservative to provide a factor of safety.
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Chapter 9
TWO YEAR FOLLOW-UP STUDY
The interpretation of the data obtained up to this point in the land
treatment demonstration has been explained in respective chapters and
assembled comprehensively in Chapter 8. The information now tentatively
known about unit performance includes:
1) degradation rate and half-life of waste organics, including
specific constituents;
2) mobility of waste constituents at varying waste loading
rates; and
3) tentative waste loading rates to be confirmed in follow-up
field monitoring.
If the waste is land treatable, determined by data collected to this
point, the follow-up study mentioned above may be needed to verify this
data for permitting Scenarios 3 and 4 {see Chapter 3). The owner/operator
of the HWLT unit applies waste to full scale land treatment plots during
the two year follow-up study. Monitoring, analysis, and interpretation is
accompl i shed according to the following schedule of sample density and
frequency.
9.1 SOIL CORE SAMPLES
Soil sampling during the two year follow-up study differs from opera-
tional monitoring at a full scale facility in that samples are taken from
the surface to 2 meters. Unsaturated zone monitoring requirements for
hazardous waste land treatment units call for sampling only the layer
immediately below the treatment zone (Part 264.278). Otherwise, the sam-
pling density and frequency are essentially comparable to an operational
monitoring plan, including compositing by pairs.
The suggested minimum number of soil cores is 6 per uniform area, to
be taken from locations chosen at random at a minimum rate of one sample
per two acres; soil core samples should be collected to a 2-meter depth in
15 cm increments. In addition to the random samples, two more cores should
be collected per uniform area if any sites on the facility are considered
to be anomalous (e.g., toe of slope or swales where waste may collect in
larger quantities than is common for the uniform treatment area). Cores
should be collected quarterly.
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9.2 SOIL-PORE LIQUID MONITORING
Soil-pore 1iquld monitoring devices should be installed at random
locations on the land treatment unit a minimum rate of one per four acres
with at least three samplers installed per uniform area. Installation and
sampling procedures are described in detail in EPA (1984A). Samples are to
be collected and analyzed quarterly.
9.3 SOIL CORE AND SOIL-PORE LIQUID SAMPLE ANALYSIS
An interpretation of data generated in the previous stages of the land
treatment demonstration may be used to reduce the list of constituents that
must be analyzed for in the follow-up study. Those constituents that
potentially pose a mobility hazard or that are resistant to degradation may
be justified as indicator parameters. Nonhazardous constituents may be
helpful in reducing the long term costs associated with monitoring; in
order to qualify, however, such a constituent's behavior must correlate
well with the hazardous constituents of concern. If a constituent is
chosen on the same basis, it is official ly termed a "principal hazardous
constituent (PHC)" according to 40 CFR 264.278(a)(2). (PHC's are defined
as "hazardous constituents contained in the wastes to be applied at the
unit that are the most difficult to treat, considering the combined effects
of degradation, transformation, and immobilization.") Analysis of both
soil core and soil-pore liquid necessarily includes these indicator consti-
tuents (i.e., "PHC's") in addition to the Tier I analysis described in
Chapter 10.
9.4 INTERPRETATION
The purpose of the follow-up study is to determine if the assumptions
made based on the short-term field plot or barrel lysimeter study will hold
for the long term under ful 1-scale operation. Success or fail ure stil 1
depends upon whether or not the waste is degraded, transformed, or im-
mobilized within the treatment zone, as determined by the monitoring
results.
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Chapter 10
TIERED SAMPLE ANALYSIS
To minimize the cost of sample analyses and still obtain sufficient
information for a treatment demonstration, three tiers of sample analyses
are employed (Table 10.1), with each higher tier involving a more intensive
group of analyses than the previous one. The intensity of the sample
analysis depends on the source of the sample and the information required.
10.1 TIER I
This tier includes gross parameters that can be measured by relatively
simple techniques. All samples collected are analyzed to at least the Tier
I level, with evaluated parameters including, but not limited to, water,
ash, solids, soluble salts, total nitrogen, total phosphorus, pH, total
organic carbon, and total extractable hydrocarbons.
10.2 TIER II
Tier II analyses include, in addition to the gross parameters
evaluated in Tier I, the hazardous organic constituents that were identi-
fied in:
1) Tier III waste analysis;
2) the preliminary reconnaissance site sampling and analysis
program (Chapter 2); and
3) (for new sites with no history of waste applications to soil
at the site or in surrounding areas) the Tier III analytical
results from the 180th day soil and leachate sampling of the
barrel Isyimeter or field plot study (Chapter 6 or 7).
The constituents analyzed in Tier II are not to be confused with the
"principle hazardous constituent" (PHC) described in the land treatment
regulations (40 CFR 264.278(a)(2)); PHC's are intended to be indicators
chosen for monitoring purposes in the final operational monitoring program.
These constituents cannot be chosen effectively until the experimental
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Table 10.1. Components of Analytical Tiers Used in the Land Treatment
Demonstration
Tier
Parameters Measured
Reference for
Analytical Procedure
Tier I
Tier II
Tier III
Water
Ash
Soli ds
Soluble Salts
Total Nitrogen
Phosphorus
Total
PH
Total
Organic Carbon
Total Extractable Hydrocarbons
All Tier I Parameters
Hazardous Organic Constituents
Identified in the Waste or
Waste-Soil Mixture
All Metals Present in Waste
(totals, NOT EP Toxic)
All Tier I Parameters
Total Metals
Total Organic Halogens
Volatile Organic Constituents
Appendix VIII Hazardous
Constituents or Those Known
or Suspected to be in the
Waste or Waste-Soil Mixture
EPA (1983A)
Rhoades (1982)
Bremner and Mulvanex (1982)
01 sen and Summers (1982)
McClean (1982)
Nelson and Summers (1982)
EPA (1982)
EPA (1982)
EPA (1982)
EPA (1982)
EPA (1982)
EPA (1982)
portions of the LTD are complete. As discussed in Chapter 3, PHC's may be
chosen for the two-year, follow-up study monitoring program since this
phase of the LTD follows the experimental phase and is, in essence, a full
scale operation.
10.3 TIER III
The most comprehensive analytical program conducted, Tier III includes
(in addition to the Tier I analyses) analyses for total metals, total
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organic halogens, volatile organic constituents, and al 1 Appendix VIII
constituents or a justifiable subset of those known or suspected to be in
the waste or its degradation product. As the organic characteristics of
hazardous waste streams are better defined by an increasing national data
base, it may be possible to eliminate some compounds from the list; how-
ever, others may possibly be added. For example, EPA (Skinner, 1984) has
compiled a list of 89 Appendix VIII constituents suspected to be present in
refinery wastes. This list may be used for Tier III analysis for these
wastes. The rapid acquisition of new data may allow further modifications
to this EPA list for refinery wastes.
10.4 QUALITY ASSURANCE/QUALITY CONTROL
Before the first sample is collected for analysis as part of a treat-
ment demonstration program, a quality assurance/quality control (QA/QC)
program must be installed to ensure the integrity of the resulting data. A
quality assurance program is an integral part of the overall program be-
cause the analytical data it generates is used to determine the treatment
potential of a specific hazardous waste. The primary goal of the quality
assurance program is to ensure the fol lowing: that al 1 testing be con-
ducted according to proper scientific procedures, that testing be directed
and performed by qualified individuals, that the physical facilities be
operated in the proper manner, and that data recording, handling, storage,
and retrieval be carried out or-maintained in a scientifically sound man-
ner. The development of standard operating procedures and a quality
assurance program will contribute significantly to the quality and reli-
ability of the analytical data. A quality assurance program for a land
treatment demonstration program should include procedures which address
laboratory testing, field studies, and data handling. Specifically, the
quality assurance program should address:
1) A detailed flow scheme of the work to be performed during the
land treatment demonstration program; individuals responsible
for each specific test procedure, including chemical analysis
and data interpretation; approximate dates of sampling and
analysis.
2) Detailed procedures to ensure the collection of representa-
tive soil or waste samples; procedures for a sample receipt
log that will include information on storage conditions,
sample distribution, and sample identification.
3) A master schedule for tracking all samples through the
screening program. This schedule should include the test
performed, individual responsible, and dates of initiation
and completion.
4) Standard operating procedures (SOP's) which outline specific
details of each test procedure and associated QA/QC require-
ments.
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5) A study folder for each waste screened that includes the
study protocol, a complete set of raw data for each test
procedure, the Individual generating the data, and the data
generating dates.
6) A complete report for each waste that includes data calcula-
tions and interpretations from each test procedure.
In addition, all analytical procedures should be done according to test
methods approved by the EPA. Any deviations from approved procedures
should first be documented for review by the laboratory QA officer and then
approved by the laboratory director. Additional information on QA/QC
procedures can be obtained from EPA (1982) and EPA (1980).
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APPENDIX A
SOIL SAMPLING AND ANALYSIS
A.I SOIL SAMPLING
The methods used for soil sampling are variable and depend partially
on the size and depth of the sample needed and the number and frequency of
samples to be taken. Of the available equipment, Oakfield augers are
useful if small samples need to be taken by hand, while bucket augers give
larger samples.
Different sections of this protocol require different methods for
sampling (e.g. for the soil survey, surface soil sampling will predominate
making the Oakfiled Auger an appropriate tool). Powered coring equipment
is the preferred choice for sampling existing sites and field plots, since
it can rapidly sample to the desired depths and provide clean, minimally
disturbed samples for analysis. Due to the time involved in coring to
1.5 m and farther, powered equipment can often be less costly than hand
sampling. In any case, extreme care must be taken to prevent cross con-
tamination of samples. Loose soil should be scraped away from the surface
to prevent it from contaminating samples collected from lower layers. For
further discussions of soil sampling please refer to
Unsaturated Zone Monitoring for HWLT Units (EPA, 1984A), Soil Chemical
Analysis (Jackson, 1967) or Methods of Soil Analysis (Black, 1965).
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Soil Moisture Sampler Sample Record
Plot No. Sample No.
Sampler Type Laboratory No.
Liquid Volume Split Sample Yes No
Collectors Name(s)
Date Time
Date Sent to Lab
Method of Preservation
Destination of Sample
Destination of Split Sample
Remarks:
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Soil Core Sample Record
Plot No. Sample No.
Composite Depth Laboratory No.
Sample Random Coordinates Split Sample Yes No
a) c)
b) d)
Collectors Name(s)
Date Time
Date Sent to Lab
Method of Preservation
Destination of Sample
Destination of Split Sample
Sample Comments:
a) c)
b) d)
87
-------
CHAIN OF CUSTODY RECORD
oo
oo
PRO). NO.
PROJECT NAME
(Si|ntl»fl)
STA.
NO.
DATE
TIME
STATION LOCATION
NO. OT
ONTAINERS
til (Si|»ll»M> Otli/Ti*f) Rtoiof'
Dill/Tint
_
(S'ifnttvrt)
REMARKS
Ditt/Tim
-------
00
UD
PROJFCT NO TRFATMFNT
OATF ppppAppn BY
SAMPI F NO S fT
CT
HIT
DA DAUPTCTD
r*A K AM c T c. n
) SAMPLE WT.tvo
)
)
) r
ng. DRY WT.Wflutlc
SAMPLE NO.
I
n
JB
«) mg H 0 1L
T*SO
FIGURE 6.1 SAMPLE DATA SHEET FOR "Bbl LYSIMETER" OR "FIELD PLOT" STUDY.
-------
A.2 ANALYTICAL METHODS FOR SOILS
A.2.1 Physical Methods
Soil physical characteristics affect the long-term use of the soil for
land treatment. In contrast, chemical properties are of extreme importance
in the short-term. Chemical properties can be more easily modified and
changed than physical properties.
A.2.1.1 Particle Size Analysis (Hydrometer Method) —
This method depends on the rate at which soil particles settle from a
water suspension. The soil particles are put into suspension by mechanical
stirring with the aid of a dispersing agent.
Temperature is reported in the sedimentation procedure since the
density and viscosity of water changes with temperature. As the tempera-
ture increases, the time required for particles to settle out of suspension
decreases. The hydrometer is usually calibrated for 19.4 or 20°C (67 or
68°F). For each °F above the hydrometer calibration temperature, 0.2 g is
added to the reading. Conversely, 0.2 g is subtracted from the hydrometer
reading for each °F below.the calibration temperature.
A. 2.1.1.1 Chemicals—
a. Dispersing agent: Dissolve 35.7 g sodium metaphosphate (NatPOo)^)
(Fisher Scientific Company No. S-333 or equivalent) and 7.94 g sodium
carbonate (NapC03) in distilled water and dilute to a volume of
1 liter. ThelJa2C03 is used as an alkaline buffer to prevent the
hydrolysis of the metaphosphate back to orthophosphate which occurs
in acidic solutions. NOTE: Instant Calgon available from Calgon Cor-
poration, Pittsburgh, PA can be substituted.
b. Distilled water.
A.2.1.1.2 Materials—
a. Bottles, French square, 1 liter (32 oz) with caps.
b. Shaker, horizontal reciprocating type, 6.3 cm (2.5 in) stroke, 120
strokes per minute.
c. Glass sedimentation cylinder with markings at the 1130 ml and 1205 ml
levels (Bouyoucos cylinder).
d. Standard hydrometer (ASTM 152 H, with Bouyoucos scale in grams per
liter).
e. Balance, can be read to 0.1 g.
90
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f. Plunger. NOTE: This can be made using 3 mm (0.125 in) diameter wire.
At one end make a circle 5.5 cm (2.125 in) in diameter. The wire
should be manipulated so the handle extends at a right angle from the
center of the circle for 56 cm (22 in). Stretched rubber bands
bisecting the wire circle are spaced around the circumference until it
is largely covered by rubber bands overlapping at the center.
g. Thermometer, 0-100°F.
.2.1.1.3 Procedure—This procedure is modified from Bouyoucos (1951).
a. Weigh 50 g (oven-dried at 105°C overnight) of a fine textured or 100 g
of coarse textured (90-100% sand) soil and place in a shaker bottle.
b. Add 125 ml of dispersing agent and 400 ml of distilled water to shaker
bottle.
c. Cap bottle snugly and place horizontally on a reciprocating shaker for
16 hours at 120 strokes per minute.
d. Remove bottle and bring suspension to room temperature.
e. Wash all contents of shaker bottle into a sedimentation cylinder.
f. Set cylinder in a place away from vibrations.
g. Place hydrometer in suspension.
h. Fill to lower mark (1130 ml) with distilled water for a 50 g sample.
Fill to upper mark (1205 ml)for a 100 g sample.
i. Remove hydrometer. Take plunger in one hand and hold the cylinder
with the other. Strongly move plunger up and down being careful not
to spill contents of cylinder.
j. After all sediment is off cylinder bottom, carefully remove plunger
and record time immediately. NOTE: Add a drop of amyl alcohol if the
surface is covered with foam and restir the suspension if necessary.
k. Record hydrometer reading at meniscus top at the end of 40 seconds.
NOTE: About 10 seconds before taking reading, carefully insert
hydrometer and steady by hand.
1. Remove hyrometer from suspension. CAUTION: Do not leave hyrometer in
suspension longer than 20 seconds as particles will settle out on its
shoulders.
m. Measure and record suspension temperature. For each °F above the
calibrated temperature of the hydrometer add 0.2 g to the reading.
For each °F below the calibrated temperature subtract 0.2 g.
n. Record corrected hydrometer reading.
91
-------
o. With the plunger, restir suspension. Take a reading at the end of two
hours. Correct hydrometer reading (see step m) and record corrected
hydrometer reading.
p. Make 3 blanks by placing 125 ml of dispersing agent in 3 sedimentation
cylinders. NOTE: Blanks should be run for each new batch of
dispersing agent.
q. Fill cylinders two-thirds full with distilled water. Insert hydro-
meter and fil 1 cylinder to the lower mark (1130 ml) with distil led
water.
r. Take hydrometer reading and temperature of suspension. Correct
hydrometer reading using step m.
A.2.1.1.4 Calculations—
a. Dispersing agent correction factor = Sum total of temperature
corrected hydrometer readings of blanks/3.
b. Weight corrected 2 hour reading = (Temperature corrected 2 hour
hydrometer reading) - (Dispersing agent correction factor).
c. Weight corrected 40 second reading = (Temperature corrected 40 second
hydrometer reading) - (Dispersing agent correction factor).
d. % Clay = (Weight corrected 2 hour reading/oven-dry weight of total
sample) x 100.
e. % Silt = [(Weight corrected 40 second reading - Weight corrected 2
hour reading)/oven-dry weight of total sample] x 100.
f. % Sand = 100 - (% clay + % silt).
A.2.1.2 Bulk Density--
Soil bulk density determination is based on two measurements, a mass
measurement and a volume measurement. The mass is measured by oven drying
the sample at 105°C until a constant weight is obtained. The bulk volume
measurement includes the space between the soil particles as well as the
space occuppied by the soil parti Ices. Bulk density, the ratio of sample
mass to sample volume, is expressed as grains per cubic centimeter (Blake,
1965). The procedure described below may be difficult or impractical to
use in soil containing rock fragments.
A.2.1.2.1 Chemicals—No chemicals are required.
A.2.1.2.2 Materials—
a. Double-cylinder core sampler with cutting edge, driving head, and
removable brass or aluminum sleeves.
92
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b. Core cylinder, 7.6 (3 in) in diameter and 7.6 cm (3 in) in height with
3.2 mm (0.125 in) thick walls.
c. Balance, can be read to 0.1 g.
d. Drying oven.
e. One-pint containers.
f. Air tight plastic bags.
g. Aluminum weighing pans.
h. Cloth diapers.
i. Desiccator containing drierite.
A.2.1.2.3 Procedure--
a. Assemble double-cylinder core sampler according to the instruction
manual.
b. Prepare a flat soil surface at depth in profile to be sampled.
c. Drive core sampler into the soil with the driving head until the soil
fills the brass or aluminum sleeve and extends slightly above it.
d. Remove driving head and twist double-cylinder core sampler.
e- Excavate soil on one side of the core sampler until the bottom of the
cutting edge can be clearly seen.
f. To ensure that the contact of the core with the main soil body is
broken, run a knife across the bottom of the cutting edge. NOTE: Do
this step taking care not to disrupt the soil core.
g. Pack a cloth diaper into the top of the double-cylinder core sampler
until it rests on the top of the soil core and hold in place with
one hand.
h. Gently tilt the top of the sampler toward the excavated side until the
cutting edge of the sampler is exposed. Put the other hand across the
bottom of the cutting edge to hold soil core in place. Remove core
sampler from excavation.
i. Remove the core and sleeve from sampler by raising the cutting edge
and applying gentle pressure to bottom of soil core while using the
cloth diaper to ensure that the soil core does not slide or fall from
the sleeve.
93
-------
j. Trim any excess soil off both ends of the soil core so a flat surface
exists flush with the edges of the sleeve.
k. Remove the soil from the sleeve ring and place in a pint container
lined with a plastic bag. Take care that no soil is lost in transfer.
1. Label the sample as to location, depth sampled and any other pertinent
information.
m. Transfer the samples to the laboratory.
n. Weigh a labeled aluminum pan and record the weight (A).
o. Transfer the moist soil sample to the pan and record the weight (B).
p. Place the pan with sample in an oven and allow to dry for 24 hours at
105°C.
q. Remove the pan with sample from the oven and cool in a desiccator.
Weigh pan and contents. Record weight (C).
A.2.1.2.4 Calculations—
a. Bulk Density = (C - A)/347.5 cc, where 347.5 cc is the volume of the
cylinder.
b. Percent Field Moisture = [(B - C)/(C - A)] x 100.
A.2.1.3 Moisture Retention (Pressure Plate Method)--
The amount of work needed to remove water from soil is measured by the
pressure plate approach. This work equals the energy with which the soil
sample holds the water. In this procedure a saturated soil sample rests on
a semipermeable membrane and is subjected to controlled pressures in excess
of atmospheric pressure. A water continuum, which is at atmospheric pres-
sure outside the apparatus, exists from the surface of the soil sample to
the open-air side of the semipermeable membrane; therefore, the compressed
gas forces water out of the pores of the sample through the membrane by way
of the water continuum. Water out-flow from the chamber ceases when
equilibrium has been reached (i.e., when the pressure exerted by the gas is
counteracted by the tension with which the soil particles hold the water).
It is possible to determine directly the moisture content of the soil at
that particular tension. Normally a moisture characteristic curve is
developed by equilibrating soils at pressures from 0 through 0.15 bars
(Richards, 1965).
A.2.1.3.1 Chemicals—
a. Distilled water.
b. Compressed nitrogen gas.
94
-------
A.2.1.3.2 Materials—
a. Five bar pressure plate extractor (Soil Moisture Equipment Company
Catalog No. 1600 or equivalent).
b. Pressure control manifold, accuracy of control within 1/100 psi in the
0.50 psi range (Soil Moisture Equipment Company Catalog No. 700-3 or
equivalent).
c. One bar pressure plate cells (Soil Moisture Equipment Company Catalog
No. 1290 or equivalent).
d. Three bar pressure plate cells (Soil Moisture Equipment Company
Catalog No. 1690 or equivalent).
e. Soil sample retaining rings (Soil Moisture Equipment Company Catalog
No. 1093 or equivalent).
f. Connecting hose (Soil Moisture Equipment Company Catalog No. 1293 or
equivalent).
g. Nitrogen gas tank gauges - 1 for tank pressure and 1 for out-flow
pressure.
h. Large spatula or small pancake turner.
i. Wax paper.
j. Plastic teaspoon.
k. Balance, can be read to 0.01 g.
1. Drying oven.
m. Aluminum pans for weighing samples.
n. Laboratory notebook.
o. Desiccator with silica gel desiccant.
A.2.1.3.3 Procedure—This apparatus and procedure are used for negative
pressures of 0i to -3 bar. Read instrument's instruction manual before
starting procedure.
a. Check pressure in the nitrogen tank.
b. Check all fittings by pressurizing system. NOTE: Take a toothbrush
and a bar of soap and mix up a soapy foam. Brush foam over each
fitting to see if there are any leaks in the system when pressurized.
95
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c. Check ceramic plates by forcing compressed air into outlet valve.
Seal off valve and submerge ceramic plate in pan of water. If any
bubbles appear, there is a hole in the rubber gasket sealed to the
plate. Repair the leak or do not use the plate.
d. Place the ceramic plate to be used in a pan of distil led water and
soak overnight (12-16 hrs). This is done when the ceramic plates have
been dried over a period of time. If the ceramic plate has been used
for a previous determination, this prolonged soaking is not necessary.
e. Take the aluminum pans and place a soil sample retaining ring inside
the pan. Draw a line around the top of the ring so that the approxi-
mate height of the ring is outlined on the inside of the aluminum pan.
The desired volume of subsample that would be put into the aluminum
pan would be slightly less than needed to fill the soil sample
retaining ring.
f. Using a thin plastic teaspoon, lift the soil from the container and
fill the aluminum pan to the volume mark. Do two replicates in the
same manner. NOTE: Be sure that all the pans are marked with the
soil sample number.
g. After the ceramic plate has been soaked overnight, place the soil
sample retaining rings on the ceramic plate in such a fashion that a
diagram can be easily made of the set up showing the sample number for
each particular ring.
h. Take the aluminum pan containing the approximate volume of soil sample
needed and carefully dump it into the proper soil sampling retaining
ring on the ceramic plate. Take the spatula or the spoon and
carefully flatten the sample until it is level with the top edge of
the soil sample retaining ring. NOTE: Do not compact this material.
Just carefully flatten by spreading.
i. After all the soil samples have been placed on the soaked ceramic
plates, add an excess of water to the surface of the ceramic plate and
allow the samples to soak for 16 hours. NOTE: Be sure there is
enough water on the ceramic plate to allow samples to wet without
removing water from the pores of the plates.
j. Cover samples and ceramic plate with wax paper to prevent evaporation.
k. After the samples have soaked overnight (16 hours), remove the excess
water from the surface of the ceramic plate by means of a pipette.
1. Remove the wax paper from the soil samples. Connect the out-flow tube
on the ceramic plate to the out-flow tube on the wall of the
extractor.
H nil
m. Cover the extractor with the metal top. NOTE: Be sure that the "0
ring seal is in place.
96
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n.
Clamp the lid to the bottom of the extractor with clamping bolts.
Tighten the wing nuts on the clamping bolts by hand.
o. With the needle valve, the "Nullmatic" type regulator, and the coarse
adjustment regulator on the manifold all closed, pressurize the system
by means of the controls on the nitrogen tank. Turn the "Nullmatic"
type regulator valve to wide open and use the coarse adjustment valve
on the manifold to get a reading on the pressure gauge of very
slightly in excess of the desired pressure.
p. Use the "Nullmatic" type regulator to get the desired pressure reading
on the manifold's pressure gauge.
q. Slowly open the needle valve at the end of the manifold and pressurize
the pressure plate extractor. NOTE: Two hours after system is pres-
surized, check pressure gauge on manifold for any final adjustment.
r. Samples that are 1 cm high can be removed any time after 48 hours from
initiation of the extraction. Some soils approach equilibrium in 18
to 20 hours; therefore, after 20 hours the out-flow tube is tested
periodically with blotter paper. If no moisture accumulates on the
blotter paper after it has been held against the out-flow tube for
approximately 1 minute, equilibrium has been reached and the extrac-
tion can be stopped.
s. Clean aluminum pan previously used. Oven dry, cool in desiccator, and
weigh to nearest 0.01 g. Record weight (A).
t. Put a piece of tubing over the out-flow tube and clamp the tubing off
with a pinch clamp. Shut the pressure source off, then drain the
system of compressed gas slowly by using the coarse adjustment valve
on the manifold.
u. After the system has been drained of compressed gas, disconnect the
hose leading to the extractor. NOTE: This will ensure that the
extractor is no longer pressurized.
v. Remove the clamping bolts and extractor lid.
w. Remove the samples one at a time and place in weighed aluminum pans.
x. Quickly weigh the aluminum weighing pan and the sample. Record weight
(B).
y. Place samples in the drying oven at 105°C. Allow samples to dry
overnight.
z. Remove samples from drying oven and place in a desiccator filled with
silica gel desiccant. Allow samples to cool.
aa. Weigh samples and weighing pan. Record weight (C).
97
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bb. Discard sample.
cc. Make sure that the pressure at which the extraction was carried out is
recorded in the laboratory notebook.
A.2.1.3.4 Calculations—
a. Legend: A = Weight of aluminum weighing pan.
B = Weight of moist sample and aluminum weighing pan.
C = Weight of aluminum weighing pan and oven-dry sample.
b. Percent moisture = [(B - C)/(C-A)] x 100.
A.2.2 Soil Chemical Methods
One method for each of the required tests is listed. The step-by-step
procedures listed in this section are from Field and Laboratory Method
Applicable to Overburden and Minesoil (EPA, 1978).The procedures in this
publication are applicable to native soil and are outlined in a very easy-
to-follow format. Other methods published elsewhere are equally effective
and may be substituted at the discretion of the laboratory.
A.2.2.1 Paste pH—
Perhaps the most commonly measured soil characteristic is pH. Al-
though pH was defined by Sorenson (1909) as the negative logarithm of the
hydrogen ion concentration, in actuality, the hydrogen ion activity is mea-
sured. Soil pH is measured by a glass electrode incorporated with a pH
meter. After water is added to the sample to form a paste, the electrode
is placed in the paste. The pH can be read directly from the meter.
Six factors affecting the measurement of pH are: 1) drying the soil
sample during preparation; 2) soil:water ratio; 3) soluble salts content;
4) seasonally influenced carbon dioxide content; 5) amount of grinding
given the soil; and 6) electrode junction potential (Jackson, 1958; Peech,
1965).
Care must be taken to ensure electrode life and accurate pH measure-
ments. The electrode should not remain in the sample longer than neces-
sary, and it should be washed with a jet of distilled water from a wash
bottle after measurement (sample or buffer). The electrode should then be
dipped in dilute hydrochloric acid and washed with distilled water to
remove any calcium carbonate film which may form. Drying out of the elec-
trode should be avoided. The pH meter should be placed in standby position
when the electrode is not in a solution (Jackson, 1958; Peech, 1965).
The following procedure describes the technique for measuring pH with
a glass electrode and meter.
A.2.2.1.1 Chemicals—
a. Standard buffer solution, pH 4.00 and pH 7.00.
98
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b. Distilled water (H20).
A.2.2.1.2 Materials—
a. pH meter (Corning model 12 or equivalent) equipped with combination
electrode.
b. Paper cups, 30 ml (1 oz) capacity.
c. Plastic cups.
d. Stirring rod.
e. Wash bottle containing distilled water.
f. Balance, can be read to 0.1 g.
A.2.2.1.3 Procedure—
a. Turn on, adjust temperature setting, and "zero" pH meter per
instruction manual.
b. Place pH 4.0 and pH 7.0 standard buffers in two plastic cups (one
buffer in each cup). NOTE: NEVER return used buffers to stock
bottles.
c. Place electrode in the pH 7.0 buffer.
d. Adjust pH meter to read pH 7.0.
e. Remove electrode from buffer solution and wash with a jet of distilled
water from a wash bottle.
f. Place electrode in the pH 4.0 buffer and check the pH reading. NOTE:
If pH meter varies more than +0.1 pH units from 4.0, something is
wrong with the pH meter, electrode, or buffers.
g. Weigh 10 g of less than 60 mesh material into a paper cup.
h. Add 5 ml of distilled water to sample. NOTE: Do not stir! Allow
water to wet sample by capillary action without stirring. With most
soils, the 2:1 (soil:water) ratio provides a satisfactory paste for pH
measurements; however, for very coarse textured and very fine textured
material, more material or water can be added to bring the soil near
saturation. At near saturation conditions, water should not be
puddled nor should dry soil appear at the surface.
99
-------
i. Stir sample with a spatula until a thin paste is formed, adding more
water or soil as required to keep soil at saturation point. NOTE: At
saturation, the soil paste glistens as it reflects light, and the
mixture slides off the spatula easily. Wash the spatula with a jet of
distilled water before stirring another sample.
j. Place electrode in paste and move carefully about to ensure removal of
water film around the electrode. CAUTION: Do not trap particles
between electrode and inside surface of the sample container.
Electrodes are easily scratched. Contact between paste and electrode
should be gentle to avoid both impact and scratching damage,
especially in sandy samples.
k. When reading remains constant, record pH and remove electrode from
paste. Carefully wash electrode with distilled water to ensure
removal of all paste. If all pH measurements are completed, the
electrode should be stored in a beaker of distilled water. NOTE:
After every 10 samples, check meter calibration with standard buffers.
A.2.2.2 Lime Requirement by SMP Buffer-
By measuring a change in pH of a buffer caused by the acids in a soil
Shoemaker et al. (1962) determine the lime requirement of a soil. The lime
requirement is read directly from a table based on the pH of a soil after
the SMP buffer has been added.
The SMP buffer method is very reliable for soils with a 2 tons per
1000 tons of material lime requirement (2 tons per acre furrow slice). An
acre furrow si ice is 6 inches (15 cm) deep over an area of 1 acre (0.4 ha).
It adapts well for acid soil with a pH below 5.8 containing less than 10
percent organic matter and having appreciable quantities of soluble alumi-
num. A sensitivity of 0.1 pH unit is needed for accurate interpretation of
this method. A difference of 0.1 pH unit will result in a lime requirement
difference of 0.5 to 0.9 tons of lime per 1000 tons of material for mineral
soils. Increased exposure time causes greater acidity, thus causing a
greater lime requirement. Increases in organic matter and/or clay content
increases absorption of acidic cations.
A.2.2.2.1 Chemicals—
a. Standard buffer solutions, pH = 4.00 and pH = 7.00.
b. SMP buffer solution: Dissolve 1.8 g p-nitrophenol (N02C6H4OH), 2.5 ml
triethanolamine (CcHjcNO-j), 3.0 g potassium chromate (K^CrO^, 2.0 g
calcium acetate (CatcOoCHoio), and 53.1 g calcium chloride
(CaClo*2H20) with distil fed water and dilute to 1 liter. Filter
througn a fiberglass sheet if suspended material is present. Connect
an air inl et with a 2.54 x 30.5 cm (1 x 12 in) cyl inder of drierite, a
2.54 x 30.5 cm cylinder of ascarite, and a 2.54 x 30.5 cm cylinder of
drierite in series.
100
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A.2.2.2.2 Materials—
a. Cup, 50 ml glass, plastic, or wax paper of similar size.
b. Pi pet, 10 ml capacity.
c. Shaker, horizontal reciprocating type, 6.3 cm (2.5 in) stroke, 250
strokes per minute.
d. pH meter (Corning model 12 or equivalent) with combination electrode.
e. Balance, can be read to 0.1 g.
A.2.2.2.3 Procedure—
a. Weigh 5 g of less than 60 mesh sample into a 50 ml cup.
b. Add 5 ml of distilled water. Mix for 5 seconds.
c. Wait for 10 minutes and read the soil pH (see Section A.2.2.1).
d. Add 10 ml SMP buffer solution to the cup for mineral soils with a pH
of 6.5 or less.
e. Shake for 10 minutes on reciprocating shaker at 250 strokes per minute
or stir.
f. Let stand for 30 minutes.
g. Read pH of the soil-buffer solution to the nearest 0.1 pH unit (see
Section A.2.2.1).
A.2.2.2.4 Calculations—
Determine lime requirement from Table A.I.
101
-------
Table A.I Soil-SMP Buffer pH and Corresponding Lime Requirement (L.R.)
to Bring Material to pH 6.5*
pH
(tons/1000 tons)1"
pH
(tons/1000 tons)1"
6.9
6.8
6.7
6.6
6.5
6.4
6.3
6.2
6.1
6.0
5.9
0.3
1.0
1.8
2.4
3.1
3.9
4.6
5.3
6.1
6.0
5.9
5.8
5.7
5.6
5.5
5.4
5.3
5.2
5.1
5.0
4.9
4.8
8.1
8.9
9.6
10.4
11.1
11.7
12.5
13.2
14.0
14.7
15.5
it
t
Adapted from
Agricultural
Shoemaker et al .
ground limestone
(1962).
TNP at least 90 percent.
A.2.2.3 Double Acid Extractable Phosphorus, Potassium, Calcium, and
Magnesium--
This method is a modified North Carolina double acid method first pub-
lished by Mehlich (1953) and then by Nelson et al. (1953). Phosphorus (P),
potassium (K), calcium (Ca), magnesium (Mg) are extracted from the sample
using a solution containing dilute hydrochloric and sulfuric acid. Phos-
phorus concentration in the extract is determined using a colorimeter and
calibration curve. The concentrations of K, Ca, and Mg in the extract are
determined using an atomic adsorption spectrometer and calibration curve.
The concentration of each element can then be converted into pounds per
1000 tons.
A.2.2.3.1 Chemicals—
a. Hydrochloric acid (HC1), concentrated.
b. Sulfuric acid (H2S04), concentrated.
102
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c. Extracting solution: To make 0.05 N HC1 and 0.025 N HoSO*, measure
about 10 liters deionized water into an 18 liter pyrex bottle. Add
12 ml H2S04 (96%) and 73 ml HC1 (37%). Make to 18 liters with dis-
tilled water and mix thoroughly by shaking. Allow 12 hours to come to
equilibrium.
d. Ammonium molybdate ((NH4)6Mo7024«4H20).
e. Ammonium vanadate
f. Nitric acid (HNOo), 1 N: Dilute 64 ml of concentrated HNOo (69.5%) to
1 liter with distilled water. J
g. Molybdate - Vanadate solution: Dissolve 25 g of ((NHd)6Mo7Oo4'4HoO)
in 500 ml of distilled water. Dissolve 1.25 g of NH4V03 in 500 ml of
1 N HN03. Store in separate bottles. Mix equal volumes of these
solutions (1 ml required per sample). Prepare fresh mixture each
week.
h. Monobasic potassium phosphate (KH2P04).
i. Phosphorus standard solution: Dissolve 0.1098 g of KH2P04 in 500 ml
of extracting solution. Dilute to 1 liter with extracting solution.
j. Potassium atomic absorption standard (1000 ppm).
k. Calcium atomic absorption standard (1000 ppm).
1. Magnesium atomic absorption standard (1000 ppm).
m. Potassium (K) standard stock solution (100 ppm): Place 10 ml of
potassium atomic absorption standard (1000 ppm) in a 100 ml volumetric
flask. Bring to volume with deionized water. Make fresh daily.
n. Calcium (Ca) standard stock solution (200 ppm): Place 20 ml of magne-
sium atomic absorption standard (1000 ppm) in a 100 ml volumetric
flask and dilute to volume with deionized water. Make fresh daily.
o. Magnesium (Mg) standard stock solution (100 ppm): Place 10 ml of
magnesium atomic absorption standard (1000 ppm) in a 100 ml volumetric
flask and dilute to volume with deionized water. Make fresh daily.
p. Lanthanum chloride (LaCl3'6H20), 5%: Dissolve 127 g of LaCl3'6H20
with deionized water and bring to a volume of 1 liter.
q. Activated charcoal (Darco G-60 or equivalent).
A.2.2.3.2 Materials—
a. Atomic absorption spectrophotometer (Perkin-Elmer Model 403 or equiva-
lent).
103
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b. Colorimeter (Bausch and Lomb Spectronic 20 or equivalent).
c. Flasks, Erlenmeyer, 50 ml.
d. Flasks, volumetric, 100 ml.
e. Flasks, volumetric, 200 ml.
f. Pipet, 1 ml.
g. Pipet, 2 ml.
h. Shaker, horizontal reciprocating type, 6.35 cm (2.5 in) stroke with
120 strokes per minute.
1. Filter paper (Whatman 40 or equivalent).
j. Pyrex bottle, 18 liters.
k. Pyrex bottle, 8 liters.
1. Balance, can be read to 0.1 g.
A.2.2.3.3 Procedure—
a. Place 5.0 g of less than 60 mesh sample in a 50 ml Erlenmeyer flask.
Add 0.2 g of activated charcoal. Prepare two blanks using only 0.2 g
of activated charcoal.
b. Add 25 ml of extracting solution and shake for 5 minutes on the
reciprocating shaker at 120 strokes per minute.
c. Filter using filter paper and save filtrate for P, K, Ca, and Mg
determinations. NOTE: If filtrate is cloudy, refliter.
d. Subdivisions 2.1.3.3.4 through 2.1.3.3.6 include the determination of
individual elements.
A.2.2.3.4 Phosphorus—These steps are used for the determination of phos
phorus.
a. Turn on colorimeter 15 minutes before use and adjust according to
instruction manual.
b. Pipet 4 ml of filtered extract into a colorimeter tube.
c. Add 1 ml of molybdate-vanadate solution and allow to stand 10 minutes.
d. Mix by inverting tube and shaking by hand for a few seconds.
e. Place tube in instrument and read percent transmission (%T).
104
-------
Using %T, determine the ppm available P from a calibration curve
prepared as follows: A) To separate colorimeter tubes, add the
amounts of chemicals given in Table A.2; B) Treat as outlined in
2.1.3.3.4 steps b-e; C) Plot ppm on the horizontal axis and % T on the
vertical axis. NOTE: If sample does not fall on calibration curve,
samples must be diluted and results multiplied by the dilution factor.
The dilution factor is obtained by taking the final volume and divid-
ing it by the initial aliquot.
Table A.2 Phosphorus Standards
Phosphorus
Standard
Solution
(ml)
0.0
0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0
Extracting
Solution
(ml)
4.0
3.5
3.0
2.5
2.0
1.5
1.0
0.5
0.0
• • •' • • ., ,fc
Molybdate-
Vanadate
Solution
(ml)
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
^MMMtf«"Hllhh«*MIMIMH^IIVBIlMH»MVIVIHBVHIVHIV«IB»«H-IBHHBI«^^
Phosphorus
in
Standard
(ppm)
0.0
2.5
5.0
7.5
10.0
12.5
15.0
17.5
20.0
A.2.2.3.5 Potassium --These steps are used for the determination of
potassium.
a. Set the atomic absorption spectrophotometer unit on emission mode
following the instrument's instruction manual.
b. Use the extractant for zero setting.
c. Put the extracted sample solution under the aspirating tube and record
readings.
d. Determine ppm of K in the sample from the calibration curve prepared
as follows: A) Into separate 100 ml volumetric flasks, dilute the K
105
-------
standard stock solution with extracting solution for a range of 0 to
80 ppm increments; B) Take reading with the atomic absorption spectro-
photometer; C) Plot available K (ppm) on the horizontal axis and the
instrument reading on the vertical axis; D) Plot a curve through the
points. NOTE: If samples do not fall on the calibration curve,
dilute samples with extracting solution and multiply results by dilu-
tion factor. The dilution factor is obtained by dividing the final
volume by the initial aliquot.
A.2.2.3.6 Calcium and Magnesium—These steps are used for the determin-
ation of calcium and magnesium.
a. Adjust the atomic absorption spectrophotometer following the instru-
ment instruction manual.
b. Pipette to 1.0 ml of sample extract and blank into separate 100 ml
volumetric flasks. Add 1.0 ml of 5% LaCl3'6H20 to each flask.
c. Bring to volume with extracting solution and mix by hand shaking.
d. In separate 100 ml volumetric flasks, prepare the calcium standards as
shown in Table A.3. Aspirate each standard into the instrument until
a steady reading is obtained. Record reading.
e. Make a calibration curve plotting Ca (ppm) on the horizontal axis and
the instrument reading on the vertical axis. Plot a curve through the
points.
f. Into separate 200 ml volumetric flasks, prepare the magnesium stan-
dards as shown in Table A.4. Aspirate each standard into the instru-
ment until a steady reading is obtained. Record reading.
g. Make a calibration curve plotting extractable Mg (ppm) on the
horizontal axis and the instrument reading on the vertical axis. Plot
a curve through the points.
h. Aspirate sample extracts into the atomic absorption spectrophotometer
and record readings.
i. Determine ppm of calcium and magnesium from calibration curves. If
samples do not fall within the range of the calibration curve, dilute
sample with extracting solution and add 5% Lado'SHoO, but not to
exceed 1% La in the final dilution. Multiply results by dilution
factor. The dilution factor is obtained by taking the final volume
and dividing it by the initial aliquot.
106
-------
Table A.3 Calcium Standards
Stock Ca
Solution
200 ppm
(ml)
0.0
1.0
2.0
3.0
4.0
5.0
LaCl3'6H20
(ml)
2.0
2.0
2.0
2.0
2.0
2.0
•
Extracting
Solution
(ml)
98.0
97.0
96.0
95.0
94.0
93.0
^^^•.^••^^^•••^•«»^»i^^i^^^^i^»«i^»»^^»^^^»^^^^* • • i •
Calcium
in
Standard
(ppm)
0.0
2.0
4.0
6.0
8.0
10.0
Table A.4 Magnesium Standards
Stock Mg
Solution
100 ppm
(ml)
0.0
0.5
1.0
1.5
2.0
2.5
3.0
LaClq'6HoO
-------
b. ppm P in the soil = ppm (read from the curve) x 6.25 x OF. NOTE: The
6.25 is obtained from the following equation: 6.25 = 25 ml extracting
solution/5 g sample) X (5 ml final volume/4 ml extract).
c. ppm K in the soil = ppm (read from the curve) X 5 X OF. NOTE: The 5
is obtained from the following equation: 5 = (25 ml extracting
solution)/(5 g sample).
d. ppm Ca in the soil = ppm (read from the curve) x 500 x DF. NOTE: The
500 is obtained from the following equation: 500 = (25 ml extracting
solution/5 g sample) x (100 ml final volume/1 ml extract).
pm Mg in the soil = ppm (read from the curve) x 500 x DF. NOTE: The
00 is obtained from the following equation: 500 (25 ml extracting
solution/ 5 g sample) x (100 ml final volume/1 ml extract).
f. pp2m of element in the soil = (ppm of element in the soil) x 2.
A. 2. 2. 4 Total Nitrogen by Kjeldahl Method—
In the Kjeldahl procedure, nitrogen is converted to the ammonium ion
by oxidation with concentrated sulfuric acid with the addition of a cata-
lyst such as copper, selenium, or mercury. This oxidation, which normally
progresses very slowly, can be accelerated by raising the boiling point.
This can be done by adding such salts as sodium sulfate or potassium
sulfate. The procedure is described below.
A. 2. 2. 4.1 Chemical s--
a. Kel-pak powder No. 3 (HgO + K2S04) (available from Matheson Scientific
Co.).
b. Sulfuric acid (hSO, concentrated.
c. Sulfuric acid (H2S04), dilute (approximately 0.1 N): Dilute 44.8 ml
of concentrated H2S04 to 16 liters with distilled water.
d. Sodium hydroxide (NaHO), 45% with sodium thiosulfate (Na2So03'5H20):
Under a fume hood in a rubber bucket mix 4545.9 g of NaOH flakes (for
nitrogen determination) with 438.0 g of Na2S203'5H20. Dissolve and
dilute to 11.355 liters (3 gal) with carbon dioxide-free water. Cool
overnight and siphon into dispensing apparatus. Protect from C02 in
the air with soda lime or ascarite in a guard tube.
e. Boric acid (H3B03), 4%: Dissolve 720.0 g of H3B03 in distilled and
deionized water on a hot pi ate. Oil ute to 18 liters with distil led
and deionized water. Add 60 ml of bromocresol green-methyl red
indicator (see below).
f. Bromocresol green-methyl red indicator: Mix 0.5 g of bromocresol
green and 0.2 g methyl red with 100 ml of ethyl alcohol (90%). Adjust
to medium color (brown) with a few drops of weak NaOH.
108
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g. Zinc (Zn), granular.
A.2.2.4.2 Materials—
a. Kjeldahl electric digestion manifold.
b. Kjeldahl electric distillation rack.
c. Room equipped with exhaust fan.
d. Flasks, Kjeldahl, 800 ml.
e. Flasks, Erlenmeyer, widemouth, 500 ml, marked at 230 ml.
f. Sieve, 20 mesh.
g. Balance, can be read to 0.1 g.
h. Asbestos gloves.
A.2.2.4.3 Procedure--
a. Place 10 g unground sample (sieved to 20 mesh) wrapped in filter paper
in Kjeldahl flask. Also prepare two blanks without soil, but
containing filter paper.
b. Add 2 packets of No. 3 Kel-pak.
c. Turn on exhaust fan.
d. Add 40 ml concentrated H2S04. NOTE: While rotating flask, run acid
down side to carry sample.
e. Mix contents by gentle swirling and place flask carefully on Kjeldahl
rack.
f. When all flasks are in place, set all knobs so that a moderate boiling
and digestion of the sample can be seen.
g. After 30 minutes, increase heat to a rapid boil for 30 minutes so that
sulfur dioxide can be released to ensure complete digestion of the
sample.
h. Rotate flasks 180° and continue heating until all the black organic
matter is digested (usually about 1 hour).
i. Allow sample to cool on digestion rack and stopper. CAUTION: Do not
place stopper in hot flask as it may implode upon cooling.
109
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j. Let stand until solution reaches room temperature and cautiously add
300 ml distilled water to each flask. NOTE: Rotate flasks while
pouring to wash neck.
k. Swirl flasks gently to dissolve crystals.
1. Add 1/4 teaspoon granular zinc to each flask.
m. Pour 30 ml ^803 (4% containing indicator) into 500 ml wide mouth
Erlenmeyer flasks. NOTE: One required for each sample and blank and
numbered to correspond to each Kjeldahl flask.
n. Place Erlenmeyer flasks on Kjeldahl distillation rack. NOTE: Top of
glass delivery tube must be below surface of H3B03.
o. Turn condenser water switch to manual. After 30 minutes turn water
switch to automatic if unit is so equipped.
p. Add 133 ml NaOH (45%) slowly to each Kjeldahl flask. NOTE: Allow
NaOH to run down side of flask so that it lies on the bottom.
q. Place each flask on Kjeldahl distillation rack as NaOH is added, using
steps r-u.
r. Wet hands with distilled water and apply water to rubber stoppers.
s. Place stopper securely in flask. Set flask on burner.
t. As soon as flask is in position, turn burner switch to make a moderate
boil but not enough to cause solution to boil into flask neck.
u. Swirl flask to mix NaOH layer with the rest of the sample solution and
set back in position making sure stopper is tight.
v. When 200 ml has distilled into receiving flask, set receiving flask
(Erlenmeyer) down and turn off heat. CAUTION: Be sure to set flask
down before turning off heat, or distillate may suck back through
condensers. NOTE: Distillate color should be green or dark blue.
w. Wash delivery tube with a small stream of distilled water from a wash
bottle before removing receiving flask.
x. When cool, titrate distillate with 0.1 N H2S04 until solution becomes
clear and then turns pink.
y. Record reading.
A. 2. 2. 4. 4 Calculations—
a. Average of sample blanks = [reading (blank 1) + reading (blank 2)]/2.
110
-------
b. Corrected sample reading = (sample reading) - (average of sample
blanks).
c. Constant = (N acid) X (meq. wt. of N) X (100) X (1/wt. of sample);
where N acid = 0.1, meq. wt. of nitrogen = 0.014, and 100 changes
constant to percent.
The equation can then be written:
Constant = (0.1) X (0.014) X (100) X (1/wt. of sample), which can be
simplified to:
Constant = (0.14) X (1/wt. of sample).
d. % nitrogen = (corrected sample reading) X constant.
A.2.2.5 Sodium Saturated Cation Exchange Capacity—
Cation exchange capacity (CEC) is defined as the sum of the exchange-
able cations in a soil. Several methods are used for determining the CEC
of a soil. In the method given here (Sobeck, 1978) the soil is saturated
with a solution of sodium acetate to replace all other exchangeable cations
on the exchange sites with sodium. Sodium is then removed from the
exchange complex by saturating the soil with an ammonium acetate solution.
CEC is measured by determining the amount of sodium in the ammonium acetate
extract.
A.2.2.5.1 Chemicals—
a. Sodium acetate (NaOAc), 1.0 N: Dissolve 136 g of NaOAc in distilled
water and dilute to 1 liter. NOTE: The pH of this solution should be
8.2. If needed, add a few drops of acetic acid or NaOH solution to
adjust the pH to 8.2.
b. Ammonium acetate (NH4OAc), 1.0 N: Dilute 114 ml of glacial acetic
acid (99.5%) with distilled water to a volume of approximately
1 liter. Then carefully add 138 ml of concentrated ammonium hydroxide
(NH4OH) and slowly add distilled water to obtain a volume of approxi-
mately 1980 ml. Check the pH of the solution and add more NH4OH as
needed to obtain a pH of 7.0. Dilute the solution to a volume of
2 liters with distilled water.
c. Isopropyl alcohol, 99%.
d. Potassium stock solution, 10,000 ppm: Dissolve 19.07 g of potassium
chloride (KC1) in 1 liter of deionized water.
e. Standard sodium solution, 1000 ppm, atomic absorption spectroscopy
grade.
Ill
-------
A.2.2.5.2 Materials—
a. Centrifuge tubes, 50 ml, round bottom polypropylene.
b. Rubber stoppers (to fit centrifuge tubes).
c. Shaker, horizontal reciprocating type, 6.35 cm (2.5 in) stroke, 120
strokes per minute.
d. Centrifuge (International Equipment Company Model K with No. 279 head
or equivalent centrifuge and 12-place head).
e. Volumetric flasks, 100 ml.
f. Atomic absorption spectrophotometer (Perkin-Elmer model 403 or
equivalent).
g. Balance, can be read to 0.01 g.
A.2.2.5.3 Procedure—
a. Weigh 4.0 g of less than 60 mesh material and transfer to 50 ml
centrifuge tube. NOTE: If the material is very coarse textured
(loamy sand or sand), a 6.0 g sample is used.
b. Record weight of sample (A).
c. Add 33 ml of 1.0 N NaOAc solution to the centrifuge tube.
d. Stopper the tube and shake in a reciprocating shaker at 120 strokes
per minute for 5 minutes ensuring that the solid material in the
bottom of the tube is completely dispersed.
e. Unstopper the tube and centrifuge until the supernatant liquid is
clear (at least 5 minutes at 2000 RPM). Decant and discard the
liquid.
f. Repeat steps c through e three more times.
g. Add 33 ml of 99% isopropyl alcohol to centrifuge tube.
h. Stopper tube and shake on reciprocating shaker for 5 minutes ensuring
that the solid material in the bottom of the tube is completely dis-
persed.
i. Unstopper centrifuge tube and centrifuge it until the supernatant
liquid is clear (at least 5 minutes at 2000 RPM). Then decant and
discard the liquid.
j. Repeat steps g through i two more times.
112
-------
k. Add 33 ml of 1 N NH4OAc to centrifuge tube, stopper tube and shake for
5 minutes ensuring that the solid material in the bottom of the tube
is completely dispersed.
1. Unstopper tube and centrifuge until supernatant liquid is clear (at
least 5 minutes at 2000 RPM).
m. Decant liquid into a 100 ml volumetric flask.
n. Repeat steps k through m two more times.
o. Fill the volumetric flask to the 100 ml mark using the 1 N NH4OAc
solution.
p. Take 10 clean 100 ml volumetric flasks and label them 0, 5, 10, 20,
30, 40, 50, 60, 70, and 80 ppm sodium.
q. Pipet 0.5 ml of the 100 ppm sodium standard into the flask labeled 5
ppm sodium. Into the flasks labeled 10 through 80 ppm, pipet 1 ml
through 8 ml, respectively, of the 1000 ppm sodium standard solution.
r. Dilute all flasks to volume with 1 N NH4OAc solution. NOTE: The
flask labeled 0 ppm will contain only the 1 N NH4OAc extracting solu-
ti on.
s. Turn on the atomic absorption unit and wet it for emission mode. Read
instruction manual carefully and set all operating parameters accord-
ing to the instrument instruction manual.
t. After the atomic absorption unit is ready, zero the instrument using
the 1 N ammonium acetate extracting solution, not distil led water.
Aspirate standards and record readings.
u. Plot a standard curve using ppm sodium on the horizontal axis and the
instrument readings on the vertical axis.
v. Record the instrument readings for all unknowns and read the
concentration (B) of sodium from the standard curve. NOTE: If the
unknown does not fall within the range of the standard curve which you
have plotted, dilute the unknown with NH4OAc and potassium stock
solution using 2 ml of the potassium stock solution for every 10 ml of
NH4Ac. Then measure the amount of sodium present.
A.2.2.5.4 Calculations—
a. Legend: A = Sample weight
B = ppm of sodium as read from the standard curve.
DF = dilution factor, which is 1 or unity if no dilution of
the unknown had to be made to get it to read within the
range of the standard curve.
113
-------
b. CEC (meq/100 g) = (B/1,000,000) x (DF) x (Volume extracting
solution/sample wt.) x (1000 meq/eq. wt Na) x 100 g.
Where: Volume extracting solution = 100 ml
eq. wt of Na = 23
The above equation can be reduced to:
CEC (meq/100 g) = (B x DF x 10) / (23 x A).
A.2.2.6 Electrical Conductance of Soil Extract
Pure water (water that contains no dissolved substances) is not a good
conductor of electric current. With the addition of absorbed salts, how-
ever, water becomes a better electric current conductor. Because of this
fact, measuring the amount of electric current conducted through a soil
extract made with pure water provides information about the amount of salt
present in the soil. This sample measurement provides an accurate indica-
tion of the concentration of ionized constituents in the soil extract. The
electrical conductivity (EC) of a soil extract is closely related to the
sum of cations (or anions) as determined chemically. This measure usually
correlates closely with total dissolved solids.
The soil material used for EC measurements should not be oven dried.
Material should be air dried and ground to pass a 60 mesh sieve.
A.2.2.6.1 Chemicals--
a. Distilled water.
b. Potassium chloride (KC1), 0.01 N: Dissolve 0.7456 g of KC1 in
distilled water, and dilute with distilled water to 1 liter. This is
the standard reference solution, and at 25°C it has an electrical
conductivity to 0.00141 mho/cm.
c. Sodium metaphosphate ((NaP03)6), 0.1%: Dissolve 0.1 g of (NaP03)6
(Fisher Scientific #S-333) in distilled water and dilute to 100 ml.
A.2.2.6.2 Materials--
a. Wheatstone bridge, alternating-current type, suitable for conductivity
measurements. (Industrial Instruments Incorporated Model RC-16B2 or
equivalent).
b. Conductivity cell, pipette-type, with platinized platinum electrodes.
The cell constant should be approximately 1.0 reciprocal centimeter.
c. Flask, volumetric, 1000 ml.
d. Balance, can be read to 0.01 g.
e. Aluminum can with lid (large enough to contain sample).
114
-------
f. Spatula.
g. Aluminum weighing pan.
h. Drying oven.
i. Dessicator, with silica gel dessicant.
j. Buchner type filtering funnel, 11 cm inside diameter.
k. Filter flask.
1. Filter paper (Whatman 42 or equivalent).
m. Vacuum source.
n. Graduated cylinder, 100 ml volume.
o. Pipette, measuring, 10 ml capacity.
A.2.2.6.3 Procedure—This procedure is modified from the U. S. Salinity
Laboratory Staff (1954).
a. Weigh 400 g of air-dried soil. Transfer the soil to an aluminum can
(with lid).
b. Add water to the sample in small increments by pouring the water down
the side of the can. Water is added to the sample in this fashion
until the saturation point of the soil is almost reached.
NOTE: Do not stir soil sample while adding water. Since water
movement through puddled soil is very slow, the soil is first allowed
to wet by capillarity and then mixed to ensure against puddling.
c. Stir the wetted soil with a spatula until a condition of saturation is
reached. Small amounts of water may be added while mixing to ensure
that the saturation point has been reached. NOTE: At saturation the
soil paste glistens as it reflects light, and the mixture slides off
of the spatula easily.
d. After the mixing has been completed, place the lid on the aluminum can
and let sample stand for 1 hour or more.
e. After the sample has set for the required amount of time, check sample
for saturation. NOTE: If the paste has stiffened or lost its
gl isten, add more water and mix it again. On the other hand, if free
water has collected on the surface of the paste, add additional air-
dry soil to absorb free water and remix the sample.
115
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f. After a saturated paste has been obtained, remove a teaspoonful of the
saturated paste for oven-drying and replace lid. Allow the saturated
soil paste to stand at least 4 hours.
g. Weigh an oven-dry aluminum weighing pan to the nearest 0.01 g.
Record weight (A).
h. Place subsample of the saturated soil paste (from step 6) in aluminum
weighing pan. Weigh pan and sample to the nearest 0.01 g. Record
weight (B).
i. Place weighing pan and sample in an oven at 105°C for 16 hours (or
overnight). Remove from oven and cool in a dessicator.
j. Weigh oven-dry sample and pan. Record weight (C).
k. After the saturated soil paste has stood for at least 4 hours (from
step f), transfer it to a Buchner funnel fitted with one sheet of
Whatman #42 (or equivalent) filter paper.
1. Attach filter flask to vacuum source, apply vacuum, and collect fil-
trate. Terminate filtration when air begins to pass through the
filter. NOTE: Refilter if filtrate is turbid.
m. Add one drop of 0.1% sodium hexametaphosphate solution for each 25 ml
of extract.
n. Allow the standard 0.01 N KC1 solution and the sample of the soil-
water extract to adjust to room temperature. NOTE: As long as the
temperature of the room is within the range of 20-30°C, the absolute
temperature of the solutions are not important. However, it is
extremely important that the standard solution and the extract be at
the same temperature. If greater precision is required, bring the
standard solution and soil-water extracts to a temperature of 25°C in
a constant temperature bath.
o. Turn on Wheatstone bridge and allow instrument to warm up.
p. When instrument is ready, rinse and fill the conductivity cell with
the standard 0.01 N KC1 solution.
q. Balance the Wheatstone bridge according to the instruction manual
provided by the manufacturer. Record the cell resistance (D) in ohms.
r. Rinse and fil 1 the eel 1 with the soil-water extract. NOTE: If the
volume of the extract is limited, rinse the cell with distilled water
followed by acetone. Dry the cell by drawing air through it until the
acetone has evaporated. Allow the cell to come to room temperature.
s. Balance the bridge and record the cell resistance (E) in ohms.
116
-------
A.2.2.6.4 Calculations—
a. Legend: A = Weight of oven-dry weighing pan.
B = Weight of saturated soil and weighing pan.
C = Weight of oven-dry soil and weighing pan.
D = Initial cell resistance.
F = Final cell resistance.
b. % Moisture of sample at saturation = [(B-C)/(C-A)] x 100.
c. Electrical conductivity (EC) mmhos/cm, at 25°C = [(0.0014118 x D)/F].
d. Total cation concentration, meq/liter = 10 x (EC).
A.2.2.7 Organic Carbon by Low Temperature Ignition
Water and hydroxides are driven off the sample by heating at 105°C.
Organic matter is oxidized by heating at 400°C for 7 hours. The percent of
organic matter can be determined by weight loss, as described below.
A.2.2.7.1 Chemicals—No chemicals are required.
A.2.2.7.2 Materials—
a. Muffle furnace.
b. Drying oven.
c. Desiccator with drierite desiccant.
d. Balance, can be read to 0.01 g.
e. Crucibles or evaporating dishes.
A.2.2.7.3 Procedure—This procedure is modified from Jackson (1958).
a. Weigh a clean and dry crucible. Record tare weight (A).
b. Weigh 10.00 g of less than 60 mesh sample in tared crucible.
c. Place in oven and heat for 4 hours at 105°C.
d. Remove sample and allow to cool in desiccator.
e. Weigh sample. Record weight (B).
f. Place sample in oven and heat for 7 hours at 400°C.
g. Remove sample and allow to cool in desiccator.
h. Weigh sample. Record weight (C).
117
-------
A.2.2.7.4 Calculatlons--
a. Legend: A = Tare weight of crucible.
B = Weight of sample and crucible after heating 4 hours at
105°C.
C = Weight of sample and crucible after heating 7 hours at
400°C.
D = Weight of sample after heating 4 hours at 105°C.
E = Weight of sample after heating 7 hours at 400°C.
b. D = B - A.
c. E = C - A.
d. Organic matter oxidized by heating = D - E.
e. % organic matter in sample = (Organic matter oxidized by heating/D) x
100.
118
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APPENDIX B
DETAILED PROCEDURE FOR COLLECTING BARREL SIZED UNDISTURBED LYSIMETERS .
B.I SCOPE AND APPLICATION
This appendix (adapted from Brown et al., 1984) provides a detailed
description of the technique for collecting barrel-sized monoliths of
undisturbed soil. Since the properties of an undisturbed soil differ from
those of a disturbed profile (Cassel et al., 1974), the use of undisturbed
monoliths is desirable for studies designed to evaluate hazardous waste
fate and contaminent movement in soil. In a land treatment demonstration,
a lysimeter can be used to measure both mobility and degradation on undis-
turbed soil monoliths collected from the site of the land treatment unit.
B.2 LYSIMETER INSTALLATION
Lysimeter casings must be special ly ordered from a barrel manufac-
turer. The straight wal 1 ed cyl indrical casing (57 cm ID and 85 cm tal 1 )
should be manufactured from 20 gauge steel, painted on the outside, and
coating-free on the inside. Both ends of the casing shoul d be rol 1 ed to
accept standard size removable lids. Prior to installation, four 2.86 cm
diameter hoi es shoul d be dri 11 ed 1 cm bel ow the rol 1 on the upper end of
the casing, and the inside 0f the casing should be cleaned and painted with
a chemical and moisture resistant non-reactive paint.
A one piece support frame (Figure B.I), required for lysimeter collec-
tion, is clamped around the casing to support the casing while it is pushed
into the soil. The bottom 10.2 cm beveled cutting edge of the support
frame is made to be the same inside diameter as that of the lysimeter
casing.
To fill the casing with an undisturbed monolith, the frame with
enclosed casing is placed on a vegetation-free soil and leveled. A steel
plate (1.9 cm thick) is placed on top of the support frame, and vertical
pressure is gently applied by means of a backhoe bucket. A trench approxi-
mately 45 to 50 cm wide by 30-45 cm deep (depending on soil texture) is
excavated with the backhoe around two sides of the support frame; then the
sides of the monolith are trimmed manually to within 2.5 cm of the proper
diameter. The frame and casing can then be forced down over the monolith
by exerting pressure on the top plate with the backhoe. The excess 2.5 cm
of soil is trimmed away by the cutting edge of the support frame as it
moves down over the monolith. An experienced operator should be able to
press the casing in increments of 15 to 25 cm between excavations without
damaging the monolith.
When the casing is filled to within 15 cm of the top, a 51 cm diameter
plywood disk is placed on the soil surface of the monolith, and two 1.9 cm
diameter steel bars placed through the holes in the top of the casing.
Pressure is again applied to the top plate until the plywood is in firm
contact with the steel bars. In a very sandy soil, it may be necessary to
119
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o
ITHAI6NT SlOCO • MII
ALL DIMENSIONS IN CENTIMETERS
I DETAIL 2
FIG. B.I. SUPPORT FRAME DESIGN FOR BARREL LYSIMETER
COLLECTION.
-------
use an hydraulic ram to push a 0.64 cm steel plate horizontally through the
soil under the cutting edge of the frame. This steel plate is secured to
the frame to prevent soil from fal 1 ing out. In a loam or clay soil, the
structure is usually sufficient to prevent soil loss during handling. At
this point, the monolith is ready for removal.
After the monolith has been tipped slightly to break it loose, the
lifting and rotating harness (Figure B.2) is used to remove it from the
hole. Next, the casing is rotated to an upside down position and placed on
two 20 x 20 x 41 cm concrete building blocks. The support frame can then
be removed from around the casing and the soil trimmed to allow installa-
tion of the leachate collection system and the lid. Three porous ceramic
suction cups (Coors Type 7001 P-6-C) are typically installed into the soil.
Suction cup installation is accomplished by excavating a hole just large
enough to receive each cup and by packing the excavated soil around each
cup. A 2.0 cm hole is then drilled through the soil from the bottom to the
top of the monolith. Next, a piece of 1.3 cm ID PVC pipe is installed in
this hole to serve as a conduit for the tubes from the suction cups through
the monolith to the soil surface. After the soil from bottom of the
monolith is leveled and the casing rim cleared, a bead of silicon adhesive
is placed on the rolled edge of the casing, and a sponge rubber gasket and
lid are installed. A lever lock type clamp is used to attach the lid. The
monolith is then turned upright and transported to the experimental site.
A barrier to minimize sidewal 1 f1ow should be instal1 ed around the
inside edge of each monolith. This is accomplished by excavating a small
trench (7.5 cm wide x 7.5 cm deep) around the upper edge of each monol ith.
The inside wall of the casing is then washed with water and air dried. The
barrier is composed of a 5 cm wide strip of duct tape, which is folded in
half and placed in the bottom of the trench. Half of the strip of tape is
then taped securely to the side of the casing wall with a second strip of
duct tape. Finally, the soil is replaced and packed into the trench on top
of the duct tape, and the lysimeter is ready to use.
121
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ro
CHAIN OR CABLE
63.5
7.0 dia.
,0.6 dia,
63.5
— -2.5
1.3
12.7
I 6.5
ALL DIMENSIONS IN CENTIMETERS
FIG. B.2. LIFTING HARNESS FOR REMOVING AND ROTATING
BARREL LYSIMETERS.
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APPENDIX C
QUESTIONS AND ANSWERS
1. The treatment demonstration standard (§264.272) requires the owner or
operator to demonstrate that hazardous constituents can be "com-
pletely" degraded, transformed, or immobilized iin the treatment zone.
In this context, what does "completely" mean?
The intent of this "complete" treatment demonstration requirement is
to ensure that during the demonstration sufficient data is generated to
allow one to predict that hazardous constituents can be treated at the
proposed unit. The extent of this predictive data will vary depending on
the treatment mechanism examined. When mobility is examined, test results
must be able to predict that no statistically significant releases of
hazardous constituents will occur from the treatment zone at the proposed
unit. Obviously, a successful demonstration must at least show "complete"
immobilization (i.e., no release) during the time frames of the demonstra-
tion. When the degradation of organic hazardous constituents is examined,
the critical results are degradation rates showing that the hazardous
constituents will be completely degraded in the proposed unit prior to
escaping from the treatment zone. A successful demonstration of treatment
via degradation does not necessarily require that the organic hazardous
constituent be completely or (i.e., 100%) degraded during the limited time
frame of the demonstration. Rather, the degradation rate data can be used
in combination with the mobility test results to predict successful treat-
ment at the proposed unit.
2. Section §264.272 requires the owner or operator to demonstrate that
hazardous constituents can be completely degraded, transformed, or
immobilized. Can this requirement be met by demonstrating that all
hazardous constituents (inorganic and organic) are treated by
immobilization only?
The preamble to the Part 264, Subpart M regulations (47 FR 32325) states
that degradation and transformation are the primary treatment mechanisms
involved in land treatment. Immobilization should be reserved as a treat-
ment mechanism only for the smaller inorganic and persistent organic con-
stituents in a land treatable waste. A treatment demonstration based
solely on immobilization as the primary treatment mode for all hazardous
constituents is unacceptable.
3. Must air emissions of hazardous constituents be addressed in the
demonstration?
In the treatment demonstration, the owner or operator must address the
mobility of all hazardous constituents, the degradation/transformation of
all organic hazardous constituents, and the toxicity of the waste to soil
microbes. At the present time, the evaluation of air emissions of hazar-
dous constituents in the demonstration is not required because of the
problems associated with air emission measurements and the absence of
regulatory standards to evaluate the results. This position modifies the
123
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guidance presented in the Permit Applicants Guidance Manual for Hazardous
Waste Land Treatment, Storage, and Disposal FacilitTeT (Final Draft,
1984) and the RCRA Guidance Document: Land TreatmentTJnits (EPA, 1983).
The appl icant wil 1, however, have to meet any state regulations on air
emissions of hazardous constituents and should be aware that the Agency is
in the process of developing regulations pertaining to air emissions.
4. If an owner/operator intends to do interim status treatment demonstra-
tion field tests on one or more plots of an existing land treatment
unit, and the EPA issues a short-term demonstration permit or a two-
phase permit to cover these tests, how is the interim status of the
remaining plots of the land treatment unit affected?
In certain cases, treatment demonstration field tests may be completed
at an existing land treatment unit provided that they are not conducted in
a manner that leads to a violation of the interim status standards. In the
event that the tests are likely to cause a violation of the ISS, a special
permit must be obtained for these tests. However, if a short term permit
or a two-phase permit is issued to allow these tests on a few plots of the
unit, the interim status of the remaining plots is unaffected, and the
owner/operator can continue to operate under ISS for the remaining plots.
In special cases, such as small land treatment units, the short-term permit
or Phase I of a two-phase permit may apply to a large part of the entire
interim status unit.
5. In a mul ti-unit facil ity, can the two-phase permit approach be used
for the land treatment unit while the remaining units are processed
according to the normal permitting approach?
Yes. Section 270.1(c)(4) states that the EPA may issue or deny a
permit for one or more units at a facility without simultaneously issuing
or denying a permit to all of the units at the facility. The interim
status of any unit for which a permit has neither been issued nor denied is
not affected by issuance or denial to any other unit of the facility.
6. Scenario 3 includes the completion of a laboratory toxicity test and a
field plot or barrel lysimeter at an HWLT unit while it is still under
interim status. Chapter 3 of this manual states that demonstration
studies may be done at an IS unit provided interim status standards
are not violated. Can these laboratory tests be done at an off-site
laboratory that has neither interim status nor a final Part 264
permit?
Yes. Part 264.4 of the regulations states that a sample of solid
waste or a sample of water, soil, or air, which is col lee ted for the sole
purpose of testing to determine its characteristics or composition, is not
subject to any requirements of Parts 262-267 or Parts 124 and 270. Part
264.4 does, however, specify certain conditions that must be met in regard
124
-------
to shipping the sample to qualify for this exemption. The laboratory test
described in this document is a short-term test on a small sample volume to
evaluate the biological toxicity characteristics of the waste. Since the
act of testing does not constitute treatment of samples, laboratories do
not need a permit to conduct such testing.
7. In determining the application rates for the demonstration, how many
rates should be considered?
Where limited data are available about the behavior of the waste(s) at
the given unit (e.g.,for new units), or where past operating practices have
been poorly defined or have resulted in poor treatment of the waste(s),
this protocol suggests that the applicant should, ideally, consider testing
three annual loading rates. More rates may lead to unnecessary costs while
testing fewer rates risks a failure of the initial LTD endeavor, leading to
costly delays in the permitting procedure and to expensive retesting, and
possibly even to permit denial and/or enforcement action. Even when a unit
is well documented and loading rates are relatively well understood, use of
only one rate in the testing, although allowable, may risk a similar LTD
failure, especially if the current waste loading rate is high. For lightly
loaded units, use of the current rate may unnecessarily limit the future
(full) utilization of the site's inherent capacity to treat waste.
8. If several hazardous wastes are treated at the same unit, must a
separate LTD be performed for each?
A single demonstration will suffice if the wastes are generated rou-
tinely (e.g., monthly) and co-mingled on the same parcel of land. In such
cases, proportional amounts of each waste may merely be combined and ap-
pliedas if they were one. This mixture should also include significant
nonhazardous wastes that are applied at the site. An alternative is to do
an LTD for the worst quality waste among those land treated at the site.
For example, if the data show no substantive differences between an API
separator sludge, DAF float, and slop-oil emulsion solids, only one may be
used to make the demonstration. If, however, the washes are maflaged1 on
separate portions of the unit, separate demonstrations should be performed
for each unless it can be shown that the wastes are not substantively
different.
9. How does one deal with wastes that are generated only infrequently?
Infrequently generated wastes should be managed on separate parcels of
land and should be demonstrated separately if there are substantive dif-
ferences between the wastes. The answer to Question 8 may partially answer
this question. The frequency of application in the LTD should be altered
from that proposed in this document to match the frequency of waste genera-
tion (i.e., wastes generated less than one per year should be tested using
a one time application).
125
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10. In choosing the constituents to be monitored in the demonstration, can
the applicant ignore hazardous constituents present in low concentra-
tions and use indicators instead?
Because of the influences of sample size, analytical detection limits,
and background concentrations, all hazardous constituents that can be
detected in the waste or its degradation products should be analyzed
throughout the experimental phases of the LTD. Since compounds or elements
that have been identified as hazardous are often so even in low concentra-
tions and because these compounds, if they are resistant to treatment, may
build up in soil over time, any identifiable constituent is of concern.
Chapter 10 of this document should give some guidance on this issue. The
authors have taken particular care to limit the analytical burden and cost
of the procedures presented in this document to that information considered
essential to the demonstration. It should also be noted that few wastes
contain a very extensive array of the constituents listed in 40 CFR 261
Appendix VIII.
11. The test protocols in this manual indicate that different soil series
should be examined separately in the demonstration. Are there any
exceptions to this general rule?
Soils with different characteristics should be examined separately in
the demonstration because these differences may significantly affect waste
treatment. The USDA, SCS classification system is used to define different
soils (i.e., "soil series") because it is a standard, widely recognized
classification system. An owner/operator may, however, demonstrate through
certification by a qualified soil scientist that the differences in the
"soil series" at his HWLT unit will not significantly affect the treatment
of hazardous waste at the unit. If this demonstration is approved, the
different soils series will be considered the same for the purposes of the
demonstration and the UZM program.
•U.S. GOVERNMENT PRINTING OFFICEI 1985-461-221/24031
126
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ERRATA SHEET
Draft Permit Guidance Manual on Hazardous Waste
land Treatment Demonstrations (12/84)
Due to an error, the following equations and the reference list were
inadverently omitted from the draft manual printed by GPO. Please make
note of these additions.
Equations
p. 49 T = _ X R _ - 1 ; where: T = gamma light decrease
_ Xg = mean chart reading for blank
X s • _ at time t; and
Xg = mean chart reading for sample
p. 50 *f = f corrected 0 time light level - 1 1
I 5 minute light level for sample j
p. 57 Dto = Can - (CTO - Cs)
^ao
p. 58 Dti = Caj - (Crj - Csj)
Cai
p. 71 Dto = Can - (Cro - Cg) ; Dti = Cai - (CH - Csi )
p. 75 Cyr = 1/2 Ccrit ; LRRDC = Cyr ; A = PR ; NA =
T 1/2 Cw LRRLC AL
x (weight fraction of residual
p. 76 UL = LCAP ; z = _ solids in waste) _ x 10~5
p. 77 n = Z In
Reference List (see next page)
-------
REFERENCES
Alexander, M. 1977. Introduction to soil microbiology. John Wiley and
Sons, Inc. New York.
Alexander, M. 1980. Biodegradation of toxic chemicals in water and soil.
pp. 179-190 In: R. Haque (ed.) Dynamics, Exposure, and Hazard Assessment
of Toxic Chemicals. Ann Arbor Science Publ., Inc. Ann Arbor, MI.
American Petroleum Institute. 1983. Land treatment practices in the
petroleum industry. Environmental Research and Technology, Inc. Concord,
MA.
Beckman Instruments, Inc. 1982. Beckman Microtox™ System operating
manual. 63 p.
Black, C. A. (ed.) 1965. Methods of soil analysis. Am. Soc. of Agro-
nomy. Madison, WI.
Blake, G. R. 1965. Particl e density. In: C. A. Bl ack (ed.) Methods
of Soil Analysis. Agron. 9:371-373. Am. Soc. of Agronomy. Madi-
son, WI.
Bououcos, G. J. 1951. A recalibration of the hydrometer method for
making mechanical analyses of soils. Agron J. 43:434-437.
Bremner, J. M. 1965. Total nitrogen. In: C. A. Black (ed.) Methods
of Soil Analysis. Agronomy 9:1149-78. Am. Soc. of Agronomy. Madison,
WI.
Bremner, J. M. and C. S. Mulvanex. 1982. Nitrogen-total, pp. 595-624.
In: A. L. Page, R. H. Miller, and D. R. Keeney (eds.) Methods of Soil
Analysis Part 2. Chemical and Micro-bological Properties. Amer. Soc. of
Agronomy. Madison, WI.
Brown, K. W., K. C» Donnelly, and L. E, Deuel, Jr. 1983. Influence of
nutrient additions, sludge application rate, and frequency on
biodegradation of two oily sludges. Microbial Ecology 9:363-373.
Brown, K. W., C. J. Gerard, B. W. Hipp, and J. T. Ritche. 1974. A
procedure for placing large undisturbed monoliths in lysimeters. Soil Sci.
Soc. Am. Proc. 38:981-983.
127
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Brown, K. W., J. C. Thomas, and M. W. Aurellus. 1984. A procedure for
collecting barrel sized undisturbed soil monoliths. Soil Sci. Soc. Am.
Proc. (in review).
Burks, S. L., M. Amalon, E. F. Stebler, J. Harmon, F. Leach, M. Sanborn,
and J. Matthews. 1982. Comparison of acute response of Microtox1",
daphnia Magna, and fathead minnows to oil refinery wastewaters. Progress
Report to Oil Refiners' Waste Control Council by Oklahoma State Univer-
sity, Water Quality Research Laboratory. Stillwater, Oklahoma. 24 p.
Cassel , D. K., T. H. Kruger, F. W. Schroer, and E. B. Norum. 1974. Solute
movement through disturbed and undisturbed soil cores; Soil Sci. Soc. Am.
Proc. 38:36-40.
Casseri, N. A., W. Ying, and S. A. Soiyka. 1983. Use of a rapid bioassay
for assessment of industrial wastewater treatment effectiveness. Presenta-
tion at the Purdue Industrial Waste Conference. 18 p.
Dindal, D. L. 1978. Soil organisms and stabilizing wastes. Compost
Sci./Land Utilization 19(4):8-11.
Edwards, N. T. and B. M. Ross-Todd. 1980. An improved bioassay technique
used in solid waste leachate phytotoxicity research. Environ, and Exp.
Bot. 20:31-38.
EPA. 1980. Guidelines for quality assurance/quality control Program.
Environmental Monitoring Systems Laboratory, Las Vegas, NY. QAMS-005-80.
EPA. 1982. Test methods for evaluating solid waste: physical/chemical
methods. Second Edition. U. S. EPA Office of Sol id Waste and Emergency
Response. 'Washington, D.C. SW-846.
/*
EPA. 1983A. Hazardous Waste Land Treatment. U. S. EPA Office of Solid
Waste. Washington, D.C. SW-874.
EPA. 19838. RCRA Guidance document: land treatment units. U. S. EPA
Office of Solid Waste. Washington, D.C.
EPA. 1984A. Unsaturated zone monitoring for hazardous waste land
treatment units. U. S. EPA Office of Solid Waste. Washington, D.C.
EPA. 1984B. Permit applicant's guidance manual for hazardous waste land
treatment, stroage, and disposal facilities, U. S. EPA Office of Solid
Waste. Washington, D.C.
Jackson, M. L. 1958. Soil chemical analysis. Prentice-Hall, Inc.
Englewood Cliffs, NJ.
Kaufman, D. D. 1983. Fate of toxic organic compounds in land-applied
waste. pp. 77-151. In: J. F. Parr, P. B. Marsh, and J. M. Kia (eds.).
Land Treatment of Hazardous Wastes. Noyes Data Corp. Park Ridge,
NJ.
128
-------
McClean, E. 0. 1982. Soil pH and lime requirement, pp. 199-224. In: A.
L. Page, R. H. Miller, and D. R. Keeney (eds.) Methods of Soil Analysis
Part 2. Chemical and Microbiological Properties. Am. Soc. of
Agronomy. Madison, WI.
Mechlich, A. 1939. Use of triethandamine acetate - barrier hydroxide
buffer for determinators of some base exchange properties and lime
requirement of soil. Soil Sci. Soc. Am. Proc. 3:162-166.
Nelson, W. L, A. Mehlich, and E. Winters. 1953. The development,
evaluation, and use of soil tests for phosphorus availability. In: W.
H. Pierre and A. G. Norman (eds.) Soil and Fertilizer Phosphorus.
Agron. 4:153-188.
Nelson, D. W. and L. E. Somrners. 1982. Total carbon, organic carbon, and
organic matter. pp. 539-580. In: A. L. Page, R. H. Miller, and D. R.
Keeney (eds.) Methods of Soil Analysis Part 2. Chemical and Microbiologi-
cal Properties. Am. Soc. of Agronomy. Madison, WI.
Neuhauser, E. F., M. R. Malecki, and R. C. Loehr. 1983. Methods using
earthworms for the evaluation of potentially toxic materials in soil. In:
R. A. Conway and W. P. Gulledge (eds.) Hazardous and Industrial Solid Waste
Testing: Second Symposium. ASTM STP 805. American Society of Testing and
Materials.
01 sen, S. R. and L. E. Sommers. 1982. Phosphorus, pp. 403-43U. In: A.
L. Pae, R. H. Mil 1 er, and D. R. Keeney (eds.) Methods of Soi 1 Analysis
Part 2. Chemical and Microbiologal Properties. Am. Soc. of Agronomy.
Madison, WI.
Overcash, M. R. and D. Pal. 1979. Design of land treatment systems for
industrial wastes-theory and practice. Ann Arbor Science Publ., Inc. Ann
Arbor, MI.
Peech, M. 1965. Hydrogen ion activity. In: C. A. Black (ed.) Methods
of Soil Analysis. Agron 9:914-920.
Peltier, W. 1978. Methods for measuring the acute toxicity of effluents
to aquatic organisms. EPAr-600/4-78-012.
Rhoades, J. D. 1982. Soluble salts, pp. 167-180. In: A. L. Page, R. H.
Miller, and D. R. Keeney (eds.) Methods of Soil Analysis Part 2. Chemical
and Microbiological Properties. Am. Soc. of Agronomy. Madison, WI.
Richards, L. A. 1965. Physical conditions of water in soi 1. In: C.
A. Black (ed.) Methods of Soil Analysis. Agron. 9:128-137. Am. Soc. of
Agronomy. Madison, WI.
Shoemaker, H. E., E. 0. McLean, and P. F. Pratt. 1962. Buffer methods for
determination of lime requirements of soils with appreciable amounts of
exchangeable aluminum. SSSAP 25:274-277.
129
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Skinner, J. 1984. Guidance on petroleum refinery waste analysis for land
treatment permit applications. Report to Hazardous Waste Permit Branch
Chiefs from Office of Solid Waste. U. S. EPA Office of Solid Waste.
Washington, D.C.
Sobeck, A. A., W. A. Shuller, J. R. Freeman, and R. M Smith. 1978. Field
and laboratory methods applicable to overburdens and minespoil. U. S. EPA
No. 600/2-78-054. U. S. Environmental Protection Agency. Cincinnati, OH.
200 p.
Sorensen, S. P. L. 1909. Cited by Peech, M. 1965.
U. S. Salinity Laboratory Staff. 1954. Diagnosis and improvement of
saline and alkali soils. U. S. Department of Agriculture No. 60. U. S.
Government Printing Office. Washington, D.C.
130
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UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
DATE:
SUBJECT-:
FROM:
TO:
Draft Permit Guidance Manuals for Hazardous Waste Land
Treatment Units^_
jf^^Sktu&r-
KennetrPA. Shuster, Chief
Land Disposal Branch (WH-565)
Addressees
Attached for your information are two draft manuals
entitled, "Permit Guidance Manual on Hazardous Waste Land
Treatment Demonstrations" and "Permit Guidance Manual on
Unsaturated Zone Monitoring for Hazardous Waste Land Treatment
Units." The availability of these draft manuals for public
comment and review was recently announced in the Federal
Register (see attachment).
"Permit Guidance Manual on Hazardous Waste Land Treatment
Demonstrations" provides detailed guidance on specific labo-
ratory and field test methods that may be used to complete the
treatment demonstration, which is required under §264.272 for
owners/operators of land treatment units. The manual also
describes alternative permitting approaches (e.g., two-phase
permit, short-term permit, etc.) for various situations.
"Permit Guidance Manual on Unsaturated Zone Monitoring for
Hazardous Waste Land Treatment Units" provides guidance on the
development and implementation of effective unsaturated zone
monitoring systems for land treatment units. The manual covers
both soil core and soil pore-liquid monitoring and addresses
equipment selection, installation, and operation, sampling
procedures, chain of custody considerations, and data analysis
and evaluation.
A limited number of additional copies of these manuals may
be obtained from the RCRA Hotline. Any comments or questions
should be directed to Mike Flynn of my staff (WH-565E) at
FTS-382-4489.
Attachments
Addressees:
OSW Senior Staff
OSW Branch Chiefs
OERR Senior Staff
OWPE Senior Staff
Mike Barclay (WH-527)
Amy Svoboda (LE-134W)
Sam Napolitano (PM-220)
Mark Greenwood (LE-132S)
Nancy Hutzel (LE-132W)
Susan Schmedes (LE-132W)
Dick Scalf, RSKERL-Ada
Norb Shomaker, SHWRD-Cinn
Les McMillion, EMSL-LV
Will LaVeille (RD-682)
EPA Headquarter's Library
EPA Regional Libraries
State Hazardous Waste Agencies
EPA Form 1320-6 (Rev. 3-761
-------
1238
Federal Register / Vol. 50, No. 7 / Thursday, January 10, 1985 / Proposed Rules
non-conveyed properties, there shall be
included on account of such costs, in
those cases involving mortgages on
which the unpaid principal obligation at
the time of the institution of foreclosure
exceeds 80 percent of the appraised
value of the property as the date the
mortgage was accepted for insurance,
an amount not in excess of the greater of
the following:
*****
(Sec. 7(d), Department of HUD Act (42 U.S.C.
3535(d)), Sec. 211, National Housing Act (12
U.S.C. 1715(b)), Sec. 204(a). National Housing
Act (12 U.S.C. 1710(a))
Dated: November 30,1984.
Maurice L. Barksdale,
Assistant Secretary forHousing—Federal
Housing Commissioner.
. [FR Doc. 85-617 Filed 1-9-85; 8:45 am]
BILLING CODE 421O-27-M
ENVIRONMENTAL PROTECTION
AGENCY
40 CFR Part 264
[OSWER-FRL-2754-5]
Hazardous Waste Treatment, Storage,
and Disposal Facilities; Availability of
Information
AGENCY: Environmental Protection
Agency.
ACTION: Notice of availability of
information and request for comments.
SUMMARY: The Environmental Protection
Agency today announces the
availability of two draft Permit
Guidance Manuals for public comment.
These manuals are (1) Permit Guidance
Manna! on Unsaturated Zone
Monitoring for Hazardous Waste Land
Treatment Units (EPA/530-SW-84-016),
and (2) Permit Guidance Manual on
Hazardous Waste Land Treatment
Demonstrations (EPA/530-SW-84-015).
The first manual provides guidance on
unsaturated zone monitoring for
hazardous waste land treatment units. It
can be used by permit applicants and
permit writers to develop effective
monitoring systems that comply with the
Part 264, Subpart M regulations. The
second manual provides guidance on
treatment demonstrations that are
required under § 264.272 for all owners
and operators of hazardous waste land
treatment units.
These manuals may be used for
information and guidance by owners
and operators of facilities that treat or
dispose of hazardous waste in land
treatment units. These manuals will
assist in the implementation of the 40
CFR Part 264 hazardous waste
management regulations by helping
owners/operators and permit officials to
design and carry out comprehensive
treatment demonstrations and to
develop effective unsaturated zone
monitoring programs.
DATE: Comments on these draft permit
guidance documents must be submitted
on or before March 11,1965.
ADDRESS: Comments should be
addressed to Docket Clerk, Office of
Solid Waste (WH-562), U.S.
Environmental Protection Agency, 401M
Street. SW.. Washington, D.C. 20460. All
communications should identify the
document title and publication number
(e.g., Permit Guidance Manual on
Hazardous Waste Land Treatment
Demonstrations (EPA/530-SW-84-015)).
Copies of these draft guidance
manuals are available for reading at the
EPA Library Public Information
Reference Unit (Room 2904} and the
Subtitle C Docket Room (Room S212),
both located at 401 M St. SW,
Washington, D.C., 20460, as well as at
all Regional Office Libraries, Monday
through Friday during the hours of 9:00
a.m. to 4:30 p.m. A limited number of
personal copies of the draft manuals
may be obtained by calling the RCRA
Hotline at (800) 424-9346 (toll free] or at
(202) 382-3000.
FOR FURTHER INFORMATION CONTACT:
RCRA Hotline, at (800) 424-8346 (toll
free) or at (202) 382-3000. For technical
information, contact Michael Flynn,
Office of Solid Waste (WH-565E), U.S.
Environmental Protection Agency, 401M
Street, SW.. Washington, D.C. 20460, at
(202) 382-4489.
SUPPLEMENTARY INFORMATION: Subtitle
C of the Resource Conservation and
Recovery Act (RCRA), Section 3004,
required the Environmental Protection
Agency (EPA) to promulgate regulations
setting performance standards for
owners and operators of facilities that
treat, store, or dispose of hazardous
waste. 40 CFR Part 265 contains the
standards applicable to owners and
.operators of interim status facilities,
while 40 CFR Part 264 contains
permitting standards for new and
existing facilities.
To help implement these standards,
the EPA has developed a series of
guidance documents. There are three •
types of documents: RCRA Technical
Guidance Documents, Permit Guidance
Manuals, and Technical Resource
Documents. The Permit Guidance
Manuals are directed to permit
applicants and EPA/State permit
writers. They describe the permitting
process, present the regulatory
requirements, and provide
recommendations for the preparation of
a permit application and the
development of the resulting permit.
Certain Permit Guidance Manuals also
provide detailed technical and policy
guidance on specific regulatory
requirements that must be addressed in
the facility's permit. The detailed policy
guidance in these documents is an
elaboration of the Agency's policy
guidance already described in the
preamble to the regulations.
Today's notice announces the
availability of two draft Permit
Guidance Manuals. These manuals are
Permit Guidance Manual on Hazardous
Waste Land Treatment Demonstrations
and Permit Guidance Manual on
Unsaturated Zone Monitoring for
Hazardous Waste Land Treatment
Units.
Permit Guidance Manual on
Hazardous Waste Land Treatment
Demonstrations provides permit
applicants and writers with guidance on
land treatment demonstrations required
under § 264.272. The manual identifies
specific laboratory and field test
methods that may be used to complete
the demonstration, and describes the
applicability of alternative treatment
demonstration approaches and
permitting procedures (e.g., short-term
permit, two-phase permit, etc.) to
various situations. The manual
addresses numerous technical and
policy questions regarding the overall
approach to the demostration, the
extensiveness of the demostration, and
the permitting of land treatment units to
accommodate the treatment
demonstration.
Permit Guidance Manual on
Unsaturated Zone Monitoring for
Hazardous Waste Land Treatment
Units is directed toward permit
applicants and permit writers who are
developing unsaturated zone monitoring
programs for hazardous waste land
treatment units required under § 264.278.
This manual covers both soil core and
soil pore-liquid monitoring. Equipment
selection, installation, and operation,
sampling procedures, chain of custody
considerations, and data evaluation are
all addressed. The installation and
sampling procedures are presented in a
step-by-step format so that the manual
may be easily used by field personnel.
The Agency requests comments on the
accuracy and cpmpletness of the
information presented in these draft
documents. EPA encourages
commenters to suggest remedies and
alternatives should inaccuracies or
incompleteness be identified.
List of Subjects in 40 CFR Part 264
Hazardous materials Packaging and
containers, Reporting and recordkeeping
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Federal Register / Vol. 50, No. 7 / Thursday, January 10, 1985 / Proposed Rules
1239
requirements, Security measures, Surety
bonds, Waste treatment and disposal.
Authority: Sees. 1006, 2002(a), 3004 and
3005 of the Solid Waste Disposal Act as
amended by the Resource Conservation and
Recovery- Act of 1976, as amended (42 U.S.C.
6905, 6912(a). 6924, and 6025).
Dated: December 26,1984.
lack McGraw,
Acting Assistant Administrator for Solid
Waste and, Emergency Response.
[FR Doc. 85-704 Filed 1-9-85; 8:45 am]
BILLING CODE (SM-50-N .
FEDERAL COMMUNICATIONS
COMMISSION
47 CFR Part 73
(Gwi. Docket No. 82-797; FCC $4-647]
Commission Policy Regarding the
Advancement of Minority Ownership in
Broadcasting
AGENCY: Federal Communications
Commission.
ACTION: Report and Order; Denial of
Proposed Rule.
SUMMARY: This Report and Order
declines to adopt the change in
Commission Rule § 73.1150 proposed in
the Notice of Proposed Rule Making in
Gen. Docket 82-797. Specifically, the
Commission determined that allowing a
seller-creditor to retain a reversionary
interest in the license in a seller-
financed sale of a broadcast property to
a minority buyer is prohibited by the
Communications Act of 1934, as
amended. The Commission further
concluded that permitting a seller-
creditor to contractually guarantee a
contingent right to reassignment of a
broadcast license would be inadvisable
as a matter of policy. The Commission
found that such action would pose a
serious threat to the ability of a minority
buyer to freely and independently
operate a broadcast station in the public
interest.
FOR FURTHER INFORMATION CONTACT
Marcia C Alterman, Mass Media
Bureau, (202) 632-7792.
SUPPLEMENTARY INFORMATION:
Report and Order (Proceeding
Terminated)
In the Matter of Commission Policy
Regarding the Advancement of Minority
Ownership in Broadcasting; General Docket
No. 82-797.
Adopted: December 21,1984.
Released: January 8,1985.
By the Commission.
1. Before the Commission for
consideration are comments filed in
response to the Notice of Proposed Rule
Making ("Notice") in the above-
captioned proceeding.' The Notice
solicited comments with respect to
permitting alternative security
arrangements in seller-financed sales of
broadcast properties to minorities.
Background
2. The Commission has long supported
increased minority participation and
ownership in the broadcast industry.
Such participation benefits not only
minorities, but the general public as
well, by diversifying control of the
media and thus the selection of
available programming. Accordingly, the
Commission is firmly committed to the
goal of encouraging minority
participation in the broadcast industry.
In 1981, we created the Advisory
Committee on Alternative Financing for
Minority Opportunities in
Telecommunications (Advisory
Committee) in furtherance of this goal.*
The Advisory Committee examined
regulatory and economic conditions
thought to hinder minority acquisition of
telecommunication properties and its
Report^ offered a number of proposals
designed to enhance minority
ownership. Several of these proposals,
such as the expanded use of distress
sales and the broader availability of tax
certificates, have already been adopted.4
This Report and Order deals with the
Advisory Committee's proposal
concerning the possible expansion of
seller-creditors' rights in seller-financed
transactions.
3. The Advisory Committee found that
obtaining "financing [particularly] has
remained the greatest obstacle" to
minorities' entrance and establishment
in the telecommunications industry. In
this regard, the Advisory Committee
observed:
many minority broadcasters do not know
how to obtain financing and financial
institutions have misconceptions about
potential minority broadcasters. * * * [Also]
the small or minority entrepreneur * * * does
not have access to fixed rate long-term funds.
As a result, that entrepreneur is subject to the
vicissitudes of short-term rates.'
' Notice of Proposed Rule Making in Gen. Docket
82-797,48 FR 5976 (February 9,1983).
'The Advisory Committee was comprised of
leaden in both the private and public sectors of the
financial and telecommunications communities.
' Strategies for Advancing Minority Ownership
Opportunities in Telecommunications: The Final
Report of the Advisory Committee on Alternative
Financing for Minority Opportunities in
Telecommunications to the Federal
Communications Commission (May 1982) (hereafter
"Deport").
' Commission Policy Regarding the Advancement
of Minority Ownership in Broadcasting, 48 FR 5943
(February 9,1983) (hereafter "Policy Statement
'Report at 25-28.
The Advisory Committee recommended
that seller-financing, already prevalent
in broadcast-sale transactions, be
further encouraged "particularly since it
is obviously one of the ways that
minorities can obtain broadcasting
properties."'Specifically, the Advisory
Committee proposed the Commission
expand the options accorded seller-
creditors to include the right to retain a
reversionary interest in the license of
the station being sold.
4. The Commission's current Rule,
found at 47 CFR 73.1150, prohibits
agreements, express or implied, which
permit a broadcast licensee to: (1)
Retain an interest in the license; (2)
claim a right to future assignment of the
license; or (3) reserve a privilege to use
the broadcast facilities, upon the sale or
transfer of its interest in a station. In
addition, as we observed in the Notice,
the Communications Act of .1934, as
amended, and longstanding Commission
precedent, as affirmed by the United
States Supreme Court, appear to support
this prohibition.7 However, the Notice
also stated that:
we believe it appropriate to inquire as to
whether certain limitations could be
removed, consistent with the provisions of
the Communications Act, so as to further
encourage the use of this financing tool,
particularly where the transaction would
enhance minority ownership of the mass
media communications.
The Notice solicited comments from the
public on this proposal, specifically
inviting interested parties to address the
following:
the type of security interest that may be
retained by a seller-creditor whether that
interest can or should include a reversionary
interest in the license itself and the legal
process, if any, that should be required before
the creditor could exercise its reversionary
interest
Comments
5. Parties supporting the expansion of
seller-creditors' rights argued that the
proposed rule was necessary to
stimulate minority acquisition of
broadcast properties.'These
commenters asserted that because the
physical assets of a station rarely
represent more than a small portion of
the purchase price, reliance on a
security interest in only those physical
assets forces a seller-creditor to place
his own capital at significantly greater
risk. To minimize the risk associated
•/Vo//ceat 5976.
'For a detailed discussion, see Notice at 5977.
•Comment* supporting the proposed rule were
submitted by: Bone and Woods. Columbia
Broadcasting Systems, Inc., and National Radio
Broadcasters Association.
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