USDA
EPA
United States
Department of
Agriculture
Science & Education Admin.
Cooperative Research
Washington DC 2O250
CR-10
United States
Environmental Protection
Agency
Industrial Environmental Research
Laboratory
Cincinnati OH 45268
EPA-600/7-80-054
March 1980
Research and Development
Properties and Plant
Growth Potential of
Mineland Overburden
Interagency
Energy/Environment
R&D Program
Report
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RESEARCH REPORTING SERIES
Research reports of the Office of Research and Development, U.S. Environmental
Protection Agency, have been grouped into nine series. These nine broad cate-
gories were established to facilitate further development and application of en-
vironmental technology. Elimination of traditional grouping was consciously
planned to foster technology transfer and a maximum interface in related fields.
The nine series are:
1. Environmental Health Effects Research
2. Environmental Protection Technology
3. Ecological Research
4. Environmental Monitoring
5. Socioeconomic Environmental Studies
6. Scientific and Technical Assessment Reports (STAR)
7. Interagency Energy-Environment Research and Development
8. "Special" Reports
9. Miscellaneous Reports
This report has been assigned to the INTERAGENCY ENERGY-ENVIRONMENT
RESEARCH AND DEVELOPMENT series. Reports in this series result from the
effort funded under the 17-agency Federal Energy/Environment Research and
Development Program. These studies relate to EPA's mission to protect the public
health and welfare from adverse effects of pollutants associated with energy sys-
tems. The goal of the Program is to assure the rapid development of domestic
energy supplies in an environmentally-compatible manner by providing the nec-
essary environmental data and control technology. Investigations include analy-
ses of the transport of energy-related pollutants and their health and ecological
effects; assessments of, and development of, control technologies for energy
systems; and integrated assessments of a wide range of energy-related environ-
mental issues.
This document is available to the public through the National Technical Informa-
tion Service, Springfield, Virginia 22161.
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EPA-600/7-80-054
March 1980
PROPERTIES AND PLANT GROWTH
POTENTIAL OF MINELAND OVERBURDEN
by
W. R. Byrnes, W. W. McFee and J. G. Stockton
Indiana Agricultural Experiment Station
Department of Forestry and Natural Resources
Department of Agronomy
Purdue University
West Lafayette, Indiana 47907
SEA/CR IAG no. D6-E762
Grant no. 684-15-18
Project Officer
S. R. Aldrich, Associate Director
Agricultural Experiment Station
University of Illinois
Urbana, Illinois 61801
Program Coordinator
Eilif V. Miller
Mineland Reclamation Research Program
Science and Education Administration - Cooperative Research
Washington, D.C. 20250
Project Officer
Ronald D. Hill
Resource Extraction and Handling Division
Industrial Environmental Research Laboratory
Cincinnati, Ohio 45268
This study was conducted in cooperation with the Science and Education
Administration, Cooperative Research USDA, Washington, D.C. 20250
INDUSTRIAL ENVIRONMENTAL RESEARCH LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
U.S. ENVIRONMENTAL PROTECTION AGENCY
CINCINNATI, OHIO 45268
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DISCLAIMER
This report has been reviewed by the Industrial Environmental Research
Laboratory-Cincinnati, U. S. Environmental Protection Agency, and approved
for publication. Approval does not signify that the contents necessarily
reflect the views and policies of the U. S. Environmental Protection Agency,
nor does mention of trade names or commercial products constitute endorse-
ment or recommendation for use.
The views and conclusions contained in this report are those of the
authors and should not be interpreted as representing the official policies
or recommendations of the Science and Education Administration, Cooperative
Research, U. S. Department of Agriculture.
11
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FOREWORD
When energy and material resources are extracted, processed, converted,
and used, the related pollutional impacts on our environment and even on our
health often require that new and increasingly more efficient pollution
control methods be used. The Industrial Environmental Research Laboratory-
Cincinnati (lERL-Ci) assists in developing and demonstrating new and improved
methodologies that will meet these needs both efficiently and economically.
Reported here is the results of a study supported cooperatively by U.S.
Department of Agriculture and U.S. Environmental Protection Agency at Purdue
University. The project was a part of the Interagency Energy-Environment
Research and Development Program. The results of this study should be of
interest to these persons engaged in the planning and reclamation of surface
mined lands, because properties of overburden materials that may serve as
predictors of potential plant growth have been evaluated.
For further information contact the authors or the Industrial Environ-
mental Research Laboratory.
David G. Stephan
Director
Industrial Environmental Research Laboratory
Cincinnati
111
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ABSTRACT
This investigation was conducted to determine physical and chemical prop-
erties of mineland overburden, to evaluate plant growth in these materials,
and to identify properties of overburden materials before mining that may serve
as predictors of potential plant growth.
Eighteen overburden materials from 5 surface coal mines in the Illinois
coal basin of southwestern Indiana were sampled and analyzed for 20 physical
and chemical properties. Twelve are unconsolldated materials, including A and
B horizons, loess, lacustrine sediments,and glacial tills, and six are rock
strata that break and weather easily. Growth potential of overburden materials,
with and without sewage sludge and fertilizer amendments, were evaluated in
greenhouse pot culture using alfalfa, wheat and white pine. Oats yield, and
survival and growth of Virginia pine and yellow-poplar were evaluted for 10
materials in outdoor containers.
Regression analysis of plant growth against chemical and physical prop-
erties of the overburden materials did not reveal properties that could be
consistently used in a formula approach to predicting plant growth material.
Electrical conductivity of the material extract and water storage capacity
were most frequently significantly related to growth.
The general ranking of overburden materials evaluated for plant growth
potential was lacustrine sediment > A horizons > B horizons = glacial tills =
loess > brown shale > sandstone > gray shale > black fissile shales. Lacus-
trine sediment and A horizons were clearly superior materials for use as sur-
face plant growth media. The B horizons, partially weathered loess and glacial
tills were similar in productivity and,are suitable for use in the plant root
zone. With amendments, B horizon and loess may be acceptable for surface use,
but are not likely to equal A horizon material 1n productivity. The sandstone
and brown shale are not suitable 1n the upper plant root zone due to undesired
physical properties and potentially phytotoxlc elements in sandstone. The
gray and black fissile shales used are unsuitable for plant growth and should
be buried to avoid direct contact with plant roots and to reduce subsequent
oxidation and leaching.
Addition of sewage sludge resulted in vastly improved growth of wheat and
to a lesser extent alfalfa on most materials in the greenhouse. Fertilization
with N-P-K was less effective than sludge but usually produced increased plant
growth. Amendment of the upper rooting zone with major nutrient elements and
organic matter from wastes such as sludge would be a beneficial practice.
This report was submitted in fulfillment of Contract No. 684-15-18 by
Purdue University 1n cooperation with the Science and Education Administration,
Cooperative Research Unit, USDA, under the sponsorship of the U.S. Environment-
al Protection Agency. This report covers the period from July 21, 1976 to
September 30, 1978 and was completed as of April 15, 1979.
iv
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CONTENTS
Page
DISCLAIMER ii
FOREWORD Hi
ABSTRACT iv
FIGURES v1
TABLES vii
ACKNOWLEDGEMENTS 1x
INTRODUCTION 1
CONCLUSIONS 2
RECOMMENDATIONS . 4
LITERATURE REVIEW 6
PROCEDURES 9
MATERIAL COLLECTION 9
CHEMICAL AND PHYSICAL ANALYSES 9
PLANT GROWTH STUDIES 15
STATISTICAL PROCEDURES 17
RESULTS AND DISCUSSION 18
PHYSICAL AND CHEMICAL OVERBURDEN PROPERTIES 18
Physical Properties 18
Chemical Properties 20
Correlation of Overburden Properties 24
PLANT GROWTH STUDIES-GREENHOUSE 24
Wheat and Alfalfa Yields 24
Elemental Content of Wheat Plants 30
PLANT GROWTH STUDIES-OUTDOOR CONTAINERS 37
Oats Yield 40
Tree Seedlings 42
Leachate Analyses 42
PREDICTION OF PLANT GROWTH POTENTIAL 44
LITERATURE CITED 48
APPENDIX 53
A. LABORATORY PROCEDURES SYNOPSIS 53
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FIGURES
Number page
1 Map of southwestern Indiana showing active coal mines
and selected study sites (A). Modified from Hutchison,
1971 10
2 Dry weight of wheat produced 1n second greenhouse
experiment as Influenced by overburden material and
treatment 32
3 Relationship between extractable boron 1n overburden
materials and uptake by plants 38
vi
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TABLES
Number Page
1 Overburden materials sampled 11
2 Generalized hlghwall log for Amax Ayrcoe mine 1n P1ke
County. Soil type: Zanesvllle silt loam 12
3 Generalized Mghwall log of Amax Chinook mine 1n Clay
County from drill log. Soil type: Iva silt loam 13
4 Generalized hlghwall log for Amax Ayreshlre mine 1n
Warrlck County. Soil type: Hosmer silt loam 14
5 Procedures used 1n chemical and physical characterization
of the overburden 16
6 Physical properties of selected overburden materials 19
7 Mean elemental content of selected overburden properties 21
8 Mean chemical properties of selected overburden materials .... 23
9 Relative variation, C.V. (%), 1n chemical properties
within strata based on analysis of selected overburden
materials collected at three sampling points at three times . . 25
10 Matrix of correlation coefficients (r) for measured
properties of selected overburden materials 26
11 Effect of overburden material and treatment on yield of
wheat and alfalfa 1n the first greenhouse study 28
12 Effect of overburden material and amendments on growth of
wheat and alfalfa in the second greenhouse experiment.
Each value 1s a mean of three replicates 29
13 Summary of analysis of variance for the greenhouse experiments . . 31
14 Emergence and height of wheat plants after four weeks growth on
overburden materials 1n the second greenhouse experiment .... 33
15 Emergence and height of alfalfa plants after four weeks growth
on overburden materials 1n the second greenhouse experiment . . 34
16 Elemental content of wheat plants grown eight weeks 1n selected
overburden materials with and without amendments 1n pot
culture 36
17 Mean oat yield, 4 weeks, and tree survival and growth, 12
weeks, 1n outdoor containers of overburden material. Each
value 1s a mean of three replicates 39
vii
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TABLES (continued)
Number page
18 Mean element content of oat plants grown four weeks 1n
outdoor containers of overburden material. Each value
1s a mean of three replicates 41
19 Chemical analysis of leachate collected in May 1978 and
April 1979 from outdoor containers of overburden
material. Each value 1s a mean of three replicates 43
20 Chemical properties of overburden materials used in
outdoor containers 45
21 Overburden properties most closely correlated by step-wise
regression to plant yield in greenhouse experiments 47
viil
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ACKNOWLEDGMENTS
This investigation was conducted by personnel of the Department of
Agronomy and Forestry and Natural Resources, Purdue University, in cooperation
with AMAX Coal Company and the Indiana Department of Natural Resources, Divi-
sion of Geological Survey. AMAX Coal Company provided access to active mine
areas, assisted with site selection and overburden sampling, and furnished
equipment for crushing of rock samples and sulfur analysis. Personnel of the
Indiana Geological Survey assisted with site selection, description of over-
burden stratigraphy, and analysis of sulfur in some overburden materials.
Appreciation is extended to Mr. V. P. Wiram, Manager of Environmental
Geology and Hydrology, and Dr. David S. Ralston, Environmental Engineer/
Agronomist, AMAX, for their encouragement in establishment of the project and
arrangement of a cooperative agreement for use of company lands. The.work of
Mr. Mike Ellis and Mr. Randy Staley, AMAX, in highwall sampling and preparation
of extracted overburden materials is also recognized. The assistance of
Mr. Ned K. Bleur, Glacial Geologist, and Mr. Don Eggert, Coal Geologist, Indiana
Geological Survey, for their helpful suggestions on site selection, identifica-
tion of geologic strata, and sulfur analysis is gratefully acknowledged. Ana-
lytical work by personnel of the Purdue Soil Testing Laboratory and assistance
of several undergraduate work-study students in various aspects of the project
are also appreciated.
Overall administration of the project was coordinated by Dr. B. J. Li ska,
Director, Indiana Agricultural Experiment Station, and Dr. Eilif V. Miller,
Science and Education Administration, Cooperative Research, U.S. Department
of Agriculture.
ix
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INTRODUCTION
With increasing demand for coal as an energy source, it is evident that
coal-mining activities will expand significantly in the United States. A
major proportion of coal extraction in the foreseeable future will be by
surface-mining which Is more disruptive to land areas than underground mining.
The Illinois Coal Basin is a major energy resource with coal reserves
estimated at 114 to 136 billion metric tons; more than 16 billion metric tons
of recoverable coal occurs in southwestern Indiana. Land disturbance from
surface coal-mining in Indiana alone exceeds 1800 ha per year for a total of
about 62,500 ha to date.
Although coal production is a necessity, the control of environmental
problems created by surface-mining and restoration of disturbed land to pro-
ductive use are also important. These aspects were emphasized in federal
legislation regulating surface-mining and reclamation (PL 95-87) enacted in
1977. In mineland reclamation, the objective 1s to leave a valuable resource,
i.e., land areas of the highest possible value following coal extraction.
One of the major problems of reclamation, however, involves requirements and
related criteria for cast overburden disposition to provide the best plant
growth media. The approach generally used is merely to require that original
"top soil" be returned to the cast overburden surface. Although this may be
satisfactory, other overburden strata may be adequate for plant growth and
could be placed near the surface more efficiently and economically. Analysis
of undisturbed overburden to determine quantity, layer thickness and volume,
and quality, physical and chemical properties, of various soil and geologic
strata above the coal seam may be a useful technique in assessment of its
potential for plant growth. Such analyses would also Identify location and
amounts of phytotoxlc and pollutant materials that should be avoided 1n the
surface plant growth zone.
The objectives of this Investigation were: (1) to determine physical
and chemical properties of undisturbed mineland overburden that predict the
suitability of various strata for plant growth; (2) to evaluate by bloassay
the potential of overburden materials as plant growth media with and without
amendments; and (3) to develop criteria based on these tests that can be used
prior to mining to determine which materials would be acceptable for place-
ment on the surface. Analyses were made on selected overburden materials
extracted from active coal mine Mghwalls in glaciated and unglaciated areas
of southwestern Indiana. Plant growth potential of overburden materials was
evaluated for selected crop and tree species in greenhouse pot studies and
large outdoor containers. Fertilizer and sewage sludge overburden amendments
were Incorporated in the greenhouse plant growth studies.
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CONCLUSIONS
The general ranking of overburden materials for plant growth potential
was lacustrine sediment > A horizons > B horizons = glacial tills = loess >
brown shale > sandstone > gray shale > black fissile shales. This ranking is
based on evaluation of physical and chemical properties, seed germination and
emergence, plant growth and yield, and uptake of nutrients and toxic elements.
Lacustrine sediment and A horizons were clearly superior materials for
use as surface plant growth media. These materials exhibited favorable physi-
cal and chemical properties and consistently produced the best growth of
alfalfa, cereal grains and tree seedlings in greenhouse or outdoor container
experiments. Also, they contain an adequate supply of most plant nutrients,
except phosphorus.
The B horizons, partially weathered loess and glacial till materials were
essentially similar in plant productivity and are suitable alone or in mixtures
for use in the plant root zone. B horizons and loess possess physical char-
acteristics such as density, texture and water-holding capacity within the de-
sired range and do not exhibit toxic chemical properties. With organic amend-
ments such as sewage sludge and fertilization, these materials may be a suit-
able alternative for use on the surface of reconstructed mineland soil, but
are not likely to equal A horizon material in productivity. Further, the
thickness of B horizon and loess as well as lacustrine sediments 1n this re-
gion make them an attractive substitute for the existing thinner surface
layers. Due to coarser textures, lower available water and weak structure,
the glacial tills are better suited for placement in the lower rooting zone.
Since the tills are alkaline, they may be beneficial in mixture with other
more acidic materials such as acid B horizon material.
The consolidated brown shale and the sandstone in the crushed condition
are physically unsuited in the upper plant root zone; the major limitations
being poor structure, coarse texture, and low water-holding capacity. Both
materials had an adverse effect on plant emergence when used as a seedbed
medium. The brown shale contains adequate amounts of most plant nutrients
and no apparent toxic elements; therefore, upon further weathering would not
be detrimental to plant growth in mixture with other materials such as glacial
till or loess. This sandstone, however, in addition to having undesirable
physical properties, contains high manganese, sulfur and soluble salts which
reduces its potential for plant growth.
The gray and black fissile shales which sometimes occur 1n close proxim-
ity to the coal strata are totally unsuitable for plant growth. They exhibit
unfavorable physical characteristics and have chemical properties such as low
pH, high potential acidity, and excessive amounts of exchangeable aluminum,
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boron, sulfur and soluble salts that directly or indirectly are toxic to most
plants. This is evidenced by low plant emergence, poor growth, high mortality,
and excessive tissue accumulations of toxic elements in surviving plants grown
on these materials. These toxic shales should be covered quickly and be placed
deep enough to avoid contact with plant roots and to reduce subsequent oxida-
tion and leaching into ground waters.
The addition of sewage sludge resulted in vastly improved growth of wheat
and to a lesser extent alfalfa on all overburden materials except black fissile
and gray shales. Fertilization with N-P-K was less effective than sludge, but
did produce increased plant growth with major beneficial responses occurring
on the unconsolidated overburden materials, It 1s evident that amendment of
overburden materials in the upper plant root zone with major nutrient elements
and organic matter from waste materials such as sludge would be a benefical
practice.
Regression analysis of the results suggested properties that should be
examined in evaluating overburden materials, but did not yield a useful pre-
dictive equation.
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RECOMMENDATIONS
Further research 1s needed to field test the physical and chemical cri-
teria developed in this work. Also, additional research 1s needed to more
fully characterize variability encountered 1n the major overburden strata and
to determine whether important properties are similar throughout the Illinois
coal basin. In the research reported here, all materials tested were used as
the entire root zone. Some of the materials appear to have properties suit-
able for subsoil, but not for surface use, therefore, experiments using A
horizon surface material and various subsoil materials are needed. Such ex-
periments should Include mixing the B horizon with other unconsolidated ma-
terials and the addition of organic residues to the subsoil.
Overburden properties are most easily used in an elimination scheme since
there are several which signal poor growth conditions even when used singly.
On the other hand, no single property assures good growth conditions in any
part of its range. The following properties, in the range shown, indicate a
high probability of poor growth unless the condition 1s corrected.
Sulfur content > 1% total S
Potential acidity > 15 meq/lOOg
Exchangeable Al > .40 meq/lOOg
Extractable Mn > 60 vg/g
pH in 1:1 H20 < 4.5
Extractable B > 1.0 yg/g
Electrical conductivity > 1.0 mmho/cm
Organic matter < 0.5% 1f used as top soil
Available H20 storage < 15% by volume
Bulk density > 1.4 g/cc after packing
These are based on results of experiments in this study plus some back-
ground knowledge and literature reports. All of the materials in this study
with significant S contents developed a low pH and some of the problems
usually associated with it. Potential acidity is another means of detecting
the same problem and requires less elaborate equipment for analysis. Low pH
is usually considered an indicator of poor growth conditions, but this is
primarily because it Increases the availability of toxic metal cations such
as A1+3 and Mn+2. Water soluble B and high electrical conductivity are fre-
quently associated together and with the presence of freshly exposed unweather-
ed materials. Either can be plant Inhibiting, but tend to leach from the media
within a few years 1n humid climates such as the eastern United States. Or-
ganic matter improves cation exchange capacity, but is probably most Impor-
tant 1n providing favorable physical conditions 1n the surface material, e.g.,
reducing crusting, stabilizing structure and Increasing available water
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storage. Texture extremes, 1n this case high clay contents or high sand con-
tents, tends to create poor physical conditions such as low available water
storage and high resistance to root penetration. Bulk density of greater than
1.4 g/cc would be considered acceptable in sandy materials, but sandy materials
have low water storage and low cation exchange capacity. If the properties
of an overburden material are not in the unfavorable ranges listed above, then
there is a high probability of good plant growth and the addition of routine
amendments such as lime and fertilizer will create a good growth medium.
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LITERATURE REVIEW
University scientists have conducted research on surface-mined coal lands
in Indiana periodically over 28 years. Investigations have focused on cast-
overburden properties (Kohnke, 1950; Byrnes and Miller, 1973); spoil bank
classification and revegetation (Stiver, 1949); tree establishment, growth and
development with emphasis on central hardwood species (Arnott, 1950; Tarbox,
1954; DenUyl, 1955, 1956 and 1962), natural revegetation (Byrnes and Miller,
1973), wildlife relationships (Mumford and Bramble, 1973), and sodoeconomic
impacts (Callahan and Callahan, 1971).
Significant research contributions also were made by other agencies and
institutions on surface-mined coal lands in Indiana. Notable among these were
investigations conducted by the U.S. Forest Service throughout the Central
States region beginning In the mid 1940's. Forest Service research, summariz-
ed by Limstrom (1960), covered many aspects of coal-mined land including physi-
cal and chemical properties of resulting spoil, kinds of parent material,
effects of grading, erosion potential, and natural and artificial reforestation,
Personnel of the Indiana University Water Resources Research Center investigat-
ed effects of surface mining on ground water storage and on water quantity and
quality in nearby streams (Corbett, 1965 and 1968; Agnew and Corbett, 1973).
Increased emphasis on coal production, changing mining technology, and
environmental awareness beginning in the 1960's have resulted in a revitali-
zation of interest and research on land disturbed by mining. Published
literature on characteristics and reclamation of surface-mined coal lands in
the Eastern Coal Region is voluminous. Funk (1962) listed 172 references on
this subject covering the period 1918 to 1960. Czapowskyj (1976) prepared
an annotated bibliography on disturbed land that systematically Indexed 591
references by mining area, type of material and subject including geology,
spoil placement and spoil characteristics. The most recent bibliography,
containing more than 1300 references, on surface mining and reclamation in
the Eastern Coal Province was compiled by the Argonne National Laboratory
(Weiss et al., 1977). Citations in this bibliography are organized into 21
categories, including overburdens and minesoils, and stored in a data base
system, BIRS, for subsequent retrieval. Symposia held at the Pennsylvania
State University 1n 1969 (Hutnik and Davis, 1973) and at Wooster, Ohio, in
1976 (Schaller and Sutton, 1978) thoroughly explored the state-of-know!edge
on ecology and reclamation of drastically disturbed lands. Current updates
in the Eastern Region also have been provided by the Research and Applied
Technology Symposiums on Mined-Land Reclamation sponsored by the National
Coal Association in Pittsburgh, Pennsylvania, in 1973 and Louisville, Kentucky,
1n 1974 through 1977 (National Coal Assn., 1973-77).
Information provided by many of these investigations has been useful in
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the formulation of state laws (State of Indiana, 1967) regulating surface
mining and reclamation, and subsequent development of guidelines and standards
(State of Indiana, 1973) for their administration. However, with the enactment
of federal legislation in 1977 (United States of America, 1977), additional and
more specific knowledge is needed on mine overburden properties, placement and
plant growth potential.
Numerous investigations have been conducted in recent years on properties
of "cast overburden" resulting from modern mining methods (Berg and Vogel,
1968 and 1973; Cummins et al. 1965; Czapowskyj, 1973; Massey, 1972; Massey
and Barnhisel, 1972; Plass, 1969; Plass and Capp, 1974; Plass and Vogel , 1973;
VanLear, 1971; Yamamoto, 1975). A current example is the work of Barnhisel
(1977), who investigated spoil (cast overburden) properties and forage yields
on four types of existing surface mine coal spoils, from neutral to very acid,
in western Kentucky. Barnhisel found that phosphorus and water are more
commonly the limiting factors in obtaining an adequate vegetation cover than
the acidic nature of spoils. Further, he indicated that acidic spoils tend
to be much more droughty than adjacent non-acid spoils as the result of a
restricted rooting depth. Armiger et al. (1976) noted that strip-mine spoils
vary greatly in chemical composition and often require markedly different rec-
lamation and revegetation procedures to alleviate toxic conditions. They
stressed the need for chemical analysis of spoil, in association with green-
house plant growth studies, to establish the presence of toxic elements and
to select amendments for effective planning of field revegetation. Such in-
formation on "cast overburden" properties is useful for classifying existing
conditions for plant growth, recommending amendments, and developing guide-
lines, but generally is "after-the-fact" in mining and grading operations.
Although the general literature on minesoils and plant growth is too ex-
pensive and varied for inclusion, several references pertinent to the topic
of overburden properties before mining and their relation to plant growth
potential are appropriate. Limstrom and Mertz (1951) described the strati-
graphy of overburden highwalls in several coal-mining districts in Ohio in
the late 1940's. They extracted samples from each highwall stratum and from
cast-overburden surfaces for laboratory analysis. Analysis was limited to
identification of type and thickness of soil and geologic strata, particle
size distribution, pH, and available phosphorus and potassium. Data were pre-
sented in tabular form with some description of resultant spoil, but with
little interpretation for plant growth. May and Berg (1967) determined acidi-
ty of hlghwall strata of five major coal seams in eastern Kentucky. They
reflected that geological and chemical characteristics of the overburden will
aid greatly in identifying and properly handling acid-bearing materials during
the mining operation. In subsequent investigations, Berg and May (1969)
measured acidity and plant-available phosphorus in overburden strata of six
Kentucky mines. Extremely acid strata were observed in all mines and plant-
available phosphorus generally was very low.
Krause (1973) Indicated that "the key to achieving a predictable growing
medium lies in Identifying which combination of overburden strata 1s best
suited for the survival and growth of vegetation", which 1s the primary ob-
jective of this project. Krause presented Information on hlghwall studies
1n Ohio which Included geology and thickness of strata and analyses for pH,
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total soluble salts, and 14 compounds and elements. He showed by diagrams
how mining operations could be handled to provide improved growing media. A
similar study conducted in eastern Kentucky (Despard, 1974) concerned the
identification of acid strata in the overburden and avoidance of its placement
in the plant growth zone of the cast-overburden. Despard emphasized the im-
portance of overburden analysis before mining is begun and indicated that color,
pyrite content, and pH of exposed overburden could serve as field guides to de-
termine potential toxicity. In a publication on rehabilitation potentials and
limitations of surface-mined land in the northern Great Plains, Packer (1974)
listed analysis of chemical and physical characteristics of surface-mine over-
burden before mining as the first priority in research needs.
Based on extensive overburden and minesoil research in the Appalachian
Coal Region, Grube et al. (1974) indicate that when specific overburden prop-
erties are known in advance of mining it is possible to plan the operation and
subsequent reclamation to take advantage of favorable physical and chemical
properties and avoid possible toxicities. They stress that advance information
should include acid-base accounts, concentrations of plant nutrients, and phys-
ical' stability of all overburden horizons when exposed to the weather. The
acid-base account was further emphasized as a primary property of overburden
materials by Sobek et al. (1976). Acid-toxic overburden is defined by the
measurement and interpretation of paste pH, total or pyritic sulphur, and neu-
tralization potential. Sobek et al. state that the test for acid-toxic ma-
terials is a paste pH reading below 4.0 or an acid-base account that shows a
net deficiency of more than 4.5 MT calcium carbonate equivalent per 907 MT of
material. When the maximum acid calculation is more than 4.5 MT calcium car-
bonate equivalent per 907 MT of material in excess of the neutralization po-
tential the material is considered toxic regardless of its pH.
Schroer (1978) recognized that at present there is little information on
the chemical and physical properties of overburdens from depths greater than
1.5 meters. Therefore, he sampled and analyzed 20 soil series to a depth of
1.5 meters and several hundred underlying overburdens to a depth of currently
mined or mineable coal in the lignite region of North Dakota. Soil horizons
were analyzed by standard soil characterization methods. Schroer observed
that physical and chemical properties varied widely with depth and across the
surface within and between mine areas. These variations were associated with
the stratified nature of the geologic materials that constitute the overburdens.
Schroer concluded that on site sampling will be needed at future mine sites to
assess overburden properties significant to reclamation.
Since the lower strata of mineland materials differ drastically from
overlying soils, special techniques may be required for their analysis. This
1s particularly true 1n the western states where salinity associated with nu-
trient deficiencies is common 1n these materials. Therefore, Sandoval and
Power (1977) developed suggested guidelines for sampling and chemical analysis
of mine spoils and overburden samples to meet the need for uniform laboratory
methods to evaluate plant growth capabilities and limitations associated with
coal lands in western United States. Appropriate uniform procedures also are
needed 1n the Eastern Coal Region for collection, preparation and analysis of
the physical and chemical properties of consolidated overburden strata.
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PROCEDURES
MATERIAL COLLECTION
Eighteen surface mine overburden materials for analysis and growth trials
were selected from five sites 1n southwestern Indiana (Figure 1). Sites were
chosen that spanned the range of major overburden types 1n the eastern edge of
the Illinois Coal Basin; then strata were selected at these sites that appeared
physically adapted to root zone construction, and commonly occurred over coal
seams mined 1n the region. Thus, materials excluded were massive, hard rock
materials such as limestone and layers too thin to be handled separately by
draglines or shovels, except that some surface soil materials (A horizons)
were collected for comparison. The materials collected are representative of
the major strata Important 1n Indiana mlneland reclamation. Twelve are uncon-
solldated materials, Including A and B horizons, loess, lacustrine deposits,
and glacial tills, and six are rock strata that break and weather easily.
Table 1 lists the materials sampled and their location by county, mine,
and rock formation; soils are Identified by series and horizon. Logs repre-
sentative of the hlghwalls at three mine sites are shown in Tables 2, 3, and
4. Several hundred kilograms of such material were collected from recently
exposed highwalls or bench cuts 1n November-December, 1976. Additional
samples of ten strata materials were collected again 1n July and December 1977
at different locations within the same mine to obtain some measure of field
variability.
CHEMICAL AND PHYSICAL ANALYSES
The rock materials, shales and sandstone, were crushed in a "chipmunk jaw"
crusher until all particles were less than 2 cm 1n diameter. Crushed samples
were used 1n the greenhouse and laboratory studies. Uncrushed material, par-
tially broken by digging from the Mghwall and handling, was used 1n the out-
door plant growth studies in large containers. Crushing was necessary for
some of the studies and approximates conditions expected after blasting,
casting, grading, and short term exposure. Each overburden material was air
dried, thoroughly mixed, and subsampled for analysis and growth trials. Ma-
terials used in chemical and physical analyses were crushed to pass a 2 ran
sieve to conform to standard soil analysis procedures.
The chemical character of the material was determined by elemental anal-
ysis for plant-available P, exchangeable K, Ca, Mg, Na, Al, extractable Mn, B,
and total sulfur. Other chemical analyses included pH, buffer pH, potential
acidity, cation exchange capacity, organic matter, and electrical conductiv-
ity. Physical properties analyzed were particle size distribution, moisture
retention and bulk density. The analyses are listed 1n Table 5 along with
-------
EXPLANATION
,-,=, , ^ I CARROLL ,'
m %-s _ I / "- -,
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O WARREN^f I CUNTON [
Strip mine that produced 2$*^ \.
mofซ than 500,000 tons -vi.^^ '->
nH FOUNTAIN^ A> *"-
i 7 i&f:.J> **
I %&*%&&
I > /: 1^
O
Strip mine that produced
less than 500.000 tons
D
Underground mine that produced
more than 500.000 tons
a
Underground mine that produced
less than 500.000 tons
A
Separate preparation plant
or loading dock
' z\
I ~
gf f
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,jip?-\PUTNAMj
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SULLIVAN A
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LOCATION OF MAP AREA \ r'
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GIBSON
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10
30 Miles
Figure 1. Map of southwestern Indiana showing active
coal mines and selected study sites ( A ).
Modified from Hutchison, 1971.
10
-------
TABLE 1. OVERBURDEN MATERIALS SAMPLED.
Overburden
material
Hosmer A-Horizon
Iva A-Horizon
Zanesville A-Horizon
Hosmer B-Horizon
Iva B-Horizon
Zanesville B-Horizon
Unweathered Illinoian Till
Weathered Illinoian Till
Wisconsin Till
Kansan Till
Loess (weathered)
Lacustrine Sediments
Black Fissile Shale 1
Black Fissile Shale 2
Gray Marine Shale
Gray Fluvial Shale
Brown Weathered Shale
Sandstone
Location
Mine
Ayrshire
Chinook
Ayrcoe
Ayrshire
Chinook
Ayrcoe
Chinook
Chinook
Universal
Universal
Ayrshire
Ayrshire
Ayrcoe
Ayrshire
Ayrshire
Minnehaha
Ayrshire
Ayrcoe
County
Warrick
Clay
Pike
Warrick
Clay
Pike
Clay
Clay
Vermill ion
Vermill ion
Warrick
Warrick
Pike
Warrick
Warrick
Sullivan
Warrick
Pike
Rock
Formation
Dugger
Dugger
Dugger
Dugger
Dugger
Dugger
11
-------
TABLE 2. GENERALIZED HIGHWALL LOG FOR AMAX AYRCOE
MINE IN PIKE COUNTY. SOIL TYPE: ZANESVILLE
SILT LOAM.
Type of Material
Average
thickness
Soil Sol urn (A and B horizon)*
Loess
Sandstone*
Gray Shale
Coal V B
Sandstone
Gray Shale
Coal V B
Gray Shale
Aslderite plus Gray Shale
Black Fissile Shale
Alum Cave Limestone
Black Fissile Shale*
Springfield Coal V
meters
1.3
4.0
0.8
6.5
0.2
0.5
5.0
0.2
5.0
0.2
0.1
0.3
1.0
1.3
*0verburden materials sampled.
12
-------
TABLE 3. GENERALIZED HIGHWALL LOG OF AMAX CHINOOK
MINE IN CLAY COUNTY FROM DRILL LOG. SOIL
TYPE: IVA SILT LOAM.
Average
Type of Material thickness
meters
Soil Solum (A and B horizon)* 1.5
Weathered Ill1no1an Till* 1.5
Unweathered HUnolan T111*t 10.5
Gray Shale 0.3
S1lty Sandstone 0.6
Gray Shale 2.4
Mixed S1lty Sandstone and Shale 4.8
Dark Gray Shale 1.0
Coal III 1.5
Underclay 0.5
Black Fissile Shale 1.5
Coal III 0.5
^Overburden material sampled.
fWeathered till was differentiated from unweathered
due to Its brown color and absence of calcium
carbonates.
13
-------
TABLE 4. GENERALIZED HIGHWALL LOG FOR AMAX AYRSHIRE
MINE IN WARRICK COUNTY. SOIL TYPE: HOSMER
SILT LOAM.
Type of Material
Average
thickness
Soil Solum (A and B horizon)*
Loess*
Brown Shale*
Gray Shale*
Black Fissile Shale*
Upper Millersburg Coal
Layered Dark Gray Limestone
and Dark Gray Shale Parting
Lower Millersburg Coal
meters
1.5
6.0
4.5
9.0
0.8
1.0
1.0
1.0
*0verburden materials sampled.
14
-------
the extractant used for elements and reference to the procedure. A brief sum-
mary of procedures used 1s given 1n Appendix A.
PLANT GROWTH STUDIES
Two greenhouse projects and one large outdoor container project evaluated
the growth of plants with and without amendments on these overburden materials.
Greenhouse project one, conducted 1n the spring of 1977, was a randomized
Incomplete block design with 10 overburden materials, 3 plant species, 2 ferti-
lizer treatments and 2 replications. Overburden materials were Iva A and B
horizon, weathered and unweathered IlUnolan till, Wisconsin till, loess, black
fissile shale No. 1, gray marine shale, brown shale and sandstone. Plant spe-
cies included alfalfa (Medlcagp satlva), wheat (Trlticum vulgare). and eastern
white pine (Pinus strobus). me" fertilizer treatments consisted of a control
and 10-10-10 applied at a rate equivalent to 74 kg/ha each of N, PaOs, and
KzO mixed throughout the overburden sample. Approximately 5.5 kg of each
material were placed 1n black, four liter clay pots. Twenty alfalfa or wheat
seeds were planted or four eastern white pine seedlings about 5 cm tall were
transplanted in each pot. After 12 weeks the plants were harvested, dried at
65 C, and weighed.
Greenhouse project two was conducted in 1978 to further evaluate the 10
overburden materials used in the first study plus 5 additional materials,
Hosmer and Zanesville A and B horizons and lacustrine sediment. The experiment
consisted of three randomized complete blocks, each containing a factorial
treatment design of the 15 materials; two species, wheat and alfalfa and three
amendment treatments, sewage, fertilizer plus lime, and control. The sewage
sludge treatment was 5.5 metric tons per hectare (mt/ha dry wt basis, calculated
assuming 2240 metric tons of soil in the plow layer of one hectare). The
sludge had 2% solids. The fertilizer and lime treatments were tailored to each
material. Lime, if needed, was added to adjust pH to 6.5, and N, P, K was
added according to Purdue Soil Test Laboratory's recommendations for the spe-
cies based on soil test results. One material, the black fissile shale, re-
ceived 22 mt/ha Hrne. More was needed to bring the pH up to 6.5, but 22 mt/ha
was considered to be the maximum practical application based on field experi-
ence. About 2 kg of overburden material with sludge or fertilizer incorporat-
ed was used 1n each 2 liter clay pot. Twenty wheat or alfalfa seeds were
planted per pot. The alfalfa was Inoculated with rhizoblum. The percent and
rate of emergence, periodic height growth, and final dry weight were recorded.
The large outdoor container study was established in the spring of 1978,
and will be continued through 1979. Approximately 100 liters (26 gallons) of
overburden material were placed 1n plastic lined cans fitted with drains for
leachate collection. Thirty containers were arranged 1n three randomized
blocks, each containing ten materials. The materials used were the A and B
horizon of the Iva soil, black fissile shale No. 1, sandstone, gray marine
shale, brown shale, weathered Illinolan till, unweathered IlUnoian till,
Wisconsin till and loess. Each container was initially planted to oats
(Avena satlva) at a rate of 5 g per container 1n the early spring. After
15
-------
TABLE 5. PROCEDURES USED IN CHEMICAL AND PHYSICAL CHARACTERIZATION OF THE
OVERBURDEN.
Characteristics
Procedure
Reference
Elemental:
available P
exchangeable K
exchangeable Ca
exchangeable Mg
exchangeable Na
exchangeable Al
extractable Mn
extractable B
extractable Mo
total S
Bray PI extraction
1 N NH^Ac extraction
1 N NH^Ac extraction
1 N NHi^Ac extraction
1 N NH^Ac extraction
1 N KC1 extraction
0.1 N H3POH extraction
Hot water extraction
pH 3.3 NHitC2Oit extraction
LECO induction furnace
(Knudsen, 1975)
(Carson, 1975)
(Walsh, 1971)
(Walsh, 1971)
(Walsh, 1971)
(Black, 1965)
(Whitney, 1975)
(Whitney, 1975)
(Black, 1965)
(Walsh, 1971)
Other chemical:
PH
buffer pH
cation exchange
capacity
organic matter
soluble salts
potential acidity
Physical:
particle size
moisture retention
bulk density
1:1 soil to water
SMP buffer pH
sum of extractable acidity
and exchangeable K, Ca,
Mg, Na
Walkley-Black wet oxidation
electrical conductivity
H202oxidation and
titration with NaOH
pipette method
pressure membrane
and pressure plate
repacked samples
16
(McLean, 1975)
(McLean, 1975)
(Black, 1965)
(Black, 1965)
(Black, 1965)
(Smith et al., 1973)
(Black, 1965)
(Black, 1965)
(Black, 1965)
-------
four weeks, the oats were harvested, dried, and weighed. The containers then
were divided into split plots for planting of two one-year seedlings each of
Virginia pine (P1nus vlrginiana) and yellow-poplar (Uriodendron tulipifera).
Tree height and root collar diameter were measured Immediately after planting
and at the end of the first growing season, Leachate from the large contain-
ers was collected periodically and analyzed for pH, soluble salts, Ca, P, and
K to determine the extent of nutrient loss in early stages of weathering.
STATISTICAL PROCEDURES
Data on plant growth were examined by analysis of variance. Significant
treatment combinations were ordered and differences between observed levels
(means) were compared with a Newman-Kuels test or Duncan's Multiple Range test.
The relationships among physical and chemical characteristics were examined
through correlation analysis. Physical and chemical properties of overburden
materials were then added in a stepwlse multiple regression program to select
1) the property most highly correlated with plant growth, and 2) those proper-
ties significantly related to plant growth in multiple correlations.
17
-------
RESULTS AND DISCUSSION
PHYSICAL AND CHEMICAL OVERBURDEN PROPERTIES
Physical and chemical properties of selected overburden materials were anal
yzed to determine their relationship to plant growth characteristics. These
properties were determined for disturbed overburden samples and are representa-
tive of materials used in greenhouse pot culture and outdoor container studies.
The data do not represent properties of various overburden materials in the na-
ural undisturbed state. It is probable, however, that they closely reflect the
ultimate cast overburden in which various strata, both consolidated and uncon-
solidated, have been subjected to disturbance by blasting, excavation, mixing,
replacement, grading and short-term weathering.
Use of disturbed materials is appropriate and generally consistent with
standard soil test procedures for determination of chemical properties and
particle size distribution, except for artificial crushing of rock strata.
Physical properties such as bulk density and moisture retention, especially at
1/3 bar tension, are normally determined on undisturbed samples indicative of
field conditions. In this study, however, bulk density and moisture retention
measurements are based on disturbed and repacked materials and therefore de-
viate from anticipated field values for the soil solum and other unconsolidated
material, but 1s the only feasible approach for rock strata. Although some of
these procedures deviate from standard soil analysis methods, they attempt to
approximate the restructured conditions typical of reclaimed mlneland.
Physical Properties
Bulk density, particle size distribution and moisture content at 1/3 bar
and 15 bar tensions were determined on three replicates each of 18 overburden
materials (Table 6). In respect to soil-plant growth factors, these properties
are Important in water relations, aeration, 1on exchange and nutrient element
availability. Available water-holding capacity was calculated as the differ-
ence in water retention at 1/3 bar tension and 15 bar tension. The textural
class for each material is based on the proportion of sand, silt and clay size
particles. Three soil series, Hosmer, Iva and Zanesville, which are repre-
sentative of upland soils In the mining region were Included for analysis of
A and B horizon soil material.
Based on the range of values for the physical properties measured, the
18 overburden materials separated into essentially three groups (Table 6).
These are:
1. A and B horizon soil, loess and lacustrine sediment. These are pre-
dominately silt loams containing 84 to 99% silt plus clay size
18
-------
TABLE 6. PHYSICAL PROPERTIES OF SELECTED OVERBURDEN MATERIALS.
Overburden
material
A Horizon
Hosmer
Iva
Zanesville
B Horizon
Hosmer
Iva
Zanesville
Loess
Lacustrine
Glacial Till
Wisconsin
Unw. Illinoian
Wx. Illinoian
Kansan
Black Fissile Shale
#1
#2
Gray Shale
Marine
Fluvial
Brown Shale
Sandstone
Bulk
density
g/cc
1.09
1.21
0.98
1.12
1.09
1.13
1.18
1.12
1.52
1.51
1.26
1.60
1.41
1.31
1.56
1.34
1.49
1.46
Moisture retention
1/3 bar
V
24.5
25.8
27.1
31.1
29.7
32.5
30.2
46.0
19.0
18.3
25.4
18.2
20.4
19.4
26.6
18.2
25.5
17.1
15 bar
by vol .
7.6
6.8
6.5
11.3
13.5
9.9
10.0
20.8
8.0
7.1
12.0
8.3
11.1
14.3
13.1
12.4
13.1
4.7
Avail.
16.9
19.0
20.6
19.8
16.2
22.6
20.2
25.2
11.0
11.2
13.4
9.9
9.3
5.1
13.5
5.8
12.4
12.4
Particle size
Sand
4.3
16.2
4.7
1.6
9.5
2.3
10.9
1.0
48.2
53.9
30.0
51.3
65.1
68.5
8.4
17.3
22.7
68.4
Silt
% _,
81.3
72.7
87.2
74.1
61.1
74.1
70.8
74.1
37.0
31.8
49.1
33.4
31.5
28.1
70.6
67.3
58.9
27.8
Clay
14.4
11.1
8.1
24.3
29.4
23.6
18.3
24.9
14.8
14.3
20.9
15.3
3.4
3.4
21.0
15.4
18.4
3.8
Text.
class
sil
sil
si
sil
sicl
sil
sil
sil
1
gsl
l
1
gsl
gsl
gsil
gsil
gsil
gsl
19
-------
particles. The bulk density was low, ranging froni 0.98 to 1.21 g/cc,
for all materials. These materials also exhibited the greatest mois-
ture retention with available water capacity in the range of 16 to
25% by volume. The lacustrine sediment with 99% silt plus clay con-
tent and nearly 2.0% organic matter had the highest, 25%, available
water.
2. Wisconsin, unweathered and weathered Illlnoian and Kansan glacial tills,
The tills are mostly loam textures with silt plus clay contents of 46
to 52% and moderate bulk densities of 1.26 to 1.60 g/cc. The bulk den-
sities are considerably lower than the tills normally exhibit in their
undisturbed state. Available water-holding capacity ranged from 10 to
13% which averages slightly more than one-half the water-holding capa-
city of the soil solum, loess and lacustrine materials.
3. Black fissile shale, gray shale, brown shale and sandstone rock materi-
als that were ground to particle sizes less than 2 cm diameter. The
resultant texture of these materials, likely due to inherent rock
characteristics, varied from silt loam with 77 to 92% silt plus clay
content for the gray and brown shales to sandy loam with 32 to 35%
silt plus clay for the black fissile shale and sandstone. All ground
rock materials contained more than 15% coarse fragments greater than
2 mm; thus, the textural classes were designated gravelly. Bulk den-
sities for the fractionated rock materials ranged from 1.31 to 1.56
g/cc and available water capacity from 5 to 13% by volume. The lowest
water retention, 5 to 9% available, occurred in the black fissile
shale and gray fluvial shale materials. The high gravel and/or sand
content of these materials likely influenced water retention capacity.
Available moisture in the rooting medium is considered a major environ-
mental factor in mineland revegetation. The quantity of available water is
directly influenced by soil texture with silt loams, loams and clay loams
generally exhibiting the greatest water-holding capacity (Brady, 1974). From
this standpoint, it is evident that the soil solum, loess, lacustrine sediment
and glacial tills analyzed in this study offer the best potential for plant-
available water. The higher gravel and sand content of most rock materials
reduce water retention capacity and tend to be more droughty. The occurrence
of high soluble salts, such as levels present in the fissile shales, also may
influence available water.
Under field conditions, the depth of soil material of a given textural
class as well as layering of materials of different textures will affect water
distribution and availability to plants. Also, materials with higher organic
matter content will indirectly influence water retention through improvements
in soil structure. Therefore, in the reconstruction of mine!and soils, it is
important to consider texture and other physical properties of soil materials
regarding their final placement and depth in the cast overburden.
Chemical Properties
Elemental content of the eighteen overburden materials is presented in
Table 7. Available phosphorus, extractable with weak acid, is generally very
low in all materials with the exception of the two black shales. The
20
-------
TABLE 7. MEAN ELEMENTAL CONTENT OF SELECTED OVERBURDEN MATERIALS.
Overburden
material
Available
P
K
kg/ha
A Horizon
Hosmer
Iva
Zanesville
B Horizon
Hosmer
Iva
Zanesville
Loess
Lacustrine
Glacial Till
Wisconsin
Unw. niinoian
Wx. Illinoian
Kansan
Black Fissile Shale #1
#2
Gray Shale
Marine
Fluvial
Brown Shale
Sandstone
6
18
6
2
6
6
12
3
2
3
14
1
61
134
6
5
3
8
76
107
132
85
222
60
98
143
74
106
113
69
146
13
435
206
224
90
Ca
3.7
8.0
2.4
2.7
9.4
3.4
4.6
18.3
16.4
15.3
7.3
18.1
30.3
13.3
10.7
4.9
7.4
9.7
Exchangeable
Mg
1.2
1.2
1.0
2.7
6.6
3.5
4.4
4.7
1.9
2.0
5.3
2.4
7.8
7.7
5.2
3.4
7.8
5.0
Na
0.03
0.02
0.01
0.09
0.14
0.08
0.36
0.15
0.03
0.08
0.17
0.00
0.19
0.02
2.21
0.16
0.91
0.22
Al
.01
.00
.06
.26
.04
.15
.02
.01
.00
.01
.01
.00
.64
.43
.02
.02
.01
.00
Extractable
Mn
11
17
35
6
28
10
18
19
9
21
51
11
67
72
44
4
28
62
B
yg/g
0.25
0.30
0.25
0.25
0.35
0.25
0.25
0.40
0.25
0.30
0.25
1.00
1.30
2.95
3.05
2.50
0.40
0.45
Total
S
%
0.09
0.12
0.11
0.16
0.10
0.16
0.11
0.14
0.27
0.11
3.27
3.63
0.65
0.56
0.13
0.62
-------
relatively high organic matter content in the black shales (Table 8) probably
accounts for their P reserves. Abailable potassium was also in short supply
in most materials. The Iva B horizon and the lacustrine material K levels
are considered "medium" to "high" by Indiana soil test standards. The gray
shales were high in K and one of the black shales had a "medium" test level.
Exchangeable calcium and magnesium levels in all of the materials appear
to be adequate. Where Mg is high and equals or exceeds calcium, in the brown
shale, for example, there is a tendency toward poor structural stability.
Sodium levels are not high enough to be of concern in any of the materials.
The highest levels are in the marine shale where exchangeable Na occupies
about 4% of the exchange capacity.
Exchangeable Al is very high in the two black shales which are also very
acidic. Aluminum toxicity is certainly likely to occur on those materials and
may be a problem in the Hosmer B where there is a pH of 4.7 and a significant
quantity of exchangeable Al, 0.26 meq/lOOg. The AT levels are generally lower
than those of West Virginia spoils reported by Plass and Vogel (1973).
Manganese is adequate in all of the materials. Manganese toxicity most
commonly occurs in soils containing high levels of Mn that are also acidic
and poorly drained such that reduction of Mn occurs. The levels in the black
shales and sandstone might be a problem for sensitive crops grown under poorly
aerated conditions.
Hot-water-extractable boron levels are high enough for most plants in all
eighteen materials. The levels near 3 ppm in the gray and black shales are
potentially toxic to sensitive plants (Sauchelli, 1969; Rogers, 1947).
There is probably adequate S for normal plant growth in all of these ma-
terials. However, the levels in the black and gray shales and sandstone ac-
count for their high potential acidity (Table 8).
The acid-base status of these overburden materials is reflected in the pH,
buffer pH, potential acidity, cation exchange capacity (CEC) and percentage
base saturation reported in Table 8. The lacustrine material, the brown shale,
and the glacial tills, with the exception of the weathered Illinoian till,
contain significant amounts of carbonates, are alkaline, and near 100% base
saturation. The A and B horizons and the loess are acid, but within a toler-
able range for many plants and could be brought to levels suitable for most
crops with reasonable lime additions. The black and gray shales and sandstone,
however, contain significant amounts of S and high potential acidity (Table 8)
which would require very high amounts of lime to correct. In spoil bank
classification for tree growth, Limstrom (1960) rated materials with pH below
4.0 as marginal to toxic.
The electrical conductivity (E.G.) of the soil solution is high enough to
be detrimental to plant growth only in the black and gray shales and sandstone.
Sensitive plants are retarded by water exceeding 1 mmho/cm in conductivity
(Nieman and Shannon, 1976). Cummins ert al_ (1965) reported that mineland spoils
22
-------
TABLE 8. MEAN CHEMICAL PROPERTIES OF SELECTED OVERBURDEN MATERIALS.
N>
Overburden
material
A Horizon
Hosmer
Iva
Zanesville
B Horizon
Hosmer
Iva
Zanesville
Loess
Lacustrine
Glacial Till
Wisconsin
Unw. Illinoian
Wx. Illinoian
Kansan
Black Fissile Shale
#1
#2
Gray Shale
Marine
Fluvial
Brown Shale
Sandstone
PH
5.3
6.9
4.9
4.7
5.5
5.0
5.8
8.0
8.2
7.9
6.8
7.7
3.7
2.7
6.6
5.4
7.3
5.5
Buffer
pH
6.8
N/A*
6.5
6.2
6.8
6.4
6.8
N/A
N/A
N/A
N/A
N/A
4.6
3.2
N/A
6.7
N/A
7.2
Potent.
acidity
meq/lOOg
N/Af
N/A
N/A
N/A
N/A
N/A
N/A
N/A
N/A
N/A
N/A
N/A
130.5
465.2
16.5
69.1
N/A
18.0
CEC
meq/lOOg
11.5
12.0
12.6
16.9
23.7
17.0
14.8
23.3
18.3
17.7
16.3
20.6
67.4
62.4
22.1
12.7
18.2
16.6
Base
Sat.
%
44.9
77.9
29.4
33.1
69.5
42.0
65.6
100.0
100.0
99.0
79.6
100.0
69.1
33.6
83.3
68.1
90.0
91.0
E.G.
mmhos/cm
0.10
0.19
0.16
0.09
0.20
0.08
0.07
0.40
0.17
0.81
0.18
0.80
5.47
8.40
2.12
1.40
0.21
2.09
Organic
matter
%
1.22
1.11
2.28
0.54
0.40
0.25
0.24
1.96
0.36
0.59
0.26
0.51
4.17
7.35
2.18
8.62
.41
1.22
CaC03
Equiv.
%
N/A
N/A
N/A
N/A
N/A
N/A
N/A
15.3
24.5
25.3
.1
15.2
N/A
N/A
N/A
N/A
3.6
N/A
*Not applicable, determined only on samples of pH 6.5 or less.
fNot applicable, determined only on samples with S > 0.5%.
-------
with electrical conductivity of 2 mmhos/cm was marginal and 3 mmhos/cm was
toxic for plant growth.
In summary, the chemical properties of the overburden materials suggest
several problems likely to occur in* using the materials for plant growth
media. Acid formation from the S in the black and gray shales and the sand-
stones is likely to cause many problems in addition to their high conductivity
and B contents. The low P and K levels in many of the materials could be over-
come with fertilizer and lime could be used to raise the pH and reduce ex-
changeable Al on the more acid unconsolidated materials. Toxicity from B or
Mn appears likely only on the same materials that have significant S content
and associated acidity.
The coefficients of variation for the chemical properties presented in
Table 9 indicate the difficulty in characterizing overburden materials with
limited sampling. In general, the rock materials exhibited the greatest vari-
ability in chemical properties. Some of this is probably a result of segrega-
tion that occurs in crushing and screening in addition to the natural varia-
tion in the field. The relatively great variation in important properties
such as available P and K, electrical conductivity, and organic matter con-
tent explain inconsistent and unusual results frequently encountered in both
field and greenhouse growth experiments.
Correlation of Overburden Properties
The results of a simple correlation analysis of twelve physical and chemi-
cal properties are presented in Table 10. The variability of properties with-
in any one material (Table 9) precludes the possibility of finding very high
correlations. However, some correlations that are common in soil materials
did appear, e.g., the positive correlation (.68) between pH and percentage
base saturation (B.S.), and the relationship of organic matter (O.M.) and
sulfur (S). The shales tended to be high in organic matter, sulfur, manganese
(Mn), and electrical conductivity (E.G.), and quite different from most of the
other materials in these properties. Thus, those three properties appear
correlated, but if the unconsolidated materials were examined separately, there
would be little relationship among them. Bulk density (B.D.) is negatively
correlated with percent silt, and this is expected in these repacked samples
where high bulk density is associated with higher percentage coarse material.
The negative relationship between electrical conductivity and percent silt is
primarily due to the two black shales which contained high soluble salts and
were low in percent silt in this analysis. The relationship is certainly not
expected to be a valid generality for overburden materials. The strong posi-
tive correlation between boron (B) and potassium (K) is interesting and may
be useful in initial screening for potential boron problems based on potassium
tests which are done much more routinely.
PLANT GROWTH STUDIES-GREENHOUSE
Wheat and Alfalfa Yields
The first greenhouse experiment utilized three plant species grown on ten
24
-------
ro
TABLE 9. RELATIVE VARIATION, C.V. (%), IN CHEMICAL PROPERTIES WITHIN STRATA BASED ON ANALYSIS OF
SELECTED OVERBURDEN MATERIALS COLLECTED AT THREE SAMPLING POINTS AT THREE TIMES.
Overburden
material
A Horizon-Iva
B Horizon-Iva
Loess
Wisconsin Till
Unw. Illinoian Till
Wx. Illinoian Till
Black Fissile Shale #1
Gray Marine Shale
Brown Shale
Sandstone
P.
37
33
77
25
33
29
129
17
69
64
K
28
9
27
44
23
17
127
36
36
75
Ca
18
19
29
4
21
6
27
78
14
7
Mg
17
6
37
5
15
4
33
44
16
20
Na
Mn
Coefficient of
25 127
34
106
22
45
13
132
141
106
131
34
37
46
30
35
50
45
76
23
B
pH
Variation (
20 5
55
0
0
10
0
28
39
28
6
5
11
1
2
1
46
15
5
5
CEC
'ฃ}
i*>l
12
6
16
4
19
6
69
52
25
12
Base
Sat.
5
4
15
0
2
3
37
6
5
9
E.C. O.M.
54 11
59 18
61 15
27 33
19 22
31 13
72 26
80 50
61 34
71 77
-------
TABLE 10. MATRIX OF CORRELATION COEFFICIENTS(r) FOR MEASURED PROPERTIES OF
SELECTED OVERBURDEN MATERIALS.
Proper-
ties
S
B
Mn
Al
Silt
PH
P
K
BD
EC
OM
BS
BS
.21
.28
.28
-.49
-.73
.68
-.08
.33
.77
.38
.12
1.00
OM
.76
.29
.72
-.27
-.36
-.37
.03
.01
.31
.75
1.00
EC
.78
.36
.82
-.24
-.78
-.31
.05
.01
.72
1.00
BD
.45
.48
.50
-.44
-.94
.24
-.22
.29
1.00
K
-.03
.78
.15
.09
-.15
.05
-.10
1.00
P pH S1H Al Mn B S
.05 -.41 -.59 -.07 .81 .18 1.00
.12 -.18 -.32 -.18 .31 1.00
.35 -.34 -.59 -.23 1.00
-.20 -.45 .29 1.00
.25 -.18 1.00
-.19 1.00
1.00
26
-------
overburden materials, both fertilized and unfertilized (control). It was a
preliminary experiment, only partially replicated, designed to refine the
technique, determine which species were adequate for testing and furnish pre-
liminary results. The dry weight of plant material produced is presented in
Table 11 with the exception of the white pine. In the limited duration (12
weeks) of the experiment, white pine seedlings growth was quite small, .06 to
.55 g dry weight per pot, and produced no statistically significant differences
among materials or treatments. Wheat and alfalfa yields in unfertilized ma-
terials indicate that Iva A horizon was the best growth medium; for wheat alone
Iva A was significantly better than the black fissile shale and for alfalfa
better than all materials except Iva B horizon, Wisconsin till, weathered
Illinoian till and brown shale. Differences among materials became much more
pronounced when they were fertilized. The fertilizer response was significant,
as expected, for most materials. The lack of response in the black and gray
shales was probably due to the presence of limiting factors such as low pH,
high B, and high soluble salt content (Tables 7 and 8). Plants in greenhouse
pot studies were watered by overhead sprinkling on a schedule designed to pre-
vent wilting. However, the water storage capacity of various materials could
become important between waterings.
The second greenhouse experiment conducted for eight weeks included 15
materials, 2 species, 3 treatments, and 3 replications (Table 12). The ferti-
lizer and sludge treatments included lime where it was needed. Across all
treatments and species, the lacustrine material produced the highest yields
with the exception of the control and sludge treatments on alfalfa, and the
black fissile shale produced the least. The A horizon materials all produced
high yields, similar to each other, and not statistically different from the
lacustrine material for alfalfa. The materials tend to form three groups if
one considers the mean of treatments and species. The A horizon and lacus-
trine materials produce the best growth and usually are the same statistically.
The B horizons, loess, glacial tills, brown shale, and sandstone tend to form
a second group which are not significantly different from each other. Finally,
the gray shale and black shale are clearly inferior growth media.
As in the firest greenhouse experiment, the addition of fertilizer usually
improved the growth of wheat with significant responses occurring on B horizon,
lacustrine, weathered Illinoian till and gray shale materials. Alfalfa yield
increased with fertilization on 11 of the 15 materials, but overall, yield
differences in comparison with the controls were not significant. In contrast,
the sludge treatment produced wheat yields significantly greater than the con-
trols on all materials except the black and gray shales. Growth responses to
sewage sludge added may be due primarily to NH$-N estimated at 200 kg/ha and P
at 165 kg/ha for the sludge rate applied. Alfalfa yields also were generally
higher on materials with sludge treatment than on the control, but differences
in mean yield were not significant except for alfalfa grown on loess.
It appears that the only overburden tested that is equal to A horizon ma-
terials 1s the lacustrine material. This is not surprising when the physical
and chemical properties are compared. The lacustrine material had a high pH,
high exchangeable Ca and Mg, high available water-holding capacity and the
27
-------
TABLE 11. EFFECT OF OVERBURDEN MATERIAL AND TREATMENT ON YIELD
OF WHEAT AND ALFALFA IN THE FIRST GREENHOUSE STUDY.
Overburden
material
A- horizon, Iva
B-hor1zon, Iva
Loess
Wise. Till
Unw. 111. Till
Wx. 111. Till
Blk. Fis. Shale
Gray Mar. Shale
Brown Shale
Sandstone
Wheat
Control
2.10a*
0.94ab
0.72ab
l.Olab
2.26a
l.OSab
0.06b
1.35ab
0.70ab
0.67ab
Fert.
3.87ab
4.02ab
3.27b
2.85b
5.25a
3.14b
0.78d
1.24cd
2.30bc
2.31bc
Alfalfa
Control
2.33a
1.19ab
0.33b
0.84ab
0.22b
0.89ab
O.OOb
O.OBb
0.77ab
O.Olb
Fert.
4.48a
4.30a
2.88abc
2.15bc
3.33ab
3.49ab
O.lOd
0.02d
3.34ab
1.47c
*With1n columns, values among materials followed by same letter
are not significantly different at the B% level. Within rows,
values between treatments differing by more than 1.07 g for
either species are significantly different.
28
-------
TABLE 12. EFFECT OF OVERBURDEN MATERIAL AND AMENDMENTS ON GROWTH OF WHEAT
AND ALFALFA IN THE SECOND GREENHOUSE EXPERIMENT. EACH VALUE IS
A MEAN OF THREE REPLICATES.
Overburden
material
A Horizon
Hosmer
Iva
Zanesvllle
B Horizon
Hosmer
Iva
Zanesville
Loess
Lacustrine
Glacial Till
Wisconsin
Unw. 111.
Wx. 111.
Blk. Fis. Shale
Gray Mar. Shale
Brown Shale
Sandstone
Control
l.SObc*
2.92ab
2.79ab
l.lObc
1.34bc
0.82c
1.14bc
3.66a
0.83c
1.25bc
0.93c
O.OOc
0.48c
1.73bc
O.SOc
Wheat
Sludge
4.82abc
4.56abc
4.10bcd
3.70bcd
3.45cd
2.58d
5.30ab
6.05a
3.71bcd
2.49d
4.03bcd
O.OOe
1.07e
4.74abc
2.52d
Fert.
per
2.32bcd
1.87bcd
3.62b
2.71bcd
3.33bc
2.14bcd
1.73cd
5.57a
1.07d
2.27bcd
2.48bcd
0.15e
l.SObcd
1.76cd
1.63cd
Control
1.36a
1.58a
1.30a
0.30a
0.89a
0.43a
O.SOa
0.96a
0.02a
0.57a
0.88a
O.OOa
O.OSa
0.35a
0.19a
Alfalfa
Sludge
1.34ab
2.23a
1.25ab
0.76ab
1.26ab
0.70ab
1.85a
1.18ab
0.78ab
0.18b
1.09ab
O.OOb
O.OSb
0.52ab
0.28b
Fert.
1.39ab
1.67ab
1.15ab
1.22ab
0.68ab
1.34ab
0.93ab
1.95a
0.43ab
0.19ab
0.94ab
O.OOb
1.02ab
0.89ab
1.42ab
*Within columns, values among materials followed by the same letter are not
significantly different at the 5% level. Within rows, values between treat-
ments differing by more than 1.26 g for either species are significantly
different.
29
-------
available K and percent organic matter are similar to A horizons (Tables 6, 7,
8). It would appear that the underlying unconsol.idated materials, the tills
and loess, and the somewhat weathered brown shale are almost as productive as
the B horizons. These materials generally are not statistically different in
plant yield from the B horizons, and in several instances, produced higher
yields; for example, wheat yields on sludge-treated brown shale and weathered
Illinoian till and untreated brown shale. It is also apparent that gray and
black shale are not likely to be productive even when amended with sludge and
fertilizer.
Table 13 summarizes the analysis of variance in the greenhouse experiments.
All of the main effects and two-way interactions were significant for plant
yield which is apparent in Tables 11 and 12. The addition of amendments ac-
cenuated the material differences, and they were more apparent with wheat than
alfalfa due to wheat's more rapid growth and its more consistent emergence.
The relationship among materials and the effects of treatments is easily
seen for wheat yields in Figure 2. The three A horizons and three B horizons
are represented by a single mean value to simplify comparisons. The addition
of sludge vastly improved the growth on all materials except gray and black
shale and was generally more effective than inorganic fertilizers. The sludge
probably improved some of the physical properties as well as supplying nutri-
ents. It appears that the addition of sludge to overburden material used in
the rooting zone might be an attractive technique for field trials. The fairly
uniform response of wheat on unamended glacial tills, loess, and B horizons
became much more variable as well as improved when sludge was added.
The poor performance of the shales and sandstone was related, in part, to
the slow and incomplete plant emergence reflected in Tables 14 and 15. Their
adverse chemical and physical properties undoubtedly retarded emergence and
growth. However, treatments with fertilizer or sludge did not consistently
bring about improvement. Sludge reduced emergence and early growth of wheat
when applied to unweathered Illinoian till and improved emergence on the brown
shale; otherwise, it had little effect (Table 14). The addition of fertilizer
caused only slight improvement in wheat and alfalfa on most materials (Table 14
and 15). In addition, surface crusting of weak structured, unconsolidated
materials such as the glacial tills may have affected seed germination and rate
of plant emergence. This appeared to be the case with alfalfa grown on un-
weathered Illinoian till when fertilizer and sludge were added.
The general ranking of overburden material for plant growth potential in
greenhouse studies is lacustrine sediment s A horizons > B horizons = glacial
tills = loess > brown shale > sandstone > gray shale > black fissile shale.
Amendments ranked sewage sludge > fertilizer > control.
Elemental Content of Wheat Plants
Wheat plants harvested after 8 weeks growth in untreated (control) over-
burden materials and those amended with sewage sludge or N-P-K fertilizer
plus lime were analyzed for elemental content (Table 16). Overburden materi-
als in all treatments were watered as needed to maintain adequate moisture
30
-------
TABLE 13. SUMMARY OF ANALYSIS OF VARIANCE FOR THE GREENHOUSE EXPERIMENTS,
Source of
variation
Study #1
Yield
Yield
Study #2
Emergence
Height
*
Overburden material
Treatment (Tr.)
Species (spp.)
Material X treatment
Material X species
Treatment X species
Material X Tr. X spp.
S
S
S
S
S
S
NS
S S
S
S
S
S
S
S
S
NS
NS
NS
NS
NS
S
S
NS
NS
NS
NS
NS
*Tested at 5% level.
31
-------
CO
ro
6
5
4
^ 3
ฃ
i
-- 2
a
/
0
.
Control
-
-
-
c
0
fM
1-
o
JC
1
ซc
,_
f
p
0 i-1 P
e ฃ T
O O (U '"*
tsl .c L. in
> *J U C
O 01 ** U tn
i C 01 *- O
00 3 3 3 1
OJ
c
i
3
_J
(U
JZ
,
OJ
in
|
CD
^
C
O
o
c
Wheat
Sewage
s/udge
i
c
O
N
O
1
ซt
=
O
fM
O
1
m
_
F
^
!^
ai
a>
i
ZZ
^
|~|
-o
M
ai
_
p
c
t/)
U
v>
3
1
01
t-
3
^
^
t/1
(I)
in
tn
U.
J2
m
.
Fertilized
r*
(O
2
o
11
JC
I/)
1
m
0)
c
o
tn
c
01
.__
c
O
O
-
c
O
N
O
1
CD
^
iE
^f
^
?!
0)
a
c
^1
^
^
T3
L.
(U
,_
J J-
c
1/1
O
3
ป
O
1
11
*-
c/)
(O
-
"
OJ ~~l
JZ
^ ซ)
*n 0)
*/> i ซ a*
t- <0 JC C
U- J= V) O
-** C i/l
> Z -o
ซ- S- 10
m o en c/i
7
6
5
4
o
I
K'
3 S
o
a>
>~
2
O
Overburden Material
Figure 2. Dry weight of wheat produced In second greenhouse experiment as
influenced by overburden material and treatment.
-------
TABLE 14. EMERGENCE AND HEIGHT OF WHEAT PLANTS AFTER FOUR WEEKS GROWTH ON
OVERBURDEN MATERIALS IN THE SECOND GREENHOUSE EXPERIMENT.
Overburden
Treatment
Control
Sludge
Fertl
lizer
material Emergence* Height Emergence Height Emergence Height
A-Horlzon
Hosmer
Iva
Zanesvllle
A-Horizon Mean
B-Horizon
Hosmer
Iva
Zanesville
B-Hor1zon Mean
Loess
Lacustrine
Glacial Till
Wisconsin
Unw. Illinoian
Wx. Illinoian
Glacial Till Mean
Black Fissile Shale #1
Gray Marine Shale
Brown Shale
Sandstone
%
85
75
90
51
70
85
80
75"
80
85
85
80
75
50"
0
40
50
55
cm
18.0
16.0
18.5
T775"
19.5
15.5
19.5
TO"
17.0
20.0
15.0
17.0
16.5
TFT
0
8.0
11.5
14.0
%
85
75
85
52"
85
65
85
75"
90
70
65
20
75
53"
5
35
85
60
cm
20.0
16.5
20.0
1575"
21.5
16.0
20.5
TO"
16.5
22.5
14.0
5.5
15.5
TTT
10.0
6.0
11.5
13.5
%
80
80
85
87
90
85
85
37
90
90
85
90
85
57
25
50
85
50
cm
21.0
20.0
21.0
2077
22.0
16.5
19.5
TO"
17.5
23.0
17.5
19.0
20.5
TO"
12.0
9.0
11.5
12.0
*Emergence percent is ratio of plants emerging/total seeds planted. Twenty
seeds with germination capacity > 95% planted per pot.
33
-------
TABLE 15. EMERGENCE AND HEIGHT OF ALFALFA PLANTS AFTER FOUR WEEKS GROWTH
ON OVERBURDEN MATERIALS IN THE SECOND GREENHOUSE EXPERIMENT.
Treatment
Overburden
material
A-Horizon
Hosmer
Iva
Zanesville
A-Horizon Mean
B-Horizon
Hosmer
Iva
Zanesville
B-Horizon Mean
Loess
Lacustrine
Glacial Till
Wisconsin
Unw. Illinoian
Wx. Illinoian
Control
Emergence*
%
95
70
80
82
75
65
80
73
60
90
45
55
55
Glacial Till Mean 52
Black Fissile Shale
Gray Marine Shale
Brown Shale
Sandstone
#1 30
50
30
30
Height
cm
14.0
10.0
15.5
13.2
15.0
11.0
14.5
IJT
11.5
17.0
8.0
8.5
10.0
"878
7.5
7.5
8.0
9.5
Sludge
Emergence
%
90
80
75
82
75
80
70
75"
85
85
0
40
80
40
0
25
65
55
Height
cm
14.5
13.5
13.0
1377
14.5
15.5
14.0
T4TT
14.0
18.0
0
4.0
13.5
TT
0
5.0
8.0
9.0
Fertil
Emergence
%
95
70
75
80
75
70
65
70
80
55
55
15
70
37
20
45
40
70
izer
Height
cm
16.5
16.0
14.0
15.5
15.5
14.5
15.5
15~T
15.0
18.5
11.5
8.0
13.0
IO"
3.5
7.0
5.5
10.0
*Emergence percent is ratio of plants emerging/total seeds planted. Twenty
seeds with germination capacity > 95% planted per pot.
34
-------
supplies during seed germination and plant growth. Elements selected for
analysis Included P, Ca, Mg, Mn, Fe, Zn, B and Al. These were compared with
interpretive standards for nutrient levels of wheat plants used by the Purdue
Plant and Soil Analysis Laboratory. Due to instrument malfunction, K was not
included in the analysis. For the black fissile shale, there was no yield of
wheat in control and sludge treatments and less than 1/4 g per pot 1n the ferti-
lizer treatment; therefore, no comparison of tissue elements was possible for
this material. Likewise, wheat yield in some replicates of glacial till,
shale and sandstone materials was too small for analysis, therefore, mean
element content is based on incomplete or partial replication.
Phosphorus content of wheat tissue ranged from "low" to "medium", .11 to
.28%, for plants grown on unamended control overburden materials. This is
consistent with the very low and low levels of available P in the overburden
itself for all materials except black fissile shale (Table 7). Amendment with
sewage sludge and fertilizer resulted in minor increases in plant P, but not
above "medium" levels, which are .21 to .50%, on Iva A and B horizon, loess,
lacustrine and gray and brown shales. Phosphorus concentration in wheat plants
grown on the three glacial tills was in the medium range for all treatments.
Plant concentrations of calcium Increased in response to both sludge and ferti-
lizer treatments from "medium" to "high" levels in A and B horizon materials.
Sludge alone resulted in higher Ca in plants grown on the tills, but little
change was noted among treatments for other materials. Magnesium content of
wheat on control treatments was "medium", .33 to .64%, for all materials ex-
cept sandstone which was "high". Wheat magnesium levels remained essentially
the same as the control, "medium" for nearly all materials, with sludge and
fertilizer amendments.
Manganese levels in wheat tissue on overburden materials without amend-
ment were "medium" to "high" for A horizon, Wisconsin and weathered Illinoian
till and brown shale, and, "very high" for B horizon, loess, lacustrine, un-
weathered Illinoian till, gray shale and sandstone. Changes in foliar Mn due
to sludge and fertilizer were erratic; however, there was some trend of in-
creased Mn levels with sludge application for B horizon, loess, Wisconsin till
and gray and brown shales and with fertilization on A horizon, loess and gray
shale. Wheat iron content was "medium", 120 to 274 ppm, on all untreated over-
burden materials. Sludge treatment resulted in "high" levels of Fe for B
horizon, loess and sandstone, but no practical change occurred in other ma-
terials. "Very high" levels of iron and aluminum occurred on two fertilized
materials, B horizon and gray marine shale. In the case of the gray marine
shale, this was probably due to the oxidation of S and resultant drop in pH.
Zinc in wheat tissue on control treatments was "low" (20 ppm) for B horizon,
"high" (103 ppm) for lacustrine and "medium" (26 to 68 ppm) on all other
materials. Zinc content increased from "low" or "medium" to "high" levels in
wheat on sludge-amended A horizon, B horizon, glacial tills and sandstone,
while no major changes occurred for materials amended with fertilizer + lime.
Boron concentration in wheat tissue was "high" for plants grown on un-
amended gray marine shale and increased to "very high" levels with sludge and
fertilizer treatments. This large accumulation in plant tissue is likely re-
lated to high extractable B in the gray marine shale (Table 7). Boron content
was "medium" in wheat for all other materials and treatments.
35
-------
TABLE 16. ELEMENTAL CONTENT OF WHEAT PLANTS GROWN EIGHT WEEKS IN SELECTED
OVERBURDEN MATERIALS WITH AND WITHOUT AMENDMENTS IN POT CULTURE.
Overburden
material
Iva A-Horizon
Iva B-Horizon
Loess
Lacustrine
Wisconsin Till
Unw. 111. Till
Wx. 111. Till
Gray Marine Sh.
Brown Shale
Sandstone
Overburden
material
Iva A-Horizon
Iva B-Horizon
Loess
Lacustrine
Wisconsin Till
Unw. 111. Till
Wx. 111. Till
Gray Marine Sh.
Brown Shale
Sandstone
C*
.20
.11
.15
.14
.22
.22
.28
.13
.18
.21
C
168
151
120
274
212
234
222
165
202
144
P
$*
%
.26
.22
.25
.15
.31
.27
.24
.16
.26
.18
Fe
S
ppm
162
332
361
204
297
205
196
182
197
338
F*
.21
.28
.28
.24
.25
.23
.26
.30
.27
.24
F
238
563
268
229
208
215
165
584
244
258
C
.96
.39
.58
1.03
1.14
.80
.84
.20
.78
.54
C
53
20
43
103
56
68
56
26
62
59
Ca
S
%
1.27
1.01
.89
1.05
1.21
1.13
1.15
.27
.71
.64
Zn
ง
ppm
73
87
69
108
75
114
89
56
61
88
F
1.01
1.25
.88
.82
1.02
.83
.72
.40
.62
.49
F
62
67
53
84
52
52
53
44
40
41
C
.47
.33
.43
.58
.60
.54
.60
.49
.64
1.19
t
12
7
22
15
16
20
16
48
11
21
Mg
S
%
.54
.64
.75
.57
.65
.62
.73
.80
.59
1.39
B
S
PPm
12
14
14
16
12
13
10
99
16
18
F
.54
.60
.75
.49
.49
.55
.54
.83
.54
.86
F
10
22
17
14
13
13
7
75
13
15
C
56
426
544
791
94
422
332
445
142
867
C
200
122
124
288
250
232
258
163
226
174
Mn
S F
ppm
60 221
455 196
655 731
450 614
442 86
319 409
232 182
733 601
351 130
291 322
Al
S F
ppm
166 288
357 622
302 219
221 230
281 202
214 204
285 202
212 624
252 337
454 296
treatments: C = Control, S = Sewage Sludge, F = Fertilizer.
36
-------
The relationship between extractable B in unamended overburden materials
and uptake of B in wheat, oats and alfalfa is shown in Figure 3. These data
are combined means of B content in materials and plants used in greenhouse and
outdoor container experiments. This comparison is of interest since gray shales,
a very abundant material in the coal region, contain plant-available B suf-
ficiently high (> 2 yg/g) to be toxic to sensitive crops (Reisenauer, Walsh
and Hoeft, 1973). In addition, reduced plant growth was observed on gray shale
that in part may be related to toxic accumulations of B. For all species,
plants grown on gray shale contained more B than those grown on any other ma-
terial. Concentrations of B in wheat and oats may have been sufficiently high
to be toxic. Alfalfa, a luxury consumer of B, had higher B accumulations on
all materials with the highest level occurring on gray shale; however, those
levels are not considered toxic for alfalfa (Jones, 1972).
Aluminum content of wheat grown in unamended overburden was "medium" in
A and B horizon, loess, gray shale and sandstone and "high" in lacustrine, the
three glacial tills and brown shale. Plant Al increased to "high" or "very
high" levels following sludge and fertilizer applications on B horizon, loess,
gray shale and sandstone. Aluminum levels of 400+ ppm are considered "very
high" and may exist at toxic levels. Although not included in Table 16, Cu
levels were "medium" in wheat tissue for all overburden materials and treat-
ments.
Based on elements analyzed, it appears that adequate concentrations
are present in wheat plants grown on unamended overburden except for P which
is low, .11 to .20%, in tissue for several materials. Element content of
wheat generally increased with sludge and fertilizer amendments for most ma-
terials, but changes were somewhat erratic and in most materials not drastic.
The "very high" to excessive tissue levels of Fe, Al and B on gray marine
shale; Fe and Al on B horizon; and Al on sandstone may be potentially toxic to
plants. Also, Mn concentrations > 351 ppm accumulating in wheat grown on one
or more treatments of B horizon, less, lacustrine, unweathered Illinoian till,
gray shale and sandstone are considered very high to excessive. Berg and Vogel
(1968) observed Mn toxicity in the form of leaf margin chlorosis on several
legume species grown in acid strip-mine spoils 1n Kentucky. Critical tissue
concentrations were not determined, but Mn toxicity symptoms were most severe
on materials with pH below 5.0
PLANT GROWTH STUDIES-OUTDOOR CONTAINERS
Ten overburden materials (Table 17) were collected from exposed highwalls
at the Ayrcoe, Ayrshire, Chinook and Universal coal mines in October 1977.
Material from the consolidated rock strata was partially fractured in extrac-
tion and placed directly in plastic-lined metal containers without further
crushing. Thirty containers, three replications of each overburden strata,
were arranged in three randomized blocks of 10 materials each at the Purdue
University Martell Forest in Tlppecanoe County, Indiana. Overburden materials
did not receive soil amendments or supplemental Irrigation.
Oats were planted 1n March and harvested in April, 1978, after 4 weeks
37
-------
C*)
00
J.\J
00
Kfl
a 2.0
ซ
Overburden
I
I
[
1
Wheat
.
_
~O"
Kl
*^
O
0
M
TI
0
.c
1
CD
^
H^
^J
"
qj
t/ป
VI
QJ
O
(U
^_
i-
VI
(J
Qj
**O
-C
c/l
2
ts
Overburden
~n
0)
Jc
to
c
I
1
f
1
1
Overburden
1
I1
Oafs
c
o
t->
0
c
eo
c
o
"^
1 _c
o
L.
o
1
-
^
,__!
a
a>
fO
a>
c
JZ
"^
P
0)
i_
"^~
0)
^
c
TT-
c
o
u
Ifl
VI
a>
o
OJ
1 iC '
CO
OJ
VI
u.
_^
u
A.
" "
OJ
*JO
J^
CO
s*
Of
w
-C
LO
c
ง
1
Alfalfa
.c
^o
I
^
1
^
"O
(U
-C
(U
1
f^
.^
VI
o
t/)
vt
a>
o
OJ
^
1-
to
=5
O
a>
*ซ
-c
to
ซ
1
1
a>
.c
t/i
c
1
-------
TABLE 17. MEAN OAT YIELD, 4 WEEKS, AND TREE SURVIVAL AND GROWTH, 12 WEEKS, IN OUTDOOR CON-
TAINERS OF OVERBURDEN MATERIAL. EACH VALUE IS A MEAN OF THREE REPLICATES.
VO
Overburden
material
Iva A-Horizon
Iva B-"Hor1zon
Loess
Unw. Illinoian Till
Wx. Illinoian Till
Wisconsin Till
Black Fissile Shale #1
Gray Marine Shale
Brown Shale
Sandstone
Oat
yield
dry wt.
9
3. 67 a*
2.64b
3.13ab
2.91ab
3.13ab
2.31bc
0.57d
1.56c
3.12ab
2.52b
Virginia Pine
Yellow-Poplar
Growth
Survival
%
100
100
100
100
100
100
33f
50
100
100
Total
height
cm
8.8a
8. lab
8.9a
4.7c
5.8abc
4.0c
0.7d
0.7d
5.3bc
4.9bc
Basal
diameter
cm
0.18a
0.19a
O.lBab
O.llab
0.14ab
0.12ab
O.OOc
0.05bc
0.15ab
0.14ab
Survival
%
100
100
100
100
100
100
0
0
100
100
Growth
Total
height
cm
34. 7a
9.9b
9.1b
4.3b
6.7b
10. 8b
O.Oc
O.Oc
6.1b
12. 5b
Basal
diameter
cm
0.41a
0.19bc
0.12c
O.lZc
O.lZc
0.25b
O.OOd
O.OOd
0.20bc
0.15bc
*Means followed by the same letter are not significantly different at P = 0.05 according to
Duncan's Multiple Range test.
^All tree seedlings were dead by December 1978, 7 months after planting.
-------
of growth. Oat tissue was analyzed for 11 macro and micro nutrient elements.
Two one-year-old seedlings of Virginia pine and yellow-poplar were planted in
each container in April, 1978. Seedling total height and basal diameter were
measured at time-of-planting and in August, 1978, after 12 weeks of growth.
Seedling survival was determined in August and December, 1978. Leachate
samples from the outdoor containers of overburden materials were collected
periodically in 1978 and spring 1979 and analyzed for pH, soluble salts and
nutrient element content. Seedling growth and leachate content will be moni-
tored through the 1979 growing season.
Oats Yield
Mean oat yield after four weeks growth ranged from 3.67 to 0.57 g dry
weight per container of 1461 cm2 surface area, for the Iva A horizon and
black fissile shale, respectively. Oat yields for the loess, unweathered and
weathered Illinoian till, and brown shale averaged 14 to 21% less than the
yield in A horizon, but these differences in mean yield were not significant
at P = 0.05. Oat yield of 2.64 g in B horizon material was significantly less
than in the A horizon, but was equivalent to yields in all other overburden
materials except gray marine and black fissile shales. The poorest oat yield,
0.57 g, occurred in black fissile shale and next poorest yield, 1.56 g, in gray
marine shale.
Oat vegetative tissue was analyzed for three macronutrients (P, Ca and
Mg), five micronutrients (Fe, Mn, B, Cu and Zn) and three other minor elements
(Na, Ba and Al) (Table 18). Due to the small sample size, less than 5 g dry
weight oats tissue from each container, analysis for other elements was not
feasible. Nutrient element concentration in oat tissue was compared to in-
terpretive standards of very low, low, medium, high and very high levels used
by the Purdue University Plant and Soil Analysis Laboratory.
Phosphorus and calcium contents of 0.23 to 0.46% and 0.24 to 0.66%, re-
spectively, in oat tissue for all overburden materials were in the "medium"
level. The highest P accumulation occurred in plants grown in brown shale
and weathered Illinolan till and was not related to soil test levels, which
were all very low. The highest Ca content in tissue was associated with A
horizon and Wisconsin till which were both well supplied with Ca (Table 7).
Magnesium concentrations ranging from 0.11 to 0.30% were in the "low" to
"medium" plant tissue levels with the highest content occurring on B horizon
which also had the highest exchangeable Mg (Table 7) and lowest on gray marine
shale. Of the micronutrients, Cu and Zn oat tissue concentrations were in the
"medium" range with the highest levels of both elements occurring on loess.
Boron and Mn levels in tissue were "medium" for oats grown in most overburden
materials. Gray marine shale contained a high level of water extractable B
and produced oats with 46 ppm, "high" level, in the tissue. The loess con-
tained only a moderate amount of extractable Mn, yet produced oats with the
highest level, 208 ppm. The plant Fe content was adequate, "medium", for all
materials except loess and brown shale where accumulations of 555 and 673 ppm
were excessive and possibly in the toxic range. Likewise, A.1 accumulations
were excessively high and probably at toxic levels for plants grown in loess
and brown shale. This 1s unexpected since the exchangeable Al levels were not
high nor were the pH's low. Aluminum was "medium" to "high" for oats grown
40
-------
TABLE 18. MEAN ELEMENT CONTENT OF OAT PLANTS GROWN FOUR WEEKS IN OUTDOOR CONTAINERS OF OVERBURDEN
MATERIAL. EACH VALUE IS A MEAN OF THREE REPLICATES.
Overburden
material
Iva A-Horizon
Iva B-Horizon
Loess
* Unw. Illinoian Till
Wx. Illinoian Till
Wisconsin Till
Black Fissile Shale #1
Gray Marine Shale
Brown Shale
Sandstone
P
0.29c*
0.26c
0.30c
0.23C
0.37b
0.29c
0.24c
0.31c
0.46a
0.25c
Ca
<
0.66a
0.48bc
0.54b
0.49b
0.40cd
0.65a
0.46bc
0.25e
0.24e
0.34d
Mg
1 - - - -
0.15e
0.30a
0.26bc
0.23d
0.28ab
0.25cd
0.24cd
O.llf
0.27abc
0.27abc
Na
0.02e
0.28b
O.lBcde
0.03e
0.42a
O.llde
O.lZde
O.Slab
0.19bcd
0.25bc
Element
Mn
63d
189a
208a
128bc
118bc
78cd
104bc
93bcd
134b
lOlbcd
r'e
lllb
215b
555a
184b
161b
178b
98b
169b
673a
175b
Cu
23b
18b
32a
19b
22b
20b
20b
26ab
24b
21b
Zn
ppm -
31c
34c
49a
32c
38bc
33c
34c
32c
39bc
45ab
B
7e
lOcde
14cd
lOcde
9de
12cde
26b
46a
15c
llcde
Al
91b
205b
835a
141b
204b
137b
98b
235b
1024a
351b
Ba
4cd
7c
25a
2cd
5cd
Id
2cd
3cd
15b
2cd
*Means in columns followed by the same letter are not significantly different at P = 0.05 according to
Duncan's Multiple Range Test.
-------
in all other overburden materials. The tissue content of Na and Ba appeared
to be within the normal range for most materials.. Overall, it appears that
tissue element concentrations were adequate or normal for most elements
analyzed. However, deficiencies may exist in B for plants grown in all ma-
terials except gray marine shale and in Mg for plants grown in gray marine
shale and A horizon material. Jones (1972) and Brady (1974) indicate that
plant B concentrations of less than 15 ppm is considered deficient. It is
probable that toxic levels of Al and Fe accumulated in plants grown in loess
and brown shale.
Tree Seedlings
Survival of Virginia pine and yellow-poplar seedlings after one growing
season, August 1978, was 100% in all overburden materials except black fissile
and gray marine shales (Table 17). Virginia pine survival was 33 and 50% in
black fissile and gray marine shale, respectively; while, survival of yellow-
poplar was zero in these materials. By December 1978, all Virginia pine in
black fissile shale were dead and no change in survival was noted for both
species in all other materials.
Virginia pine height growth of 5.8 to 8.9 cm in 12 weeks was superior in
A and B horizon soil, loess and weathered Illinoian till. The poorest growth,
consistent with low survival, occurred in the black fissile and gray marine
shales. Virginia pine basal diameter growth was generally slight with little
variation among overburden materials except for significantly lower growth
in black fissile and gray marine shale.
Height and basal diameter growth of yellow-poplar, 34.7 cm and 0.41 cm,
respectively, in Iva A horizon were significantly better than all other ma-
terials. No net growth was observed on yellow-poplar in black fissile and
gray marine shales and all seedlings were dead by August 1978. Growth of
yellow-poplar was not significantly different in all other overburden materials.
Under conditions of this outdoor container study and based on first-year
growth characteristics of oats, Virginia pine and yellow-poplar, it is evident
that the black fissile and gray marine shales without amendments are unsuitable
as a plant growth medium. The A horizon soil provides the best overall plant
growth potential. Other materials studied appear to support adequate plant
growth and may be suitable media alone or in mixture in the rooting zone. The
excessive plant accumulations of Fe and Al from loess and brown shale did not
appear to affect the short-term growth evaluated in outdoor containers.
Leachate Analyses
Chemical analysis of leachate samples from outdoor containers of over-
burden materials are reported for the May 1978 and April 1979 collection
periods (Table 19). Leachate was available from only a few of the coarse ma-
terials in summer 1978 and therefore was not summarized since all materials
could not be compared. Leachate analysis was limited to pH, electrical con-
ductivity and four essential nutrient elements.
42
-------
TABLE 19. CHEMICAL ANALYSIS OF LEACHATE COLLECTED IN MAY 1978 AND APRIL 1979 FROM OUTDOOR CONTAINERS OF
OVERBURDEN MATERIAL. EACH VLAUE IS A MEAN OF THREE REPLICATES.
Overburden
material
PH
5/78
4/79
Elect. Cond.
5/78
4/79
mmhos/cm
Iva A-Horfzon
Iva B-Horizon
Loess
Unw. minoian Till
Wx. Illinoian Till
Wisconsin Till
Black Fissile Shale #1
Gray Marine Shale
Brown Shale
Sandstone
7.7
6.9
6.8
8.0
7.0
7.6
7.5
7.3
8.1
7.8
7.3abc*
6.9abc
6.1bc
7.8a
6.8abc
7.9a
3.6d
5.7c
6.7abc
7.5ab
0.44
0.23
0.12
1.97
0.23
0.32
2.37
5.35
0.21
0.38
0.50b
0.20b
0.12b
0.89b
0.17b
0.35b
5.30a
4.80a
0.15b
0.37b
P
5/78
0.05
0.05
0.05
0.07
0.07
0.15
0.03
0.05
0.00
0.13
4/79
0.00
0.00
0.00
0.00
0.00
0.00
0.43
1.27
0.05
0.00
K
5/78
2.6
0.6
0.5
11.5
0.3
4.0
16.7
29.2
72.0
25.5
4/79
ppm
4. Ob
0.4b
0.4b
4.6b
0.2b
0.7b
8.1b
11. 6b
78. 3a
l.lb
Ca
5/78
67
20
12
240
18
45
300
360
23
18
4/79
99bc
17d
15d
146b
13d
61cd
367a
377a
12d
22d
Mg
4/79
15c
lie
6c
55c
8c
17c
2067 a
1480b
lie
15c
*Means in columns followed by the same letter are not significantly different at P = 0.05 according to
Duncan's Multiple Range Test.
-------
Leachate from all materials was slightly acid to alkaline, pH 6.8 to 8.1,
in May 1978. By April 1979, there was a decrease in pH for leachate from all
materials except Wisconsin till and B horizon soil. A major decrease 1n pH
occurred in leachate from black fissile, gray marine and brown shales. This 1s
likely due to rapid weathering of these soft shales and the formation of acid
as the exposed S compounds, probably pyrites, oxidized. Calcium and magnesium
were especially high 1n leachate from the black fissile and gray marine shales
and moderately high from unweathered IlUnoian till.
Phosphorus 1n the leachate was negligible from all overburden materials
except black fissile and gray marine shales in April 1979. Moderate levels
of potassium, 25 to 72 ppm, occurred in leachate from the gray marine and
brown shales and sandstone 1n May 1978; however, by April 1979 only leachate
from brown shale had significant potassium content. Electrical conductivity
exceeded 1 mmhos/cm in leachate from unweathered Illinolan till, black fissile
shale and gray marine shale 1n May 1978. In April 1979, electrical condictivity
of leachate was excessive, 4.8 to 5.3 mmhos/cm, for only the gray marine and
black fissile shales. This high level of soluble salts in the soil solution
could be detrimental to seed germination and plant growth.
Chemical properties of overburden materials used in the outdoor contain-
ers (Table 20) varied somewhat from those used 1n greenhouse studies (Tables
7 and 8). The material was collected from the same mines and strata but at
different locations and therefore further reflects variability encountered.
The major differences occured 1n the rock strata. The pH was less acidic, 6.5
versus 3.7, 1n black fissile shale and more alkaline, 8.1 versus 5.5, in sand-
stone at time-of-collection 1n October 1977 as compared with previous samples.
After one year of weathering, April 1979, the pH of material 1n the surface 2
inches of outdoor containers decreased, with the most dramatic adjustment oc-
curring in the black fissile and gray marine shales (Table 20). Electrical
conductivity, organic matter and P content were lower in the black fissile
shale, gray marine shale and sandstone; and, K content was higher in all shales
and sandstone than material collected for previous studies.
PREDICTION OF PLANT GROWTH POTENTIAL
It 1s apparent when plant growth in greenhouse and outdoor container ex-
periments (Tables 11, 12 and 17) are compared with physical and chemical over-
burden properties (Tables 6, 7 and 8) that no single property is a reliable
predictor of plant growth. Variability in Individual overburden properties
within strata accounts for some of the difficulty in identifying specific pre-
dictors. However, the occurrence of properties known to cause severe plant
toxicity, suppressed growth or mortality in a given material can be identified
and used to rule out that material as plant growth media. This is evident in
the case of the black fissile and gray shales where some critical or limiting
factors occur at extreme levels. Certain Individual easily measured factors
such as pH, electrical conductivity, potential acidity or soil texture may be
adequate to eliminate the material from consideration 1f the tolerance range
1s known for given plant species.
44
-------
TABLE 20. CHEMICAL PROPERTIES OF OVERBURDEN MATERIALS USED IN OUTDOOR
CONTAINERS.
Overburden
materials
W77 4/79
Electric Organic
conduc. matter
mmhos/cm %
Iva A-Horizon 7.0 6.6 .15 1.0
Iva B-Hor1zon 5.8 5.5 .33 0.4
Loess 5.7 5.2 .03 0.2
Unw. Illinolan Till 8.1 7.7 .65 0.4
Wx. Illinolan Till 6.9 6.8 .12 0.2
Wisconsin Till 8.1 7.7 .13 0.5
Black Fissile Shale #1 6.5 2.7 2.80 3.3
Gray Marine Shale 6.2 3.0 3.80 3.4
Brown Shale 7.0 7.0 .24 0.5
Sandstone 8.1 7.7 .39 0.2
kg/ha-
ll
7
11
2
11
3
6
7
6
2
81
246
103
83
123
83
358
616
314
166
45
-------
Plant yields from greenhouse studies and corresponding overburden proper-
ties were examined by step-wise regression techniques. The results (Table 21)
indicate the limited usefulness of such an approach when single factors ex-
hibit overriding importance in some materials and are unimportant in others.
This may lead to fortuitous correlations that are unrelated to cause-and-effect.
When the overburden properties (Tables 6, 7 and 8) and greenhouse yield data
(Tables 11 and 12) are evaluated in accord with regression results, it becomes
apparent that some properties normally considered desirable (e.g. high levels
of K, P, Ca, Mg and CEC) occur in the same materials that produce low yields
because of very low pH or other detrimental factors. This results in the
favorable properties disappearing from the regression equation.
Electrical conductivity of the soil solution and water storage capacity
were the properties that occurred most frequently as the best single factor
in the regressions (Table 21). Manganese, magnesium and bulk density were
the best factors 1n some equations. The negative regression of Mg with plant
yield is unexpected in this region and is due to the occurrence of high Mg in
a few overburden materials that were very undesirable in other respects.
Potassium, B, Al, pH, P and % clay appear as additional factors in the multiple
correlation. The relationship of these factors with yield was in the expected
direction with the exception of P which was negative instead of positive as one
would anticipate. The explanation for the negative correlation of P is similar
to that for Mg.
The single factors alone were poor to moderate predictors of plant growth,
R2 = .39 to .68, and the addition of one or two other factors in step-wise re-
gression gave only modest improvement. It appears that measurement of only
those properties listed 1n these equations (Table 21) would not allow adequate
prediction of plant growth response. However, it is obvious that these prop-
erties should be examined along with others Indicated 1n previous studies and
1n agriculture and forestry practice.
46
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TABLE 21. OVERBURDEN PROPERTIES MOST CLOSELY CORRELATED BY STEP-WISE
REGRESSION TO PLANT YIELD IN GREENHOUSE EXPERIMENTS.
Experiment
Treatments
Species
Best single factor
Factor* R2
Multiple correlation
Factor(s)* R2
Experiment 1
Control
Alfalfa -EC1
Wheat -Mg
Fertilizer
Alfalfa -EC
Wheat -Mn
.39
.42
.68
.50
-EC
-Mg, +K
-EC, -B
-Mn, -Mg
.39
.76
.80
.67
Experiment 2
Control
Alfalfa
Wheat
Fertilizer
Alfalfa
Wheat
Sludge
Alfalfa
Wheat
-BD
+H20
+H20
+H20
-BD
-EC
.47
.42
.56
.51
.46
.58
-BD, -Al, -Clay
+H20, +pH
+H20
+H20, -P
-BD, +pH
-EC, -B
.71
.58
.56
.62
.62
.67
*Factor symbols: EC, electrical conductivity of soil solution; Mg, ex-
changeable Mg; K, exchangeable K; Mn, extractable Mn; B, extractable B;
BD, bulk density of repacked materials; Al, exchangeable Al; Clay, per-
cent clay; HzO, percent water by volume between 1/3 and 15 bars; P,
available P by Bray PI extraction; pH, 1:1 soil to water by volume.
fSign indicates positive or negative correlation with yield.
47
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LITERATURE CITED
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flood-control reservlors and coal surface-mining activity, southwestern
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Publishing Co., NY, 639 p.
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Callahan, J. C. and J. G. Callahan. 1971. Effects of strip mining and tech-
nological change on communities and natural resources in Indiana's coal
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Corbett, D. M. 1968. Ground-water hydrology pertaining to surface mining
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49
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LlmstroiD, G. A. 1960. Forestation of strip-mined land in the central states.
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-------
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51
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52
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APPENDIX A
LABORATORY PROCEDURES SYNOPSIS
1. Elemental Analyses
Phosphorus: Bray No. 1, F1ske-Subbarrow Method. Use 1.5 g of soil in
15 ml of 0.025 NH^Cl 1n .03 N NH^F. Shake 5 min at 200 opm. Fil-
ter. Take a 5 ml aliquot, acTd 2 ml acid ammonium molybdate solution
and mix. Add 2 ml P-C agent (Aminonaphthol-sulfonlc acid) and mix.
Develop color. Read between 15 m1n - 45 m1n at 600 my. Compare
with standards.
Potassium: 1.5 g soil in 15 ml of 1 N ammonium acetate, pH 7.0. Shake
5 m1n at 200 opm. Filter. Read on AA. Compare with standards.
Calcium and Magnesium: To 1.5 g soil add 15 ml 1 N ammonium acetate
pH 7.0. Shake 5 m1n at 200 opm and filter. DTlute with Lanthanum
Chloride (1500 ppm). Read on AA Spectrophotometer. Compare with
standards.
Sodium: To 5 g soil add 15 ml 1 N ammonium acetate pH 7.0. Shake 5 m1n
at 200 opm. Do not filter. Read supernatant liquid on AA Spectro-
photometer. Compare with standards.
Aluminum: Leach 10 g of soil with five 20 ml allquots of 1 N KC1. Add
10 drops of O.U phenolphthaleln to filtrate. Titrate the filtrate
to a permanent pink endpoint using standardized 0.1 N NaOH. Add
more Indicator, 1f necessary, as some may be precipitated with the
A1(OH)3. Record base. Add one drop of 0.1 N^HC1 to bring the fil-
trate back to colorless. Add 10 ml of 4% to filtrate and stir.
If the filtrate contains exchangeable Al, the pink color returns.
Stirring constantly, titrate the filtrate with 0.1 N HC1 until
color disappears. Add 1 or 2 drops of Indicator. Tf color returns,
titrate until no color returns for two minutes. The meq. of add
used is equal to the meq. of exchangeable Al.
Manganese: 10 g soil are extracted with 50 ml 0.1 N phosphoric acid,
shake 15 m1n, filter 20 ml, add 2 ml of cone. H^Oi*, evaporate.
Organic matter 1s oxidized with Ha02. Add distilled water and 0.3
g of tr1sod1um perlodote. Heat 20 m1n. Dilute to exactly 20 ml
with distilled water. Read color on Coleman Model 8 Photo-Electric
Colorimeter at 540 my.
Boron: Add 40 ml of nearbolUng distilled \\20 to 20 g of soil and re-
flux 5 min. Add 2 drops of 20$ Caclz solution, cool, and filter
through boron-free filter paper. Take 0.5 ml aliquot of the soil.
53
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extract, add 2 ml of curcumin reagent and mix thoroughly. Evapo-
rate to dryness in a 55ฑ 3 C water bath or oven. Heat 15 m1n,
dissolve in 10 ml of 95% ethyl alcohol and transfer to a colorimeter
tube. Allow any turbidity present to settle out. Read in color-
imeter within 2 hours at 540 my. Evaluate against a standard curve.
Molybdenum; Extraction is made with pH 3.3 NH^O^ using a 10:1 di-
lution factor. Extract is centrifuged and analyzed directly with
atomic absorption.
Sulfur: The Leco Sulfur Analyzer is used. Ground samples are treated
with combustion accelerations (iron and tin) and heated to ca 1,600
C in a stream of purified 02. The high temperature is generated
by using an induction furnace to indice an electrical field in the
accelator-treated sample. The S02 liberated is collected in dilute
HC1 containing potassium iodide, starch and trace amounts of potas-
sium iodate. This is titrated automatically with KI03 through the
use of a photocell to maintain the initial optical density of the
blue color formed by reaction of the starch with the iodine formed
by reaction of KI03 and KI in the presence of HC1.
2. Other Chemical
pH: 1:1 soil to water volume. Mix 5 seconds. Let stand 10 min. Stir,
read pH with pH meter.
Buffer pH: Add 10 ml of SMP buffer solution (pH 7.5). Shake at 200
opm for 10 min. Let stand 30 min. Stir and read pH.
Cation Exchange Capacity:
Extractable acidity. To 10 g of air dry soil add 100 ml of extrac-
tion solution (BaCl2ป triethanolamlne). Stopper, shake well,
and let stand overnight. Run blank. Filter, wash with ex-
tracting solution. Bring up to 250 ml. Add indicator (brom-
cresol green and methyl red) and titrate with 0.2 N_ HC1 to
pink orange end-point. Calculate.
Base extraction. Use macerated paper in 60 ml fritted glass funnels,
Extract with a total of 100 ml 1 lฑ ammonium acetate pH 7.0
(allow to sit overnight in 30 ml extracting solution). Run Ca,
Mg, K, and Na on extract. Calculate C.E.C. and report 1n meq.
Calculate percent base saturation.
Organic Matter: Oxidize with potassium dlchromate and cone, sulfuric
add by standing for 30 min; add water, phosphoric acid, sodium
fluoride, and dlphenylamine indicator. Titrate with 0.5 N^ ferrous
ammonium sulfate.
Soluble Salts: To 25 g of air-dry soil add 50 ml of distilled water
and shake well for 1 min. Cover and let sit for 30 minutes. Fil-
ter into test tube. Determine K-value of unknowns after standardiz-
ing solubrldge with 0.01 ^ KC1 set at 141.
Potential Acidity: FeS2 is completely oxidized with H202 and the pro-
duct, H2S04, 1s measured titrametrically with 0.01 N NaOH.
54
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3. Physical Analyses
Particle Size: Samples are sieved to remove particles larger than
2 mm. The remaining sample is dispersed with sodium hexameta-
phosphate, placed in settling containers and subsampled at
appropriate intervals with a pipette. The subsample is dried
at 105 C and weighed.
Moisture Retention: Two samples of disturbed overburden were measured.
Moisture retained at 15 bar tension was measured by placing about
10 g of material passing a 5 mm sieve in a pressure membrane ap-
paratus. Fifteen bars of pressure was applied and the sample was
allowed to equilibrate. The sample was removed, weighed, dried at
105 C, and weighed again. Moisture retained at 1/3 bar tension
was measured by placing loose, unsieved material in metal cans
(8 cm diameter x 5 cm deep, small hole in bottom) and wetting the
material to saturation. Saturated samples were placed in a pres-
sure plate apparatus, put under 1/3 bar pressure and allowed to
equilibrate. The samples were then removed, weighed, dried at
at 105 C, and weighed again.
Bulk Density: Determined using 8 cm x 5 cm metal cans. Loose samples
were placed in the cans, wet to saturation, dried at 105 C and
weighed.
55
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TECHNICAL REPORT DATA
(Please read Instructions on the reverse before completing}
1. REPORT NO.
EPA-600/7-80-054
3. RECIPIENT'S ACCESSION NO.
4. TITLE AND SUBTITLE
Properties and Plant Growth Potential of Mineland
Overburden
5. REPORT DATE
March 1980 issuing date
6. PERFORMING ORGANIZATION CODE
7. AUTHOR(S)
W. R. Byrnes, W. W. McFee and J. G. Stockton
I. PERFORMING ORGANIZATION REPORT NO.
CR-10
9. PERFORMING ORGANIZATION NAME AND ADDRESS
Indiana Agricultural Experiment Station
Departments of Forestry .& Natural Resources and Agronomy
Purdue University
West Lafayette, IN 47907
10. PROGRAM ELEMENT NO.
1NE623
11. CONTRACT/GRANT NO.
EPA-IAG D6-E762
CR-684-15-18
12. SPONSORING AGENCY NAME AND ADDRESS
Industrial Environmental Research Laboratory
Office of Research and Development
U. S. Environmental Protection Agency
Cincinnati, Ohio 45268
13. TYPE OF REPORT AND PERIOD COVERED
Final
14. SPONSORING AGENCY CODE
EPA/600/12
15. SUPPLEMENTARY NOTES
This project is part of the EPA-planned and coordinated Federal Interagency Energy/
Environment R&D Program.
16. ABSTRACT
Overburden materials from surface coal mines in southwestern Indiana were analyzed
for physical and chemical properties. Plant growth potential of selected materials,
with and without sewage sludge and fertilizer amendments, was evaluated in greenhouse
pot culture and outdoor containers using alfalfa, small grains and tree seedlings.
The general ranking of overburden materials for plant growth was lacustrine
sediment > A horizons > B horizons = glacial tills = loess > brown shale > sandstone
> gray shale > black fissile shale. Amendments ranked sewage sludge > fertilizer >
as surface plant growth media. The B horizons, partially weathered loess and glacial
tills were similar in productivity and are suitable for use in the plant root zone.
The sandstone and brown shale are not suitable in the upper root zone due to undesired
physical properties or content of phytotoxic elements in sandstone. The gray and black
fissile shales are unsuitable for plant growth and should be avoided in the rooting
zone.
Regression analysis did not reveal overburden properties that could be used con-
sistently for predicting plant growth potential. Electric conductivity of the material
extract and water storage capacity were most frequently significantly related to
growth.
7.
KEY WORDS AND DOCUMENT ANALYSIS
DESCRIPTORS
b.lDENTIFIERS/OPEN ENDED TERMS C. COSATI Field/Croup
Ecology
Environments
Soils
Soil Tests
Surface Mining
Coal Mines
Inorganic Chemistry
Vegetation
Mineland Overburden
Geology
Indiana
Overburden
Root Zone
Shales
Ecological Effects
Coal
Sewage Sludge
A Horizon
6F 8A 8F
8H 10A 10B
7B 7C 13B
8. DISTRIBUTION STATEMENT
Release to the Public
19. SECURITY CLASS (ThisReport)
Unclassified
21. NO. OF PAGES
66
20. SECURITY CLASS (ThUpage)
Unclassified
22. PRICE
EPA Form 2220-1 (Rซv. 4-77) PREVIOUS EDITION is OBSOLETE
56
ป u 5 eovtBNMEid mipftnwOfFKt: 1W0.657-146/56Z9
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