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Scholars' Mine Scholars' Mine Masters Theses Student Theses and Dissertations 1970 Clay mineralogy and compaction characteristics of residual clay Clay mineralogy and compaction characteristics of residual clay soils used in earth dam construction in the Ozark Province of soils used in earth dam construction in the Ozark Province of Missouri Missouri Arthur David Alcott Follow this and additional works at: https://scholarsmine.mst.edu/masters_theses Part of the Civil Engineering Commons Department: Department: Recommended Citation Recommended Citation Alcott, Arthur David, "Clay mineralogy and compaction characteristics of residual clay soils used in earth dam construction in the Ozark Province of Missouri" (1970). Masters Theses. 7177. https://scholarsmine.mst.edu/masters_theses/7177 This thesis is brought to you by Scholars' Mine, a service of the Missouri S&T Library and Learning Resources. This work is protected by U. S. Copyright Law. Unauthorized use including reproduction for redistribution requires the permission of the copyright holder. For more information, please contact [email protected].

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Scholars' Mine Scholars' Mine

Masters Theses Student Theses and Dissertations

1970

Clay mineralogy and compaction characteristics of residual clay Clay mineralogy and compaction characteristics of residual clay

soils used in earth dam construction in the Ozark Province of soils used in earth dam construction in the Ozark Province of

Missouri Missouri

Arthur David Alcott

Follow this and additional works at: https://scholarsmine.mst.edu/masters_theses

Part of the Civil Engineering Commons

Department: Department:

Recommended Citation Recommended Citation Alcott, Arthur David, "Clay mineralogy and compaction characteristics of residual clay soils used in earth dam construction in the Ozark Province of Missouri" (1970). Masters Theses. 7177. https://scholarsmine.mst.edu/masters_theses/7177

This thesis is brought to you by Scholars' Mine, a service of the Missouri S&T Library and Learning Resources. This work is protected by U. S. Copyright Law. Unauthorized use including reproduction for redistribution requires the permission of the copyright holder. For more information, please contact [email protected].

CLAY MINERALOGY AND COMPACTION CHARACTERISTICS OF RESIDUAL CLAY SOILS USED IN EARTH DAM CONSTRUCTION

IN THE OZARK PROVINCE OF MISSOURI

BY

ARTHUR DAVID ALCOTT, 1941-

A

THESIS

submitted to the faculty of

UNIVERSITY OF MISSOURI - ROLLA

in partial fulfillment of the requirements for the

Degree of

MASTER OF SCIENCE IN CIVIL ENGINEERING

Rolla, Missouri

1970 19C853

ii

ABSTRACT

The clay mineralogy and Standard Proctor compaction

characteristics of clayey residual soils developed on the

Salem Plateau of the Ozark Physiographic Province and used

in earth dam construction were studied.

A review of the geology of the Salem Plateau is

presented along with a discussion of the factors controlling

the development of soils on carbonate bedrock in a high

leaching environment. The predominant soil clay mineral

was found to be a poorly crystallized kaolinite rather

than halloysite as has been postulated by others. Minor

amounts of triple-layer minerals and an undetermined amount

of an alumino-silicate gel are indicated. The effects of

particle size and degree of crystallinity on the tests

used to determine clay mineralogy are discussed.

The effects of several soil properties on the

laboratory compaction of the clayey residual soils were

investigated. Since the clay mineralogy was similar for

all of the soils investigated, this factor was discarded

as not being responsible for compaction differences. The

percent clay was found to have the highest correlation

with the maximum dry density and the optimum moisture

content of the soils. The plastic limit and cation­

exchange capacity were also closely correlated with the

compaction characteristics.

lll

It was determined that the pedular structure character­

istic of the residual soils was not destroyed upon laboratory

compaction, particularly compaction dry of optimum moisture

content. A theory of the compaction of clay soils is

postulated which deals primarily with the behavior and

changes in this ped structure with increasing moisture

content.

Scanning electron microscopy was used to illustrate

points brought out in the discussions on the morphology of

the soil clays and on the compaction characteristics of

the clays.

iv

ACKNOWLEDGEMENT

I wish to thank my adviser, Dr. N. 0. Schmidt, for his

assistance and guidance during the period that I have

attended graduate school and particularly during the period

that this paper has been written.

I also wish to express my appreciation to Dr. William

Hayes, Chief Geologist, and the Missouri Geological Survey

for financing the expenses related to the gathering of the

test soils and other field data and for allowing the author

to initiate an electron microscope study at the Survey's

expense. Without this assistance, the project would not

have been feasible.

The clay mineralogy investigation required equipment

and technology found only from outside sources. I wish to

thank Mr. W. M. Dressel for permitting the DTA and TGA

studies to be performed at the U.S. Bureau of Mines, Rolla,

Missouri. I also acknowledge with thanks the assistance of

Mr. R. Rickey and Mr. M. Adams for performing the tests and

for their suggestions with regard to interpretation.

The transmission microscopy was performed by

Mr. Kuldip Chopra at the Ceramics Department, University of

Missouri - Rolla. The scanning electron microscopy

investigation was performed at the Materials Research Center,

also at the University of Missouri - Rolla. My sincere

thanks for their assistance.

Dr. W. D. Keller was most helpful in allowing the

v

author to use the x-ray diffraction facilities at the

University of Missouri - Columbia. His discussions regarding

testing technique and data interpretation were invaluable

to this study.

Special thanks is also offered to Dr. J. L. Eades of

the Geology faculty of the University of Illinois. His

independent analysis of the nature of the clay mineralogy

substantiated that of the author and is most appreciated.

The encouragement and assistance over the past two

years of Mr. J. H. Williams and Mr. E. E. Lutzen of the

Missouri Geological Survey is gratefully acknowledged.

Finally I wish to thank my wife, Molly, for her

understanding and help, particularly during the period

when this paper was being prepared.

vi

TABLE OF CONTENTS

ABSTRACT . . . .

ACKNOWLEDGEMENT

LIST OF FIGURES

LIST OF TABLES .

Page

ii

iv

X

xiv

I.

II.

II I.

IV.

v.

INTRODUCTION

LITERATURE REVIEW . .

A. GEOLOGY . . . . ..

B. SOIL FORMATION

1

5

5

8

1. Soils derived from limestones . . . . 8

2. Formation of Kaolins 11

3. Kaolinite morphology . . . . . 12

C. COMPACTION CHARACTERISTICS . . . . 15

1. Soil gradation and index properties . 16

2. Cation-exchange capacity

3. Clay particle structure .

FIELD INVESTIGATION . . . . . . . .

MATERIALS . . . . . .

TEST PROCEDURES . . . . . . . A. SOIL GRADATION . . . . . . . . . . . .

1. Sample preparation . . .

2. Coarse sieve analysis . . . .

3. Hydrometer analysis . . . . . . . . ·

B. ATTERBERG LIMITS TESTS ....... · · ·

1. Liquid limits .. . . .

18

26

32

35

40

40

40

40

41

41

41

Table of Contents Continued

2. Wet liquid limits

3. Dispersed liquid limit .

4 . Plastic limits .

C. MOISTURE-DENSITY RELATIONSHIPS

1 . Natural samples . . 2 . Dispersed samples . . .

D. X-RAY DIFFRACTION . . . . . . . 1. General . . . . . . . . . . . . 2 . Preparation of samples . 3. Powdered samples . . . . . . . 4. Potassium acetate treatment

E. DIFFERENTIAL THERMAL ANALYSIS . 1. General . . . . . 2 . Sample preparation and testing .

F. THERMOGRAVIMETRIC ANALYSIS . . . . . G. TRANSMISSION ELECTRON MICROSCOPY (TEM)

H. SCANNING ELECTRON MICROSCOPY (SEM) . I . LOW-POWER MICROSCOPY (LPM)

J. SOIL CLAY CHEMISTRY . . . . . 1 . General . . . . . . . . 2 . Chemical analysis . . . . 3 . Soil pH in water . . . 4. Cation-exchange capacity

5. Flame photometry . . . . . 6. Absorption spectrophotometry . .

K. SPECIFIC GRAVITY . . . . . . . . . .

. .

. .

. .

. .

. .

. .

. .

. .

. .

. .

. .

. .

. .

. . .

. .

. .

.

.

.

.

.

.

.

.

.

.

.

.

.

.

.

vii

Page

41

42

53

53

53

53

55

55

57

58

58

60

60

61

63

64

66

72

72

72

72

73

75

75

77

77

viii

Table of Contents Continued Page

L. CORRELATION TESTS 79

VI. ANALYSIS OF RESULTS 82

A. CLAY MINERALOGY . 1 . X-ray analysis . 2 . Differential thermal analysis

3 . Thermogravimetric analysis

4. Electron microscopy

5 . Chemical analysis

6. Summary . . .

. . . 82

82

90

100

102

110

112

B. SOIL CLASSIFICATION AND CATION-EXCHANGE CAPACITY . . . . . 113

C. COMPACTION CHARACTERISTICS 123

1. Atterberg Limits . . . 123

2. Gradation and cation-exchange capacity 135

3. Soil clay structure 135

VII. CONCLUSIONS 147

A. GENERAL . 147

B. CLAY MORPHOLOGY 147

C. SOIL CLASSIFICATION AND CATION-EXCHANGE CAPACITY . . . . . . . . . . . 148

D. CORRELATIONS WITH COMPACTION RESULTS 150

E. THEORY OF RESIDUAL SOIL COMPACTION 150

F. APPLICATION OF TEST RESULTS . 152

1. Correlations 152

2. Dam design - construction 152

G. RECOMMENDATIONS FOR FURTHER STUDY 157

VIII. APPENDIX A - Dam Reports 159

Table of Contents Continued

IX. BIBLIOGRAPHY .

X. VITA ....

lX

Page

176

184

Figure

1.

2 •

3 .

4 .

5 .

6 .

7 .

8.

9 .

10.

11.

1 2 .

13.

14.

15.

16.

17.

18.

LIST OF FIGURES

Clay Distribution in Clarksville Soil (from Scrivner, 1960).

Location of Dam Sites.

Particle-Size Analysis of Masters #1 and Masters # 2 .

Particle-Size Analysis of Terre Du Lac and Timberline .

Particle-Size Analysis of Sayers, Little Prarie, and Blackwell.

Particle-Size Analysis of Floyd, Ft. Westside, and Rice .

Particle-Size Analysis of Sunrise Central, Sunrise South, and Fabick.

Particle-Size Analysis of Hornsey, Elsey, and Sunnen .

Plasticity Chart Plot of Ozark Soils .

X-Ray Diffractograms of the Sayers Soil.

X-Ray Diffractograms of the Masters #1, Timberline, and Terre Du Lac Soils .

Shift in 001 Peak of Georgia Kaolinite When Treated With Potassium Acetate . Differential Thermal Analysis of Georgia Kaolinite and Indiana Halloysite . Differential Thermal Analysis of Ozark Soils

Differential Thermal Analysis of Ozark Soils

Differential Thermal Analysis of Ozark Soils

Differential Thermal Analysis of Ozark Soils

Thermogravimetric Analysis .

X

Page

10

33

44

45

46

47

48

49

52

85

86

87

93

. 94

. 95

. 96

. 97

101

List of Figures continued

Figure 19. TEM Terre DuLac Suspended Sample

2 0 •

21.

2 2.

2 3.

24.

25.

26.

2 7.

28.

29.

30.

31.

(57000X) ..... .

TEM Terre Du Lac Suspended Sample (52000X) ..... .

TEM Terre Du Lac (28000X) .....

Suspended Sample

TEM Terre Du Lac Suspended Sample (20000X). . ..

SEM Terre Du Lac (1000X) .

Powdered Sample

SEM Hornsey (3000X)

Powdered Sample

SEM Hornsey (3000X) ...

SEM Hornsey (10000X).

SEM Hornsey (10000X). . .

Ped Sample

Ped Sample . . . . . . . . Ped Sample . . . . . .

SEM Terre Du Lac Ped Sample (10000X) .......... .

SEM Timberline (10000X) ....

Ped Sample

. .

Clay Content Versus Liquid Limit (Clay Residual Soils) . . . . . .

Clay Content Versus Plastic Limit (Clay Residual Soils)

.

.

xi

Page

103

103

104

104

105

105

106

. . . . . . 106

. . . . . . 108

108

109

115

116

32. Cation-Exchange Capacity Versus Liquid Limit (Clay Residual Soils) . . . . . . . . . . . 118

33. Cation-Exchange Capacity Versus Plastic Limit (Clay Residual Soils) . . . . . . . . . . . . . 119

34. Cation-Exchange Capacity Versus Clay Content (All Soils) . . . . . . . . . . . . . . . 120

35. Clay Content Versus Maximum Dry Density (Clay Residual Soils) . . . ... 124

List of Figures continued

Figure

36.

37.

38.

39 .

40.

41.

42.

43.

44.

45.

46.

47.

48.

49.

50.

Clay Content Versus Optimum Moisture Content (Clay Residual Soils). . . . . . .

Cation-Exchange Capacity Versus Maximum Dry Density (Clay Residual Soils) .

Cation-Exchange Capacity Versus Optimum Moisture Content (Clay Residual Soils) ..

Liquid Limit Versus Maximum Dry Density (Clay Residual Soils).

Liquid Limit Versus Optimum Moisture Content (Clay Residual Soils). . ..

Plastic Limit Versus Maximum Dry Density (Clay Residual Soils). . . ..

Plastic Limit Versus Optimum Moisture Content (Clay Residual Soils). . . . . ..

Clay Content Versus Maximum Dry Density (All Soils) ....

Clay Content Versus Optimum Moisture Content (All Soils) .

Optimum Moisture Content Versus Maximum Dry Density (Clay Residual Soils)

LPM a.) b . )

LPM a.) b.)

SEM a.) b.)

SEM a.) b.)

SEM a.) b.)

Terre Du Lac (Black and White) Compacted 3% Dry of Optimum Compacted 5% Wet of Optimum

Terre Du Lac (Color) Compacted 3% Dry of Optimum Compacted 5% Wet of Optimum

Terre Du Lac (lOOX) •• Compacted 3% Dry of Optimum Compacted 5% Wet of Optimum

Terre DuLac (300X). Compacted 3% Dry of Optimum Compacted 5% Wet of Optimum

Terre Du Lac (3000X) Compacted 3% Dry of Optimum Compacted 5% Wet of Optimum

. . . .

xii

Page

125

126

127

128

129

130

131

132

133

134

137

138

140

141

142

xiii

List of Figures continued

Figure Page

51. The Effect of Dispersion of the Standard Proctor Compaction of Clayey Residual Soils. . 146

52. Graphical Relationship of the Maximum Dry Density to the Plastic Limit and the Clay Content of the Clayey Residual Soils . . 153

53. Graphical Relationship of the Optimum Moisture Content to the Plastic Limit and the Clay Content of the Clayey Residual Soils . . 154

54. Graphical Relationship of the Maximum Dry Density to the Plasticity Index and the Liquid Limit of all Soils. . 155

55. Graphical Relationship of the Optimum Moisture Content to the Plasticity Index and the Liquid Limit of all Soils . . 156

Table

I.

II.

I I I.

IV.

V.

VI.

VII.

VIII.

IX.

X.

XI.

XII.

XIII.

XIV.

XV.

LIST OF TABLES

Affect of Crystal Structure on Cation­Exchange Capacity (after Kelley and Jenny).

Material of Dams Investigated

Comparison of Natural Field Moisture With Atterberg Limits .

Summary of Particle Size Analysis .

Comparison of Wet Liquid Limit And Natural Atterberg Limits.

Comparison of Natural and Dispersed Atterberg Limits.

Summary of Atterberg Limits Tests

Result of Moisture-Density Tests.

X-Ray Machine Specifications.

Summary of Major DTA Temperature Peaks.

Chemical Analysis of Ozark Soils.

Summary of pH and Cation-Exchange Capacity of Ozark Soils.

Concentration of Mg, Ca, Na, and K Cations in meq/100 grams.

Specific Gravity of Ozark Soils

Correlations for Clayey Residual Ozark Soils.

xiv

Page

22

36

39

43

so

so

51

54

56

62

67

74

76

78

80

1

I. INTRODUCTION

Missouri has approximately 1600 man-made earth dams, as

many or possibly more than any other state in the Union.

About 700 of these dams are located in the Ozark

Physiographic Province, a series of plateau surfaces

developed principally on Paleozoic carbonate bedrock

formations. A mantle of clayey residual soils up to 200

feet thick overlies these bedrock surfaces.

Earth dams constructed in this area, particularly

those constructed of the clayey residual soils, have a

history of poor performance. Excess seepage, slope

instability, piping, and total embankment failures have

occured. Further problems will emerge as urban expansion

and increasing numbers of recreational lake developments

extend into the area. The purpose of this investigation

is to study the nature of these residual soils, the factors

which affect the compaction of the soils, and to recommend

procedures to improve the performance of the dams.

The stony nature of most of the embankments prohibited

the collection of near surface undisturbed samples with hand

tools. Owner resistence and the expenses involved in

mobilizing and using mechanized equipment further prohibited

undisturbed sampling.

Only dams with a reservoir surface area greater than 15

acres were investigated. The expectation was that this

restriction would limit the investigation to dams which were

2

constructed using accepted engineering practices. This was

not the case. Almost anything passes for accepted construc­

tion practice in this state where there is no legislation to

regulate dam design and construction. Therefore, attempts

to relate dam performance with the nature of the embankment

materials or with the embankment performance were not

feasible. One dam with flat slopes utilizing good materials

but poorly constructed might perform less satisfactorily

than another constructed with steep slopes and less suitable

materials, but well compacted.

The investigation has been directed, therefore, to a

study of the nature of the soils used in dam construction

and to the factors which affect the compaction of these

soils. With this knowledge, it should be possible to assess

the potential for dam construction if good construction

techniques are followed.

The effect of significant soil properties on Standard

Proctor compaction parameters were investigated. These

properties were chosen considering the clayey nature of

the soils. They are: (1) clay mineralogy, (2) Atterberg

Limits and grain-size distribution, (3) cation-exchange

capacity, and (4) soil clay structure.

Evidence indicates that the Tertiary climate of the

Ozark region was semi-tropical or tropical. Where carbonate

bedrock is located in this type of climate, chemical

leaching is prominant and conditions favoring the formation

3

of kaolinitic and halloysitic soils are developed. Terzaghi

(1958) reports the characteristics of a halloysitic soil of

tropical Kenya to be similar to that of the Ozark soils,

Graham (1969) sites the probable presence of halloysite in

the Ozark soils as being responsible for the low maximum

dry density and the high optimum moisture content of the

Springfield soil, an Ozark residual clayey soil. The

mineralogical investigation was designed to determine more

explicitly the nature of the clay and possible changes in

its morphology from one portion of the Ozark Province to

another.

X-ray diffraction, differential thermal analysis,

thermogravimetric analysis, chemical analysis, transmission

electron microscopy, and scanning electron microscopy

techniques were chosen for this investigation. The results

of several of these tests are shown to be affected by

mineral particle size, degree of crystallinity, and other

factors. These factors can lead to errors in interpretation

if they are not recognized and considered. The electron

microscopy studies, particularly those of the transmission

electron microscope, provide keys to clay mineral

identification.

Harris (1969) has made numerous correlations between

independent soil properties as the percent fines, the percent

clay, the liquid and plastic limits and the Standard Proctor

compaction test variables, the maximum dry density and the

optimum moisture content. It was decided to determine if

4

similar correlations exist for the Ozark residual soils.

It was chosen to study the nature of the clay structure

of the laboratory compacted samples with the scanning

electron microscope at various magnifications 1 particularly

samples compacted wet and dry of the optimum moisture

content.

5

II. LITERATURE REVIEW

A. GEOLOGY

The geology of the Missouri Ozarks is illustrated on

the Geologic Map of Missouri published by the Missouri

Geological Survey. The general geology of the Ozark

Plateaus is that of a horizontal sequence of sedimentary

formations deposited by shallow marine seas which moved

onto and off of a Precambrian dome centered in the St.

Francois Mountains. The Ozark Province has been divided

into four subprovinces by Thornbury (1965): (1) the

St. Francois Mountains - the Precambrian igneous core of

the province; (2) the Salem Plateau - underlain by

Cambrian and Ordovician dolomites with some sandstones;

(3) the Springfield Plateau - underlain primarily by

Mississippian and Pennsylvanian limestones; and (4) the

Boston Mountains - rugged topography developed on shales,

limestones and sandstones.

The topography of the northern flank of the Salem

Plateau where the darns investigated are located is char­

acterized by steep-sided ridges with closely spaced

drainage. Broad uplands are developed in portions of

Phelps, Dent, and Crawford Counties on the Roubidoux and

Jefferson City formations.

The youngest formation exposed in the area is the

Ordovician Jefferson City dolomite, and oldest is the

6

Cambrian Potosi dolomite. The stratigraphy of these

formations is described in detail in The Stratigraphic

Succession in Missouri published by the Missouri Geological

Survey.

Bretz (1965) attributes the plateau development to

weathering cycles which extended through three periods

of peneplanation forming the three plateau levels. These

stages of peneplanation correspond to, and are the result

of, tectonic pulses triggered within the province dome.

Evidence of later, minor pulses are noted in terraces and

rejuvenated streams.

He dates the plateaus as follows: (1) Boston Mount­

ains (pre-Tertiary?), (2) Springfield Plateau (early Ter­

tiary?), and (3) Salem Plateau (post-early Eocene). The

minor pulses are dated as Pliocene (?) and pre-Pleisto­

cene(?). According to the theoretical cycles of pene­

planation, the Salem Plateau is now in the early mature

stage. Bretz bases his postulation on the following

evidences of peneplanation noted in the area: (1)

accordant summits, (2) flat interfluvial divides, and

(3) monadnocks.

Quinn (1956) disputes the hypothesis of peneplanation

and postulates that the plateaus, ". . were eroded in

place by alternating periods of stream entrenchment

providing the escarpments, and periods of escarpment

retreat (pedimentation), forming the plateau surfaces."

7

Valley entrenchment occurs during periods of high

moisture which results in rejuvenation of streams resulting

in erosion. During alternating periods of arid conditions

streams aggrade and mechanical weathering predominates.

Quinn relates these alternating cycles to correspond with

the glacial and interglacial climatic conditions.

The two proposals vary considerable in dating the

development of the Salem Plateau. Bretz dates the plateau

as post-Eocene, pre-Pliocene; Quinn dates the plateau as

late Pleistocene. The age of the residual soils must coin­

cide with or be somewhat younger than the plateau itself.

The soils must be older than the Pleistocene loess deposits

which often covers the residium, particularly in the north­

eastern portion of the plateau. The exact age of the soils

has not been determined.

During the Tertiary period, what is now the Gulf

of Mexico extended far up into the Mississippi River Valley.

This near-shore (probably tropical) environment could

have provided the moisture required to produce a climate

favorable to laterization forming the clayey residual

soils on carbonate bedrock. Toward the end of the Tertiary

with the advent of the Pleistocene glacial stages, these

favorable conditions ceased and the existing soil forming

cycle was terminated.

8

B. SOIL FORMATION

1. Soils derived from limestones. The residual soils

investigated in this study are classified as Ultisols

(U.S.D.A., 1960). Earlier systems classified the soils

as Red-Yellow Podzolics. Where Red~Yellow Podzolics are

usually developed in tropical climates, Ramann (as reported

in Miller, 1965) noted a tendency of tropical soils to pen­

etrate into temperate climates on limestone formation.

This is possible because the permeable limestones, or

dolomites, permit rapid percolation with a resultant

decrease in ground water influence on soil formation.

The principle clay minerals in these Red-Yellow

Podzols developed on limestones are kaolinites and

halloysites. The soils also exhibit an increase in iron

and clay content with depth (Scrivner, 1960).

The laterization process is considered to be the

dominant process in the genesis of these residual soils

(Simonson, 1949). There is little evidence that eluviation

and illuviation have acted as a major process to concen­

trate clay in the B horizon. Simonson further suggests

that the dominant process in these soils is the destruction

of clays in the upper horizons and the formation of new

clay minerals in the deeper horizons.

Jenny (1941) notes that in humid regions the limestone

derived soils are closely related to the impurities in the

9

parent material. Carroll and Hathaway (1953) discuss the

soils developed on the Lenoir limestone in Virginia. The

limestone contains partings of hydrous mica and montmoril-

lonite. Their investigation shows that the mica and mont-

morillonite were changed during the leaching process to

kaolinitic and chloritic clay soils. The clay content,

particularly that of kaolinite, and the cation-exchange

capacity increased with depth through the soil profile.

Scrivner (1960) notes this variation of clay content with

depth and a graph from his study illustrating this

variation is presented as Figure 1.

In a study of the Lebanon soil in Missouri, Scrivner

(1960) reports that a limestone which contains illite

weathered by chemical leaching to produce a soil profile

which contains predominantly kaolinite. The soils also

contain some montmorillonite, an intermediate product of

illite weathering.

Miller (1965) studied four Ozark soils developed by

chemical weathering of four different carbonate bedrock

formations. The formations ranged in age from Ordovician

to Mississippian and the sources of the samples were

separated by distances of up to 100 miles. There is a

marked similarity in the soil profiles and mineralogy, 0

which consists primarily of kaolinite and some 14 A

minerals. The only clay mineral present in any

significant amount in the bedrock formations is illite.

10

10

Clay ( 0.002 mm) as 20 percent of less

than 2 mm soil

30

Limestone

40

50

,.-.... . 0 60

·r-f ..__,

...c: .j.J 70 0. Q)

0

80

90

100

110

120

0 10 20 30 40 50 60 70 80 90 100

Clay Content (%)

FIGURE 1. Clay Distribution in Clarksville Soil

(from Scrivner, 1960)

11

2. Formation of Kaolins. The most common minerals

of the kaolin group or family of minerals are allophane,

halloysite (hydrated and non-hydrated), and kaolinite.

Investigators present two primary modes of kaolin for­

mation; as precipitated gels and as particles from

solution. Hauser (1952) postulates that after chemical

leaching, hydration and adsorption of ions, the silica and

alumina gels react to form halloysite. Then, by conden­

sation, kaolinite and montmorillonite, mica and other

minerals may be formed depending on what ions are present.

Bates (1952) favors the theory of formation of

particles from solution. The kaolin mineral produced

depends on many factors; time, temperature, pressure,

humidity, pH, and the composition of the solution. Sherman

(1952) relates the kaolinite formation to the intensity of

the chemical weathering (amount, intensity, and distri­

bution of annual rainfall) and the length of time the

material has been subjected to weathering. Kaolin

formation is maximized by moderate, non-cyclic annual

rainfall and good internal drainage. With increased age

and/or greater annual rainfall, the kaolinitic clays

decompose into their individual hydrated oxides which are

concentrated to form laterites.

Keller (1968) presents a detailed study of the cry­

stallization of clay minerals from solution which is beyond

the scope of this investigation. In his summary he states,

" . it may be said that the factors which are important in the development of kaolin-type minerals from alumino-silicates are the complete removal of the metal cations (other than Al and Si) and the introduction of H ions (Ross, 1943), and a relatively low silica~alumina ratio."

12

The conditions required to produce the above factors are

a humid climate where precipitation exceeds evaporation,

permeable bedrock to allow continued leaching, and an

oxidizing environment to remove Fe from solution.

Scrivner (1960) presents a mechanism whereby alumino­

silicates arrive in solution from which they are subse-

quently precipitated as kaolins. His research describes

the destruction o£ the illite, alumina feldspars, and

quartz from the carbonate bedrock by an acid soil

environment to produce a solution of alumino-silicates.

The metallic Mg and Ca ions are removed by leaching from

the solution and the Fe is oxidized to Fe 2o3 . The

requirements outlined above by Keller have been satisfied.

A pH change immediately above bedrock from acidic to

basic keys the precipitation of a kaolinitic mineral out

of solution.

3. Kaolinite morphology. In the preceeding

paragraphs the formation of kaolinitic minerals from

solution has been discussed, but the morphology of these

minerals has not been considered. A number o£ minerals

from well-crystallized kaolinite to halloysite to

13

allophane may be the product of this precipitation.

Keller et al (1970) emphasize the question of kaolin

group morphology when they state,

" A long-standing problem of the kaolin group minerals has been the question: 'What geologic or geochemical environments determine whether well­crystallized kaolinite; b-axis disordered, 'fire-clay' mineral; kaolinite of hexagonal, elongate plate, tubular or other external morphology; endellite, halloysite, allophane, dickite of differing IR absorptions; or possible other varieties, are formed?' A corallary question asks 'is there a sequence, either possible or necessary, in either direction, between allophane, endell1te, kaolinite, dickite. . ?'"

In a discussion of the interrelationship of morphology

and chemistry, Bates (1959) cites the following factors

that determine the degree of curvature and therefore the

shape of the minerals. The first is the degree of misfit

between the tetrahedral and octahedral sheets which are

affected by the number and size of cations. The second is

the strength of the interlayer bond which is a product

of the size and polarizing power of the cations and the

distribution of H ions. The platy kaolinites are favored

over the lath or tubular materials as the H20 content

decreases and as the Si0 2 :Al 2o3 increases (as the number

of cations decreases).

Bates further postulates that there is a complete

morphological cycle in the kaolin group from the well­

crystallized hexagonal plates of kaolinite to elongate

plates, to laths with crystallographic terminations to

curved laths to tubes of halloysite (4H 20). A

halloysite-allophane transition has also been postulated

14

(Sudo and Takahashi, 1956). It is therefore possible that

a complete morphological series from allophane to

well-crystallized kaolinite exists.

In his discussion of soil clays Bramao (1952) notes

three morphological classes: (1) hexagonal plates, (2)

cylindrical or rod-like particles, and (3) irregular

layered particles having curved surfaces. This third

class exhibits x-ray and thermal properties of both

halloysite and kaolinite. The clay particles are

generally fine, have roughly hexagonal or elongate shape

with rounded edges, and a roughness of texture.

Bramao further summarizes the conditions under which

this irregular soil clay kaolin would form.

"The small particle size and evident poor crystallinity of much of the soil kaolin are results of the weathering conditions in soils. Soils are subject to wetting and drying cycles; a kaolinite crystal may begin to synthesize in one part of the cycle, and its growth may be interrupted or retarded during another part. The next increment of crystal growth might be more hydrous, or have a slightly different chemical composition and physical structure. Soil formation is characterized by the simultaneous presence or a large number of free ions and colloidal systems; the latter, particularly the hydrous oxides of aluminum and iron, may well

affect the development of clay mineral crystals. Where halloysite and kaolinite can grow undisturbed in an ideal environment, they can attain their characteristic euhedral forms. Where weathering conditions are dynamic and reflect the interplay of a host of variables, as in soils, perfect crystal formation would be only fortuitous."

Bramao further postulates that halloysite may be a

special form of kaolinite, one which has been deformed by

the presence of excess water molecules. He believes that

the poorly developed kaolin which forms in the above type

of environment is not necessarily a transitional crystal-

line form but one which, ". . may be an equilibrium

form peculiarly developed in a soil environment."

C. COMPACTION CHARACTERISTICS

The compaction of soils is affected by many factors

including such natural variables as mineralogy, gradation,

classification, moisture content, and mechanical variables

as type and intensity of compactive effort. This inves-

tigation proposes to study the effect of three of these

variables; soil gradation and index properties, cation­

exchange capacity, and clay-particle structure, on the

compaction characteristics of the Ozark soils. Corre-

lations are made of the interrelationships between these

factors and the compaction characteristics of the soils.

These characteristics are the maximum dry density and

15

16

optimum moisture content as defined by ASTM D 1557-66.

1. Soil gradation and index properties. The effect

of the gravel content of the soil (percentage of material

retained on the No. 4 sieve) has been discussed by several

authors. Holtz and Lewitz (1957) note that the compaction

of the fines is not affected if the soil contains less than

about 30% gravel. For soils containing from 30-50% gravel

there is some interference with the compaction of the fines.

As the plasticity of the fines increases, the soil is able

to tolerate a greater percentage of gravel before the com­

paction of the fines is affected.

Zeigler (1948) discusses the effect on the moisture­

density relationship which occurs when varying amounts of

gravel are added to a loamy sand. The addition of SO%

gravel (material finer than 3/4" and retained on the No. 4

sieve) increases the maximum dry density from 119.2 pcf

to 133.5 pcf and the optimum moisture content from 13.5%

to 7.5%. The trend of the increase approaches linearity.

Harris (1969) has conducted a detailed investigation

into the interrelationships between independent variables

(soil gradation, index properties) and dependent variables

(engineering properties as cohesion, angle of internal

friction, and compaction characteristics). The major

objection of his study was to develop predictive

relationships for evaluating the dependent variables.

Two recent studies noted by Harris concentrate on the

prediction of the moisture-density values of soils. Ring

et al (1962) conducted studies for the Bureau of Public

Roads. The first study produced curves relating the

liquid and plastic limits to the maximum dry density and

the optimum moisture content. A later study reported by

the same authors developed equations and curves relating

17

the plastic limit and fineness average (defined as one-sixth

of the summation of the percentage of particles finer by

weight than the following sizes in millimeters: 2.0,

0.42, 0.074, 0.020, 0.005, 0.001). It was found that the

values of optimum moisture and maximum dry density are

more closely predicted when related to plastic limit and

fineness average than when related to the plastic limit

and liquid limit. These studies utilize linear regression

to analyze the relationships.

Harris summarizes a report by the U.S. Army Engineer

Waterways Experiment Station (1962) which presents the

relationships between compaction, consolidation and

strength characteristics and the index properties of the

soils. The study develops correlations between index

properties and soil gradation, index properties and

specific gravity of the soils, and the index properties

and the compaction characteristics.

Harris (1969) concentrates his study to correlations

involving plastic fine-grained soils. He finds that the

compaction values are significantly related to the plas­

ticity indices and the percent clay. The liquid limit

provides the highest degree of simple correlation. A

very high degree of correlation was obtained for the

optimum moisture content versus maximum dry density.

His study indicates that a high degree of correlation

between the compaction characteristics and the liquid

limit holds also for residual soils. A lesser correlation

is noted with the plastic limit. The correlation of

compaction values with soil gradation is less significant.

For the glacial soils the gradation is more closely

correlated with the optimum moisture and maximum dry

density than with the index properties. The specific

gravity correlates poorly with other properties.

Few of the residual soils studied by Harris exhibit

18

the high percentage of clays, the high degree of plasticity,

or the low density characteristics typical of the soils

tested in this study of Ozark soils. It may well be that

the relationships determined by Harris will not hold for the

Ozark residual soils.

2. Cation-exchange capacity. That cations exdst in

the clay-water system and that they affect the properties

of the system has been known for some time. During the

18th century, it was determined that the process of cation-

exchange occurred and that the phenomenon was restricted

to the clay fraction of the soil (Grim, 1952). Other

19

early studies were carried out by investigators in the field

of soil chemistry.

Hauth and Davidson (1950) and Grim (1953) discuss

three methods by which clay minerals adsorb these cations.

In the first, cations are attracted to the edges of the

clay plates which hold a negative charge. The second

occurs as a result of substitution within the clay lattice.

Substitution of divalent ions for trivalent aluminum ions

results in a deficiency of positive charges which is

satisfied by cations which become strongly attached to the

clay particles. The third method involves the exchange

of the hydrogen in exposed hydroxyls by other cations.

The first method, while active in all clays, is responsible

for most of the exchange capacity of the kaolinite family

minerals. The platy kaolinite minerals which have a layer

of hydroxyls exposed along their basal cleavage surfaces

may also derive some of their exchange potential from

method three. The substitution of cations within the

clay lattice is most prevalent in the triple-layer minerals

where it is responsible for up to 80 percent of the total

cation-exchange capacity (Grim, 1953).

The exchange reaction in clay is very complex and as

of 1958 no one had been able to develop a qualitative

hypothesis which completely describes the reaction or the

sequence in which different cations would become involved

in the exchange reaction (Grim, 1958). As early as 1939,

Grim gave the following approximate order of cation

exchangeability; Na>K>NH 4>Mg>Ca. It appears that divalent

cations replace monovalent cations more readily than vice

versa. Other factors involved in the exchange reaction

include the total population of exchange positions, the

concentration of the replacing ions, the nature and

concentrations of the anions, the size and polarity of the

ions, and the hydration tendency of the ions (Grim, 1952).

20

Certain exchange relationships have been observed and

reported in the literature. Grim (1953), and a number of

other authors, report typical values of the cation-exchange

capacity of clay minerals:

CEC meq/100 gr.

Kaolinite 3 - 15

Halloysite zH 2o 5 - 10

Halloysite 4H 2o 40 - 50

Illite 10 - 40

Montmorillonite 80 - 150

Grim and Bray (1936) examine the properties of a number

of ceramic clays and showed that the cation-exchange capa­

city increased as particle size decreases. Harmon and

21

Fraulini (1940) studied the properties of a kaolinite as

a function of particle size. They note a pronounced

increase in the cation-exchange capacity, about four-fold,

as particle size decreased from 10-20 microns to less than

0.1 microns. The authors also devoted a portion of the

study to the relationship between cation-exchange capacity,

specific surface, and permeability showing an increase in

permeability with increasing cation-exchange capacity and

decreasing particle size.

Kelley and Jenny (1936) determined that the cation­

exchange capacity of clay minerals increased markedly upon

the breakdown in crystal structure caused by grinding.

Table I modified from Kelly and Jenny shows that the

cation-exchange capacity of a kaolinite increased from 8

to 100 meq/100 gr. as the mineral was ground for 7 days.

Data for other minerals are also included in the Table.

These authors postulate that upon grinding, many OH ions

of the kaolinite lattice become exposed as breaks are

produced across the octahedral layer or parallel thereto.

The increased exchange capacity is due to these exposures

of unsatisfied negative charges.

These studies seem to indicate that the cation-exchange

capacity is a more dominant factor in montmorillonites than

in kaolinites and halloysites, and as the clay particle

size and degree of crystallinity decrease the cation­

exchange capacity increases.

22

TABLE I

Affect of Crystal Structure on Cation-Exchange Capacity

(after Kelley and Jenny)

Minerals 100 Mesh Grinding Time

48 hr 72 hr 7 days

Muscovite 10. 5 . . . 76.0 . . . Biotite 3.0 62.0 72.5 . . . Kaolinite 8.0 57.5 70.4 100.5

Montmorillonite 126 I . . . 238 . . .

Baver (1930) shows that the divalent cation Mg and Ca

flocculate at much lower concentrations than Na and K

cations and that they produce a structure which is favorable

to the movement of water and air; a structure which is

relatively stable. Baver (1956) notes that, "The high

hydration and dispersive action of the Na ion makes the

plasticity of the Na-saturated soil greater than those

soils saturated with divalent ions."

Winterkorn and Moorman (1941) present data illustrating

the effect of different exchange ions on Atterberg Limits,

optimum moisture content and maximum dry density, total

consolidation and rate of consolidation, permeability, and

shear strength of compacted samples. Saturating the soils

with different cations also causes changes in the results

with different cations also causes changes in the results

of hydrometer particle size analysis showing the effect of

each cation on the flocculated or dispersed nature of the

clay particles.

23

Davidson and Sheeler (1952) relate the cation-exchange

capacity of loess in southwestern Iowa to certain engineer­

ing properties of the soil. At exchange capacities greater

than about 20 meq/100 gr. the curves relating CEC to

Atterberg Limits and percent clay appear to approach

linearity. At least a very strong correlation is established.

Along with these investigations on the nature of the

cation-exchange reaction and its affect on the engineering

properties of clay soils were investigations into the clay­

water system itself and how the cation affected the system.

Winterkorn (1940) describes the oriented water film

surrounding clay particles and how if affected the plasticity

indices.

Grim (1952 and 1958) has expanded this explanation.

The properties of the clay-water system are a function of:

(1) the bond between the particles, (2) the amount of

water between the particles, and (3) the nature of the

water adsorbed on the surfaces of the clay mineral

particles.

The bond between particles is dependent largely on the

cations held on the basal and edge surfaces of the clay

24

particles. The valence, geometric size, and tendency of

the ion to hydrate affect the bonding strength. The

geometric nature of this bonding restricts to a degree the

amount of water which can penetrate between particles. The

exchangeable ions also affect the configuration of the water

molecules that envelope the clay surfaces. The water for

some distance out from the surface is not a true liquid

since the molecules are probably arranged in a preferred

orientation different from that of liquid water. There is

an indication that the nature of the water molecule

orientation may vary with the exchangeable ion and the

thickness of the adsorbed water later.

The Na ions tend to develop thick surrounding layers

of oriented water whereas Ca and Mg ions develop only thin

layers; tens of molecular layers for the Na ion versus only

about four for the Ca and Mg ions. In addition there

appears to be no distinct boundary between the oriented and

liquid water systems when the Na ion is involved (Grim,

1958).

The "swarm" of water molecules and cations surrounding

the clay particles have been referred to as the double

layer. A decrease in the thickness of the double layer

causes a reduction in the electrical repulsion between clay

particles. Lambe (1960) has graphically illustrated the

effect of electrolytic concentration, ion valence, dielectric

25

constant, and temperature on the electrical potential of the

double layer system. The higher the ion concentration of

the pore fluid, the greater the particle-to-particle

attraction and the less diffuse the double layer. A similar

relationship exists as the valence of the ions in the pore

fluid increases.

Lambe and Martin (1960) note that the only exchangeable

ions likely to be important in soils are Na, K, Ca, Mg, Fe,

and Al and that of these Ca and Mg generally account for

50 to 90 percent of the exchangeable ions except on extremely

acid soils of humid regions.

Recently in the field of soils stabilization research

the effects of exchangeable cations have been extensively

studied and utilized. Vees and Winterkorn (1967) found that

the liquid and plastic limits of a kaolinitic soil increases

with the valence of the exchangeable ions and that this

indicates an increase in the flocculation effect of the

higher valence ions. The addition of lime to soils acts to

decrease the dry density and to increase the optimum

moisture content of compacted samples (Ladd et al, 1960).

The addition of 10 percent lime caused a drop in dry density

from 98 to 87 pcf for a heavy clay with a liquid limit of

60 and a plastic index of 20.

Lambe (1962) extends the results of earlier studies to

cover the general effects of the addition of aggregates and

26

dispersants to compaction samples. The aggregates produce

a strongly random structure which resists compaction effort

and results in a lowering of the maximum dry density and an

increase in the optimum molding water content. Dispersants

such as sodium tetraphosphate reduce the electrical

attraction between particles causing a decrease in cohesion.

This leads to a significant decrease in the liquid limit.

The repelled clay particles can be easily moved relative to

each other and may be molded into a dense mass by mechanical

compaction. The result is an increase in compaction with

the dispersed structure and a lowering of the optimum

moisture content.

3 • Clay particle structure. Lambe (1953) shows that

marine clays have a more flocculated structure than fresh­

water samples. His research also shows that remolded

samples have a more oriented (parallel) fabric. Mitchell

(1956) used a petrographic microscope to illustrate the

improved orientation of clay samples with remolding.

Lambe (1958) contributed a classic paper postulating

the effect of structure on compacted clay samples. In this

paper, Lambe reviews the factors which affect the structure

of natural soils. He also lists several variables which can

be altered by the engineer which will change the structure:

(1) type of compaction, (2) amount of compaction, (3) amount

of water, and (4) additives. Lambe concludes that: (1)

clays compacted dry of optimum owe their low density to a

flocculated structure; (2) this flocculated structure

results in part from a high electrolytic concentration of

ions with strong bonding capacity which prohibits the

development of a thick diffused double layer; and (3) wet

of optimum a dispersed structure is developed which allows

more efficient particle arrangement.

Seed and Chan (1959) conducted a number of tests on

clay samples compacted by different methods wet and dry of

optimum. They investigated and reported the effect of

27

particle arrangement or structure on sample shrinkage,

swelling, and total and effective strength characteristics.

The results of these tests when interpreted in light of

Lambe's theory substantiate his conclusions with regard to

particle structure. The authors also note the effect of

different methods of compaction. They found that the soils

which had undergone the greatest amount of shear strain

had the greater degree of particle orientation and a

lower shear strength.

In his discussion of the physico-chemical properties

of soils, Michaels (1959) reports the possibility of

"packets" of parallel clay particles. He believes the

packets act as "rigid solid entities" which resist attempts

at being forced into a coherent mass because the area of

contact between packets is so small. Relative to

28

individual clay particles, there are few points of attraction

(cohesion) between packets of compacted, dry clay.

Trollope and Chan (1960) discuss a mechanism whereby

packets are formed. They attribute the packets to a

strong electrolytic environment which forces particles to

move together. The authors contend that only in zones of

large shear strains are the particles reoriented and that

compacted clay soils which are generally considered to be

remolded are for the most part not remolded.

Alymore and Quirk (1962) used transmission microscopy

to study the natural structure of clay soils. They report

a "turbostatic" microstructure of clay particles.

"Turbostatic" structure refers to a twisted, swirl-like

clay particle arrangement similar to that noted by Borst

and Keller (1969) and discussed in a later section of this

paper. This type of structure is noted in natural clays,

particularly kaolinite and illite.

Sloan and Kell (1966) used transmission microscopy to

illustrate the structure of compacted kaolin samples. Their

study illustrates the predominance of packets of clay

particles in the compacted samples. Few individual clay

particles were noted. The packets appear to exhibit the

compacted arrangement (flocculated and dispersed) that

Lambe had postulated for single particles. The kaolin

compacted dry of optimum exhibited random packet orientation.

29

Zones affected by higher shear strains (as those close to

the top of each layer in a compacted sample) show greater

orientation. As water is added beyond that required for

optimum, greater packet orientation is observed. Sloan and

Kell further state:

"The addition of molding water in amounts less than that required to produce a slurry or viscous suspension would probably not disrupt the packets; hence persistence of the packets through the compaction process over the relatively limited moisture range in this study could be expected. The relative absence of individual particle edge-to-edge relationships would seem to support this view."

The investigation by Barden and Sides (1970) utilized

the scanning electron microscope to illustrate the compacted

structure of a clayey soil. The structure of the soil

compacted at one-half Standard Proctor compaction effort at

2.8% dry of optimum and 5.2% wet of optimum was investigated.

Their study indicates that at low to moderate magnification

(20-SOOX) the structure of the compacted samples appears to

vary appreciably depending on the molding moisture content.

Dry of optimum, distinct "pellet-like" macropeds were

predominant. Macropeds are packets or groupings of clay

particles. Wet of optimum the structure was more

homogeneous, offering little evidence of macropeds. At

higher magnification (1900-9500X) there was no marked

difference between the micrographs of samples compacted

wet and dry of optimum. This would indicate that the

intrapacket or microstructure of samples is not dependent

on the molding water content. Indeed, there appeared

30

to be little difference between high magnification

micrographs of the natural soils and those of the compacted

samples.

Barden and Sides postulate the following compaction

sequence. At low compaction, moisture, the macropeds appear

to resist deformation and macrospaces filled with air exist

between the macropeds. As more water is added the macropeds

become weaker and distort under compactive effort to reduce

and finally eliminate the macrospaces. At this point the

soil appears fairly homogeneous and the dry density is at

a maximum. The addition of more water causes a reduction

in the dry density as the water layers between soil

particles increases.

Obviously this explanation varies considerably from

that postulated by Lambe (1958) and Seed and Chan (1959)

where the change in particle orientation with change in

molding water content determines the compacted density.

To varying degrees Trollope and Chan (1960) and Sloan and

Kell (1966) had hinted at the compacted nature of clay

soils as outlined by Barden and Sides.

The significance of this "new" explanation of compacted

clay soils is evident. The theories of soil swelling,

shrinkage, consolidation, and shear strength of compacted

clays based on the Lambe (1958) theory must undergo some

re-examination and revision to allow for the presence and

influence of the pedular nature of the compacted samples.

31

32

III. FIELD INVESTIGATION

Sixteen Missouri Ozark earth dams were investigated.

Where possible soils were obtained from the borrow source

of the dams. Where this was not possible, soils from the

vicinity of the dams were sampled. Figure 2 shows the

locations of the dams investigated.

The physical parameters of the dams were determined with

a 100 ft. chain, an abney, and a Brunton compass. The

parameters determined were the width, height, length,

location of water level, and the dimensions of upstream and

downstream embankment slopes. The upstream slope values

are based on the angle of the slope above the reservoir

level. The exact location of the darns were spotted in the

field on U.S.G.S. Quadrangle sheets.

Early attempts to obtain moisture content and

undisturbed samples from the darns with agricultural probes

and small augers were abandoned when it became obvious

that the hand equipment was not adequate to sample the

stony embankment material.

The location of the principle source of embankment

material at each darn was generally apparent or was obtained

from someone in the vicinity of the site. At these sites

approximately 40 pounds of soil were obtained and placed

in a plastic sample bag.

Each darn was visually inspected to assess its per-

forrnance. Particular attention was given to evidence of

34

slope instability and seepage below, around, and through

the darns. The field investigation was completed during

the dry summer months of 1969 making seepage relatively

easy to locate and to differentiate from precipitation. An

attempt was made to determine from the owners which darns

were constructed with a cut-off trench.

The general characteristics of the soils and bedrock

were noted in the field and compared with geologic and

soils maps to determine the soil series and bedrock

geology at each site. Mr. James H. Williams, engineering

geologist with the Missouri Geological Survey, visited a

number of the sites with the investigator and was very

helpful in differentiating between the dolomitic

formations.

The bedrock formations, soil series, the darn parameters,

and a summary of the laboratory soils tests for each darn

site are presented in Appendix A as Darn Reports. A typical

cross-section or cross-sections for most of the darns are

also illustrated.

35

IV. MATERIALS

The soils investigated basically fit into three cat­

egories: (1) alluvial-colluvial soils, (2) residuals

developed on sandstones, and (3) residuals developed on

carbonate rocks. Table II outlines the geologic formations

and soil series present at each site. The Sunnen sample

is an alluvial deposit or reworked Gasconade clay residium.

The Masters #1 and Elsey soils appear to be colluvial

deposits also derived from Gasconade clay residium. The

Rice, Fabick, and Ft. Westside soils were developed all or

in part from the sandstones within the Roubidoux formation.

The remaining soils are residuals developed on the

Jefferson City, Gasconade, Eminence, and Potosi formations.

The clay residuals are classified as the Clarksville gravelly

or stony loams. The Hanceville loam and the Lebanon silt

loam are characteristic of the non-clay residuals.

An attempt was made to collect each sample from the

lower B and C horizon. Some, as the Sayers, Terre Du Lac,

and Sunrise Central were collected immediately above bed-

rock. Depth to bedrock at the other sites was not apparent.

The Clarksville cherty residium is the typical soil

developed on the carbonate bedrock of the Salem plateau.

The percent of chert in the soil is highly variable from

site to site and throughout the profile at any one site.

The surface and upper horizons often have a heavy

36

TABLE II

Materials of Dams Investigated

Soil (Dam) Location Bedrock Soil Series (county) Formation

Timberline St. Francois Potosi Clarksville gv.

Terre Du Lac St. Francois Potosi Clarksville gv.

Masters #1 Dent colluvial (?) Clarksville st. Gasconade

Masters #2 Dent Gasconade Clarksville st.

Sunrise South Jefferson Potosi Clarksville st.

Sunrise Cent. Jefferson Potosi Clarksville st.

Elsey Washington Gasconade Clarksville st.

Blackwell Dent Gasconade Clarksville st.

I Floyd Dent Gasconade Clarksville st.

Sayers Washington Potosi Clarksville st.

Hornsey Washington Eminence Clarksville st.

Sunnen Washington alluvial Clarksville st. Gasconade

Rice Crawford Roubidoux Lebanon slt. lm.

Fabick Dent Roubidoux Hanceville lm.

Ft. Westside Crawford Roubidoux (?) Lebanon slt. lm.

Lt. Prarie Phelps Jefferson Ct. Lebanon slt. lm.

37

accumulation of chert. Sloping surfaces accumulate chert

as fines are washed downslope. The Terre Du Lac and

Masters #2 samples contain almost no chert, whereas the

Blackwell and Floyd samples contain up to 50% chert. The

quartz druze (secondary crystalline quartz deposits)

typical o£ the Potosi formation was found in the Timberline

and Sunrise samples.

The clay residuals exhibit many similarities from

one location to another. They are generally deep red in

color~ an indication of high iron content. A high degree

o£ blocky to sub-angular structure is developed throughout

the profiles. The natural aggregate structural units of

soil particles are called peds. The peds occur from coarse

sand to gravel sizes. As a result of this structure which

exists throughout the profile, the natural soil deposits

are well-drained.

There are several factors related to the origin of the

soils which may have contributed to forming this pedular

structure. The formation of the soil is associated with

the solution and lowering of the bedrock level. This

lowering is accompanied by an adjustment (drop) in the

level of the residual mantle. This adjustment could

fracture the soil mass resulting in the ped structure.

The slicken-sided ped surfaces may reflect this movement.

The ped structure may also be the result of dessica-

tion. Later sections of this investigation will show that

38

the residual soils have rather high liquid limit values.

It was noted that the field moisture of the soils was

closer to the plastic limit than the liquid limit, Table III.

This is generally regarded as an indication of dessication.

The soils were formed ( and probably continue to be formed

at a reduced rate) in a humid warm climate.

Baver (1956) notes the specific effect on aggregate

formation caused by drying of the clay-soil mass. He

related the unequal strains developed in the soil caused by

non-uniform drying as a cause of "shrinkage" cracks which

form the peds. Wetting of the dried peds causes unequal

swelling which results in ped fragmentation and development

of smaller peds. Upon wetting, unequal air pressure in

the peds caused by capillary adsorption of water also acts

to break down the larger peds.

The iron may play an important role in prohibiting the

breakdown of the peds by both water and mechanical action.

Iron acts to "cement" the particles together and/or to

increase the cationic concentration and attraction between

particles.

The alluvial deposits do not exhibit well-developed

profiles. The residual clay structure has been modified

but not totally destroyed in most cases. As the residuals

were water-worked, some of the clay was lost and sand was

concentrated. The result is a deposit containing less

clay and more sand than the parent residuals.

TABLE III

Comparison of Natural Field Moisture

With Atterberg Limits

I Field Soil (Dam) LL PL Moisture

Fabick 25 16 17

Rice 27 15 14

Lt. Prarie 57 23 26

Masters #1 84 25 35

Masters #2 103 34 44

Floyd 85 35 38

39

40

V. TEST PROCEDURES

Tests on the Ozark soils were performed to determine

results in four general areas: (1) soil gradation and

Atterberg Limits, (2) compaction characteristics, (3) clay

mineralogy and (4) soil clay chemistry. The procedures

used to determine these values are presented in sections

essentially as outlined above.

A. SOIL GRADATION

1. Sample preparation. A portion of the field sample,

approximately 1 lb., was prepared for soil classification

tests essentially as directed in ASTM D421-58, Dry

Preparation of Soil Samples for Particle-Size Analysis and

Determination of Soil Constants. A Lancaster mixer was

used to break down the air-dried clay soil aggregates

after the stone portion, where size exceeded that of a No.

4 sieve, had been removed by hand. A mortar and pestle

was used to further pulverize the soil for particle-size

analysis (No. 10 sieve) and tests for soil index properties

(No. 40 sieve).

2. Coarse sieve analysis. The pedular structure of

the clayey residual soils investigated in this study does

not break down completely during dry or wet sieving.

Representative 500 gr. samples which passed the No. 4

sieve were presoaked for 24 hours in a 4% sodium

hexametaphosphate (Calgon) solution, mixed in a dispersion

41

cup, and washed through a No. 10, a No. 40, and a No. 60

sieve. The amount of the sample retained on each sieve

after oven drying was recorded and calculations made to

determine the amount finer than each of the sieves. These

values are recorded in Table IV.

3. Hydrometer analysis. Hydrometer analyses were

performed as recommended in ASTM D422-63 except that the

sedimentation cylinders were not placed in a constant

temperature bath during tests. Temperature corrections

were made later. After sedimentation, the samples were

passed through a No. 60 and a No. 200 sieve for comparison

with the hydrometer analysis.

The results of the particle-size analyses were plotted

on grain-size distribution charts which are presented in

Figures 3 - 8. The results are summarized in Table IV.

B. ATTERBERG LIMITS TESTS

1 . Liquid limits. Liquid limit test samples were

prepared and values determined in accordance to ASTM

D423-66 except that a Casagrande grooving tool was used.

Water was added to the pulverized samples until the soil

appeared to be slightly wet of liquid limit and then

allowed to age for 24 hours to allow water to be adsorbed

by the clay particles. The liquid limit tests were

performed wet to dry.

2. Wet liquid limits. Graham (1969) noted a sizeable

difference between the wet and air-dried liquid limit

42

values of a residual soil similar to the soils investigated

in this study. Several of the thesis soils were tested to

determine if a similar pattern was noted.

The wet liquid limit was determined by taking the soil

at field moisture, soaking it for 24 hours in distilled

water, mixing in a dispersion cup, and passing the mixture

through a No. 40 sieve. The prepared mixture was then

placed in a dish and allowed to air dry to a consistency

just wet of the liquid limit. The liquid limit was then

determined as previously. These values are reported along

with normal air dry values in Table V, and compared with

Graham's results for a similar soil.

3. Dispersed liquid limit. In another portion of

this study, samples were mixed with sodium hexametaphosphate,

a dispersant, prior to performing compaction tests. Small

portions of these air-dried samples were prepared and tested

to obtain Atterberg Limits as described in the previous

sections.

It was noted that the samples were particularly sen­

sitive to manipulation and that the liquid limit values

vary depending on how long the samples were manipulated

before testing. An attempt was made to be consistent in

preparing and mixing samples in each test, but it is

suggested that the values obtained are only approximate.

These values are reported in Table VI along with normal

air dry values for the same soils.

43

TABLE IV

Summary of Particle Size Analysis

PERCENT FINER

Soil (Darn) #10 #40 #60 #200 10]J 2]J l]J

Terre Du Lac 100.0 99.9 99.4 98 94 92 90

Hornsey 99.4 98.6 98.5 97 95 93 91

Timberline 99.5 94.8 91.2 85 80 79 78

Sunrise Cent. 98.9 94.9 93.4 92 87 83 82

Sunrise South 98.8 92.5 91.0 89 80 72 70

Sunnen 99.6 96.9 92.3 87 57 38 37

Elsey 99.2 97.6 96.0 94 86 71 69

Masters #1 100.0 99.8 99.6 96 83 76 71

Masters #2 100.0 99.6 99.4 99 99 95 94

Sayers 99.8 99.1 98.6 98 96 93 90

Blackwell 98.6 95.3 93.0 85 77 64 56

Ft. Westside 99.8 98.2 94.2 83 56 38 37

Rice 99.8 88.4 70.8 58 35 21 18

Fabick 99.6 94.0 78.0 61 38 19 16

Lt. Prarie 99.5 97.8 97.8 95 80 58 44

Floyd 99.3 98.0 98 98 97 87 83

Sieve Size

100 No. 4 No. 10 No. 40 No. 200 -

I' II I ---~ @ r---I I I ~----I I ~

80

I I I : ~ I I r------I I I I ~

+J ..c: bO

•rl <l)

:s: 60

I II I I

"' I I I I 0 ~ I u I L I I I I I I I I II l

:>, .0

I I I I I I 1

~ <l) ,::::

•rl 40 r.....

+J ,::::

I I I I I I I I I' I

I I I I I ~ I (!) u ~

~ 20 'I

I I I 1 Maste s #2

I I I I 2 Maste s #1

I I I I I u I I I

0

I I I I I I I

II - U.---~ - _j_ l 0 0 rl rl rl rl 0 rl . 0 0

rl 0 . 0 0

0

Particle Diameter in ~1illimeters ~ ~

FIGURE 3. Particle-Size Analysis of Masters #1 and Masters #2

100

80

+J .£.: bO

•rl Q)

~ 60 :>. .0

H Q)

s:: •rl 40 ~

+J s:: Q) u H ~ 20

0 0 0 rl

1

2

Terre

Timbe

Du l ac

line

0 rl

Sieve Size No. 4 No. 10 No. 40 No. 200

fT --r--........ I I ~ I

I I

I I ............... ~ : I l I ..__

I II I I I I I ! I I

I I I I ,! I ! I

I I ! I I I I I II

I I I I I I I !

II I I I I I I I

II I I I I I I I I

1l I I I II I I I I I T

II I I I I

I I rl rl

0

Particle Diameter in ~1illimeters

r-l 0

0

0

FIGURE 4. Particle-Size Analysis of Terre Du Lac and Timberline

0

r-l 0 0

0

.j:lo.

U'1

100

80

.f-1 ..c: bO

•r-l Q)

:3: 60 :>. ..0

~ Q)

s:: •r-l 40 r.....

.f-1 I:: Q) () ~

~ 20

0 0 0 r-1

Sieve Size No. 4 No. 10 No. 40 No. 200

I' I' --...... ~ -K I

I I ---r--..... It

"""""' II I I ~

~ r---...... 0 <D I I II I I I r----.::: -....... 'I II I I

0 ~

~ I I I I I ~ I I ~ I I I i ~ I I 1 I ' II II I I I

I

1\" I I I I ll

I I I I \ I I I I lj I

I 1 Sayer I I I I

jrie 11 I I I

2 Littl Pra I I I I II I I I 3 Black, ell I I I I I I lj I l ~ I I

_l _l

0 r-1 r-1 r-1 r-1

r-1 . 0 0

0 . 0 0 .

0

Particle Diameter in ~1illimeters

FIGURE 5. Particle-Size Analysis of Sayers, Little Prarie, and Blackwell .p. 0\

100

80

+' ..c: bO

•r-i (I)

3 60 :>. ..0

~ (I)

J:! •r-i 40 ~

+' J:! (I) {)

~

~ 20

0 0 0 ,..;

1

2

3

Floyd

Ft. W

Rice

stsi de

0 ,..;

Sieve Size No. 4 No. 10 No. 40 No. 200

I

I ~

" ~ I

I ,! "" I II

I 1\ ' l I ~ I I

II II

!\ I~

~ I I ! I I II I \ I I ! ~ I It II I I !

,.,.

~ "" I I

I " I I I ! I I I

11 I I I I I I I

'I I I I I I l I

II I I I I I I I I I I

I l II I ! ,..; ,..; .

0

Particle Diameter in ~1illirneters

~

1\ \ ~0

1\ (3)' ~

,..; 0

0

" "

~

Q"

'" -... "'

!'.......

!'--..

r---

,..; 0 0 . 0

FIGURE 6. Particle-Size Analysis of Floyd, Ft. Westside, and Rice

.j::. -....]

100

80

f.J ..c:: bO

•o-1 (l)

:3 60 :>,

..0

H (l)

s:: •o-1 40 ~

f.J s:: (l) {)

H ~ 20

0 0 0 rl

1 Sunri:

2 Sunrit

3 Fabid

No. 4 No. 10

Sieve Size No. 40 No. 200

II

I I I I I I I I I

! I ! I I

[I

e Ce ~tra : II

e So ~th I I

0 rl

I

: I

tl

r--.:: r-::: ~ I

I ~ : II

I i \ T-

~ I I I

II I \ I I I ! II I

I I ~ I I ! r---..!.. I I

I

"' I I I

I I I I I I .I I I I I

!I I I I I I I ! I I I I I I

I I I I I I

I I

rl rl

0

Particle Diameter in :1i llimeters

---..... .........___

' •0'

\ 0' "

rl 0

0

"

r--

~'---._

""

0

I'--

rl 0 0

0

FIGURE 7. Particle-Size Analysis of Sunrise Central, Sunrise South, and Fabick

~ 00

100

80

.f.J

.c: bO

•.-! Q)

:3 60 ~

..0

~ Q)

1=: •.-! 40 JJ...

.f.J 1=: Q) ()

~

~ 20

0 0 0 rl

1

2

3

Horns ~y

Elsey

Sunne~

FIGURE 8.

0 rl

Sieve Size No. 4 No. 10 No. 40 No. 200

'I II I

I I --- I

~ -I .....,._

r---. ""'" II

I I ........ H--I I ~ I I I I !I

I I I \ I I I

I I I

I I I I I I ! I I I

I I I I

I I I I I

I I I I I I I ! I I I I I I I I I

I I I I

I I I ! I I I I I II I I I I I I I

tl I I I II I I

rl rl

0

Particle Diameter in 11illimeters

0 ' \

\ ' 1\.

rl 0

0

"

~

~ (j)'

Particle-Size Analysis of Hornsey, Elsey, and Sunnen

G) ~

-

..___

r-1 0 0

0

... \.0

TABLE V

Comparison of Wet Liquid Limit And

Natural Atterberg Limits

% Change Soil (Dam) Wet LL LL PL in LL

Terre Du Lac 132 96 35 37

Hornsey 121 90 43 34

Sunnen 52 42 21 24

Springfield 144.8 105.6 34.0 37

* from Graham (1969)

TABLE VI

Comparison of Natural and Dispersed Atterberg Limits

Natural Dispersed

Soil (Dam) LL PL PI LL PL PI

Terre Du Lac 96 35 61 73 34 39

Floyd 85 35 50 55 28 27

50

I

51

TABLE VI I

Summary of Atterberg Limits Tests

% Soil (Dam) LL PL PI Clay

Timberline 69 30 39 79

Terre Du Lac 96 35 61 92

Masters #1 84 25 59 76

Masters #2 103 34 69 95

Sunrise South 68 30 38 72

Sunrise Central 70 33 37 83

Elsey 84 25 59 71

Blackwell 60 23 37 64

Floyd 85 35 so 87

Sayers 105 41 64 93

Hornsey 90 43 47 93

Sunnen 42 21 21 38

Rice 27 15 12 21

Fabick 25 16 9 19

Ft. Westside 48 21 27 38

Little Prarie 57 23 34 58

52

80

0 Clayey Residual Soils 0

D Sandy Residual Soils 0 60 0

"'"' ~ '--"

~ QJ

'"0 l=l

H

C) 0 ·r-l 0 +J (/)

Cll r-1 A< D

20

D D

0 0 20 40 60 80 100

Liquid Limit (%)

FIGURE 9. Plasticity Chart Plot of Ozark Soils

53

4. Plastic limits. Water was added to the powdered

samples until the approximate consistency of the plastic

limit was reached; the samples were then aged for 24 hours.

The plastic limit was determined in accordance with

ASTM D424-59, and the plasticity index calculated. The

Atterberg Limits for all soils investigated are reported

in Table VII. Figure 9 illustrated how these values plot

on the Plasticity Chart.

C. MOISTURE-DENSITY RELATIONSHIPS

1. Natural samples. Soils for compaction tests were

prepared and tested in accordance with ASTM D698-70,

Moisture-Density Relations of Soils Using 5.5-lb. Rammer

and 12-in. Drop. Method A in which all material larger

than the No. 4 sieve is discarded, was followed. After

mixing with an amount of water predetermined to produce the

desired moisture, the samples were aged 24 hours before

testing.

2. Dispersed samples. Approximately 20 to 25 lb.

samples of several soils were crushed to pass the No. 4

sieve. Each sample was soaked in a 4% solution of sodium

hexametaphosphate (Calgon). The mixture was stirred to

assure that all of the sample was wetted.

After 24 hours of soaking, the sample was further

worked by mixing in a dispersion cup. Additional distilled

water was required to dilute the mixture to a consistency

which could be handled by the dispersion apparatus. Each

54

TABLE VI I I

Result of Moisture-Density Tests

--Soil (Dam) Maximum Optimum

Dry Density Moisture (pcf) (%)

--Timberline 82 36

Terre Du Lac 79 37

Masters #1 84 25

Masters #2 81 36

Sunrise South 88 31

Sunrise Cent. 85 33 --

Elsey 89 26

Blackwell 92 24

Floyd 83 34

Sayers 74 42

Hornsey 77 38

Sunnen 108 18

Rice 121 13

Fabick 121 13

Ft. Westside 100 22

Lt. Prarie 94 27

Floyd - D 87 30 --

Sayers - D 75 35

T. D. Lac - D 80 33

Sunnen - D 107 17

55

portion of the sample was mixed until all lumps had disap­

peared, about 5 minutes. The dispersed mixture was then

placed in two, 2' by 2' pans to a depth of less than 1

inch.

The pans were placed before a 20 inch fan and a small

electric heater until the soil dried; generally 3 days

were required.

The dried soil was again crushed to pass a No. 4 sieve,

the moisture content determined, and the sample separated

into portions. Predetermined amounts of water were mixed

with each portion of soil to attain the desired moisture

content and the soil placed in plastic bags to age. After

24 hours the samples were compacted by a procedure identical

to that used for the standard moisture-density tests. The

results of all compaction tests are given in Table VIII.

Portions of the dispersed, dried, and crushed soil mixtures

were saved for Atterberg Limits testing.

D. X-RAY DIFFRACTION

1. General. A number of authors including Bragg

(1949), Brindley (1951), Grim (1953), and Bradley (1964)

discuss the basic principles of x-ray diffraction theory

and technique. The essence of these discussions are out­

lined by Schmidt (1965) where it is noted that clay mineral

analysis using x-ray diffraction is basically a determina­

tion of the thickness of a unit sheet of the mineral. The

angle of incidence at which reinforcement occurs is directly

related to the thickness of a monomolecular layer of the

Location of Machine

Geology Dept.

UMC

Geology Dept. UMR

TABLE IX

X-Ray Machine Specifications

Type of Time Delay Machine (seconds)

Norelco Wide-Angle 4

Diffractometer

General Electric 2 - 4

Model XRD-5

Counts per Second

100 - 200 i

1000 - 2000

U1 0\

57

mineral. The results of x-ray scanning are recorded on a

chart called a diffractogram which graphs twice the angle

of incidence of the x-ray against the magnitude of the count

of reflected x-rays.

For economic reasons, two x-ray machines were utilized

in this study. This is not ideal since analysis and

comparison of diffractograms from different machines is

difficult. Table IX gives pertinent data for the machines

used.

2. Preparation of samples. An attempt was made to

prepare sample slides using a procedure similar to that

described by Schmidt (1965) where 50 gram portions of soil

were soaked in distilled water for one week, mixed in a

dispersion cup, and sedimented in a 1000 ml. hydrometer

cylinder. Some samples flocculated and settled rapidly.

The supernatent water was poured off, fresh distilled water

added, and the sample sedimented again. After 3 cycles of

mixing with fresh distilled water had failed to disperse

these samples, 5 grams of sodium hexametaphosphate (Calgon)

had to be added to the mix for the samples to be success­

fully dispersed.

According to Stokes' Law, after 24 hours all particles

larger than 2 microns (all sand and silt) had settled out

of suspension and a portion of the clay fraction was

siphoned off and concentrated by evaporation. A few drops

of the concentrate was pipetted onto a 1" X 3" X 1 mm.

58

microscopic slide and dried before a heater. The clay

plates tend to orient themselves upon drying.

It was this tendency of the clay plates to so com­

pletely orient themselves which rendered the sedimentation

method unsatisfactory in this study. As shown in Brindley

(1951), Bramao (1952) and Grim (1953), the comparison and

identification of the kaolinite group minerals required

in part an analysis of the 020 peak which is not developed

in the oriented sedimented slides.

3. Powdered samples. Samples, pulverized to pass a

No. 200 sieve, were mixed with denatured alcohol before

being poured onto the 1n X 3" slides. As the alcohol

evaporated, a film of sample adhered to the slide. Best

results were obtained when a thin film of powder was pro­

duced. This was especially evident at low 8 angles where

a thick film placed the reflection surfaces inside the

focal plane of the scanner resulting in a scattering of

the x-ray.

Powdered samples also develop a preferential orienta­

tion due to their platy structure, but there is enough

random orientation to allow development of other peaks not

associated with the c-axis, including the 020 peak

required in analysis of the kaolin group (Figures 10 and 11).

4. Potassium acetate treatment. Halloysite (4H 20) 0

with a basal 001 spacing of about 10.0 A is known to 0

collapse to around 7.2 A as the soil is dried. Early

59

researchers thought this process was irreversible. Wada

(1961) showed the process was reversible and expanded the 0

kaolin group mineral lattice to 14.1 A using potassium

acetate. Upon washing with distilled water the kaolinites 0

collapsed back to 7.2 A whereas the halloysites collapsed 0

to about 10.1 A retaining a water molecule in the expanded

lattice. Miller and Keller (1963) refined the procedure

by using ethylene glycol which helps to retain the expanded 0

10.1 A lattice since ethylene glycol evaporates more

slowly than water.

In accordance with this method, with some modifica-

tions discussed with one of the authors C Keller, 1970),

1.5 grams of potassium acetate was mixed in a small mortar

and pestle with 2.0 grams of air-dried soil passing the

No. 200 sieve. This mixture was allowed to rest for 24

hours in a high humidity environment, after which it was

washed several times through filter paper with distilled

water. A final wash using a solution of equal portions of

distilled water and ethylene glycol was used. The washed

sample was diluted with ethylene glycol and placed on a

glass slide in a thin film. The slide was subjected to

x-ray scanning while the film was still moist. It is

noted that the specimens prepared in this manner remained

moist for longer than 24 hours.

The method of sample preparation used in this study

was tested to check its workability. A sample of pure

60

Georgia Kaolinite was diffracted to determine its base

pattern. Then a sample was x-rayed which had been treated

with potassium acetate and ethylene glycol as described 0

above. There was no shift in the 7.2 A peak indicating no

permanent lattice expansion of the reference kaolinite.

A sample of pure Indiana Halloysite was x-rayed along

with a treated sample, Figure 12 shows the results for

this reference mineral with a definite shift in the basal 0 0

001 peak from 7.2 A to 10.0 A for the treated sample. This

indicated the sample was halloysite and that the method

of sample preparation used in this study did produce the

expected results in the differentiation between control

specimens. The results of similar tests on some of the

Ozark soils are described and presented in a later section.

E. DIFFERENTIAL THERMAL ANALYSIS

1 . General. Differential thermal tests were performed

at the U.S. Bureau of Mines, Rolla, in two furnaces

designed to conform with the specifications outlined by

Berkelhamer (1944). Nickel specimen holders with a capacity

of approximately 0.5 grams were used with chromel-alumel

thermocouples, recommended for their sensitivity. A Leeds

and Northrup automatic programmer was used to control the

rate of heating, 12°C/min. A Leeds and Northrup multiple

thermal differential recorded of the automatic pen-and-ink

type recorded the curves.

61

Samples of Georgia Kaolinite and Indiana Halloysite

were tested to obtain reference curves. They are shown in

Figure 13. Grim and Rowland (1942) show a number of curves

for various clay minerals which can be used for comparison

with test curves of the Ozark residual soils.

2 . Sample preparation and testing. Specimens were

prepared for DTA by sieving a sample of air-dried soil

through a No. 200 sieve. Mackenzie (1957) notes that

sieve size has little influence on the curves but that

the sample should be fairly fine (100 - 200 mesh) to

insure good packing of the specimens.

The nature of the low temperature peak system is

dependent to a degree upon humidity variations, therefore,

the use of air dried samples may result in erroneous low

temperature peaks (Mackenzie, 1957). Similarly, using

samples which have been oven-dried at about 100°C may lead

to the eradication of the low temperature peaks altogether.

Mackenzie suggests that samples be equilibrated over a sat­

urated solution of Mg(N0 3 )·6H 20 in a dessicator for

several days. This procedure standardizes the moisture

content of the test samples. Eades (1970) suggests that

the procedure while important for the triple-layer minerals

is not required for the kaolinite group minerals. The

samples tested in this study were not pretreated as

described above.

Where small or very reactive samples are tested, they

62

TABLE X

Summary of Major DTA Temperature Peaks

Peak Temperatures (OC)

Low Major Soil (Dam) Endothermic Endothermic Exothermic

--Masters #1 100 560 minor ?

Masters #2 120 550 925

Sunnen 90 ? 545 905

Terre Du Lac 115 560 925

Sunrise South 120 550 920

Sayers 120 545 915

Blackwell 110 535 minor ?

Timberline (1) 118 555 916

Timberline (2) 120 555 915

Timberline - leached 120 540 945

Hornsey 105 ? 550 915

Hornsey - leached 128 562 930

Elsey (1) 125 540 920

Elsey (2) 110 545 920

Floyd 110 560 930

Floyd oven dried 3 no peak 530 935 -hr. 700C at

Indiana Halloysite 120 580 973

same - oven dried 12 135 595 987 hr. at 70°C

Georgia Kaolinite (1) no peak 605 966

Georgia Kaolinite (2) no peak 610 970

63

are often mixed with an inert material such as calcined

kaolinite or aluminum which has been ground to a particle

size which approaches that of the sample. Base line drift

and sample shrinkage can often be corrected with this

procedure. The DTA base line is a horizontal line along

which the curve should return after recording each

endothermic and exothermic reaction. A disadvantage of

mixtures with inert materials is that they effect the

areas under the peaks which distorts quantitative

determinations. Samples tested in this study were not

mixed with inert material.

Some base line drift was encountered in early tests,

Figure 14, but this was corrected by packing the samples

more firmly in the specimen holder. Factors such as

heating rate, size and construction of specimen holders,

and the degree of packing can radically alter the resulting

DTA curves. Consistency of technique is the key to

obtaining curves which can be compared and analyzed.

Figures 14 thru 17 show DTA curves for a number of the

Ozark soils. Table X summarizes the temperatures of the

important reactions.

F. THERMOGRAVIMETRIC ANALYSIS

Portions of the minus 200 mesh samples prepared for

DTA were saved for thermogravimetric analysis, TGA. A

Ugine-Eyraud Model B-60 Automatic Recording Balance and

furnace were used. The heating rate, 10°C/min., was

64

programmed by a Bristol's Model 565 Round-Chart Dynamaster

Pyrometer. Test results were recorded by a Bristol's

Model 760 Strip-Chart Dynamaster. The equipment and method

of testing is discussed at length in Duval (1963).

One hundred mg. samples of the powder were placed in

the sample holder in the furnace. The balance was zeroed

and the sample heated to approximately 50°C which temper-

ature was held until there was no further noticeable weight

loss. It is believed that most of the hygroscopic moisture

is expelled in this manner. A heating process was utilized

0 in which the temperature was raised in steps of about 50 C

and held until the weight was stabilized. The tests were

terminated at 1000°C,

The data has been transformed to dehydration curves.

Curves for the standard minerals, Georgia Kaolinite and

Indiana Halloysite, were determined, converted to dehydra­

tion curves, and plotted along with the curves for several

of the Ozark soils in Figure 18.

G. TRANSMISSION ELECTRON MICROSCOPY (TEM)

A Hitachi Model HU-llA transmission electron microscope

was used to study the size and shape of clay particles of

several soils in this investigation. Both powdered and

colloidal suspension specimens were prepared for analysis.

The major reference for transmission microscopy is an

extensive study performed for the American Petroleum

Institute (Davis et al, 1950). Later studies by Bates and

and Cromer (1955), Brindley and Cromer (1956), and Bates

and Cromer (1959) concentrate on applying transmission

microscopy in determining the morphology of the kaolin

group minerals.

65

A thin carbon film was evaporated (sputtered) onto

glass slides in a vacuum chamber. The powdered sample

(finer than 200 mesh) was dusted onto the film which was

then floated off of the glass slide in a beaker of water.

An electron microscope grid was used to lift the carbon

film with sample from the beaker and mount the specimen in

the microscope. The magnified image of the particles so

mounted was projected onto a screen for viewing and glass

plate photographic slides were obtained.

The 200 mesh powder specimens produced images of

aggregates of clay particles rather than of individual

particles. These were difficult to analyze for particle

parameters such as size and shape.

Soils which had never been air-dried were suspended

in distilled water for a week before testing. They were

agitated often to separate the particles. Before testing,

the suspension was again agitated and a drop of the mixture

placed on the floated carbon film. The sample was then

mounted as before. This method of sample preparation

resulted in a much better segregation of the particles.

Photographs taken of the soil particles when utilizing this

method of sample preparation are presented in Figures 19-22.

66

H. SCANNING ELECTRON MICROSCOPY (SEM)

The scanning electron microscopic investigation was

conducted at the Materials Research Center, University of

Missouri - Rolla. A JEOLCO (Japan Electron Optics Labora­

tory Company, Ltd.) Scanning Type Electron Microscope,

Model JSM-2 was used. Samples were mounted on copper

disks, placed in a vacuum and subjected to electron

scanning. Micrographs were taken with a mounted Polaroid

camera.

Initially, specimens were prepared by mounting air­

dried pulverized minus 200 mesh samples on the copper disk

with silver paint. Figures 23 and 24 present several

micrographs taken from this portion of the study.

Borst and Keller (1969) present a technique of

mounting samples for scanning with a minimum of sample

disturbance. Air-dried peds were broken to expose a

fresh surface. These chips, about 1 em. by 1 em., were

mounted with silver paint on the disks and coated with a

thin film of gold in a vacuum chamher. The specimens were

then exposed to scanning. Micrographs resulting from this

portion of the study are presented in Figures 25 thru 29.

Compacted clay samples were also analyzed. Chips

with fresh surfaces, as described above, were prepared for

testing. These chips were mounted to expose to scanning

planes oriented perpendicular to and parallel to the dir­

ection of applied compactive effort. Micrographs of this

Name of Lake

Analysis

Si0 2 Al 2o3 Fe 2o3 Ti0 2 MnO

CaO

MgO

Na 2o K20

Ignition Loss

- H2o 105°C

+ H20 1000°C

HCl Insol. Residue

HCl Soluble Si0 2 HCl Soluble Al 2o3 HCl Soluble Fe 2o3 Oxides of Al, Fe,

Ti, Mn, P.

Totals

TABLE XI

Chemical Analysis of Ozark Soils

U.S. Bureau of Standards Sample #98

Plastic Clay

59.11

25.54

2. OS

1. 43

0.005

0.21

0. 72

0. 2 8

3.17

7.28

M.G.S. Lab Analysis S amp 1 e # 9 8

Plastic Clay

57.90

27.28

2.33

1. 03

0.16

0.70

0.35

2.40

8.17

0.84 7.33

83.72

0.71

5.36

1. 04

30.64

100.32

Blackwell

%

50.40

24.48

6.81

0.46 --- --

0.50

1. 60

1. 97

1.15

12.18

3.93 8. 2 5

-----

---- -

--- --

7.11

31.60 0\ '-]

99.40

TABLE XI - continued

Name of Lake Sayers Sunnen Sunrise South

Analysis % 0 0 ~0 'o

Si02 40.86 53.06 41.04 Al 2o3 27.06 23.53 27.97 Fe 2o3 9.99 7.84 11. 49 Ti0 2 0.43 0. 71 0.46 MnO - -- -- ----- - -- - -

CaO 0.46 0.18 0.38 MgO 2.20 1.10 1. 31 Na2o 0.23 0.20 0. 13 K20 0.94 1.14 0. 7 2. Ignition Loss 17.96 12. 51 16. 55

- H 0 2 105°C 7.04 4.97 6.36 + H20 1000°C 10.92 7.54 10.19

HCl Insol. Residue 41. 52 ----- -----

HCl Soluble Si0 2 0.79 ----- - ----

HCl Soluble A1 2o3 25.57 ----- -----

HCl Soluble Fe 2o3 9.98 7.59 11.18

Oxides of Al, Fe, 37.48 32.08 39.92 Ti, Mn, P.

0\

Totals 100.13 100.27 100.05 00

TABLE XI - continued

Name of Lake Timberline Terre du Lac Hornsey

Analysis % % !!: 0

Si0 2 42.04 42.6 8 42.32 A1 2o3 28.08 28.60 29.21 Fe2o3 9.99 10.16 8.33 Ti0 2 0.51 0.46 0.36 MnO ----- ----- -----GaO 0.4.8 0.40 0.40 MgO 1. 30 1. 07 1. 61 Na2o 0.13 0.18 0.13 K2o 1. 03 0.65 0.87 Ignition Loss 16.13 16.05 16.73

- H 0 2 105°C 5.59 5.73 6.03 + H20 1000°C 10.54 10.32 10.70

HCl Insol. Residue ----- 45.20 43.11 HCl Soluble Si0 2 ----- 0.75 0.87 HCl Soluble Al 2o3 ----- 26.47 27.56 HCl Soluble Fe 2o3 10.06 10.47 8.91 Oxides of Al, Fe, 38.58 39.22 37.90

Ti, Mn, P. (]\

\.0

Totals 99.69 100.20 99.93

TABLE XI - continued

Name of Lake Floyd Masters #1 Elsey

Analysis % % ~ 0

Si0 2 52.20 56.88 50.68 Al 2o3 24.24 21.17 22.76 Fe 2o3 7.16 6.16 7.42 Ti0 2 0.46 0.41 0.46 MnO ----- ----- -----

CaO 0.10 0.37 0.42 MgO 1. 2 7 1. 58 2.15 Na2o 0.13 0.13 0.23 K20 1. 30 1. 20 1. 33 Ignition Loss 11.96 12.44 15.08

- H 0 2 105°C 3.38 4.81 6.44 + H20 1000°C 8.58 7.63 8.64

HCl Insol. Residue ----- ----------

HC1 Soluble Si0 2 ----- ----- -----

HCl Soluble Al 2o3 ----- ----- -----

HCl Soluble Fe 2o3 7.15 6.15 6.95

Oxides of Al, Fe, 31.86 27.74 30.64 Ti, Mn, P.

"'-J

Totals 98.66 100.30 100.45 0

TABLE XI - continued

Names of Lake Sunrise Central Masters #2

Analysis % %

Si02 40.96 46.30 Al 2o3 29.44 24.68 Fe2o3 10.41 9.66 Ti0 2 0.41 0.36 MnO ----- -----CaO 0.52 0.64 MgO 1. 38 1. 77 Na2o 0.13 0.16 K2o 0.73 1. 00 Ignition Loss 16.29 16.56 - H 0 2 105°C 5.08 6.79 + H20 1000°C 11.21 9.77

HCl Insol. Residue ----- -----HCl Soluble Si0 2 ----- -----HCl Soluble Al 2o3 ----- -----HCl Soluble Fe 2o3 10.38 8.78 Oxides of Al, Fe, 40.26 34.70

Ti, Mn, P. '-I

"'"' Totals 100.28 101.17

72

portion of the study are presented in Figures 48, 49, and SO.

I. LOW-POWER MICROSCOPY (LPM)

A low-power (10-SOX) microscope study of the compacted

samples was conducted at the U.S. Bureau of Mines, Rolla,

Missouri. Micrographs were taken at 17X both in black-and­

white and in color of samples of Terre Du Lac compacted

3% dry of optimum and 4.5% wet of optimum. Micrographs

were taken with a Polaroid MP-3 Land Camera adapted to

accept Bausch and Lomb lenses. A 72 mm lense was used.

These micrographs are presented in Figures 46 and 47.

J. SOIL CLAY CHEMISTRY

1. General. All samples tested for chemical

properties were first air-dried and passed through a No. 4

sieve. Where further preparation was required for specific

tests, it will be noted in the discussion.

2 . Chemical analysis. In general, methods of chemical

analysis as outlined by Scott (1948), Standard Methods of

Chemical Analysis, were followed. All tests were performed

on the clay fraction of the soils and major tests are out-

lined below with results presented in Table XI.

a. Si0 2 - gravimetric. Clay is fused with sodium car-

bonate (Na 2co 3), taken up in dilute hydrochloric

acid, dehydrated, filtered, ignited and silica

volatilized with hydroflouric acid. (Scott,

p. 797-801)

73

b. Al 20 3 - gravimetric. filtrate from Si0 2 is used.

Ammonium hydroxide is added to precipitate hydro­

xides of Al, Fe, Ti, etc. Al 2o 3 is calculated

by difference after determination of Fe 2o 3 ,

Ti0 2 , P2o5 , and MnO.

c. Fe 2o 3 - volumetric. Oxides are fused with potas­

sium acid sulfate (KHS0 4), taken up in dilute

sulfuric acid (H 2so 4), reduced with test lead,

and titrated with potassium permanganate.

(Scott, p. 470)

d. Tio 2 - colorimetric. Determination of titanium

with hydrogen peroxide. (Scott, p. 987)

e. CaO - volumetric. Oxalate is added to filtrate

from precipitation of Al, Fe, hydroxides, etc.

forming a precipitate of calcium oxalate - dissolved

in dilute H2so 4 and titrated with potassium

p erma n g an ate . ( S cot t , p . 21 0 )

f. MgO - gravimetric. Ammonium acid phosphate

(NH 4) 2HP0 4 is added to filtrate of calcium oxalate

precipitation - forms precipitate which is ignited

to form magnesium pyrophosphate from which MgO

is calculated. (Scott, p. 532)

3. Soil pH in water. Various soil-water ratios have

been used in pH determinations with a pH increase noted as

the soil-water ratio decreases. As recommended by Peech

(1965) in Methods of Soil Analysis a 1:1 ratio was used in

I

TABLE XI I

Summary of pH and Cation-Exchange

Capacity of Ozark Soils

Soil (Darn) pH CEC (rneq/100 gr)

Timberline 5.1 27.8

Terre Du Lac 7.1 27.9

Masters #1 5.4 21.9

Masters #2 7.5 35.8

Sunrise South 6.5 24.6

Sunrise Central 4.9 30.6

Elsey 7. 7 26.9

Blackwell 7.5 24.1

Sayers 7. 5 44.9

Hornsey 4.8 42.1

Sunnen 4.9 11.5

Rice 5.2 8.7

Fabick 5.6 7.6

Ft. Westside 4.6 19.1

Little Prarie 7.8 13.7

Floyd --- ----

74

Si02/Al 20 3

2.55

2.53

4.57

3.20

2.52

2.38

3.79

3.50

2.56

2.46

3.82

----

----

----

----

3.66

75

this study. Twenty grams of soil were added to 20 grams of

distilled water, stirred for several minutes, and allowed

to sit for one hour. A Corning Model 12 Research pH Meter

with a glass electrode was used to measure the pH. Two

readings were taken and their average recorded in Table XII.

4. Cation-exchange capacity. The cation-exchange

capacity, CEC, was determined essentially as outlined by

Chapman (1965). The method utilizing ammonium acetate to

saturate the sample was used.

Two hundred ml. of 1 N ammonium acetate were filtered

through 10 grams of soil placed in a Gooch crucible over a

500 ml. Erlenmeyer flask. The leachate was saved for fur-

ther analysis. The soil was then filtered with 100 ml. of

ethyl alcohol to wash out the excess ammonium acetate.

The leached soil was then placed in a Kjeldahl flask

with about 30 grams of magnesium oxide, a catalyst, and 200

ml. of distilled water and boiled for distillation. Fifty

ml. of 4% boric acid was mixed with 150 ml. of the distillate

with the mixture then titrated with .1 N hydrochloric

acid. The amount of acid in ml. required to reach the

end point is noted and recorded as the value of the

cation-exchange capacity in meq/100 grams. Two samples

of each soil were tested, the results averaged and

reported in Table XII.

5. Flame photometry. Na+ and K+ were determined by

use of a Coleman Flame Photometer with a Coleman Electric

TABLE XIII

Concentration of Mg, Ca, Na

and K Cations in meq/100 grams

Soil (Dam) Mg++ Ca++ K+

Timberline 9.3 10.1 0.50

Terre Du Lac 10.1 12.2 0.40

Masters #1 11.7 5.8 0.36

Masters #2 20.6 11.6 0.76

Sunrise South 11.0 9.4 0.48

Sunrise Cent. 9.3 9.0 0.75

Elsey 21.3 6.5 0.79

Blackwell 14.6 13.6 0.60

Sayers 34.3 12.5 0.71

Hornsey 13.5 10.8 0.90

Sunnen 2. 8 1.4 0.45

Rice 1.4 5.1 0.31

Fabick 1.8 2.7 0.20

Ft. Westside 3.6 4.0 0.42

Lt. Prarie 7. 7 15.3 0.38

76

Na +

0.40

0.90

0.39

1. 50

0.66

0.46

0.41

0.30

1.15

0.41

0.20

0.19

0.21

0.22

0.68

77

Colorimeter. The theory is explained in the article by

Rich (1965) in Methods of Soil Analysis.

The leachate from the CEC determination was placed in

a 250 ml. volumetric flask and brought to volume with the

addition of ammonium acetate. Standard solutions contain-

. k fN+ d + .. lng nown amounts o a an K ln ammonlum acetate were

tested and the results used to construct graphs of colori-

meter readings versus ion concentration of meq/100 gr. of

soil. Two samples of each soil were then tested for each

ion, correlated with the graphs to determine concentration,

the values averaged, and reported in Table XIII.

6. Absorption spectrophotometry. The leachate from

the CEC determination was also used in the determination of

++ ++ Mg and Ca . Five ml. of the leachate was placed in a

50 ml. volumetric flask and brought to volume with 1000

ppm. lanthanum. A Jarrell-Ash Atomic Absorption Flame

Emission Spectrophotometer was used to analyze the samples.

Standard solutions of Mg++ and Ca++ were tested to construct

graphs relating the cation concentrations and the spectra-

photometer values. Two samples of each soil were tested,

the values averaged, and reported in Table XI I I. This

method of testing is described by Prince (1965) in Methods

of Soil Analysis.

K. SPECIFIC GRAVITY

Specific gravity tests were performed essentially as

outlined by ASTM D854-58 (1965). The results of testing

78

TABLE XIV

Specific Gravity of Ozark Soils

Soil (Dam) Specific Gravity

Fabick 2.68

Rice 2.70

Ft. Westside 2. 7 2 ' 2.72

Sunnen I 2. 7 2' 2.73

Blackwell 2.74

Lt. Prarie 2.77

Elsey 2.79

Floyd 2. 8 0' 2.80

Sunrise Cent. 2.82

Sunrise South 2. 8 2

Terre Du Lac 2.82

Timberline 2.83

Masters #1 2.83

Masters #2 2.84

Sayers 2.84

Hornsey 2.84, 2.84

79

are presented in Table XIV. The dessicated nature of the

samples required some special procedures to be followed

to assure sample dispersion. The samples tested were air­

dried. Two samples identical to the one tested were oven-

dried for 24 hours at 105°C. The average moisture content

for the two samples was calculated and used as the moisture

content for the tested sample.

The samples were soaked for longer than 24 hours in

distilled water before testing. The method of air

removal by boiling the sample for 10 minutes was followed.

As Table XIV indicates, several soils were tested twice

and reproductive results were obtained~

L. CORRELATION TESTS

Data to be correlated was analyzed by a computer

program written by Capt. W. Vogel, U.S. Army Corps of

Engineers, a graduate student in Civil Engineering at the

University of Missouri - Rolla. A P-PLOT option was

implemented to plot the data and curves developed by the

analysis. A least squares polynomial of the form:

Y = A(O) + A(l)X + A(2)X 2 + •.• + A(N)XN was used to

analyze the data and to evaluate A(O), A(l), ... A(N).

Two values, sigma (a) and the correlation coefficient

(r) were used to evaluate the curve fit where:

where: x = X - X

y = y - y

TABLE XV

Correlations for Clayey Residual

Ozark Soils

x- axis y-axis Sigma Correlation Coordinate Coordinate (a) (r)

Plastic Limit Optimum Moist. 7. 9 0.92

Liquid Limit Optimum Moist. 10.6 0.90

Cation-Exc. Cap. Optimum Moist. 14.3 0.86

% Clay Optimum Moist. I 9.7 0.90

9-D Clay* Optimum Moist. 8.8 0.95

Plastic Limit Max. Dry Density 8.1 -0.89

Liquid Limit Max. Dry Density 19.2 -0.88

Cation-Exc. Cap. Max. Dry Density 23.0 - 0. 8 7

9-0 Clay Max. Dry Density 5.9 -0.96

% Clay* Max. Dry Density 10.9 -0.97

Optimum Moist. Max. Dry Density 15.1 0.90

Cation-Exc. Cap. * % Clay 155 0.88

Cation Exc. Cap. Plastic Limit 9. 2 0.91

Cation Exc. Cap. Liquid Limit 139 0.81

% Clay Plastic Limit 13.4 0.87

% Clay Liquid Limit 61.1 0.95

80

Coef.

------

*Correlations include values for sandy residual soils

and,

a =

2 E(y - Ycalc)

N - k - 1

where:

81

N = no. of data points

k = degree of polynomial

Ycalc = calculated y value for a given x value

The correlation curves resulting from this analysis

were plotted and presented as Figures 30 thru 45 along

with the values of sigma (cr) and the correlation

coefficient (r). These values are summarized in Table

XV.

The correlation coefficient, r, has a range in values

from -1.0 to +1.0. Perfect correlation is demonstrated

where r = ±1.0. Sigma (cr) is a common statistic used in

the earth sciences to express the summation of deviations

of data from a curve fitted through that data. The value

of sigma which indicates a significant relationship depends

on the order of magnitude of values being correlated.

82

VI. ANALYSIS OF RESULTS

A. CLAY MINERALOGY

The mineralogy of the residual soils will be discussed

in sections corresponding to the method of testing. No

method of testing in itself produced definitive data on

which to identify the clay mineralogy of the soils, but

when they are considered along with the probable environ-

ment of soil formation, a clear picture of the mineralogy

is developed.

1. X-ray analysis. Several x-ray diffractograms of

the soils investigated in this study are shown in Figures 10

and 11. Powder slides were x-rayed to produce the diffracto-

grams.

The major peaks shown on these diffractograms are

0 0 located at the following 28 angles: 12.0-12.4 , 20.0 , 0

21.0°, 25.0-25.4°, and 26.7°. The peaks at 21.0° (4.26 A) 0

and 26.7° (3.34 A) are quartz peaks. The 12.0-12.4° 0 0

(7.15± A) and 25.0-25.4° (2.54± A) peaks represent basal 0

001 and 002 kaolinite reflections and the peak at 20.0 0

(4.45± A) represents the 020 kaolinite mineral reflection.

The reflections which occur for some soils at 20 angles of 0 0

24°± (3.71 A) and 33°± (2.72 A) appear to represent the

021 and 022 reflections of the same group. 0

The reflections which occur at 10± A (Masters #1 and

Floyd) are probably basal illite peaks whereas those in the

83

0

area of 13.4-15± A (Timberline, Terre DuLac, etc.)

probably represent chlorite or montmorillonite group

minerals in the soil. The weak peaks indicate that only

minor amounts of these minerals are present.

The apparent major constituent of the soils studied,

based on the spacing~ magnitude and size of the reflection;

is a mineral of the kaolin family, probably halloysite or

kaolinite. Brindley (1961) describes the x-ray character-

istics of each in detail. In attempts to distinguish

between the two~ he used the relative intensity of the 0

basal 001 peak and those near 4.4 A, the 020 reflection.

For kaolinites, the usual situation is for the magnitude

of the 001 reflection to be twice that of the 020 reflection.

For poorly crystallized kaolinites, the reflections may be

more nearly equal; for halloysite the 020 reflection is

usually greater than that of the 001 reflection (Figure 10) .

Bramao et al (1952) compares the 002 and 020 reflec­

tions. Where the intensity of the 002 peak is greater

than that of the 020 peak, kaolinite is indicated; where

the intensity of the 020 peak exceeds that of the 002 peak,

halloysite is predominant. In the diffractograms of the

residual soils studied in this investigation, the 020 peak

intensity exceeds that of both the 001 and 002 basal peaks;

therefore, halloysite is indicated. The broadness of the

basal 001 and 002 peaks is also a characteristic of hal­

loysites (Grim, 1953).

84

Several features of the x~rays indicate that halley~

site may not be the major clay constituent of the Ozark

soils. The 001 peak for most of the samples occurs between 0

7.0 and 7.2 A. This peak is generally located between 0 0

7.35 and 7.5 A for halloysites versus 7.15 A for kaolinites,

even poorly crystallized kaolinites.

Tests of several samples treated with potassium acetate

and ethylene glycol, as recommended by Miller and Keller

(1963), indicate no permanent expansion of the crystal

lattice from the area of the 001 peak at 7.2 A. Figure 12

illustrates the results of these tests. This indicates

that halloysite is not a major constituent of these

samples.

Grim (1953) discusses three factors which affect the

diffractograms of the kaolin minerals. The first is the

effect of displacement of the unit sheets with respect

to each other, particularly in the a and b~axis directions.

The displacement results in broad diffraction patterns

rather than sharp peaks. Secondly, a particular kaolin

mineral may be interlayered with another kaolin mineral or

a number of other clay minerals. Weakened and displaced

peaks result. Finally he notes that the shape and size

of particles affect the diffractograms.

Brindley (1961) discusses the affects of b~axis

disordered kaolinites (similar to the kaolinite pM of

Mackenzie, 1957) on x~ray patterns. He states that the

85

Treated with Potassium Acetate

Untreated

002

30 26 24 22 20 18 16 14 12 10 8 6

2 8 in Degrees

FIGURE 10. X-Ray Diffractograms of the Sayers Soil

28

Masters Ill

Timberline

Terre Du Lac

24 22 14

2 8 in Degrees

FIGURE 11. X-Ray Diffractograms of the Masters #1,

Timberline, and Terre Du Lac

86

26

Shift in

Kaolinite Treated with

Potassium Acetate

Untreated Georgia Kaolinite

24 22 20 18 l6 14 12 10 8

2 6 in Degrees

FIGURE 12. Shift in 001 Peak of Georgia Kaolinite

When Treated With Potassium Acetate

87

6

88

only visible effect of this disordering is the strengthening

of the 020 diffraction band and a sharp low-angle termin­

ation of that peak. These features are evident in the

diffractograms of most of the soils tested in this study,

including the Sayers soil, Figure 10.

Brindley and Robinson (1947) illustrate broadening

and lowering of intensity of peaks with a decrease in cry­

stallinity. Murray and Lyons (1956) present data to sub­

stantiate this effect of degree of crystallinity. They

also demonstrate that particle size varies directly with

the degree of crystallinity, larger particles being better

crystallized.

Conflicting data for the special case of a b-axis

disordered kaolinite are presented in Robertson et al

(1954). This kaolinite exhibits very good crystallinity

even with very fine particle size, on the order of 0.2

microns. The low intensity and broad peaks of the

diffractograms are the result of fine particle size, not

of poor crystallinity. It would appear that in most

soils, both decreasing clay mineral particle size and

degree of crystallinity act to broaden and weaken the

reflections of x-ray peaks.

The residual soil x-rayed in this study shows a

marked degree of asymmetry of the 001 peak sloped to the

low-angle side. Keller (1968), in a study of flint clays

which shows similar patterns, attributes this feature to

89

mixed layering of the kaolinite, probably with water but

possibly with illite. Mixed layering of kaolinite and

chlorite (Brindley and Hillery, 1953) also produces 0

similar asymmetry. The reflection around 10 A and 0

13-15 A noted in several of the sample diffractograms may

be an indicator of mixed layering.

Grim (1953) states that chlorite may be confused with

kaolinite, especially if the clay is iron rich. The iron 0

can result in weak first order (14 A) and third order 0

(4.7 A) basal peaks. This leaves the second order 0

chlorite peak at 7.2 A to be confused with the 001 basal

peak of kaolinite. A sample of Sayers soil was leached

with HCl and showed no reduction of the intensity of the 0

7.2 A peak. This indicates that chlorite which is more

soluble in HCl than kaolinite is probably not a major

soil constituent.

The possibility that iron oxide might "coat" the clay

particles in some manner scattering the x-rays and contri-

buting to the broadness and lack of intensity of the 001

peak was considered. The Sayers sample which was leached

with HCl to remove the acid soluble oxides, including

iron, when x-rayed showed no sharpening of the 001 peak.

This indicates that the iron oxide is not the factor

responsible for the shape of the peaks (Figure 10).

In summary, the diffractograms show some character­

istics of halloysite, kaolinite, some mixed layering, and

90

minor amounts of chlorite, illite, and montmorillonite.

First appearances suggest halloysite to be the major clay

mineral in the soils. Further study shows that these fea­

tures which suggest halloysite may also be the product of

a fine-grained and/or poorly crystallized kaolinite which

possibly exhibits some b-axis disordering.

Some mixed layering, probably with water, is indicated

and adds to the confusion. Results of tests on the samples

treated and x-rayed as outlined by Miller and Keller (1963)

are a solid indicator that halloysite is not the major

clay mineral. Several authors note the risks of clay

mineral identification based on x-ray data alone since

so many factors may combine to affect the final diffrac­

tograms.

2. Differential thermal analysis. Differential ther­

mal curves for the clay minerals vary with several factors

related to both test procedures and the nature of the

minerals tested. Careful and consistent sample preparation

and testing should eliminate variations between curves due

to these factors.

The curves obtained in the current study all show

to varying degrees the following characteristics: (1) a

low temperature endothermic peak which generally occurs

between 100-135°C, (2) a major endothermic peak which

occurs in the area of 535-560°C, and (3) an exothermic

peak generally developed between 910-930°C. A number of

91

these curves are presented as Figures 13 thru 17. A

summary of the temperatures at which the endothermic and

exothermic peaks occur are reported in Table X. Two samples

of several soils (Timberline, Elsey, Georgia kaolinite) were

tested and the peak temperatures of the two samples agree

very well.

According to Mackenzie (1957) the low temperature

(100-135°C) peak is due to the removal of: (1) water

adsorbed on the surface of clay particles, (2) interlayer

water, or (3) water associated with amorphous silica or

alumina gels. The major endothermic peak at 535-560°C is

related to the expulsion of water from the crystal lattice.

There is disagreement as to the cause of the exothermic

peak, but researchers believe it is due to the formation

of a-Al 2o3 and/or mullite. This reaction begins at a

temperature of about 900°C and extends well past 1000°C.

Bradley and Grim (1951) present a more detailed investi­

gation of the nature of the high temperature reaction

which goes beyond the scope of this investigation.

Kaolinite pM (Mackenzie, 1957), which has disordered

shifts in the stacking of the unit sheets, and halloysite

produce differential thermal curves which appear much like

those obtained in this study. The curves also have many

of the features of a mixture of illite and kaolinite as

studied by Grim (1947). Mixtures of kaolinite with other

triple-layer minerals might also produce these features.

92

Two features of the curves tend to indicate that the

soils are not predominantly halloysite. A sample of the

reference halloysite, Indiana Halloysite, was dried in an

oven for 12 hours at 70°C and then subjected to DTA. This

sample shows a pronounced low temperature water loss even

after oven drying. A sample of Floyd soil was oven dried

for only 3 hours at 70°C, but all trace of the low

temperature water loss disappeared. If a significant

amount of halloysite was contained in the Floyd sample,

some low temperature water loss should have been indicated.

These comparisons are illustrated in Figure 16. A sample

of Masters #2 which was oven dried for 12 hours at 70°C

still showed a significant low temperature peak.

Bramao (1952) studied the shape of the major endo­

thermic curve, particularly the degree of asymmetry devel­

oped when halloysite soils were analyzed. He expresses

the asymmetry as the Slope Ratio (S.R. = tana/tanS), and

found values for kaolinites varied from 1.78 to 2.39 with

a mean of 1.55 while values for halloysite varied from

2.50 to 3.80 with a mean of 3.11. Correlation with test

results of other published DTA curves for the two minerals

confirmed his observations. The maximum slope ratio for

soils tested in this study is in the order of 2.10, indi­

cating that halloysite is not a major constituent of the

soil, but other factors as particle size and degree of

crystallinity probably affect values of slope ratio.

GEORGIA KAOLINITE

INDIANA HALLOYSITE

FIGURE 13. Differential Thermal Analysis of

Georgia Kaolinite and Indiana Halloysite

;0 ... 0.

1.0 VI

M A S T E R S n o. 2

M A S T E R S n o. 1

BLACKWELL

E L S E Y

FIGURE 14. Differential Thermal Analysis of Ozark Soils \.0 ~

TIMBERLINE no.l

T I M B E R Ll N E no. 2

He a ted for 12 H o u r s at 7 o· c

Leached in HCI

FIGURE 15. Differential Thermal Analysis of

Ozark Soils •o .. Ill

·.., -0.

.Ill

1.0 (/1

HORNSfY

HORNSfY-Ieached

fL 0 Y D

FLOYD- dried for 3 h o u r s a t 7 o' c

FIGURE 16. Differential Thermal Analysis

of Ozark Soils

0 Ill

o-

\D 0\

SUNRISE SOUTH

TERRE DULAC

SAYERS

~

FIGURE 17. Differential Thermal Analysis of Ozark Soils

..... ~ .,

"o " 0.

~ "'-l

98

Some features of these curves do not correlate with

curves of kaolinite, even the disordered kaolinite pH.

They show the major endothermic peak reaction around 535~

560°C versus 550-580°C for kaolinite pM and about 580°C

for halloysite. The depressed exothermic peak for the

soils tested in this study occur at 910-930°C versus

960-980°C for kaolinites and 970~980°C for halloysite.

Several factors might act singularly or together to

lower these peak temperatures. Speil (1944) reports sev­

eral effects of a decrease in particle size induced by dry

grinding including: (1) a gradual increase in the size of

the low temperature endothermic peak, (2) a decrease in

the size and reduction of the temperature of the major

endothermic peak, and (3) a reduction in the size of the

exothermic peak. The curves of the Ozark soils, when compared

with the standard kaolinite and halloysite, exhibit these

effects. Carthew (1955) substantiates Speilts findings but

found the effect of particle size only related to the minus

2 micron fraction.

In reporting their study of refractory clays,

Grimshaw et al (1945) produce data which conflicts with

Speil's and Carthewts finding in that they noted a lowering

of the peak temperatures due to a decrease in crystallinity,

but not due to a decrease in particle size alone, This

conclusion has been substantiated in a study by Volostnykl

99

(1966) in which he points to the regularity, or lack of

regularity, of the stacking of kaolinite plates as the

dominant factor controlling the temperature of the major

endothermic peak. Obviously, there remains a question as

to the effect of the decreasing particle size on the

temperature at which the major endothermic reaction occurs.

The effect of iron oxides on the thermal activity of

kaolinites was studied by Saunders and Giedroyc (1950).

They report that iron oxides lower the temperature of the

exothermic peak (but not to a temperature as low as that

of the Ozark soils). As shown in Figure 15, leaching the

acid soluble oxides, including iron, from the Timberline

soil resulted in an increase in temperature of the exother­

mic peak from 915°C to 945°C. Caillere et al (1946), as

reported in Mackenzie (1957), found the presence of alkali

ions decreases the size of the exothermic peak.

Kerr et al (1949) discuss several factors which affect

the temperature at which the exothermic reactions occurs.

They note that fine-grained, poorly crystallized, or

interlayered kaolinites present exothermic peaks at much

lower temperatures, peaks which are more rounded. Reactions

for interlayered or disordered kaolinites have been

observed which barely show an exothermic peak, presumably

because of the small particle size and/or the broad

temperature range over which the reaction occurs.

In summary of the results of differential thermal

100

analysis, the similarity of curves for most of the soils

studied indicates similar mineralogy. Analysis of the

DTA curves and the factors which might have affected them

indicate the probability that the major constituent of the

soils is a kaolinite with perhaps a minimum amount of hal­

loysite with the possibility of triple-layer clay minerals.

The size and generally low temperature at which the various

endothermic and exothermic reactions occur is probably the

result of poor crystallinity and small particle size of

the clay minerals. The iron content, the presence of

alumino-silicate gels, possibly allophane, and the nature

and concentration of adsorbed cations each probably have

an effect to an undetermined degree on the curves.

3. Thermogravimetric analysis. Ross and Kerr (1931,

1934), Nutting (1943), and Mielinz et al (1953) present a

number of dehydration curves of kaolin group minerals.

Dehydration curves of several of the Ozark soils are pre­

sented in Figure 18 along with the curves of the reference

halloysite and kaolinite. Except for the curve obtained

from the test on Georgia Kaolinite, the curves display

some low temperature water loss, major water loss between

500-600°C (related to the major DTA endothermic peak) and

very little water loss above 600°C.

Grim (1953) notes, "Variations in the specific char­

acteristics of the minerals being studied, such as grain

size, crystallinity, nature of adsorbed ions, etc., affect

,......_ ~ ..._,

UJ UJ 0

,...l

1-< (!)

4-J

~

16~-4------~------~~~~======!

10

8

6

• Sayers

• Terre Du Lac

4 • :f\fasters 1

• Georgia Kaolinite .. Indiana Ha1loysite

2

0 ____ _. ________ ~--------~~--------~------~

200

FIGURE 18.

400 600 0

Temperature C

800

Thermogravimetric Analysis

1000

] 0 1

102

dehydration results." The Ozark soils do exhibit rather

high initial water loss which even exceeds that of the

reference halloysite. The factors of fine particle size,

poor crystallinity, and/or presence of alumino-silicate

gels probably produce this unusual water loss. It is not

possible to isolate the exact clay mineralogy from these

curves.

4. Electron microscopy. Clay particle size and shape

parameters are best determined from transmission electron

micrographs. The moderately well-developed hexagonal

clay plate and the elongated plate shown in Figures 19

and 20 illustrate the highest degree of crystal development

of any particles observed during this investigation. This

hexagonal plate was the only one observed in a study of

two soils (Hornsey and Terre DuLac); the elongated plates

were fairly common. The several particles in the aggregates

shown in Figures 21 and 22 are somewhat less well developed

and illustrate the most common degree of crystallinity

observed in the micrographs.

These micrographs also illustrate the predominant

particle size range determined from the transmission

microscopy portion of the study. This size is in the

order of 0.4 to 1.0 microns.

The scanning electron micrographs of the powdered

samples also indicate that the clay minerals are poorly

crystallized. Most of the particles appear to exist in

FIGURE 19. TEM Terre Du Lac

Suspended Sample

(57000X)

¥IGURE 20. TEM Terre DuLac

Suspended Sample

• ( SZOOOX)

I-' 0 VI

FIGURE 21. TEM Terre Du Lac

Suspended Sample

(28000X)

4

FIGURE 22 . TEM Terre Du Lac Suspended Samp le

(20000X)

t-' 0 -+:>

FIGURE 23. SEM Terre Du Lac

Powdered Sample

(lOOOX)

FIGURE 24. SEM Hornsey

Powdered Sample

( 3000X) f-' 0 (Jl

FIGURE 25. SEM Hornsey

Ped Sample

(3000X)

FIGURE 26. SEM Hornsey

Ped Sample

(lOOOOX) t-' 0 0\

107

aggregates of several particles which are difficult to

analyze. A number of the particles or aggregates display

curved surfaces. These aggregates average 1 to 10 microns

in length (Figure 23 and 24).

The scanning micrographs of the broken chips of the

air-dried peds show several features of interest. They

substantiate the general low degree of crystallinity of

clay particles shown in the earlier micrographs except for

the Terre Du Lac sample where a fair degree of platy

hexagonal or elongate crystallinity has been developed,

Figure 28.

The crumpled, swirl-like laminated structure exhibited

by the micrographs of the Hornsey sample, Figures 25 and

26, and to a degree by the Terre Du Lac micrographs is

almost identical to that developed in the kaolinitic ball

clays described and photographed by Borst and Keller

(1960). They attribute the probable cause of the deforma­

tion in structure to post-depositional stresses. Forces,

possibly due to dessication, which were responsible for the

pedular nature of the Ozark soils may also be responsible

for the distorted structure.

It had been hypothesized by this investigator that as

the dessication process removed moisture from the soil-water

system and the interparticle bonding became stronger, the

clay particles would be drawn into a low density

flocculated position. This does not appear to be the

FIGURE 27 . SEM Hornsey

Ped Sample

(lOOOOX)

FIGURE 28. SEM Terre Du Lac

Ped Sample

(lOOOOX) !-" 0 00

109

(])

!=: •r-1 1'"-i

(])

~

1'"-i ,--.,.

(]) p..

:>< ..0

IS

0 IS

C1l 0

•r-1 rJ)

0 E-<

0 '"d

1'"-i (])

'--'

~

p.. ~

rJ)

Gl

N

~

p:: :::::> (.9

H

~

110

case as a strong degree of parallel particle orientation

is observed in the scanning micrographs. Michaels (1959),

Trollope and Chan (1960) and other authors have postulated

this parallel orientation of particles in packets.

Microscopy studies by Sloan and Kell (1966) and others

have shown this structure to exist. The peds exhibit a

noticeable volume of voids which is probably responsible

in part for the low density of the clay soils in their

natural state.

The microscopy study shows that halloysite, if

present at all, is a minor soil constituent. No transmis­

sion micrographs and only one scanning micrograph, Figure 29,

shows a tabular or tubular form which may be halloysite,

but could also be chrysotile or a number of other clay

minerals.

5. Chemical analysis. The results of chemical anal­

yses performed at the Missouri Geological Survey on a

number of the soils investigated in the study are presented

as Table XI. A summary of pH, cation-exchange capacity,

and silica-alumina ratio is presented in Table XII. The

content of Na, K Mg, and Ca in meq/100 gr. as determined

at the University of Missouri - Columbia is presented

in Table XIII.

Grim (1953) presents typical values of the chemical

composition of a number of clay minerals; Ross and Kerr

1 1 1

(1934) give values for allophane. A common value used to

compare clays is the silica-alumina ratio, Si0 2/Al 2o3 .

Average values of the silica-alumina ratio as reported by

the above authors for kaolinite (theoretically 2:1) are

2.00:1 to 2.12:1; for halloysite, 2.00:1 to 2.10:1; for

allophane, 1.20:1 to 1.80:1; for illite, 3.20:1 to 4.00:1;

and for montmorillonite, 5.10:1 to 5.95:1. As Table XII

indicates, the typical values for the Ozark clay residual

soils are 2.45:1 to 2.55:1. Higher values are noted in

the alluvial-colluvial soils where silica has been

concentrated. Higher values are also noted in the soils

which have a high chert (silica) content as Floyd and

Blackwell.

The silica-alumina ratio for the residuals of 2.45:1

to 2.55:1 may be caused by a mixing of some illite and

montmorillonite in with kaolinite. Another cause may be

that some octahedral layers may have iron replacing

alumina which would result in a higher ratio. Still

another cause could be the presence of silica-rich gels in

the clay.

The Ozark soils exhibit a relatively high (6-12%)

iron content. A number of possible effects of this

occurrence have been discussed in earlier sections.

Table XI shows that for three soils tested (Sayers,

Terre Du Lac, Hornsey) approximately 90 percent of the

Al 2o3 is soluble in 12.1 normal HCl. This indicates that

112

a majority of the alumina in the soil is not crystallized

or is poorly crystallized. When results of other tests

are considered along with this evidence, the latter,

poorly-developed crystalline state is indicated. Keller

(1970) notes that soil acids can cause the breakdown of

even well-crystallized kaolinites. This effect is thought

to be much more severe for poorly-crystallized or

disordered kaolinites.

6. Summary. The x-ray diffraction, differential

thermal analysis and the thermogravimetric analysis com­

bined with a study of the electron micrographs indicates

that the major clay minerals of all of the residual Ozark

soils investigated in this study are poorly crystallized

kaolin minerals. If placed in Bates' (1959) morphological

series, these minerals would be classified as elongate

kaolinite crystals with possibly some particles as a

transitional phase between the elongate crystals and

halloysite.

Two or more phases of clay morphology may be repre­

sented in the Ozark soils. One may be the better

crystallized, elongate platy crystals. Another phase

represented by less well-developed crystallinity may be a

precurser (Keller et al, 1970) of kaolinite or halloysite.

This phase or other phases may be the result of post­

formational crystal destruction enhanced by soil acids.

Bramao's discussion of the probable mode of formation

113

of these soil clay kaolins aptly describes the Ozark setting

in which the clays were formed. It is to be expected that

the result of changing soil conditions and interrupted

formational cycles would be poorly developed and varying

clay morphology.

Minor amounts of chlorite, illite, and montmorillonite

are indicated. The presence of an undetermined amount of

allophane or an alumino-silicate gel of some nature is

also indicated.

B. SOIL CLASSIFICATION AND CATION-EXCHANGE CAPACITY

The results of Atterberg Limits tests are presented in

Table VII with results plotted on the plasticity chart,

Figure 29. Results of gradation tests are presented as

Figures 3 thru 8. Table IV summarizes the results of the

gradation tests.

Before sieve analysis, all materials retained on the

No. 4 sieve was discarded. This material was predominantly

chert. Earlier sections of this discussion noted that the

proportion of chert throughout the soil varies widely and

that the percentage in any one sample is not a diagnostic

value. The fines is defined as that material passing the

No. 200 sieve. Clay is defined as that material (colloids)

finer than 2 microns (0.002 mm).

Except for the sandy residual soils, the soils invest­

igated have 85 percent or more fines and 60 percent or more

clay. Several of the clay residuals have greater than 90

114

percent clay. ThB sandy residual soils have 60 to 80

percent fines but only 20 to 40 percent clay. These soils

are composed primarily of fine sand and silt size particles.

All but three of the soils plot as CH or CL on the

plasticity chart. The Hornsey soil plots just below the

A-line as a MH soil. The Rice and Fabick sandy residuals

are CL-ML soils.

Definite relationships are noted between the Atterberg

Limits and the percent clay. Davidson and Sheeler (1952)

note a general relationship between the clay fraction and

the liquid limit and plastic limit.

The clay content of the clayey residual soils was

correlated with the liquid limit and the plastic limit,

Figures 30 and 31. A linear curve fits both sets of data

fairly well, but a concave upward second or third degree

curve fits both sets of data more closely. It is suggested

that at higher clay contents, notably above 90 percent,

that the soil is more "sensitive" to other factors than to

increases in percent clay. For high clay content soils,

as water is added up to the liquid limit the electro-chemical

nature of the soil-water system has a noticeable effect on

the Atterberg Limit values. The cation-exchange capacity is

a measure of this electro-chemical potential of the clay

soils. Values of the cation-exchange capacity determined

for the Ozark soils are presented in Table XII along with

soil pH and silica-alumino ratio.

"""' IN! '-./

.u ·r-1 s

•r-1 ....:l

"0 •r-1 ;:1 0"

•r-1 ....:l

100 Linear y = -3.81 + 1.05 X rr = 61.1 r = 0.95 2

Best Fit y = 49.47 - 0.61 X+ 0.012 x tr = 50.2

I 0 80

I ~~ 0 0

60

40

20_~------~--------~--------L-------~--------~--------L-------~--------jL 55 -~ 6u 65 85 70 80 75 90 95

Clay Content (%)

FIGURE 30. Clay Content Versus Liquid Limit (Clay Residual Soils) f---0 f---0 Ul

"" ;;-e "-'

+J -M a -M ~

0 ·rl +J {/)

til ..... fl.!

Linear

Best Fit 40

35

30

25

y = 2.52 + 0.36 x cr = 13.4 2 y = 32.70- 0.56 X+ 0.007 X

r = 0.87

cr = 9.6

0

0? '/

/ /0

,

// / 0

0// /, 0

//

0

I

0

o I I

I I

0

20 ' I I I I I I I 30 40 50 60 70 80 90 100

0--:------

Clay Content (%)

FIGURE 31. Clay Content Versus Plastic Limit (Clay Residual Soils)

f-' f-' 0\

117

The Sayers and the Hornsey soils both contain 93

percent clay but the liquid limit of the Sayers is 105

compared to 90 for the Hornsey. The cation-exchange

capacity of the Sayers is 44.9 whereas that of the Hornsey

is 42.1. Masters #2 has 95 percent clay and a cation­

exchange capacity of only 35.8. The result is that Masters

#2 has a lower liquid limit and plastic limit than does

Sayers.

This does not mean that the cation-exchange capacity

is by itself the factor controlling the limit indices. The

cation-exchange capacity was correlated with the liquid

and plastic limit, Figure 32 and 33. The degree of

correlation is similar to that of the correlation of the

clay content versus the limit indices. This similarity

suggests that a combination of influence of clay content

and cation-exchange capacity on the limit indices exist.

Data presented above indicates that at higher clay contents,

the cation-exchange capacity of the soil has the dominating

effect on Atterberg Limits.

Cation-exchange capacity is a property of the clay

fraction of the soil. The degree of correlation between

these two factors, cation-exchange capacity and clay content,

was determined and presented in Figure 34. A fairly linear

relationship appears to exist between these factors up to

a clay content of about 90 percent. Above that point the

curve flattens and it is postulated that again the cation-

exchange capacity becomes more important. The soils which

40 0

20L_--~L---~----~----~----~----~----~----~ 5 10 15 20 25 30 35 45 40

Cation-Exchange Capacity (meq/100 gr.)

FIGURE 32. Cation-Exchange Capacity Versus Liquid Limit (Clay Residual Soils)

I-" I-" 00

......._ N .......,

.j.J

•rl a

•rl ...:1 t)

•rl .j.J (I)

t\1 ...-t ~

40

35 r 30 r

25

20 5

Linear and Best Fit

0

0

y = 12.04 + 0.66 X cr = 9.3 r = 0.91

0

/ 0

0

0 0

0

20 25 30 35 40

Cation-Exchange Capacity (meq/100 gr.)

FIGURE 33. Cation-Exchange Capacity Versus Plastic Limit (Clay Residual Soils)

45

f-1 f-1 \.0

"'"" IN! .._,

.j.J

~ Q) .j.J

~ 0 u :>. ~ r-i u

100

80

60 I

40

20

0 // / .

~ ~

0

0

/

0 ,o/ //

/./'0 0

// ~o/

Linear y = 15.81 + 2.02 X

Best Fit 2

y = -17.74 + 5.21 X- 0.06 X

0

A"',..... _....~

a = 155.1

a = 89.2

r = 0.88

oL---~----~L------L------L------J------~------~----~--40 45 10 15 20 25 30 35

Cation-Exchange Capacity (meq/100 gr.)

FIGURE 34. Cation-Exchange Capacity Versus Clay Content (All Soils)

1-' N 0

121

appear to control the deviation from linearity of the curve

(Terre Du Lac, Sayers, Masters 2) are the same soils which

have high cation-exchange capacities. The concentrations of

the more common exchangeable cations which compose the

cation-exchange capacity are presented in Table XIII.

These observations are consistent with discussions by

Grim and others covered in the literature review with regard

to the clay-water system and the effect of cation concen-

tration on the system. Increased cation concentration

results in an increase in the attraction between the

particles. More water is required to dilute the concentra-

tion to reduce particle attraction, and to reduce

flocculation, which allows the liquid limit shear failure

to develop.

With regard to the plastic limit, the higher cation

concentration produces a flocculated microstructure which

resists deformation at a fairly high moisture content.

Conversely, soils with lower cation concentrations have a more

dispersed structure which allows manipulation and water

expulsion until a lower moisture content is reached.

The effect on Atterberg Limits of dispersing the clay

soil with sodium is illustrated in Table VI. It is

thought that the sodium acts to lessen the attraction

between clay particles and allows more water between

particles. The result is a lowering of the limit values

as the degree of flocculation and particle attraction

decreases.

122

Table IV illustrates the difference in the liquid

limit values of soils which have never been air dried and

those which have. Though the cation-exchange capacity

of wet samples was not determined, it is thought that the

exchange capacity for soils which have never been dried

would be higher than that of soils which have. This

reduction in capacity would occur if upon drying the

concentration of cations in the clay soil increases as water

evaporated and micropackets of clay particles are formed.

These packets would tend to trap cations, thereby reducing

the cation-exchange potential. Upon rewetting with

distilled water for the limit tests, the packets are not

completely destroyed and all cations would not be available

in the clay-water system, some still being bound up between

plates in the packets. This decrease in cation-exchange

capacity would result in lower particulate attraction and

lower Atterberg Limit values.

Another aspect is that the micropackets which are

formed upon air drying and which do not disperse when

mixed with distilled water effectively reduce the percent

clay-size fraction of the soil. Though the packets them­

selves probably have a water film as would the individual

clay particles, the attraction between packets is less;

therefore, less water is required to reach the liquid limit.

The liquid limit of samples which have never been dried and

have the higher cationic concentration and greater particle

attraction would require more water to disperse the structure

123

to a point of failure in the liquid limit device.

C. COMPACTION CHARACTERISTICS

Three factors; soil gradation and Atterberg Limits,

cation-exchange capacity, and clay structure, were studied

with relation to their effect on laboratory compaction of

the Ozark soils. No gross difference was noted in the

clay mineralogy of the soils investigated in this study

so this was eliminated as a prime cause of compaction

differences.

The results of soil compaction tests are presented in

TableVIII. Figures 35 thru 45 illustrate the relation­

ships between the factors listed above and the optimum

moisture content and maximum dry density of the soils

tested. Table XV illustrates the correlation coefficient

and sigma value for each relationship tested.

1. Atterberg Limits. As discussed previously, Harris

(1969) showed the best correlation tested was between the

liquid limit values and the maximum dry density and optimum

moisture content. The correlation coefficient for this

relationship for residual soils was on the order of 0.90.

This same range of values (0.88 for maximum dry density

and 0.90 for optimum moisture content) was noted for the

Ozark clayey residuals. The plastic limit was found to

exhibit even a slightly better degree of correlation than

the liquid limit. A correlation coefficient in the order

of 0.90 signifies a high degree of relationship (Harris,

........ 4-4 tJ ~ .....,

:>. ...., ..... til ~ Q) ~

:>. ~ ~

~ ~ ~

90

85

80

75 Linear

Best Fit

y = 125.09 - 0.51 X

2 y = 138.85 - 0.93x + 0.003 x

0

a= 5.9

a = 5.4

0

0

0

~--... ,.... ........ ~ .................

r = -0.96

0

70 I I I I I I I I I 55 60 65 70 75 80 85 90 95

Clay Content (%)

FIGURE 35. Clay Content Versus Maximum Dry Density (Clay Residual Soils)

~

N .s;:.

,-... ~ '>.,/

+.1 !::: Q) +.1 !::: 0 u Q) I-I ::l +.1 fJl •rl

jl

~ ·rl +.1 p.. 0

40

35

30

25

20

Linear and Best Fit

y = 2.73 + 0.37 X (j = 9.7 r = 0.90

0

~ 0

~~ 60 65 70 75 80 85 90 95

Clay Content (%)

FIGURE 36. Clay Content Versus Optimum Moisture Content (Clay Residual Soils)

I-' N tn

/""'>

4-1 () 0.

'-../

:>. -IJ ·ri

11.) Q (I)

A

:>. ~

~ ·ri

><

:2

120

110

100

90

80

0

\ \

"

Linear

Best Fit

'\

0

y = 108.40 - 0.80 X

2 3 y = 158.16 - 6.66 X+ 0.21 X - 0.002 X

a = 23.0

0 = 18.8

r = -0.87

70 35 40 45 10 15 20 25 30

Cation-Exchange Capacity (meq/100 gr.)

FIGURE 37. Cation-Exchange Capacity Versus Haximum Dry Density (Clay Residual Soils)

f-'

N 0\

""' ~ '-'

.j..J

Q Q) .j..J

Q 0 u Q) ~ ::l

.j..J

rn ..... :S

~ ..... .j..J

0. 0

40

I /. 0

0 I

35

I 0

30

25 ~ 0

/ 0

0

0

20- Linear and y = 13.83 + 0.62 X cr = 14.3 r == 0.86 Best Fit

0

15 10 15 20 25 30 35 40 45

Cation-Exchange Capacity (meq/100 gr.)

FIGURE 38. Cation-Exchange Capacity Versus Optimum Moisture Content

(Clay Residual Soils)

f-' N "-J

"'"" 11-1 () llo '-'

~ ~ •rl Ill s:: Q)

Q

~

'"' Q

~ or! :< ~

110 t-'\.o Linear y = 117.80- 0.41 X cr = 19.2 r = -0.88

" Best Fit y = 154.50 - 1.44 X+ 0.007 X 2 cr = 13.8

" " 100 " " ~ 90

' 0

80

70 ~------~------~------~-------L------~------~------~~-------30 40 so 60 70 80 90 100

Liquid Limit (%)

FIGURE 39. Liquid Limit Versus Maximum Dry Density (Clay Residual Soils)

..... N 00

50

"""" N "-../

+J 40 !:I Ill +J !:I 0 u Ill

~ +J

.~ 30 ~

Linear y = 8.93 + 0.30 x

Best Fit y = -17.90 + 1.06 x- 0.005 x2

j I ~ / o +J .

0.. 0

20

10 30 40 50 60 70

Liquid Limit (%)

a= 10.6

a= 7.6

80

r = 0.90

90 100

FIGURE 40. Liquid Limit Versus Optimum Moisture Content (Clay Residual Soils)

1-' N \D

,....... ~ u 0..

'-./

:>. .j..l

•r-i (I)

I:: Q) t:l

:>. 1-1

Q

~ 13

•r-i X

:ill

110

100

I

90 t-I

80

Linear and y = 109.1 - 0.80 x Best Fit

--............_ 0

~0

............ 0

0

a = 8.1 r = -0.89

70 ~------~--------~--------L-------~--------~------~~------~~-----10 15 20 25 30 35 40 45

Plastic Limit (%)

FIGURE 41. Plastic Limit Versus Maximum Dry Density (Clay Residual Soils)

....... tN 0

;-..

N '-"

.j.J

g .j.J

1=1 0

c.>

<1.1

~ .j.J

Ul •r-1

~ § ~ .j.J p.. 0

50

40

30

' 20

Linear y = 3.79 + 0.90 X

Best Fit y = -29.72 + 3.12 x -0.04 x2

0 -~g

a= 7.9

a = 5.6

r = 0.92

10 ~------~--------~-------L--------~------~------~~------~-------10 15 20 25 30 35 40 45

Plastic Limit (%)

FIGURE 42. Plastic Limit Versus Optimum Moisture Content (Clay Residual Soils)

f-' VI f-'

120

110

"'"' Il-l () Q. ......,

t' 100 'rl !ll 1::: Q) ~

>.

'"' ~

m 90

'rl X )!

80

20

Linear y = 128.30 - 0.55 X

Best Fit 2 3 y = 149.52- 1.79 X+ 0.019 X - 0.0004 X

"· ',

30

', '-...,

' 0 ',

40

' ',o ""-, 0

.........

', -o -.........:

so 60 70

Clay Content (%)

80

0 = 10.9

0 = 7.6

r = -0.97

0 ~........ 0

~._,

. ::--.o, 0~ 0

90

FIGURE 43. Clay Content Versus Maximum Dry Density (All Soils)

...... Vl N

50

,....._ N '-"

I +J

40 l=l Q) +J l=l 0 u

I Q)

1-4 ;:I +J til 30 •rl

~

~ •rl +J

I p. 0

20 I

10 20

Linear and Best Fit

30

0

0

y = 6.30 + 0.33 X a= 8.8 r = 0.95

40 50 60 70

Clay Content (%)

FIGURE 44. Clay Content Versus Optimum Moisture Content

0

~ 0

80 90

....... (.N

(.N

(All Soils)

120

110L

""' I 4-l t) p.

'-"

:>-. 1001 -1-1 "T"4 Cll !:l (!) Q

:>-. ~ Q

m 90

•.-1 X til ~

' 80

70 10

Linear

Best Fit

y = 121.19 - 1.14 X

2 3 y = 296.70- 19.01 X+ 0.58 X - 0.006 X

(J = 15.1

(J = 7.3

\ 0

~ \ \

~

0

15 20 25 30 ' 35 40

Optimum Miosture Content (%)

FIGURE 45 • Optimum Moisture Content Versus Maximum Dry Density

(Clay Residual Soils)

r = -0.90

45 1-' V-1 +:>.

135

1969).

2. Gradation and cation-exchange capacity. The

percent fines was not found to have a significant relation­

ship with either the maximum dry density or optimum moisture

content. The correlation between the percent clay of all

the soils and the compaction characteristics was very

high, -0.97 for the maximum dry density and 0.95 for the

optimum moisture content. The cation-exchange capacity

also has a high degree of correlation with the optimum

moisture content (0.86) and the maximum dry density (-0.87).

The high degree of correlation between the Atterberg

Limits and the compaction characteristics indicate that the

factors which influence the values of the limit indices also

influence the compaction characteristics. The clay content

and the cation-exchange capacity were determined to strongly

affect the limit values; similarly, they have been shown

to be strongly related to the optimum moisture content and

the maximum dry density.

Lambe (1958) has postulated that the compacted nature

of clayey soils is a result of clay particle structure.

Clay content, cation concentration, and other factors not

studied in this investigation have a strong influence on

the compaction process which is manifested in their affect

on the clay structure.

3. Soil clay structure. The Atterberg Limits and the

cation-exchange capacity are considered indirect measures

136

of clay structure. No direct quantitative measures of

differences in clay structure in compacted samples were

determined, but a qualitative low-power and scanning micro­

scopy investigation of the clay structure was conducted.

Particular attention was made in comparing the apparent

validity of the particle-to-particle concept of the structure

of compacted samples and changes in this structure with

different compacting moisture contents as postulated by

Lambe (1958) to the packet-to-packet compacted structure

as postulated by Sloan and Kell (1966) and Barden and

Sides (1970).

Low-power micrographs of the Terre Du Lac soil are

presented in Figures 46 and 47 for two samples; one com­

pacted 3% dry of optimum, the other compacted 5% wet of

optimum. Samples compacted at all moisture contents contain

a large number of particles which exhibit residual pedular

structure which apparently has not been destroyed or altered

significantly by the compaction process.

Some differences are observed between the samples

compacted dry and wet of optimum. The dry sample has a

much "rougher" texture, the wet sample an apparent uniform

texture. A large volume of voids, or macrospaces, are also

obvious in the dry sample and which do not appear in the

wet sample. The size of the packets, or macropeds, in

the dry sample is highly variable whereas less variation

is exhibited in the wet sample.

a.) Compacted 3% Dry of Optimum b.) Compacted 5% Wet of Optimum

FIGURE 46. LPM Terre Du Lac (Black and White)

t-' lN -....}

- ~ ~

.a;j IE1 aJ

P!l ,.

~

~

R I

'A·.. .f '•i . )' ~·ij,:r· . ~ ~k.~

, f •.•.' .. , ~~ • io " ..

liiC

~

I ~

[J!l

• • ,":f ~ •fv '9. " 1~ . ! ' ·~ • '·' .. .; . ,~ .• . K .

. . ~· ~, ·\ : ·~. ·,,. ·.• · .. t. -~~

~ ~~. ·~·t· ".· ·~ r ' 'I :li ji . •I'. ,. ... ' • •

• _. ~ I r" , ·-~ ~ ~' .. · . ~ . ;;r 'f. .

··., ~.4·--·· ....... :·,.,

~ :.,)-, • • I' •

~- f~ .. ).' . ... . . ~-\ . '-4···. . ~ .. .. . -. ..

a.) Compacted 3% Dry of Optimum b,) Compacted 5% Wet of Optimum

FIGURE ~7. LPM Terre DuLac (Color)

f-> (A

co

It is suggested that the sample compacted wet of

optimum has been more altered by wetting and compaction

139

than that compacted dry of optimum. Part of this alteration

is probably manifested in the breakdown upon wetting of the

peds due to differential swelling pressure and differential

air pressure as suggested by Baver (1956).

A study of the microstructure was initiated to further

investigate the macropeds and to investigate the particle­

to-particle structure of compacted samples with variations

in the compaction moisture content.

Figures 48, 49, and 50 compare the structure of Standard

Proctor samples compacted dry and wet of optimum at magni­

fications of lOOX, 300X, and 3000X. All micrographs are

of sample surfaces oriented parallel to the direction of

applied compactive force. At a magnification of lOOX,

the outline of the macropeds are still apparent with similar

patterns of texture, macrospaces, and ped sizes as was

evident in the low-power micrographs. The scanning micro­

graphs (lOOX) enhance the significant textural differences

between the samples compacted wet and dry of optimum; the

dry sample with a very random pattern of macropeds, the

wet sample with a uniform pattern. These patterns are still

evident in the 300X micrographs.

Quite a different pattern is observed in Figure 50

for those micrographs taken at 3000X. The microstructure,

or "intra-pedular" structure, is very similar for both wet

'-- · · ---..a._ -

t;,.,

a.) Compacted 3% Dry of Optimum b.) Compacted 5% Wet of Optimum

FIGURE 49. SEM Terre Du Lac (300X)

T

I-' ~ I-'

a.) Compacted 3% Dry of Optimum b.) Compacted 5% Wet of Optimum

FIGURE SO. SEM Terre Du Lac (3000X)

""

,__. -+>o N

and dry samples, apparently independent of compaction

moisture content.

143

The theory of the compactive process which emerges from

this study is considerably different from that postulated

by Lambe (1958). There is little indication in the micro­

graphs of single particle activity being prominant in the

compaction process. This is particularly true for samples

compacted dry of optimum. On the wet side of optimum where

samples appeared uniform under relatively low magnification,

clay particles seem to form a cement between macropeds.

The following theory, similar to that postulated by

Barden and Sides (1970), of laboratory compaction density

is primarily a function of the degree of fit between

macropeds of clay. Dry peds at low moisture content are

resistant to deformation and a relatively loose compacted

structure is obtained. With the addition of moisture, two

factors are thought to influence the compacted density.

First, upon adsorption of moisture, the macropeds tend to

break down forming a better gradation of particles which

can result in a more dense arrangement without major ped

deformation. Also, as Barden and Sides postulate, with

additional moisture the macropeds become "softer" and can

be forced by outside forces into a more compact arrangement.

At the optimum moisture content, the effects of ped

breakdown and deformation are maximized. Macrospaces are

minimized.

144

Wet of optimum the influence of individual particles

and the smaller peds are predominant. With increased

moisture and further deterioration, more particle-to­

particle reaction may occur. As water layers are adsorbed

by particles and small peds, they are pushed apart and

density decreases. A decrease in cation concentration may

play an important role as the water film expands. Even wet

of optimum, a large portion of the peds remain relatively

unaffected by the increased moisture and their internal

structure is essentially unaltered.

The micrographs of the natural air-dried soil has

indicated a natural essentially parallel particle orienta­

tion. When this structure is affected by moisture, no

major reorientation of particles may be required, as from

flocculated to parallel structure; just a separation of

parallel plates.

Assuming the natural ped structure is the result of

dessication, the forces responsible for the particle

orientation were very large. Once the ped structure has

been destroyed by moisture, the effort expended in a

compaction test in an attempt to force the particles back

into a dense state is considerably less than were the

dessication forces. The water film surrounding the

particles and peds resists the compactive effort.

The natural low density of the peds (Scrivner, 1960)

which is not destroyed by the compaction process is one

145

factor responsible for the low compacted densities of the

Ozark clayey residual soils. As would be anticipated, the

soils tested with higher non-clay contents (primarily

quartz, S.G. - 2.66) have higher compacted densities. Soils

with high cation-exchange capacities, particularly those

high in the sodium ion, appear to adsorb moisture more

readily with an accompanying breakdown in ped structure.

The greater the degree of particle reorientation, the lower

the compacted dry density and the higher the optimum moisture

content.

Figure 51 demonstrates the results of the Standard

Proctor tests on the soils dispersed with sodium metahexa-

phosphate. The dispersed soils demonstrate a higher maximum

dry density and lower optimum moisture which agrees with

Lambe's (1962) discussion of the effects of aggregants and

dispersants.

It is postulated that the sodium treatment acts to

breakdown the peds more than the normal addition of water

reducing the macrospaces and allowing a more dense particle

arrangement at a lower optimum moisture content. As more

water is added, particularly past the optimum, the particles

adsorb water layers reducing the particle-to-particle

attraction and the dry density.

....... 4-1 0 s:l.

'-J

~ .j,J

...... !I)

90

85

!:1 80 Q) Q

~ ~ Q

~ ......

i 75

70

20

0~ / ~ / ""

25 30 35

Moisture Content (%)

40

Floyd - natural

Floyd - dispersed

Terre Du Lac - natural

Terre Du Lac - dispersed

Sayers - natural

Sayers - dispersed

45

FIGURE 51. The Effect of Dispersion of the Standard Proctor Compaction

of Clayey Residual Soils

50

I-' .f::o 0\

VII. CONCLUSIONS

A. GENERAL

This study of residual soils used in earth dam

construction in the Ozark Province of Missouri centered

147

investigation in four general areas. First was a determina-

tion of the clay morphology of the soils and the extent of

any changes in this morphology from one site to another.

Second was a study of the soil gradation, Atterberg Limits

and cation-exchange capacity. This was followed by a study

of the correlation between these soil properties and the

compaction maximum dry density and optimum moisture content.

Finally, the effect of the pedular nature of the clay soils

on the Standard Proctor compaction characteristics was

investigated.

B. CLAY MORPHOLOGY

Regardless of differences in the parent material or the

geographical location of the dam sites within the portion of

the Ozark Province investigated, the morphology of the

clayey residual soils is similar. The relative location of

the samples within the vertical soil profile appears to

determine to a great extent the clay content in percent.

It is shown that the climatic conditions which existed

in the Ozarks during the Tertiary Period were probably

f laterl·zation process which conducive to the development o a

has resulted in the formation of halloysite-rich soils in

other areas under similar conditions. The numerous tests

148

which have been performed to determine the mineralogy of

the clays have shown that the residuals do not contain

halloysite in any significant amounts. It is suggested that

the continuous, extensive leaching process associated with

halloysite formation was never completely developed within

the Ozark area. Instead of halloysite, clays with a

morphology more closely resembling kaolinite were formed.

The major clay morphology is expressed in poorly

developed elongate platy kaolinite crystallinity. Other

kaolin morphologies even less well developed, including

possibly some alumino-silicate gels, are indicated by some

of the tests. A minor amount of illite, chlorite, and

possibly some montmorillonite is also present.

The soils are characterized by the presence of an

aggregated structure which separates the soils into units

called peds. This ped structure is probably the result of

soil collapse as the bedrock is chemically leached and of

dessication of the soil mass. These peds are thought to

affect the results of all tests performed on the soils to

determine their engineering properties.

C. SOIL CLASSIFICATION AND CATION-EXCHANGE CAPACITY

When the Atterberg Limits test results are plotted on

the plasticity chart, the clayey residuals and the alluvial­

colluvial soils are classified as CL and CH. The liquid

·d 1 ·1 as high as 105 with limits of the clayey res1 ua so1 s were

a corresponding plasticity index of 69. The stone-free

149

residuals contain up to 95% clay.

as

The cation~exchange capacity of the residual soils was

high as 45 meq/100 gr. for those soils with greater than

90% clay. This is very high for kaolinitic soils. The fine

clay particle size and poor crystallinity have been shown

to act to increase the cation~exchange capacity of kaolinitic

soils. These high values may also reflect the presence of

some illite and/or montmorillonite.

The value of the liquid limit of samples never allowed

to air~dry in considerably (30~40%) higher than that of

samples which were tested after air~drying. It is thought

that the process of air-drying enforces and strengthens the

natural ped structure to a point that it fails to break down

completely when wetted for the liquid limit test. The

result is that only moderate particle-to-particle (ped-to­

ped) attraction develops and less water is required to

facilitate shear failure in the liquid limit device.

The liquid limit of the sodium dispersed samples was

found to be less than the natural air-dried liquid limit for

several of the soils. This agrees with results presented by

White (1958) in his discussion of the effects of the

exchangeable cation on the liquid and plastic limit of clay

minerals. An explanation fitted to the pedular nature of

the soils is that the samples treated with a sodium dispersant

reacts in one of two ways or in a combination of the two:

(1) the dispersant completely breaks down the ped structure

allowing the sample to behave as described by White, and/or

150

(2) the ped structure is partially retained but the sodium

attracts to the peds a film of water which acts to separate

the clay peds and reduce ped~to~ped attraction. In either

case, the liquid limit value is lowered,

D. CORRELATIONS WITH COMPACTION RESULTS

Several factors were studied to determine their

correlation with the Standard Proctor laboratory compaction

parameters of the clayey residual Ozark soils: (1) soil

gradation, (2) Atterberg Limits, and (3) cation-exchange

capacity. The percent clay had the best correlation tested

with both optimum moisture content (r = 0.95) and the

maximum dry density (r = -0.97). The plastic limit also

correlated well with both factors, particularly the optimum

moisture content; the liquid limit exhibited only fair

correlation. The cation-exchange capacity also had only

fair correlation with the compaction characteristics. This

might be anticipated since the cation-exchange effect is more

pronounced in a more fluid environment than that of the

normal compaction test.

There appeared to be no significant relationship between

the percent fines and the optimum moisture content and the

maximum dry density. The relationship between the optimum

moisture content and the maximum dry density is good

(r = 0.90).

E. THEORY OF RESIDUAL SOIL COMPACTION

The Standard Proctor compaction tests yielded low values

151

of the maximum dry density with corresponding high values of

the optimum moisture content for the clayey residual soils.

The electron microscopy investigation has shown that the

pedular structure of the clayey residual soils is not

destroyed during laboratory compaction. This is thought to

be the key factor controlling the low density of the

compacted samples.

The low-power micrographs illustrate that dry of

optimum most of the clay remains bound in macropeds with a

large volume of macrospaces between them. As more water 1s

added and optimum is approached, the moisture breaks down

some of the larger peds to form smaller peds and other peds

are probably completely destroyed. A better ped-particle

gradation and perhaps a softening of some peds with

increased moisture allows the soil to be forced into a more

dense arrangement with a minimum of macrospaces.

Wet of optimum, even more peds are reduced in size

and/or destroyed with clay particles and small peds

develop water layers which force them apart, reducing

the compacted density. These particles appear to form a

cementing bond between the remaining peds, which still

comprise the majority of the compacted sample.

High magnification micrographs show that the micro­

structure of the clay peds is not destroyed during the

compaction process. Indeed, it does not appear to be changed

significantly from that of the natural soil peds.

152

F. APPLICATION OF TEST RESULTS

1. Correlations. Several correlations have been

presented which may be useful in estimating the optimum

moisture content and maximum dry density from more commonly

available data. The clay content and plastic limit were

noted to be closely correlated to the optimum moisture

content and maximum dry density. Curves relating these

factors have been plotted and presented as Figures 52 and

53. Similar curves are presented, Figures 54 and 55,

relating the plasticity chart values, liquid limit and

plasticity index, to the optimum moisture content and maximum

dry density. At best these curves yield approximate values,

show trends. Better estimates can be obtained using the

equations presented along with the illustrations which show

the correlations.

2 . ::.D..:::a=m~d.:;_:_e..:::s_i~g"n=---c.:...:..o_n_s_t_r_u_c_t_i_o_n_. The m a j or pro b 1 em

observed in the earth dams investigated was seepage through

and around the dams. The seepage is often noted high up on

the downstream slope of dams, even on those dams with moderate

slopes. The seepages are often associated with surface slips

on the steeper dam slopes. The additional driving force

exerted by the saturated areas overcomes the resisting forces.

It is probable that the resisting forces are reduced signifi­

cantly as the nature of the ped structure of the embankment

clays is altered upon saturation. A large portion of the peds

are believed to swell and deteriorate, destroying much of the

intergranular frictional resistance which is thought to provide

........ ~ '--"

+J 'r'l s •n ~

t) ·r-1 +J 1:1)

til ...-! ll-o

75

80 •77\ a~' \ •74 \ 401-

~~~ \ \ ~

"-s~ \ \ 75 v\, f5 ~

e83 \. 79

/ 3l ~4,.

\ ~s'\-\ ~~

• 81 ~ \ • 85 "'-~ \ ~\,~ \ \0 .\ • 88 80

30

82 \ \ \ \ \95 \ \ • 84 85 25L

\ \. 89

\ • 94 e92 \ e108 \

\90 \ 201 I I

30 40 50 60 70 80 90 100 Clay Content (%)

FIGURE 52. Graphical Relationship of the Maximum Dry Density to the

Plastic Limit and the Clay Content of the Clayey Residual Soils

....... U1 w

40

35 ,-... ~ '-"

.1-J •r-1 13

•r-1 ....:l 30 (.)

'1"'1 .1-J Cll t1l

.-1 p..

25

• 18

40

~~

~~~ va~<'\-

/

.s~~ '-.:

6\o

~~~ ~~~

I 30

\ s<'\;,

~~-<..;

~Ay# \ 25

\)~ e31 ~~ \

\ \

' • 26 •25

" • 27 •24 ' .........

25

50 60 70 80

Clay Content (%)

I 35

\ \ \

38 •

42 •

40

I \

\ "40

34 ·" • 37

•33

' ,30

" • 36

" ........... 35

90 100

FIGURE 53. Graphical Relationship of the Optimum Moisture Content to the

Plastic Limit and the Clay Content of the Clayey Residual Soils

1-' V1 +;>.

"'"' ~ '-"

~ QJ

"' s:: H

:>. .j.J

-M 0

-M .j.J {/J

!11 .-I p..

80

60

40

120

20 r

\ \

•113 113.

~~~

100

I

"" ~(j\.

-v-¢s'\-~ "V'Q;-4,.

90

9Z. / .az ba • • 1 /as 94.

108•

l \-100

\ \

\....S~"V

84,

•"'-o-v'~ --#~""

fO 1 79•

• 81

70

0 I \ V I I I I

100

0 20 40 60 80 100 Liquid Limit {%)

FIGURE 54. Graphical Relationship of the Maximum Dry Density to the

Plasticity Index and the Liquid Limit of all Soils

._. tn tn

,..-.,. N '-'

>< G)

"' .e :>. .j.J ..... t)

..... .j.J en ~

....... p.,

C)))l

~<'\,~

80 ~ ls<'\-"

"\o 40 /

36. I ~~<'\, d:;)~~

~ ·:P . 60 1-s<'\-~

~()'\. 30 • 25 '\>~~

I # I ~

()~<'\,~ I I

20 40 I 24 •

I • 27 /1 40 10

I I I 20 ,.18

I I 13.

0 I I 0 20 40 60 80 100

Liquid Limit (%)

FIGURE 55. Graphical Relationship of the Optimum Moisture Content to

the Plasticity Index and the Liquid Limit of all Soils

1-' V1 0\

157

the mechanism of slope stability (Terzaghi, (1958).

Where these clayey soils are utilized in dam construc­

tion, compaction on the wet side of optimum would signifi­

cantly reduce the susceptibility of the embankment to

seepage. The macrospaces which exist in the samples

compacted dry of optimum offer ideal channels for water flow.

Samples compacted wet of optimum contain less macrospaces

and should be more resistant to water flow. Post-construc­

tion loss of shear strength due to ped deterioration upon

saturation would also be reduced. The possibility of piping

would also be reduced.

It is also recommended that the dam embankments be

designed based on the results of Modified Proctor compaction

results rather than Standard Proctor. This would result in

higher densities with higher shear strength and less

macrospaces with a corresponding decrease in seepage.

G. RECOMMENDATIONS FOR FURTHER STUDY

The discussion presented above relating dam design and

construction to the nature of compacted soils assumes that

the soils compacted in dam embankments behave as those

compacted in the laboratory. It is believed that the theory

of compaction as outlined previously does apply to embankment

soils, but that the degree of soil structure evident in the

laboratory soils is not developed in the field.

The major recommendation based on this study is that a

darn constructed of the residual clay soils be thoroughly

158

investigated. This investigation should be centered around

the gathering and testing of undisturbed samples from the

dam itself. This investigation would be facilitated by

selection of a dam constructed of relatively stone-free clay.

Where ped structure is exhibited by the in place soil, even

slight sample disturbance could alter the apparent density.

Both a low-power and a scanning electron microscopic

investigation of the sample taken from the embankment would

aid in determining the validity of the ped or packet theory

of clay soils compacted in the field.

VIII. APPENDIX A

Dam Reports

159

DAM: Fa RESERVOIR SIZE: 23--Acres !BEDROCK FORMATION: ___ --t Roubidoux

Sec. 4 T.35 N. R.7 W.

LOCATION: Dent County EMBANKMENT: HEIGHT 3 3 ft · LENGTH 530 ft. lsoiL SERIES: Hanceville

Loam

TYPICAL DAM SECTION SOIL CLASSIFICATION:

+ ' zo

j

LL 25 PL 16 PI 9

GRADATION: % FINER

#Ul 100 #40 94 #60 78 #100 64

#200 61 10t.L 3 8

2J1. 19 tp_ 16

COMPACTION CHARACTERISTICS ASTM D 1557-,.66

MAX. DENJ21 lb/cu foPT. MOIST. --=.1~3.JL.% __

!PREDOMINANT CLAY MINERALS:

Kaolinite

COMMENTS: CEC-7.6 pH-5.6 Gs-2.68

water level 20 ft. below crest

water not passing through dam_

drop inlet W/ 3 ft. ¢ concrete pipe cutoff trench

I

I-' 0\ 0

DAM: Horns ey RESERVOIR SIZE: 40 + Acres

Sec. 6 T.37 N. R.Z E.

EMBANKMENT: HEIGHT 50 ft · LENGTH 875 ft.

LOCATION: Washington County

BEDROCK FORMATION: ___ -t Eminence

SOIL SERIES: Clarksville Stony Loam

TYPICAL DAM SECTION SOIL CLASSIFICATION:

LL 9 0 PL 4 3 PI 4 7 I

GRADATION: % FINER

#Ul 99 #200 9 7 #40 99 #60 98 #100 9 8

10/,L 95 2J.L 9 3 1~ 91

COMPACTION CHARACTERISTICS ASTM D 1557 " 66

MAX. DEN. 77 lb/cu foPT. MOIST. 38 %

PREDOMINANT CLAY MINERALS:

Kaolinite

COMMENTS: CEC- 42.1 pH- 4. 8 7 ft. freeboard

Gs-2.84

steep slopes w/ minor slides near toe--tilted fence line along toe of downstream slope

cutoff trench I-' 0'\ I-'

DAM: Blackwell RESERVOIR SIZE: l ~ Acres jBEDROCK FORMATION: ___ --f Gasconade

LOCATION: Dent County .

Sec. 26 T.35 N. R.4 W.

EMBANKMENT: HEIGHT 2 2 ft. LENGTH "530 ft. !soiL SERIES: Clarksville

Stony Loam

TYPICAL DAM SECTION SOIL CLASSIFICATION:

l

LL 60 PL 23 PI 3 7

GRADATION: % FINER

#l.Q. 99 #200 85 #40 95 #60 93 #100 89

10t,t. 77 2JL 64 1/L 56

COMPACTION CHARACTERISTICS ASTM D 1557-66

MAX. DEN. 92 lb/cu ftoPT. MOIST. 24 %

'PREDOMINANT CLAY MINERALS: ,------~ I K 1· . ao 1n1te

COMMENTS: CEC-24.1 pH- 7 .5 G -2.8 0 s 6 ft. freeboard concrete spillway drop inlet w/ 24 in. CMP previous embankment f ailure ( ? )

I

!---" 0\ N

DAM: Masters #2 RESERVOIR SIZE: 24 Acres BEDROCK FORMATION: Gasconade - Eminence

LOCATION: Dent County EMBANKMENT: HEIGHT 36 ft.

LE_NGTH 700 ft . SOIL SERIES: Clarksville Sec. 16 T. 35 N. R. 5 W. Stonx: Loam

TYPICAL DAM SECTION SOIL CLASSIFICATION:

LL 103 PL 34 PI 69

GRADATION: % FINER

#1.0 100 #200 99

#40 100 10tL 99

#60 99 2JL 95

#tOO 99 1J.L 94

SE.c /vftJ:srsli!S #I COMPACTION CHARACTERISTICS

ASTM D 1557-66

MAX. DEN. 81 lbLcu ftoPT. MOIST. 36 %

PREDOMINANT CLAY MINERALS:

COMMENTS: CEC-35.8 pH-7.5 Gs-2.84

see Masters #1

I I

1--' 0\ tN

DAM: Sunnen RESERVOIR SIZE: 40+ Acres

LOCATION: Washington County EMBANKMENT: HEIGHT 50 ft .

Sec. 4 T.37 N. R.l W~ LENGTH 1300 ft.

BEDROCK FORMATION: ___ -' Colluvial on Gasconade

SOIL SERIES: Clarksville S tony Loam

TYPICAL DAM SECTION SOIL CLASSIFICATION:

WAS H&O

LL 4 2 PL 21 PI 21 I

GRADATION: % FINER

#Ul 100 #200 87 #40 97 #60 92 #100 88

10J.L 57 2JJ- 38 1JL 3 7

COMPACTION CHARACTERISTICS ASTM D 1557-66

MAX. DEN.l08 lb/cu fbPT. MOIST. ~1..;;.8...::.% __

PREDOMINANT CLAY MINERALS: Kaolinite

COMMENTS:CEC-11.5 pH-4.9 G -2.72 s

13 ft. freeboard 150 ft. paved spillway drop inlet w/ two 4 ft. ¢ concrete

pipes tilted slope indicators

1--' 0\ +>-

DAM: Masters-~# 1

LOCATION: Dent County

Sec. 16 T.35 N. R.S w:

RESERVOIR SIZE: 24 Acres BEDROCK FORMATION: ___ -! Gasconade - Eminence

EMBANKMENT: HEIGHT 36 ft. LENGTH 700 ft • !soiL SERIES: Clarksville

Stony Loam

TYPICAL DAM SECTION SOIL CLASSIFICATION:

LL 8 4 . PL 2 5 PI 5 9 I

GRADATION: % FINER

#Ul 100 #200 96 #40 100 1011. 83

2JL 76 #60 99 #100 98 1/.L 71

COMPACTION CHARACTERISTICS .

ASTM D 1557-66

MAX. DEN. 84 lb/cu ftoPT. MOIST. --.::2:.;;;:;5....::% __

"PREDOMINANT CLAY MINERALS:

Kaolinite

COMMENTS: CEC- 21. 9 pH-5.4

5 ft. freeboard

36 in. CMP w/ hooded inlet cutoff trench spring below toe of dam

G -2.83 s

I-' 0\ V1

DAM: Sunrise South RESERVOIR SIZE: .i:::> ACres JBEDROCK FORMATION: ___ _, Potosi

Sec. 36 T.39 N. R.4 E.

LOCATION: Jefferson County EMBANKMENT: HEIGHT 35 ft · LENGTH 550 ft. lsoiL SERIES: Clarksville

Grvl. Loam

TYPICAL DAM SECTION SOIL CLASSIFICATION:

-413'~ ~

t

(rJ

LL 6 8 PL 3 0 PI 3 8 I

GRADATION: Ofo FINER

#Ul 99 #200 89 #40 93 #60 91 #100 90

10J,L 80 2JL 7 2 1J.L 70

COMPACTION CHARACTERISTICS ASTM D 155 7 -66

MAX. DEN. 88 lb/cu ftoPT. MOIST. __;;.3..;;;1~% __

PREDOMINANT CLAY MINERALS:

Kaolinite

COMMENTS:CEC-24 . 6 pH-6 .5 G -2.82 s 6 ft . freeboard

60 ft. wide unpaved spillway

seepage--marshy at toe of dam ....... 0\ 0\

DAM: Sunrise Central

LOCATION: J efferson County

Sec. 36 T .39 N. R.4 E:

BEDROCK FORMATION: ___ _, Potosi

RESERVOIR SIZE: 2 S Acres

EMBANKMENT: HEIGHT 35 ft · LENGTH 525 ft. lsoiL SERIES: Clarksv ille

Grvl. Loam

TYPICAL DAM SECTION SOIL CLASSIFICATION:

E~tooi!D

LL 7 0 PL 3 3 PI 3 7 I

GRADATION: % FINER

#l.Q 9 9 #200 92 #40 95 #60 93 #100 93

10J,L 8 7 2P- 83 1J..L. 82

COMPACTION CHARACTERISTICS ASTM D 1557-66

MAX. DEN. 85 l b / c u fbPT. MOIST. 33 %

PREDOMINANT CLAY MINERALS: Kaolinite

COMMENTS: CEC- 30.6

5 ft . freeboard

pH-4.9 G -2 . 82 s

90 ft. wide paved spillway seepage through east abutment eroded toe lake 20 ft. from toe of dam

....... 0\ -.....)

DAM: Ft. Westside RESERVOIR SIZE: !BEDROCK FORMATION:------4 Roubidoux (?)

LOCATION: Crawford County

Sec. 2 T.39 N. R.4 W~

EMBANKMENT: HEIGHT 23 ft · LENGTH 9 00 ft · lsoiL SERIES: Lebanon

Silt Loam

TYPICAL DAM SECTION SOIL CLASSIFICATION:

LL 4 8 . PL 21 PI 2 7 I

GRADATION: % FINER

#1.0 100 #40 99 #60 94 #100 89

#200 83 10J,L 56 2JL 38 1J.L 37

COMPACTION CHARACTERISTICS ASTM D 15 57 , .66

MAX. DEN}-00 lb/cu ftoPT. MOIST. 22 %

PREDOMINANT CLAY MINERALS:

Kaolinite

COMMENTS: CEC-19.1 pH-4.6 G -2. 7 2 s 3 ft. freeboard earth spillways steep slopes--but no apparent

seepage

cutoff trench

1--' 0'\ 00

RESERVOJR SIZE: 15 Acres jBEDROCK FORMATION: ___ ---t Roubidoux

DAM: Rice

LOCATION: Crawford County

Sec. 17 T.39 N. R.3 W. EMBANKMENT: HEIGHT 4 2 ft.

LENGTH 960 ft. !soiL SERIES: Lebanon Silt Loam

TYPICAL DAM SECTION SOIL CLASSIFICATION:

_, 1s'\-_ LL 2 7 PL 15 PI 1 2 1

GRADATION: % FINER

#Ul 100 #40 88 #60 71 #tOO 60

#200 58 10J,L 35

2JJ.. 21 1J.L 18

COMPACTION CHARACTERISTICS ASTM D 1557-66

MAX. DEN.121 lb/cu ftoPT. MOIST. l 3 %

.PREDOMINANT CLAY MINERALS:

Kaolinite

COMMENTS: CEC- 8. 7

3 ft. freeboard

pH-5.2 G -2.72 s

seepage below toe into marsh varment dens in backslope at water

line no cutoff trench ?

...... 0\ 1.0

DAM: Say ers RESERVOIR SIZE: 43 Acres BEDROCK FORMATION: ___ -! Potosi

Sec. 2 8 T .38 N. R.l E.

LOCATION: Washing ton County EMBANKMENT: HEIGHT 60 ft · LENGTH 900 ft · !soiL SERIES: Clark s v ille

Stony Loam

TYPICAL DAM SECTION SOIL CLASSIFICATION:

LL 1 0 5 PL 41 PI 6 4 1

GRADATION: % FINER

#Ul 10 0 #40 99 #60 99

#200 9 8 10t,t. 9 6 2t,i. 9 3

#100 9 8 1J.L 90

COMPACTION CHARACTERISTICS ASTM D 155 7-6.6

MAX. DEN. 7 4 l b / cu f t OPT. MOIST. __;,4.;;;.2..;;.% __

PREDOMINANT CLAY MINERALS:

Kao lini,te

COMMENTS: CEC-44 . 9 pH-7 . 5 G -2 . 84 s 3 f t. f r eeboar d s l ides and seepage through steep

crest section 40ft . wide - spillway- eroded cutoff trench (?)

...... -....]

0

DAM: Litt-le Prar1e

LOCATION: Phelps County

Sec. 21 T.38 N. R.7 W.

RESERVOIR SIZE: l.UU Acres jBEDROCK FORMATION: ___ --t Jefferson City

EMBANKMENT: HEIGHT 40 ft · LENGTH 1300 ft · lsoiL SERIES: Lebanon

Silt Loam

TYPICAL DAM SECTION SOIL CLASSIFICATION:

LL 57 PL 23 PI 34

GRADATION: % FINER

#Ul 99 #40 98

#200 9 5 10/.L 80

#60 98 #100 9 7

2JL 58 1/L 44

COMPACTION CHARACTERISTICS ASTM D 1557-66

MAX. DEN. 94 lb/cu ftoPT. MOIST. 27%

PREDOMINANT CLAY MINERALS: Kaolinite

COMMENTS: CEC-13.7 pH-7.8 G -2.72 s 8 ft. freeboard

granular toe drain

drop inlet

cutoff trench

I

..... --..J .....

DAM: - -~ - RESERVOIR SIZE: 6 0 Acres fBEDROCK FORMATION: ___ --t Gasconade

Sec. 20 T.35 N. R.S W. EMBANKMENT: HEIGHT 9 .~~ ~~ · I E Clarksville St. LENGTH · SOIL SERI S;_:._ ______ _

LOCATION: Dent County

TYPICAL DAM SECTION SOIL CLASSIFICATION:

LL 85 PL 35 PI 50 I

GRADATION: % FINER

#1.0 9 9 #40 98 #60 98 #100 9 8

#200 98 10tL 9 7 2JL 87 1JJ- 83

COMPACTION CHARACTERISTICS ASTM D 1557-66

MAX. DEN. 8 3 lb/cu ftoPT. MOIST. ~3....:.4....::;% __

PREDOMINANT CLAY MINERALS:

. Kaolinite

COMMENTS: Gs-2.80

6 ft. freeboard unlined spillway--eroded· very wet to~--marsh several zones of seepage through

dam and abutments

f-' -....]

N

RESERVOIR SIZE: j_ 1 ACres !BEDROCK FORMATION: ___ -! Gasconade

DAM: Elsey

LOCATION: Washington County

Sec. 30 T.37 N. R.2 E. EMBANKMENT: HEIGHT 18 f t .

LENGTH 770 ft. -- lsoiL SERIES: Clarksville Stony Loam

TYPICAL DAM SECTION SOIL CLASSIFICATION:

LL 8 4 PL 2 5 PI 5 9 1

GRADATION: % FINER

#Ul 9 9 #200 94 #40 98 10tL 86 #60 96 #100 9 5

2JL 71 1J..L. 69

COMPACTION CHARACTERISTICS ASTM D 1557-66

MAX. DEN.89 lb /cu ft .OPT. MOIST. 26 . 5%

PREDOMINANT CLAY MINERALS: Kaolinite

COMMENTS: CEC- 26. 9

4 ft. freeboard

cutoff trench

pH-7.7 G -2.79 s

two 50 ft. wide shallow spillways 1-' -.....! VI

DAM: I~II~ D:u I.a!; RESERVOIR SIZE:

LOCATION: St. Francois County EMBANKMENT: HEIGHT LENGTH

TYPICAL DAM SECTION

BEDROCK FORMATION: Potosi

SOIL SERIES:Clarksville Grvl. Loam

SOIL CLASSIFICATION:

LL 96 PL 35 PI 61

GRADATION: ~ FINER

#Ul 100 #200 98

#40 100 10tL 94

#60 99 2P. 92

#100 98 tJj. 90

COMPACTION CHARACTERISTICS

MAX. DEN. 79 lb/cu ft OPT. MOIST. 37%

PREDOMINANT CLAY MINERALS:

Kaolinite

COMMENTS: CEC- 2 7 • 9 pH-7.1 Gs-2.82 10 ft.± freeboard rock spillway massive rock downstream bench marshy valley floor

-~

...... "'-1 ~

DAM: Timberl1ne RESERVOIR SIZE: ~~ Acr~~ BEDROCK FORMATION: Potosi

LOCATION: St. Francois County EMBANKMENT: HEIGHT 75 ft. LENGTH · 67S±ft. SOIL SERIES: Clarksville

Grvl. Loam

TYPICAL DAM SECTION SOIL CLASSIFICATION:

LL 69 PL 30 PI 39

GRADATION: % FINER

#Ul 99 #200 85 #40 95 10tL 80 #60 91 2JL 79 #100 88 1J.L. 78

COMPACTION CHARACTERISTICS

MAX. DEN. 82 lbLcu fbPT. MOIST. 36%

PREDOMINANT CLAY MINERALS: Kaolinite

COMMENTS: CEC- 2 7. 8 pH-5.1 Gs-2.83 4 ft.± freeboard rock spillway eroded seepage through dam at several

locations bench added to stabilize slope

---------- ---- --------- --- ------------ -- ---- ----- ----

f-' -....J V1

176

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184

X. VITA

Arthur David Alcott was born on 28 April, 1941 in

Asheville, North Carolina. He received his primary and

secondary education in Sumter, South Carolina. After high

school graduation, he attended Colorado School of Mines,

Golden, Colorado where he received a Geological Engineering

Degree in June, 1964.

He worked as a highway engineer for the Colorado

Department of Highways until January, 1966, and as a soils

and foundations engineer for Sverdrup & Parcel and

Assoc., Inc., St. Louis~ Missouri until August, 1968. He

has attended the University of Missouri - Rolla since that

time and was a graduate assistant during the 1969-1970

school year.

The author is a registered "Engineering-in-Training"

with the Colorado Board of Professional Registration. He

is married to the former Molly Ann Orr of Lancaster,

Pennsylvania and has two daughters, Laura Ann and

Jennifer Ashley.