determination of effective porosity of soil materials

148
Agronomy Reports Agronomy 8-1988 Determination of effective porosity of soil materials Robert Horton Iowa State University, [email protected] Michael L. ompson Iowa State University, [email protected] John F. McBride Iowa State University Follow this and additional works at: hp://lib.dr.iastate.edu/agron_reports Part of the Agricultural Science Commons , and the Agronomy and Crop Sciences Commons is Report is brought to you for free and open access by the Agronomy at Iowa State University Digital Repository. It has been accepted for inclusion in Agronomy Reports by an authorized administrator of Iowa State University Digital Repository. For more information, please contact [email protected]. Recommended Citation Horton, Robert; ompson, Michael L.; and McBride, John F., "Determination of effective porosity of soil materials" (1988). Agronomy Reports. 5. hp://lib.dr.iastate.edu/agron_reports/5

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Page 1: Determination of effective porosity of soil materials

Agronomy Reports Agronomy

8-1988

Determination of effective porosity of soil materialsRobert HortonIowa State University, [email protected]

Michael L. ThompsonIowa State University, [email protected]

John F. McBrideIowa State University

Follow this and additional works at: http://lib.dr.iastate.edu/agron_reports

Part of the Agricultural Science Commons, and the Agronomy and Crop Sciences Commons

This Report is brought to you for free and open access by the Agronomy at Iowa State University Digital Repository. It has been accepted for inclusionin Agronomy Reports by an authorized administrator of Iowa State University Digital Repository. For more information, please [email protected].

Recommended CitationHorton, Robert; Thompson, Michael L.; and McBride, John F., "Determination of effective porosity of soil materials" (1988).Agronomy Reports. 5.http://lib.dr.iastate.edu/agron_reports/5

Page 2: Determination of effective porosity of soil materials

Determination of effective porosity of soil materials

AbstractThe performance of a compacted soil liner is partly a function of the porosity, which is important because thetransport of materials through the liner occurs via the pore space. This project studies the pore spaces ofcompacted soil materials to estimate the effective porosity, which is the portion of the pore space where themost rapid transport of leachate occurs. Pore space of three soil materials, till, loess. and paleosol, was studiedby using mercury intrusion porosimetry, water absorption, and image analysis. These analyses providedcumulative porosity curves from which the pore size distribution of soil samples were estimated. Theory wasdeveloped to estimate the effective porosity of a compacted soil material based upon a model of its pore sizedistribution and pore continuity. The effective porosities of compacted till. loess. and paleosol materials areestimated-to be 0.04. 0.08. and 0.09. respectively. These values are 10 to 20% of the total porosities.Comparisons between measured and predicted C1 travel times through compacted soil samples were made inorder to verify the estimated effective porosities. The estimated effective porosities are reasonable becausepredicted C1~ first breakthrough times are similar to the measured first breakthrough times in the,soilsstudied. For these three soils predicted first breakthrough times are 5 to 10 times earlier when effectiveporosity is used.in the Darcy-equation based calculations as compared to Darcy-equation-based calculationsthat utilize total porosity.

DisciplinesAgricultural Science | Agronomy and Crop Sciences

RightsWorks produced by employees of the U.S. Government as part of their official duties are not copyrightedwithin the U.S. The content of this document is not copyrighted.

This report is available at Iowa State University Digital Repository: http://lib.dr.iastate.edu/agron_reports/5

Page 3: Determination of effective porosity of soil materials

'-

//

i

l PB88·242391~ 1111111 111111111111111111111111111111

'--------------EPA/600!2-88/045August 1988

DETERMINATION OF EFFECTIVE POROSITYOF SOIL MATERIALS

by

Robert HortonMichael L. Thompson

John F. McBrideIowa State University

Ames, Iowa 50011

Cooperative Agreement No. CR-811093-01-0

Project Officer.

Walter E. Grube, Jr.Land Pollution Control Division

Hazardous Waste Engineering Research LaboratoryCincinnati, Ohio 45268

HAZARDOUS WASTE ENGINEERING RESEARCH LAB0RA.TORYOFFICE OF RESEARCH AND DEVELOPMENT

U.S. ENVIRONMENTAL PROTECTION AGENCYCINCINNATI, OHIO 45268

rIIi'-~--

REPROOUCEDBV,U_S. DEPARTMENT,OF COMMERCE.

"NATIONAL-TECHNICAL' .INFORMATION SERVICESPRINGF:IELD, VA 22161.',.'-c

"'<' , ...

~--~-----------~------j

Page 4: Determination of effective porosity of soil materials
Page 5: Determination of effective porosity of soil materials

TECHNICAL REPORT DATA(P/eaSt! read Instructions on the reverse before completing)

1. REPORT NO.12. 3'1I81'8N~S~74~°B"911ASEPA/600/2-88/045

4. TITLE AND SUBTITLE 5. REPORT DATE

August 1988Detennination of Effective Porosity of Soil Materials 6. PERFORMING ORGANIZATION CODE

-7. AUTHOR(SI ~. PERFORMING ORGANIZATION REPORT NO.

Robert Horton, Michael L. Thompson, John F. McBride -

9. PERFORMING ORGANIZATION NAME AND ADDRESS 10. PROGRAM ELEMENT NO.

-Iowa State University 11. CONTRACT/GRANT NO.

Ames, Iowa 50011CR 811093-01-0

12. SPONSORING AGENCY NAME AND ADDRESS 13. TYPE OF REPORT AND PERIOD COVEREDHazardous Waste Engineering Research Laboratory ~; n;l 1Office of Research and Development . 14. SPONSORING AGENCY CODE

U.S. Environmental Protection Agency EPA/600/12Cincinnati, OH 4526815. SUPPLEMENTARY NOTES

Project Officer: Walter E. Grube, Jr. (513) 569-779816. ABSTRACT.. > The performance of a compacted soi 1 1i ner i spa rt 1y a function of the porosity,which is important because ,the transport of materials through the liner occurs vi a thepore space. This project studies the pore spaces of compacted soil materials to esti-mate the effective porosity, which is the portion of the pore space where the mo?trapid transport of leachate occurs. Pore space of three soil materials, till, loess.and paleosol, was studied hy using mercury intrusion porosimetry, water desorption,and image analysis. These analyses provided cumulative porosity curves from which thepore size distribution of soil samples were estimated. Theory was developed to esti-mate the effective porosity of a compacted soil materi a1 based upon a model of itspore size distribution and pore continuity. The effective porosities of compactedtill. loess. and paleosol materials are estimated-to be 0.04. 0.08. and 0.09. respec-tively. These values are 10 to 20% of the total porosities. ~Comparisons betweenmeasured and predi cted -C1 ..: travel times through compacted soil sampl es were made inorder to verify the estimated effective eorosities. The estimated effective porosi-ties are reasonahle because predicted Cl~ fi·rst breakthrough times are similar to themeasured first breakthrough times in the,soils studied. For these three soils pre-dicte9 first breakthrough times are S to ao times earlier when effective porosity ~s

used.'~the Oarcy-equation based calculatnons as compared to Darcy-equation-basedcalculations that utilize total porosity.117.

.- J! .'" ;.-~ KEY WORDS AND DOCUMENT ANALYSIS.-

.1. DESCRIPTORS b.IDENTlFIERS/OPENENDED TERMS c. COSATI FieldfGroup

,--

1B. DISTRIBUTION STATEMENT 19. SECURITY CLASS (Tllu Report) 21. NO. OF PAGES

Unclassified 130

Release·to Public. 20. SECURITY CLASS (Tllis pIIlt) 22. PRICE

Unclassified /;07 •EPA Form 2220-1 (R .... 4-77) PREVIOUS EDITION IS OBSIH.I:TE -L

Page 6: Determination of effective porosity of soil materials
Page 7: Determination of effective porosity of soil materials

NOTICE

The information in this document has been funded wholly or in part

by the United States Environmental Protection Agency under assistance

agreement CR-811093-01-0 to Iowa State University. It has been

subjected to the Agency's peer and administrative review, and it has

been approved for publication as an EPA document. Mention of trade

names or commercial products does not constitute endorsement or

recommendation for use.

ii

Page 8: Determination of effective porosity of soil materials

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Page 9: Determination of effective porosity of soil materials

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Today's rapidly developing and changing technologies and indusfria1I I

products and practices frequently carry with them the increased generationt

of solid and hazardous wastes. Theselmateria1s, if improperly dealt with,can threaten both public health and the environment. Abandoned waste sitesand accidenta1:re1eases of toxic and hazardous substances to the environ­ment also have I important environmental and public health implications. TheHazardous Wast~ Engineering Research Laboratory assists in providing an

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authoritative and defensible engineer~ng basis for assessing and solving !

, these prob1ems~ Its products supportjthe policies, programs and regulations!l of the Environ~nta1 Protection Agencr, the permitting and other responsi- "! bi1ities of State and local governmenFs and the needs of both large and~ma11j)usiness,~s.Jn5~a'!l.d1ing.~hei~af.tes-J:eSpousib1¥-aJ1d ~onom:tcan¥_ - )2'0..!

iiI Ii This report 'describes the results of a study of the pore spaces of soil iI compacted to engineering specificatiops for a land-fill liner. Effective iI porosity, which is that portion of thr pore space where where the most f

rapid transpor:ti3b'f fluids takes p1ace~ is a parameter important to Iengineers designing earthen barrier structures. The data in this report I

will be usefu1:to earth science and engineering professionals involved in Idesign, constrtiction, and testing of ~arthen barriers for waste management. i

! II

For information, please contact the Land Pollution Control Division ofIThe Hazardous Waste Engineering Research Laboratory.I

Thomas R.IHauser, DirectorHazardouslWaste EngineeringResearch Laboratory

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Page 10: Determination of effective porosity of soil materials
Page 11: Determination of effective porosity of soil materials

ABSTRACT

Hazardous waste disposal landfills require liners constructed of

compacted soil material to help prevent the migration of hazardous

wastes. The performance of a compacted soil liner is partly a function

of the porosity. Porosity is important because the transport of

materials through the liner will occur via the pore space. The main

purpose of this project is to study the pore spaces of compacted soil

materials and to estimate the effective porosity, which is the portion

of the pore space where the most rapid transport of leachate occurs.

The pore space of three soil materials, till, loess, and paleosol,

is studied by using mercury intrusion porosimetry, water desorption, and

image analysis. These analyses provide cumulative porosity curves from

which the pore size distribution of a soil sample may be estimated.

Theory is developed to estimate the effective porosity of a

compacted soil material based upon a model of its pore size distribution

and pore continuity. The effective porosities of the compacted till,

loess, and paleosol materials are estimated to be 0.04, 0.08, and 0.09,

respectively. These values are 10 to 20% of the total porosities.

Comparisons between measured and predicted Cl travel times through

compacted soil samples are made in order to verify the estimated

effective porosities. The estimated effective porosities are reasonable

because predicted Cl- first breakthrough times are similar to the

measured first breakthrough times in compacted till, loess, and paleosol

materials. For the three soil materials used in this study., predicted

first breakthrough times are 5 to 10 times earlier when effective

porosity is used in the Darcy-equation-based calculations as compared to

Darcy-equation-based calculations that u~ilize total porosity.

This report was submitted in fulfillment of cooperative agreement

CR-811093-01-0 by Iowa State University under the sponsorship of the

U.S. Environmental Protection Agency. This report covers a period from

10/1/83 to 4/30/86, and work was completed as of 12/31/85.

iv

Page 12: Determination of effective porosity of soil materials
Page 13: Determination of effective porosity of soil materials

CONTENTS

Abstract ..•• "" """""""""""""""""""""""""""""""""."""."""""" """"." •. . ,.Figures" ......• "..••. ".•.. "•.•..•••.. "... "..••.•...• "••...•......••.Tables .....•..........•........••...•.........•....•.•............Acknowledgments •••••••••••••••••••

ivvi

xxii

1­2.3.4.5.6.

Introduction ......•.•...•...........•.......•............Conclus ions " " " " """""""""""""""""Recommendations"" """"""""""" """" " """" " """ """"""" """""""""Materials and Methods ••••.•••••••.••••.••••••••••••••••••Theoretical."""",,""""""" e,e""""""""""" """"" """""""""""""""Results and Discussion •••••.•••...••...••••..•••••••••••.•

1578

1936

Refer'ences.""""""""" •••••••••••••••••••••••••••••••••••••••••••••••• 113

v

Page 14: Determination of effective porosity of soil materials
Page 15: Determination of effective porosity of soil materials

Number

1

2

3

4

5

6

7

8

FIGURES

Schematic diagram of the experimental set-up usedfor the measurement of soil permeability andfor solute breakthrough curves.

Influence of n on effective porosity (E) atvarious values of 9s (9r = 0.05).

Secant CD corresponds to the pair (r.9). CDis a distance r fr~ the center of the circle.O. The normal to CD through 0 makes theangle 9 with respect to the angular origin OK.

Construction of a pattern inside a circleof radius 1 with: 9 = n/2. 92 = n/2. ~ = Sin.P(pore) = 0.3. Draw a circle with radius r =1 and choose an angular origin (1). Equation(13) shows that N = 5 for this case. Choosefive (r.9) pairs using the method describedin the text and draw the corresponding secants(2). Assign each region formed to the states"p" and "M" (pore and matrix) so that eachregion has a probability of 0.3 of beingassigned to the pore state (3). Color thepore cells black and erase the lines dividingthe matrix cells (4).

++Segment GR represents all points along line ORwhich have secantJL-intersecting ___the line segment AB. Note that AB makesthe angle B with respect to the angular origin.

Moisture density relations for (a) the tillderived soil. (b) the loess derived solI.and (c) the paleosol soil material.

Mercury intrusion porosimetry~etermined

pore size distributions for till samplesusing three drying techniques.

Mercury intrusion porosimetry determined poresize distributions for compacted loesssamples using three drying techniques.

vi

14

25

30

31

33

394041

44

45

Page 16: Determination of effective porosity of soil materials
Page 17: Determination of effective porosity of soil materials

Number FIGURES (continued)

9 Mercury intrusion porosimetry determined poresize distributions for compacted paleosol samplesusing three drying techniques.

10 Mercury intrusion porosimetry determined poresize distributions for undisturbed till samplesusing three drying techniques.

46

47

11

12

13

14

15

16

17

18

Mercury intrusion porosimetry determined poresize distributions for undisturbed loess samplesusing three drying techniques.

Mercury intrusion determined pore size distribu­tions for undisturbed paleosol samples usingthree drying techniques.

Mercury intrusion porosimetry determined cumula­tive porosity curve for compacted till samplesusing three drying techniques.

Mercury intrusion porosimetry determined cumula­tive porosity curves for compacted loess samplesusing three drying techniques.

Mercury intrusion porosimetry determined cumula­tive porosity curves for compacted paleosolsamples using three drying techniques.

Mercury intrusion porosimetry determined cumula­tive porosity curves for undisturbed till samplesusing three drying techniques.

Mercury intrusion porosimetry determined cumula­tive porosity curves for undisturbed loesssamples using three drying techniques.

Mercury intrusion porosimetry determined cumula­tive porosity curves for undisturbed paleosolsamples using three drying techniques.

48

49

50

51

52

53

54

55

19 Water desorption curves for compacted soil materials. 59

20 Water desorption curves for undisturbed till materiaL 60

21 -Water desorption curves for uriaisturbed loess material. 61

22 Permeability as a function Of time for compacted 63till material.

vii

Page 18: Determination of effective porosity of soil materials

Number FIGURES (continued)

23 Permeability as a function of time for compactedloess material.

24 Permeability as a function of time for compactedpaleosol material.

64

65

25

26

Cl breakthrough curves for compacted till material.

Cl breakthrough curves for compacted loess material.

67

68

27 Cl breakthrough curves for compacted paleosol material.69

28

29

30

Three replicates of measured and fitted (solutionto convective-dispersive equation) Cl- break­through data for compacted till materials.

Three replicates of measured and fitted (solutionto convective-dispersive equation) Cl break­through data for compacted loess materials.

Three replicates of measured and fitted (solutionto convective-dispersive equation) Cl- break­through data for compacted paleosol materials.

70

71

72

31 Cl breakthrough curves for undisturbed till material. 73

32 Cl breakthrough curves for undisturbed loess material. 74

33

34

35

36

37

38

39

Cl breakthrough curves for undisturbed paleosolmaterial.

Theoretical cumulative porosity curves asinfluenced by the n-parameter (a = 1.0,S = 8/8s )'

Measured and curvefitted cumulative porosityfor compacted till material.

Measured and curvefitted cumulative porosityfor compacted loess material.

Measured and curvefitted cumulative porosityfor compacted paleosol material.

Theoretical relative permeabil{ty (Kr ) curvesas influenced by the n-parameter (S ~ 8/8s )'

Porosity image obtained by photographing fluourescentdye in soil pores with a 35-mm camera and a macrolens. Diameter of soil sample = 5.5 em.

viii

75

77

78

79

80

82

88

Page 19: Determination of effective porosity of soil materials

Number

40

41

42

43

44

45

46

47

48

49

50

51

52

53

54

FIGURES (continued)

Example of an image of soil porosity obtainedwith circularly polarized light. UndisturbedClarinda soil materials. Frame length = 6.6 mm.

Example of a backscattered electron image of acompacted Clarinda soil sample showing holes in thesurface. Frame length = 100 1~.

Image analyzer determined pore size distributionhistogram for compacted till material.

Image analyzer determined pore size distributionhistogram for compacted loess material.

Image analyzer determined cumulativeporosity curves for (a) till materialsand (b) loess materials.

Original and Markov-generated pore patternsfor soil material A.

Original and Markov-generated pore patternsfor test image B.

Original and Markov-generated pore patternsfor soil material C.

Original and Markov-generated pore patternsfor soil material D.

Image analyzer determined pore size distri­bution histograms for the original and Markovgenerated pore patterns of soil material A.

Image analyzer determined pore size distri­bution histograms for the original and Markovgenerated pore patterns of soil material C.

Image analyzer determined ,pore size distri­bution histograms for the original and Markovgenerated pore patterns of soil material D.

Image analyzer determined cumulative porositycurves for the original and Markov-generated porepatterns of soil material D.

Original and Markov-generated pore patternsfor test image E.

Original and Markov-generated pore patterns for testimage F.

ix

90

91

96

97

99

102

103

104

105

106

107

108

109

111

112

Page 20: Determination of effective porosity of soil materials

-'

Page 21: Determination of effective porosity of soil materials

Number

1

2

3

4

5

6

7

8

9

10

11

12

13

TABLES

Listing of the values of N(L,S) forthe four possible cases.

Particle size distribution, liquid limit,plastic limit, and plasticity index ofsubsoil materials.

Classification of subsoil materials according toUSDA, AASHTO, and Unified classifications.

Particle density, undisturbed bulk density,optimum bulk density and moisture content ofsubsoil materials.

Total porosity of soil materials before andafter drying.

Volumetric soil water content at four tensionsfor compacted 'soil samples.

Permeability of three replicates of. eachProctor-type compacted subsoil material.

Permeabilities of compressed and extrudedsubsoil materials.

Permeabilities of undisturbed soil samples.

Total porosities of compacted soil materialsbefore and after freeze drying.

Parameters used with equation (8) todescribe the cumulative porosity of thesoil materials.

Measured permeabilities and times of firstchloride breakthrough and predicted effectiveporosities and noninteracting'~ollutant

breakthrough times for compacted soil materials(permeameters were 11.64 cm long).

Results of porosity analyses obtained byLeitz TAS image analyzing computer.

x

35

36

37

37

42

58

62

62

66

76

81

84

94

Page 22: Determination of effective porosity of soil materials
Page 23: Determination of effective porosity of soil materials

Number TABLES (continued)

14 Markov probability statistics for selectedpore patterns. The transitional probabilitiesare for pore to pore (P+P), pore to matrix (P+M) ,matrix to pore (M+P) , and matrix to matrix (M+M).The corresponding patterns are shown in Fig. 45,46, 47, 48, 53, and 54.

xi

100

Page 24: Determination of effective porosity of soil materials

.,!

J

Page 25: Determination of effective porosity of soil materials

ACKNOWLEDGMENTS

The authors are indebted to many individuals for their

contributions to this study. Major contributions were made by J.

Barmettler, H. Bruce, L. Wolf, T. Meyer, and G. J. Kluitenberg in

conducting laboratory experiments. We thank Dr. Darrell Norton and the

National Soil Erosion Laboratory, West Lafayette, Indiana, for access to

the Leitz image analysis system and for assistance with the image

analysis data. P. Murphy and D. Kyle contributed with the clerical work

of the project.

The study was supported by the U. S. Environmental Protection

Agency under Cooperative Agreement CR-811093-01-1 to Iowa State

University, by Iowa Agriculture and Home Economics Experiment Station

Project No. 2556, and by an Iowa State University Research Grant.

We thank Dr. Walter E. Grube, Jr., the U. s. EPA Project Officer

for providing helpful comments, discussions, and support during the

course of the project.

xii

Page 26: Determination of effective porosity of soil materials
Page 27: Determination of effective porosity of soil materials

SECTION 1

INTRODUCTION

Our technological society produces a variety of hazardous chemicals

that must be disposed of. For the foreseeable future, landfills will be

used for the disposal of these hazardous wastes. Ideally, the disposal

of hazardous wastes in landfills should be done with minimal effects on

the environment.

Compacted clay is frequently used to line hazardous waste disposal

landfills. The purpose of the compacted clay liner is to restrict the

movement of hazardous liquid materials out of the landfill. Currently,

saturated hydraulic conductivity (usually referred to as soil

permeability in the Environmental Protection Agency's design standards)

is the most common measurement used to estimate the ability of liner

material to contain wastes (USEPA, 1978). Soil saturated hydraulic

conductivity, K (L3/L2/T), is defined from Darcy's equation:

K = J/I [1)

where J is the fluid flux density (L3/L2/T) and I is the hydraulic

gradient (L/L). Soil saturated hydraulic conductivity has dimensions of

volume per unit area of liner per unit time, and thus, it is a bulk

parameter related to the areal average fluid flow in the liner.

Saturated hydraulic conductivity is often used to make preliminary

estimates of solute transit times, but knowledge of average fluid flow

alone is not adequate for accurate prediction of pollutant breakthrough

or travel time. Nonuniform flow velocities through a cross-sectional

area should be accounted for because faster-than-average fluid flow may

be responsible for the first appearance ~f the pollutant below the

liner.

The convective-dispersive equation is commonly used to model

1

Page 28: Determination of effective porosity of soil materials

miscible displacement processes in porous media. The diffusive­

dispersive coefficient in this equation attempts to describe the

nonuniform solute velocities (Van Genuchten and Wierenga, 1986).

Because the nonuniform velocities are described, this model is an

improvement over the areal average velocity approach. The disadvantage

of the convective-dispersive equation is that empirical measurements of

the diffusive-dispersive coefficient are required for each soil and set

of flow conditions. The breakthrough curve is generally the basis of

the determination (Nielsen and Biggar, 1961). With compacted clayey

materials of low permeability, the measurement of a solute breakthrough

curve may take months. Moreover, the solute breakthrough curve itself

yields a direct measurement of travel time, thereby decreasing the need

for the convective-dispersive equation for prediction of first

breakthrough time.

Effective porosity, E, has been described as that portion of the

total liner porosity that contributes significantly to fluid flow.

Effective porosities are less than total porosities because some of the

pore space is discontinuous (dead end) and some of the pore space is so

narrow that fluids in these spaces are essentially immobile. Coats and

Smith (1964), Skopp and Warrick (1974), and Van Genuchten and Wierenga

1976) all prOVide mathematical models that explicitly include effective

pore space. They describe how to use numerical solutions and

experimental breakthrough curve data to solve for effective porosity.

This report will not address these approaches in detail, but rather,

will develop a new technique based upon Darcy's equation for estimating

effective porosity and solute travel time. Because the fluid flux

density through a clay liner can be determined by using Darcy's

equation, the mean effective fluid velocity, VE, can be described by:

VE = KItE [2]

With a constant hydraulic gradient and the liner K and E both known, the

average pollutant travel distance per un~t time can be estimated. Thus,

the time of first breakthrough, T, of a noninteracting pollutant can be

predicted by the equation:

2

Page 29: Determination of effective porosity of soil materials

[3]T = EL/KI

where L is the liner thickness (m).

The Environmental Protection Agency, requires that a disposal unit

liner prevent migration during the active life of a unit (USEPA,

1982). The active life of a unit containing noninteracting pollut~nts

can be estimated by using Eq. (3). Knowledge of the liner permeability

alone is not sufficient information to accurately estimate the length of

time of liner effectiveness. When a disposal unit is constructed with

known liner thickness, L, and designed for a known hydraulic gradient,

I, measurement of both permeabilit~and effective porosit~ are required

to estimate the active life of the unit with Eq. (3). Although methods

of measuring permeability of compacted clay materials have received much

attention in the literature (Olson and Daniel, 1981), determination of

effective porosity has received little attention.

This report presents a method for estimating the effective porosity

of compacted clay materials. This method is based upon the soil pore

size distribution. The estimates of effective porosity are used in Eq.

(3) to predict the travel time of a noninteracting solute through

samples of compacted materials, independent of solute breakthrough

experiments. This work adds to the previous capillary-tube based

efforts of modeling miscible displacement (Lindstrom and Boersma, 1971;

Rao et al., 1976; Reddell and Smajstrla, 1983) by providing a simple

method for predicting solute travel time through compacted soil

material. The proposed method is tested by comparing predicted and

measured travel times.

The specific project objectives are:

1. To determine saturated hydraulic conductivities and solute break­

through curves for undisturbed and remoulded samples of till, loess,

and paleosol soil materials.

2. To obtain morphometric measurements of porosity for the soil

materials.

3. To correlate measured solute breakthrough curves with predicted

values based on the morphometric porosity measurements.

3

Page 30: Determination of effective porosity of soil materials

4. To develop a model to predict the effect of changes in porosity on

leachate breakthrough.

The study consisted of laboratory measurements to describe physical

properties of the soil materials. Theory predicting solute travel time

through the soil materials was developed and tested.

4

Page 31: Determination of effective porosity of soil materials

SECTION 2

CONCLUSIONS

1. The theory that utilized pore size distribution determined by

mercury intrusion porosimetry provided reasonable

estimates of effective porosity for compacted soil materials.

2. Predictions of Cl first breakthrough made by using effective

porosity and permeability were reasonably close to measured Cl

breakthrough for all three compacted soil materials.

3. The active lifetime of hazardous-waste-disposal units may be over­

estimated if liner effective porosity is not properly estimated and

used in the prediction of pore-fluid velocity.

4. The permeabilities of till. loess. and paleosol samples compacted

at water contents 1 to 2% higher than optimum on the moisture­

density relation curve were less than 10-9 m/s.

5. The effective porosities of the compacted till. loess. and paleosol

soil materials were estimated to be 0.04. 0.08. and 0.09.

respectively.

6. The effective porosities of the three compacted soil materials

studied were between 10 and 20% of the total porosities.

7. Undisturbed samples of the till, loess. and paleosol soi1 materials

had permeabilities greater than 10-9 m/s.

8. Cl breakthrough curves of undisturbed cores were highly skewed,

indicating the presence of macropores and thus a bimodal

distribution of pore sizes.

9. Removal of water from large samples of soil materials containing

smectitic clay was difficult to do ~ithout causing samples to

shrink, causing a decrease in total porosity.

10. Shrinkage of soil samples occurred when standard acetone

replacement techniques were used to remove water.

5

Page 32: Determination of effective porosity of soil materials

11. Removal of water without observable l~rge changes in soil structure

was possible by using methanol replacement prior to acetone

exchange.

12. Compared to oven drying and acetone drying, freeze drying caused

minimal loss of soil porosity.

13. Freeze dried samples of compacted soil materials seemed to have

increased the volume of pores in the 0.2 to 2.0 um range compared

with the original porosity before drying.

14. Impregnating samples of compacted soil material with plastic with­

out altering the porosity was very difficult.

15. Once soil samples were impregnated with plastic the task of

discerning pores from matrix required considerable human judgment

and could not be left to a computer alone.

16. Image analyzers had a difficult time describing soil porosity in

reasonable ways.

17. Use of Markov statistics to describe soil pore patterns was found

to be simple and promising for compacted materials with unimodal

pore size distributions.

18. The Markov method was difficult to use effectively on patterns

with bimodal pore size distributions and non-random spatial

distributions of pores on an image.

6

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SECTION 3

RECOMMENDATIONS

1. An estimate of effective porosity of the clay liner should be used

to calculate the active life of a disposal unit.

2. Careful mixing and compacting of soil materials is necessary to

remove the cracks and pores that occur in undisturbed soil

materials.

3. The proposed theory for estimating effective porosity should be

tested on other compacted soil materials by comparing predicted

and measured solute breakthrough times.

4. The theory should be tested with a retardation term, R,

(T = ELR/KI) that reflects positive or negative adsorption.

5. The theory should be tested by comparing predicted and measured

breakthrough times for low hydraulic gradient «25) flow

conditions.

6. Further work should be done to determine if methanol exchange and

acetone replacement methods will preserve soil porosity before

resin impregnation.

7. Further work should be done with soil impregnation techniques to

try to find a way to impregnate soil without first removing the

water.

8. Further work should be done to account for pore shape and

continuity in order to estimate the effective porosity.

9. Methods should be developed to quantify pore

structure in three dimensions in order to better characterize

the porosity.

7

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J

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SECTION 4

MATERIALS AND METHODS

SOIL MATERIALS

We collected subsurface samples from three soils developed in major

Iowa parent materials: till, loess, and paleosol. The till-derived

soil was Nicollet, a fine-loamy, mixed, mesic Aquic Hapludoll. The

loess-derived soil was Fayette, a fine-silty, mixed, mesic Typic

Hapludalf. Clarinda, an exhumed paleosol, is a fine, montmorillonitic,

mesic, sloping Typic Argiaquoll. The clay fraction of each material was

dominated by smectite, with small amounts of clay mica and kaolinite.

Undisturbed cores were collected with a hydraulically driven tube

0.065 m in inner diameter. The cores were cut into segments about 0.076

m long, placed in plastic bags, and stored at 40 C. Bulk samples of each

soil material were collected by shovel excavation. The disturbed

samples were air-dried, crushed, sieved, and stored in labeled

containers.

General Physical Properties

After the bulk samples were air-dried and ground to pass a 2-mm

sieve, selected physical properties were determined. The particle

density of each subsoil material was determined with pycnometers

according to Blake (1965a). Sand, silt, and clay contents were

determined either by total fractionation (sedimentation and weighing) or

by a pipette technique similar to that of Day (1965). Atterberg limits

(plastic limit, liquid limit, plasticity index) were obtained for each

subsoil material with standard methods of the American Society for

Testing Materials, ASTM (1964).

The particle size distribution data and the Atterberg limits were

used to classify each soil material according to the United States

8

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Page 37: Determination of effective porosity of soil materials

Department of Agriculture (USDA) textural triangle. the American

Association of State Highway and Transportation Officials (AASRTO)

classification. and the Unified classification.

The bulk density of each subsurface material was determined with

undisturbed samples. The paraffin coating technique described by ,

Blake(1965b) was used on core fragments of 70 to 100 cm3 •

Moisture-Density Relationship

The standard Proctor moisture-density relations of each air-dried.

ground subsoil material were determined. Several sub-samples of each

subsoil material were re-wetted to a range of moisture contents and then

compacted in a 0.102-m diameter mold by using a 2.49 kg rammer with a

O.305-m drop. according to the ASTM Test D-698-78. Method A (1982).

A measured mass of air-dried. sieved soil was spread thinly on a

sheet of plastic. Distilled water was misted on by using a spray bottle

until the soil at the surface was wetted. Then the soil was massed in

the center of the sheet by moving the corners of the plastic towards the

middle. The soil was further mixed by gently rubbing it between the

hands in order to break any clods that may have formed. Next. the soil

was spread out again and the above repeated until the predetermined

amount of water was applied. A uniformly moist. clod-free. friable soil

was thus obtained. which was then placed in a dishpan. sealed in a

plastic bag, and stored in a constant temperature and humidity room for

a minimum period of time as specified by ASTM standards. Finally. a

standard moisture-density relation test was performed.

Mercury Intrusion Porosimetry

The pore size distribution of undisturbed and compacted samples of

each subsoil material was determined by mercury porosimetry. Compacted

samples were prepared at moisture contents 1 to 2% higher than

"optimum", which was obtained from the moisture-density relations.

First, the undisturbed and compacted samples were broken into fragments

of -2 cm3 • Second. the fragments were p~ungedinto liquid nitrogen and

then dried in a freeze dryer for 4 to 5 days (Zimmie and Almaleh. 1976).

An alternative method of removing water from the samples was also

sought. We compared the effects of acetone drying to freeze drying and

slow oven drying on subsamples about 2-6 cm3 by using mercury

9

Page 38: Determination of effective porosity of soil materials

porosimetry. Fragments of compacted samples were dried in three ways.

Some were dried for one week in an oven set at 400 C. Some were plunged

into liquid nitrogen and then dried in a freeze dryer for'4 to 5 days

(Zimmie and Almaleh, 1976). Finally, some fragments were dried by

acetone vapor exchange by a method similar to that of FitzPatrick and

Gudmondsson (1978). These fragments were exposed to acetone vapor in

increasing concentrations of up to 100%. Then the fragments were placed

in contact with liquid acetone for 24 hours (to be strictly comparable

to resin-impregnation techniques). Finally, the acetone was allowed to

evaporate before intrusion of Hg.

Porosities of triplicate fragments (~1 cm3) of each subsoil

material and each drying method were measured by using a Quantachrome

SP-200 mercury porosimeter in four intrusion steps: 0 to 0.1 MPa, 0.1 to

8.3 MPa, 8.3 to 41.4 MPa, and 41.4 to 414 MPa (60,000 psi). Because the

volume of mercury intruded was recorded continuously as a function of

pressure, cumulative pore size could be calculated with the capillary

rise equation: r (l/p)(iy cos if», where r is the equivalent pore

radius (m), P is the pressure (Pa), y is the surface tension of mercury

(N/m), and if> is the wetting angle of mercury (assumed to be 1400 C).

Cumulative porosity was plotted as cumulative intruded volume versus

equivalent pore radius.

The specific methodology used on our soil samples after drying was

to carefully reduce samples to approximately a 1.0-cm length and O.S-cm

width; the sample chamber could hold about 3 such pieces which together

weighed around 2.0 g. Then. the sample was weighed to the nearest one

hundredth gram. Next, the sample was placed into the sample holder,

which consisted of a sample chamber attached to a bored stem; the bore

had a volume of 0.5 cm3 , which was the maximum volume of mercury that

could be intruded. An electrode plate was placed over the opening of

the sample chamber after coating with a thin layer of vacuum grease.

Then, a plastic housing was fitted over the sample chamber and an endcap

was screwed on, assuring a tight seal between electrode plate and sample

holder. The system was weighed to the nearest one hundredth gram.

Next, the above system was inserted into the filling apparatus,

consisting of a rotating jar (one-quarter-filled with mercury) and a

10

Page 39: Determination of effective porosity of soil materials

vacuum pump. Air was evacuated from the filling apparatus until -1

kg/cm 2 of pressure was reached. Then, the bell jar was rotated from a

horizontal position to a vertical one until the stem of the sample

holder was immersed in mercury. Next, air was allowed to enter the bell

jar in small increments. Since the sample chamber was sealed by the

pool of mercury, a pressure gradient developed. At -0.76 kg/cm 2 dials

indicated that mercury had filled the stem and sample chamber. The bell

jar was then rotated to the horizontal, the volume readout dial zeroed,

the microprocessor initialized, and pressure allowed to go from -0.763kg/cm to ambient. Once at ambient, the microprocessor was switched to

recall and the volume, percent volume, D (r), and surface area versusvpressure plots were drawn on graph paper.

To prepare for the high-pressure intrusion, the sample holder was

removed from the fi~ling apparatus. Upon visual inspection, one could

see that mercury was not to the top of the stem since some had already

intruded into the sample~ At this step, the stem could be topped off

either with mercury and weighed in order to calculate the bulk density

or with hydraulic oil for high-pressure intrusion; there must be a I-cm

length of hydraulic oil along the end of the stem for this. Next the

sample holder was encased in a thick metal sheath and subsequently

dropped into the high-pressure chamber. Then, the chamber was sealed

and hydraulic oil pumped in to bleed the system of air.

At this point, the pressure and volume dials were zeroed, the

maximum pressure (psi) for the run set, the microprocessor initialized,

and the pressurizing motor turned on. Pressurization continued until

the maximum was reached; the rate of pressurization was adjustable.

When the maximum press~re was reached, the pressure and volume were

recorded. Then the porosimeter began its depressurizing cycle and shut

off automatically at zero pressure; again, the pressure and volume were

recorded. Next, the plots were drawn on the appropriately scaled graph

paper. NOTE: By the time of the start 9f the next pressure intrusion,

the volume readout had decreased some more; this lower number served as

the zero for the next plot since the microprocessor zeroed the x-y scale

every time it initialized.

The above steps were repeated for all of the desired pressure

11

Page 40: Determination of effective porosity of soil materials

intrusions except that the volume dial was not zeroed. At the end of

the 0-60,000 psi intrusion the sample holder was removed from the

pressure chamber and sheath and the stem was topped off with mercury;

the system was weighed in order to calculate the bulk density after

intrusion to 60,000 psi (414 MPa).

We calculated initial total porosity (£) of the samples from the

relation £ = 1- (Pb/pp )' where Pb = bulk density and Pp = particle

density. Bulk density of compacted samples was known because a known

mass of soil material was compacted to a known volume. Particle density

for each soil material was determined with a pycnometer, according to

Blake (1965a).

Bulk density of freeze-dried samples at 0.1 MPa (i.e., ambient

pressure) in the porosimeter was calculated by using the relation:

~ = mIl {(v1+v 2)- [(m3-m2)/PHg]) [4]

where m1 = sample mass (Mg), VI = volume of sample holder (m3), v2 =3volume of mercury intruded at 0.1 MPa (m ), m2 = mass of sample holder

(Mg), m3 = mass of mercury-filled sample holder with sample after

intrusion to 0.1 MPa (Mg), and PHg = density of mercury (13.541 Mg/m 3 at

200 e). Total porosity calculated from these bulk density values and the

pycnometer-determined particle density was consistently very close

(within 0.01 to 0.02 cm3 of porosity per cm3 of soil) to total porosity

values calculated for freeze-dried samples after mercury intrusion to

414 MPa, suggesting that total porosities at ambient pressure and after

pressurization were essentially equal. Total porosity of oven-dried and

acetone-dried samples was calculated solely from mercury intrusion data.

Water Desorption

Standard soil-water characteristic data were obtained for compacted

samples by determining soil water contents of duplicate samples at 0.05,

0.1, 0.2, and 1.5 MPa. These pressures correspond to equivalent pore

radii of 3, 1.5, 0.75, and 0.1 urn, respectively, and were chosen to

measure pores in size ranges roughly comparable to those measured by the

mercury porosimeter. Samples were equilibrated at those pressures by

using a standard pressure plate apparatus (Bouma et al., 1974). The

water contents of undisturbed till and loess materials were determined

at 0.01, 0.025, 0.05, 0.075, 0.10, 0.20, 0.30, and 0.40 MPa.

12

Page 41: Determination of effective porosity of soil materials

Permeability

Permeability of compacted soil materials was measured in two

ways. The first method used compressed and extruded samples, and the

second method used Proctor-type, compacted samples.

From the moisture-density relation data, a point one or two

percentage points above "optimum" moisture content was chosen. A

calculation was made to determine the mass of moist soil at the given

moisture content needed to form a 6.35 cm diameter by 2.54 em high

cylinder at the corresponding dry density. The loose, moist soil was

placed into a mold consisting of a base-plate, cylindrical wall and

plunger. A hydraulic press was used to force the plunger down until a

mark was reached indicating that the plunger was 2.54 em from the base

plate; the hydraulic press did not indicate a load-pressure at this

stage. Next, the compacted soil sample was extruded by forcing the

plunger through. Then, the sample was placed in a properly labeled

plastic bag and stored in a refrigerator.

The pressed soil samples described above were placed in 7.62-cm

diameter acrylic permeameters. Paraffin, kept at 600 C, was poured

between the wall of the permeameter and the sample in 0.5-cm increments

until the top of the sample was reached; the paraffin was allowed to

solidify between increments. In this manner, any gaps formed when the

paraffin cooled were filled by the next increment.

Next, a solution of de-aired, saturated CaS04 with 0.06%

formaldehyde to control microbial growth, was introduced into the

permeameter and pressurized from an air-pressure source. The air was

separated from the solution by means of a rubber membrane within the

solution container (Figure 1 displays the physical set-up). Hydraulic

gradients in the range of 100-200 were used. Because of the relatively

small sample height, this required a hydraulic head of approximately

250-500 em H20 (3.5 - 7.5 psi). Once the hydraulic gradient was

established, a minimum of 5 pore-volumes was passed to obtain a constant-'

flux from which to calculate the hydraulic conductivity.

With the second method, the permeability of each compacted subsoil

material was measured by using a 0.102-m diameter, 0.116-m long

permeameter. Three replicates of each subsoil material were compacted

13

Page 42: Determination of effective porosity of soil materials

< Air pressure from regulated source

Flexible membrane

Pressurized chamber-#------(contains leaching solution)

Tomanometer

<

leachate intest tube

-++--- Paraffin wax

Soil sample ---------+l-~~

Paraff i n wa x ---------+I-

Chemi ca1ana lys i s ~------=----_....

Schematic diagram of the experimental s.et-up used for the-measurement. 0 f -soilpermeabi lit:y-and for -so1ute--hreakthr-Dugh-curves.

Chamber

Rotating fractioncollector

Figure 1.

14

Page 43: Determination of effective porosity of soil materials

at moisture contents ~1 to 2% above optimum, determined from the

moisture-density relation. De-aired, saturated CaS04 solution (adjusted

to 0.06% formaldehyde to control microbial growth) was introduced at 6.9

kPa pressure at the bottom of the permeameter to slowly saturate the

compacted sample. The source of the pressure was compressed air. _ The

air was separated from the saturated CaS04 solution by a rubber membrane

within the solution container to help prevent the desaturation of the

soil material. After saturating the material, the CaS04 solution was

introduced at the top of the permeameter at hydraulic gradients of ~170

to 270, and the rate of solution movement through the sample was

measured over time.

Permeability was determined on undisturbed soil samples for each

soil material. The undisturbed materials were placed into permeameters

and sealed with paraffin wax. Constant-head methods (Klute, 1965) were

used to determine soil permeability.

Solute Breakthrough

Solute breakthrough measurements were made for compacted and

undisturbed soil samples. The breakthrough measurements were made on

the same soil samples used to determine permeability. Thus,

breakthrough measurements were made on two sizes of disturbed samples

and one size of undisturbed sample.

Solute breakthrough curves were obtained for each compacted and

undisturbed subsoil sample. A de-aired, 0.05N CaC1 2 solution with

0.016% Acid Fuchsin (a red dye), and 0.06% formaldehyde was used as the

tracer solution. The dye gave a visual test for any permeameter wall

leakage. The tracer solution was exchanged for the saturated CaS04

solution and allowed to leach through the compacted soil sample under

the same hydraulic gradient used in the permeability test. The leachate

was collected in equal-volume increments with a fraction collector and

the leachate was analyzed for chloride concentration with an automatic

titrator.

IMAGE ANALYSIS

Sample preparation techniques

We "fixed'· the pores of soil samples by filling them with a plastic

resin (impregnation) and hardening the resin (curing) by heating it.

is

Page 44: Determination of effective porosity of soil materials

Because the resin was not miscible with water. it was necessary to

remove all water from the samples before impregnation. The standard

method among soil micromorphologists to remove water is by replacement

with acetone (Miedema et al •• 1974; FitzPatrick and Gudmundsson. 1978).

and this was the first method tried.

Typically. a compacted sample about SO cm3 was placed either in

contact with acetone or in 100% acetone vapor for a period of about one

week. The acetone was changed every day or every other day until it

contained less than 3% water. At that point. the sample was impregnated

with a mixture of polyester resin and acetone (SO/SO by volume) and

placed under a vacuum for 2-3 hours. The sample was left to sit.

covered. for a period of 2 to S days. then it was uncovered and left in

a laboratory hood for another 2 to Sdays. Finally. the sample was

gradually heated over a period of 2 to S days from 300 C to 60oC. This

slow heat treatment normally caused the samples to harden well enough

that they could be cut open with a diamond trim saw. Details of

treatments similar to those described above may be found in

FitzPatrick's (1984) book.

We removed water from the high-clay soil samples (Fayette and

Clarinda) by a two-step process that employed methanol. We immersed

moist, compacted samples of about SO cm3 in 100% methanol in a covered

container. Each day for a week the methanol was changed until the

amount of water in the methanol was <S%. Then the samples were immersed

in acetone in the same covered container. The acetone was changed each

day until the level of methanol in the acetone was <S%. Following these

treatments. the samples were impregnated with a resin/acetone mixture in

the normal way.

Obtaining an image

The primary technique that we used to obtain an image of the

porosity of impregnated soil samples was with a macro lens and a 3S-mm

camera. In the resin/acetone mixture us~d for impregnation we dissolved

a small amount (~.3%) of a dye (Uvitex-OB, CIBA-GEIGY Chemicals Corp.)

that is sensitive to ultraviolet light. After the impregnated sample

was cured. cut open, and polished by standard petrographic techniques,

it was photographed under ultraviolet light by using Kodak Ectagraphic

16

Page 45: Determination of effective porosity of soil materials

He (high contrast) film. Because only pores contained resin and dye,

only pores were exposed on the film. Following printing, these images

were typically about 2X the size of the original samples. This

technique was originally developed by Murphy et ale (1977a).

We experimented with two other techniques to obtain porosity

images. In the first instance, we prepared thin sections of the

hardened soil blocks by standard petrographic techniques. These

sections were about 30urn thick, as measured by the birefringence of

quartz in the samples. When viewed in circularly polarized light, all

mineral materials should have some birefringence unless they are opaque

or the c-axis of the mineral is exactly perpendicular to the stage of

the microscope (Pape, 1974). By using this principle, we made

photographs in circularly polarized light with a modified petrographic

microscope and high-contrast film. After printing, these images were

typically about 20X the size of the original samples.

The final technique used to obtain images of soil porosity employed

a scanning electron microscope and backscattered electron detectors. A

hardened block of soil was cut into pieces measuring about 2.5 x 2.5 x

1.2 cm. One face of each piece was polished with polishing grits,

gradually changing from 180 grit to 600 grit to I-urn diamond grit. A

200-~ coating of gold was put on the polished surface with a vacuum

sputter coater. The sample was then viewed with a JEOL U3 scanning

electron microscope operated in backscatter mode at 25 kV. In theory,

the difference in atomic number between resin in the pores and minerals

in the soil matrix should provide significant enough contrast for the

two phases to be distinguished. Images were typically magnified

1000X. This approach to obtain soil porosity images was first reported

by Jongerius and Bisdom (1981). Problems that we identified with each

of the imaging techniques we used are discussed in the Results and

Discussion section.

Analyzing the images _'

Once obtained, images of soil porosity are normally very complex.

While it is possible to digitize such images by hand, this would be an

enormous task. Therefore, we sought image analyzing computers that

would automatically digitize each image and then quantify the digitized

17

Page 46: Determination of effective porosity of soil materials

elements. We took three approaches.

First, we utilized a microcomputer, a digitizing board compatible

with the microcomputer, and a video camera that captured the porosity

image and sent it to the digitizing board. We adapted the algorithms of

Lin and Harbaugh (1984) to perform a pattern analysis of each image.

Second, we employed an image analyzing computer manufactured by

LeMont Scientific, Co. This computer is capable of digitizing an image

into 4096 x 4096 pixels, but there is no way to edit the image

manually. Algorithms used in measuring objects in the image are

proprietary, but indexes of area, perimeter, length, width, and

orientation for each object in the image are obtained. The accuracy of

area and perimeter measurements depends upon the intensity of

digitization chosen by the operator, the available computer memory, and

the algorithm. itself. "Length" and "width" measurements are actually

projections of an object onto certain coordinate axes specified by the

algorithm. Orientation is the angle made by the long axis of an object

with respect to the horizontal.

Third, we employed a Leitz Texture Analysis System (TAS). This

computer is capable of digitizing an image into 512 x 480 pixels. In

addition, each image can be edited manually and complex operations such

as erosion and dilation can be performed on the image by computer

programs. Individual objects in the image are measured with respect to

equivalent spherical diameter (derived from an area measurement),

perimeter, orientation, Feret minimum, and Feret maximum. Feret

dimensions are measurements made by projecting each object onto chosen

coordinate axes •. Although the specific algorithms used by the Leitz TAS

are proprietary, their principles have been discussed by Serra (1980).

All three of our approaches to automatic image analysis had the

same basic mechanics: a video camera, a digitizing board, and a

computer. There were differences in the amount of computer memory

available to store and manipulate each i~age and in the sophistication

of the programs used in analysis. The LeMont image analyzer was also

set up to obtain a digital image directly from a scanning electron

microscope without the intermediary of a video camera.

18

Page 47: Determination of effective porosity of soil materials

SECTION 5

THEORETICAL

This section contains description of the theory developed to

estimate the effective porosity of compacted soil materials. Also in

this section is a description of the Markov analysis techniques used in

this study.

In general, there are two ways to investigate soil porosity:

behavioral measurements and morphological measurements. The behavior of

fluids (both liquids and gases) in soils is largely determined by the

morphology of the pore space. To make predictions about fluid behavior

in soils under field conditions, one normally measures fluid behavior

under laboratory conditions and then makes extrapolations.

Alternatively, it is possible to make morphological measurements of the

pores in a soil (e.g., size, shape, and continuity), and then make

behavioral predictions based on fundamental theory of fluid behavior.

Morphological measurements are also used to distinguish one soil from

another or to identify the effects of soil treatments (e.g., compaction

or tillage).

The simplest method of morphological measurements relies on the

principle that the pressure (or tension) at which a fluid is held in a

capillary tube depends on the radius of the tube and on the surface

tension and wetting angle of the liquid. This principle is formalized

in the capillary rise equation:

r = -(1/P)(2y cos ~) [5]I

where r = equivalent pore radius (m), P = pressure (Pa), y = surface

tension of the liquid (N/m), and ~ = wetting angle of the liquid.

Two common techniques are based upon this equation: water retention

measurements and mercury intrusion porosimetry. In water desorption

i9

Page 48: Determination of effective porosity of soil materials

measurements, water is gradually pulled out of a saturated soil sample

stepwise by equilibration at different pressures. In mercury intrusion

porosimetry, mercury is gradually pushed into the soil sample with

increasing pressure. In both instances, the volume of fluid pulled out

or pushed in at known pressures or tensions gives information about pore

sizes in the sample. Typically, a continuous distribution of pore radii

is obtained. Such a distribution assumes that all pores in the sample

act like continuous, discrete capillary tubes. Even though these

assumptions are an inaccurate description of soil porosity, the

information gained from capillary-rise measurements can be used as a

starting point for modeling soil porosity and for making predictions of

fluid behavior based on porosity. In this regard, we have employed the

approaches of Van Genuchten (1980) and Mualem (1976).

Another general approach to morphological measurements of soil

porosity uses visual images of the pores in a soil sample. Of course,

the image itself is a simplified model of the porosity, especially

because the image is normally two-dimensional. But information

different from that of capillary-rise techniques can be obtained from

images. Besides pore size, characteristics such as pore shape and pore

patterns can be studied.

There are three different conceptual approaches to image analysis

of soil pores: measurement of individual pores, stochastic modeling, and

stereology. In our work, we have employed the first two methods. The

third method, which has its roots in analysis of biological micrographs

(Weibel, 1979) has only recently been directed to soil porosity images

(Ringrose-Voase and Nortc1iff, 1987).

Measurements of individual pores on photographs can be made

manually, but it is the image analyzing computer which has made this

approach practical. For each pore on an image, indexes of size and

shape are obtained by counting pixels (picture points) covered by the

pore. Statistics for individual pores a~e summed and distributions of

pore size and shape on the image are calculated. These techniques have

been discussed by Bullock and Murphy (1980), among others.

Instead of measuring individual pores on an image, it is also

possible to analyze the pattern of pores on an image, if one assumes

20

Page 49: Determination of effective porosity of soil materials

that the pores are randomly distributed in the two-dimensional space of

the image. Dexter (1976) first developed this approach for soil

porosity images, and a similar approach has been used by Lin and

Harbaugh (1984) to model porosity in rocks. Briefly, a two-dimensional

image is again digitized into pixels. The probabilities of transition

from pore to pore or from pore to non-pore (i.e., soil matrix) are

compiled. Probabilities so measured may be used to compare one image to

another or to generate another, statistically identical, image.

Although Lin and Harbaugh (1984) have extended the theoretical approach

from two to three dimensions, serial-section images are required, and

their preparation is very time-consuming.

Although considerable effort has been made to develop image

analysis techniques for soil porosity studies, there have been\

relatively few predictions of soil behavior based on image analysis

measurements. Bouma et al. (1979), for example, needed a matching

factor to compare predicted saturated hydraulic conductivity with

hydraulic conductivity measured in the laboratory. Walker and Trudgill

(1983) attempted to correlate image analysis measurements with tracer

breakthrough measurements in laboratory columns. Dexter (1978) found

image analysis to be most useful as part! of a computer simulation model

of root movements in tilled soil. Image analysis has also been used to

identify the effects of soil compaction on pore shape and orientation

(Murphy et al., 1976).

EFFECTIVE POROSITY

To estimate the travel time of noninteracting pollutants through a

liner by Eq. (3), the liner's effective porosity must be determined.

Earlier, effective porosity was described as that portion of total

porosity that contributes significantly to fluid flow. We now define

"significantly" by defining effective porosity as that portion of total

porosity that conducts fluid faster than the average pore-water

velocity •. Large continuous pores conduc; fluid faster than do small

continuous pores. Therefore, in a porous medium that exhibits a range

of pore sizes, a range of pore-water velocities will exist as a fluid

passes through. Higher-than-average pore-water velocities will be

responsible for the first appearance of pollutants, whereas lower-than-

21

Page 50: Determination of effective porosity of soil materials

average pore-water velocities will not. Thus, the determination of the

soil porosity versus soil pore-water velocity distribution is crucial to

the evaluation of the soil's effective porosity.

The pore-water velocity distribution can be calculated from the

unsaturated permeability, K(S), as a function of fluid-filled porosity,

S. Based upon theory developed by Mualem (1976), Van Genuchten (1980)

showed that the unsaturated permeability could be predicted from the

total porosity, the residual porosity (i~e., the volumetric water

content when water films lose effective continuity), and a measure of

the uniformity of pore sizes by the equation:

[6]

where Ss is the total porosity, Sr is the residual porosity, and m = [1­

(l/n)] for O<m<I, where n is an empirical parameter that describes the

uniformity of pore size. Ss' Sr and n can be determined from a

cumulative porosity curve.

Cumulative porosity curves may be obtained by either soil-water

desorption techniques, image analysis, or mercury-intrusion

porosimetry. For recompacted material, the latter method is generally

preferred because of its speed and range. Both approaches are based on

the capillary-rise equation, which for mercury porosimetry may be

formulated:

r = - (I/P)(2r cos~) [7]

where r = pore radius (m), P = pressure (Pa), r = surface tension of

mercury (N/m), and ~ = wetting angle of mercury (1400). To obtain Ss'

Sr and n from mercury-intrusion curves, we adapted an equation

originally developed by Van Genuchten (1980) for soil-water desorption

curves:

S = S + (S -S )[1 + (a/r)n](I/n)-1r s r

where r is the pore radius from Eq. (7) and a is an empirical./

[8]

parameter. To use Eq. (8) to model mercury-intrusion curves, we define

Ss as equal to the total porosity of the freeze-dried samples, and we

transform the mercury-intrusion cumulative porosity curve to a form

similar to the soil-water characteristic curve as follows: S

22

Page 51: Determination of effective porosity of soil materials

where SRg = mercury-filled porosity. Once the cumulative porosity

curves are transformed, the Sr' n and a parameters (Eq. 8) can be

determined by using nonlinear regression techniques (Van Genuchten,

1978).

The Sr and n parameters can also be estimated from a graphica~

display of the transformed data. The residual porosity, Sr' is

approximated as the value of S that the cumulative porosity curve

asymptotically approaches as limiting pore size decreases. Mercury­

intrusion cumulative porosity curves for compacted soil samples

generally have Sr-values approximately equal to their non-mercury-filled

porosities after intrusion to 414 MPa (60,000 psi). For soil materials

considered for hazardous waste disposal liners, Sr is generally less

than 0.1. The n-parameter is estimated as follows: the cumulative

porosity data is plotted as S vs log r; next, the absolute value' of the

slope, s, of the cumulative porosity data is calculated at a value of e

and Ss. The n-parameter is then

(following Van Genuchten, 1980):

approximately halfway between Sr

determined by using the equation

n =Jexp (0.8 Sp)

{.11 (0.5755 0.1 0.025)Sp - Sp2 -:sp3

(O<Sp~ 1)

( Sp>l) [9 ]

where Sp is equal to s/(Ss - Sr).

The pore fluid velocity distribution can be described by

differentiating Eq. (6) and multiplying by the hydraulic gradient.

I(dK( S)/dS)

[(1_Sl/m)m-1 - (1_Sl/m)2m-1] [10]

where S = (S -SriSs -Sr). Equation (10) is monotonic in that (dK(S)!de)

continuously decreases as S decreases.

A design engineer determines soil permeability by measurement and-'

controls the hydraulic gradient and total porosity, Ss' by

construction. This information allows the calculation of an average-

fluid velocity, V, for a liner (V = KI/S s ). But some portion of the

total porosity conducts fluid at a velocity greater than the average

23

Page 52: Determination of effective porosity of soil materials

velocity, and some portion conducts fluid at a velocity less than the

average velocity. We defined effective porosity, E, as that portion of

the total porosity that conducts fluid faster than the average fluid

velocity. Therefore a minimum cutoff pore-fluid velocity, Vmin , is set

equal to V. Once Vmin is selected, I(dK(S)/dS) is set equal to Vmin and

Eq. (10) is solved for S. The determined value of S represents a

porosity cutoff point, Sc' i.e., all values of S larger than Sc have an

associated pore-fluid velocity greater than Vi' and all values of Sm nsmaller than Sc have an associated pore-fluid velocity less than Vmin •

Thus, the effective porosity equals that proportion of the pore space

greater than or equal to Sc. Effective porosity, E, can be determined

from· the equation:

E = (I-Sc)(Ss - Sr) [11]

Once the effective porosity is estimated, the time required for

noninteracting pollutants to first appear at the bottom of a clay liner

can be predicted by Eq. (3).

Our method to estimate the effective porosity determines the

portion of total porosity that conducts fluid faster thanVmin • This

portion is assumed responsible for the total Darcian fluid flux

density. In reality, this assumption is not entirely correct because

the portion of porosity that conducts at less than Vmin is responsible

for a small part of the Darcian fluid flux density. The mean velocity

of pore water in the range of pore space that we refer to as effective

porosity is actually:

VE = [K - K(S )] II (S - S )c s c

where S represents the cutoff value of water filled pore space.c

Equation (2) provides a slightly elevated value of VE because in Eq. (2)

the K(S ) term is assumed to equal zero. In reality, K(S ) # 0, butc cK(S ) is much less than K so that it can be conveniently ignored.c

Equation (II) shows that effective porosity is a function of Ss'

Sr' and Sc' Sc can be determined as the~root of Eq. (10) once Vmin , K,

I, and n are specified. We have proposed selecting Vmin by setting it

equal to V. Because V is directly proportional to K and I, Vmin must

also be directly proportional to K and I. A result of this specified

equality, Vmin = V, is that Sc becomes independent of K and I; i.e., the

24

Page 53: Determination of effective porosity of soil materials

3.53.212.52.21n

1 . 5

.03

· 021 w::;...__--L --'- ...1-_....:......_L-__--.J

1 • 21

\,~

· 15es=0.,5.·

· 12Els=0.4

.219

E8s=0.3

.216

Figure 2. Influence of n on effective porosity (E) at variousvalues of e (8 = 0.05).

s r

25

Page 54: Determination of effective porosity of soil materials

same value of Sc will be calculated as the root of Eq. (10) for all

values of K and I as long as the product of K and I is greater than

zero. Therefore, the effective porosity, E, as defined in this paper,

is a function only of es' er , and n. The relationship between E and n

for a range of es with er = 0.05 is shown in Fig. 2.

Once es and n are estimated from the measured cumulative porosity

data, the effective porosity can be estimated from Fig. 2. With an

estimate of the effective porosity, the time required for the first

appearance of noninteracting pollutants at the bottom of a clay liner

can be predicted by using Eq. (3).

Markov Analysis

Much of the theory and terminology used in our Markov analysis

comes from Markov statistics. Markov statistics are useful for

analyzing systems that have two somewhat contradictory properties (1)

randomness in time or space, and (2) relatedness in time or space.

Relatedness is said to exist if all events are influenced in some way by

preceeding events. Any system that displays these properties can be

called Markovian.

For example, the weather system is strongly Markovian in that

weather conditions on one day influence conditions on the following

day. Markov statistics allow us to analyze this kind of dependence and

use it to model a system more accurately than if we had assumed the

system to be totally random.

An ordered sequence of events is spoken of as a Markov chain. In

our analysis we are interested in first-order, discrete Markov chains.

First-order indicates that the influence of only the immediately

preceeding event will be analyzed, although a given event may be

influenced by several preceding events. The word discrete indicates

that each event can have only a finite number of states. The change of

state value from one event to the next is called a transition (this is

true even if the state value remains the same between events).

For example, consider a system in which I ask my friend to have

dinner with me. The events correspond to replies. Each event has one

of two states: 'yes' or 'no.' We assume that a sequence of responses

are: no, no, no, yes, yes, yes, yes, yes, no, no, no, yes, yes.

26

Page 55: Determination of effective porosity of soil materials

The marginal probability of a state is defined as the ratio of the

frequency of the state to the total number of events in the chain. In

our example, the marginal probability of a 'yes' is 7/13.

Using this same example, we can see how the influence of events on

each other can be determined. In the above chain there are four no->no

transitions; five yes->yes transitions; two no->yestransitions; and one

yes->no transition. Altogether there are 12 transitions. The

probability of a given type of transition can be found by dividing its

frequency by the total number of transitions.

This information can be arranged as follows:

Initial State

Yes No

Final State Yes 5/12 2/12

Final State No 1/12 4/12

At this point it is convenient to introduce the notation p(AIA),

which we will interpret to mean the probability of an event with state A

immediately following an event with state A in a Markov chain. By using

only marginal probabilities to estimate P (yes I no), we arrive at P

(yes I no) = 7/13. An estimate of P (yes I yes) is also 7/13 because

marginal probabilities give us no information about how the preceding

state affects the following state. However, using transitional

probabilities we arrive at P (yes I no) = 2/12 and P (yes I yes) =5/12. The motivation of computing transitional probabilities is that

they allow us to more accurately predict the state of events following a

given event and are better descriptors of the existing data than the

marginal probabilities alone.

Many properties of soil, such as thermal diffusivity, water

retention, compactability, hydraulic conductivity, and miscible

displacement, depend largely on the spatial arrangement of pores in the

soil matrix. Often the matrix-pore arrangement is modeled assuming that

the matrix elements or the pores have a ~imple uniform geometry. For

example, the capillary tube models and the packed sphere models are

often assumed. Naturally these simplified geometries do not reflect the

range of complexity and irregularity of soil structure. One method of

describing soil structure that puts fewer restrictions on the sizes and

27

Page 56: Determination of effective porosity of soil materials

shapes of the pore and matrix elements involves Markov statistics.

Markov statistics have been used in the consideration of

transitions between pores and matrix elements along a straight line of a

soil surface. A one-dimensional Markov analysis has been used to

compare tillage effects on soil properties and to predict root gr~wth

(Dexter, 1976,1978). Multidimensional Markov analyses may prove to be

even more useful.

Multidimensional applications of Markov statistics in the'

literature are few. Pielou (1964) treated vegetation patterns in the

plane, and Kretz (1969) produced a statistical study of mineral grains

also in the plane. Lin and Harbaugh (1984) proposed an algorithm,

intended for computer image analysis, to compute Markov statistics from

two- and three-dimensional geological data. These statistics were used

in combination with a random number generator to produce patterns with

Markov statistics similar to the ?riginal data. Lin and Harbaugh

empirically demonstrated the consistency between the statistics of the

original patterns and of the patterns produced with the random number

generator. Lin and Harbaugh did not establish whether the generated

patterns shared properties beyond similar Markov statistics with the

original patterns, or whether the algorithm was applicable for any given

original pattern. We have attempted to determine whether the algorithm

of Lin and Harbaugh is appropriate for use in soil porosity studies and

to suggest the circumstances under which the algorithm used by Lin and

Harbaugh does not apply.

Presented in this section is the theory behind the algorithm of Lin

and Harbaugh (1984). A restricted case of this algorithm is considered

in which planar patterns consist of only two states (pore and matrix).

By using this algorithm, pore-matrix patterns are obtained by

assigning independently and randomly the states "pore" or "matrix" to

cells that subdivide a circular region. The geometry of these cells is

governed by three parameters: 81, 82' an~ A. The parameters 81 and 82

limit the range of elongation directions for .individual cells. The

parameter A affects both the total number and the sizes of the cells.

To understand how cells are determined, consider a circle of radius

R whose center is the pole of a set of polar axes. The cells that

28

Page 57: Determination of effective porosity of soil materials

subdivide this circle are formed by the intersections of secants to the

circle. Each secant corresponds to an ordered pair (r, e) where rand e

are restricted as follows:

R < r < -R

e1 ~ e ~ eZ

-n/Z ~ e1 < eZ ~ n/Z [lZ]

For an ordered pair (r, e) the corresponding secant is the unique secant

at distance r from the pole whose normal through the pole makes the

angle e with respect to the angular origin (see Figure 3).

The pairs (r, e) are chosen from a rectangular region in the

*Cartesian r- e plane. Letting R represent this region, then

* *R = {(r, e): -R < r < R, e1 < e ~ eZ)}. Each pair is chosen from R by

using a planar Poisson point process with average density A per unit

area. (One can generate (r, e) pairs corresponding to a planar Poisson

process by choosing randomly and independently rand e and then pairing

them, keeping in mind the restrictions of Equation 1Z.)

The number of secants comprising a pattern is assumed to be

determined by a random variable with a Poisson distribution and mean N

where:

N = A .rJ R* drde [13]

A complete set of parameters for generating a pattern consists of

e 1 , eZ' A and P(pore), i.e., probability that any given cell will be

assigned to the pore state. When generating a pattern from a set of

model parameters, the number of secants is best chosen to be N (rounded

to an integer). Figure 4 shows the stepwise graphical construction of a

pore-matrix pattern.

The parameters e 1 and eZ can be estimated by simply noting the

range of elongation directions of the pores in a given pattern. The

smaller limit of elongation direction corresponds to e 1 and the larger

to eZ• If there is no particular orientation to the pores then e1 =-n/Z and eZ = n/Z. .'

Naturally, the pore-matrix patterns encountered in practice will

not be composed of cells generated by random secants. However, to

estimate A it is assumed that the patterns of interest are generated by

the procedure shown in Figure 4. (The validity of this assumption has

29

Page 58: Determination of effective porosity of soil materials

c

Figure 3. Secant CD correspond to the pair (r,e). CD is adistance r from the center of the circle, O. Thenormal to CD through 0 makes the angle e withrespect to the angular origin OK.

30

Page 59: Determination of effective porosity of soil materials

Figure 4. Construction of a pattern inside a circle of radius 1with: 8 = n/2, 82 = n/2, A = SIn, P(pore) = 0.3.Draw a circle with radius r = 1 and choose an angularorigin (1). Equation (13) shows that N = S for thiscase. Choose five (r,e) pairs using the methoddescribed in the text and draw the correspondingsecants (2). Assign each region formed to thestates "p" and "M" (pore and matrix) so that eachregion has a probability of 0.3 of being assigned tothe pore state (3). Color the pore cells black anderase the lines dividinE the matrix cells (4).

31

Page 60: Determination of effective porosity of soil materials

not yet been analyzed in the literature). To arrive at an estimate of

~, estimates of the expected number of secants intersecting a segment

lying within a pore-matrix pattern are made using two different methods.

The value of N(L,a), the expected number of secants intersecting a

segment of length L that makes an angle a relative to the angular _

origin, does not depend upon the position of the segment within the

pattern. Thus the general segment with length L and orientation a will

be referred to as segment AB.

Let Si represent the state of the point with label i. For two

points (A and B) in different cells, p(SAISB) represents the conditional

probability that point A is in state SA given that point B is in the

same state. P(SA) is the overall or marginal probability of state SA

within the pattern. In an extension of a theorem by Switzer (1965), Lin

and Harbaugh (1984) show:

p(SAISB) = P(SA) [l-exp(-N(L,a»] + exp(-N(L,S» [14J

where N(L,a) is the expected number of secants intersecting AB.

Solving for N(L,S) yields:

N(L,a) = In {[p(SAISB) - P(SA»)/[l-P(SA)]} [15J

N(L,a) can also be written in terms of the sampling density, ~.

This is done by determining which (r, a) pairs correspond to secants

intersecting AB. By letting R~ symbolize the region of all (r, a) that

correspond to secants intersecting AB in a Cartesian r, e-plane , and

from the definition of A:

N(L,a) = A ffR, drda [16]

(R~ depends on the position of AB, but the value of the integral does

not.)

As an example, N(L,S) is computed here for the case: Ie-all < n/2

and la-a2 1 < n/2.

For this case consider any fixed a strictly between a 1 and a2 •

There is a set of points, GR, along the line (r, a) whose normals

intersect AB. The length of GH can be f9und by drawing an extension++

line through point A parallel to the line GR. See Figure 5. Next the++

secant CD normal to the line GR and passing through point B is drawn.

If the intersection of CD and the extension line is labeled point E,

then AE has the same length as GR. Trigonometry shows the length of AE

32

Page 61: Determination of effective porosity of soil materials

Figure 5.

,,",,,,',,," ({j-e),,

Segment GH represents all points along line OH whichhave secants intersecting the line segment AB. Notethe AB makes the angleB with respect to the angularorigin.

33

Page 62: Determination of effective porosity of soil materials

*is L cos (a-e). By usinge

ffR, drde = fe1

2

this result, one_can see that:

L* cos (a-e) de [17]

By using equation 16 and integrating,

[18]

The value of N(L,a) for the other three possible cases is computed

by using an analogous technique. Table 1 shows a listing of all four

cases and the corresponding values for the area of R~.

Equating the values of N(L,a) in equations 15 and 16 and

rearranging terms yields:

[19]

The subscript on A indicates that the estimates of this parameter

depend on the value of a. This dependence on a comes from the fact thatI

both p(SAISB) and the integral in equation 19 depend on a.

To arrive at estimates for P(SA) and p(SAISB)' the pattern can be

sampled at equally spaced rectilinear grid points corresponding to a

standard set of x- and y-axes. P(SA) is independent of direction.

There will be two estimates for P(SA):one for each possible value of SA

(pore and matrix). P(SA) can be found by dividing the number of sample

points in state SA by the total number of points in the sample.

p(SAISB) is estimated by assuming that all points in the sample are from

different cells. The value for p(SAISB) is computed for two directions

(the x and y directions) by Lin and Harbaugh (1984). Let S(x,y) be the

state of the sampling point with coordinates (x,y). Let the function F

be defined

F(xl • [~for points (x,y) within the pattern:

if S(x+l,y) # S(x,y), or if (x+l,y) lies outside the pattern.

if S(x+l,y) = S(x,y)

Then for the x direction:

p(SAISB) = LX Ly F(x,y) / Lx Ly 1

p(SAISB) can be computed in a similar fashion for the y-direction.

Notice that for each direction there are two values of p(SAISB); one for

34

Page 63: Determination of effective porosity of soil materials

each possible value of S. Appropriate values of the terms of equation

19 for the two different states and two directions can be used to obtain

four estimates of A. It is not known how to best combine these four

estimates of A, therefore both arithmetic and geometric means will be

shown for each pattern.

Table 1. Listing of the Values of N(L,a) for the Four Possible Cases.

Case ffR, drd8

la-811 < 71/2 and I a-02 1 > 71/2 sin [(82-°1)/2] cos [a-(82+81)/2]

Ia-81I < 71/2 and I a-82 1 < 71/2 1+ sin [a-(82+81)/2] cos [( 82-(1) /2]

la-81 1 > 71/2 and I a-82 1 < 71/2 1- sin [a-( 82+(1) /2] cos [(82-81)/2]

I a-811 > 71/2 and 16- 82 1 > 71/2 sin [(81-82)/2] cos [a-(82-81)/2/]

35

Page 64: Determination of effective porosity of soil materials
Page 65: Determination of effective porosity of soil materials

SECTION 6

RESULTS AND DISCUSSION

GENERAL PHYSICAL PROPERTIES

Table 2 presents the particle size distribution, liquid limit,

plastic limit, and plasticity index determined for subsoil materials of

Nicollet, Fayette, and Clarinda. Nicollet material had the least clay

and the most sand, whereas Clarinda material had the most clay and an

intermediate sand content. Fayette material, derived from loess, was

highest in silt. The percentage clay in each subsoil material is

reflected by the values of the Atterberg limits. As percentage clay

increases, the Atterberg limits increase.

Table 2. Particle size distribution, liquid limit, plastic limit,

and plasticity index of subsoil materials.

Particle size distribution

Clay Silt Sand

( (2) (2-50) (50-2000) Liquid Plastic Plasticity

Soil ( ll!!1) (ll!!1 ) ( ll!!1) limit limit index

------------ % ------------

Nicollet 21 25 54 28 15 13

Fayette 35 57 8 35 21 14

Clarinda 44 35 21 56 28 28

Table 3 presents the classification of each subsoil material

according to the USDA, AASHTO, and Unified classifications. According

to the AASHTO classification, which classifies soil material according

to its suitability for engineering uses (A-1 is the highest suitability

class), the Clarinda subsoil material is the least suited for

36

Page 66: Determination of effective porosity of soil materials

\

Page 67: Determination of effective porosity of soil materials

engineering uses (A-7 is the next to lowest suitability class). In

addition, according to the AASHTO and Unified classifications, Clarinda

subsoil materials are subject to extremely high volume change.

Table 3. Classification of subsoil materia1s~according to USDA, AASHTO,

and Unified classifications.

Soil USDA AASHTO Unified

Nicollet sandy clay loam A-6 (3) CL

Fayette silty clay loam A-6 (10) CL

Clarinda clay A-7-6 (18) CH

Moisture-Density Relationships

Table 4 presents the particle density, undisturbed bulk density,

and the optimum bulk density and moisture content from the moisture­

density relations determination. Nicollet subsoil material compacts to

the highest bulk density. Compacted Clarinda subsoil material has an

optimum bulk density lower than undisturbed Clarinda subsoil material.

Thus, the compactive force experienced in the past by the undisturbed

Clarinda subsoil material was greater than the compactive force during

the moisture-density relations test.

Table 4. Particle density, undisturbed bulk density, optimum bulk

density and moisture content of subsoil materials.

Particle Undisturbed Optimum Optimum

density bulk density bulk density moisture

Soil (Mg/m3 ) 3 (Mg/m3) (%)(Mg/m )

Nicollet 2.59 1.66 1.84 14

Fayette 2.71 1.41 1.67 18

Clarinda 2.69 1. 59 1.45 27

37

Page 68: Determination of effective porosity of soil materials

)

Figure 6 presents the moisture-density relations for Nicollet,

Fayette, and Clarinda subsoil materials. From the figure, one can see

that the compaction of the subsoil materials at higher-than-optimum

moisture content provides bulk densities slightly lower than the maximum

values. The subsoil materials were compacted at higher-than-optim~m

moisture content to obtain higher percentage water saturation.

Mercury Intrusion Porosimetry

The calculated total porosity of the samples after drying was

always lower than the calculated initial total porosity (Table 5). For

all compacted samples, oven drying resulted in the greatest -absolute

loss of porosity. For example, in Clarinda materials, total porosity

dropped from 0.46 to 0.25 cm3fcm3 , i.e., about 46% relative change. On

the other hand, freeze-dried samples shrank the least; for example,

total porosity of Fayette freeze-dried samples changed very little. For

compacted samples, relative shrinkage was consistently greatest for

Clarinda materials and least for Fayette materials. There was no

discernible pattern related to particle size distribution, although the

greatest shrinkage occurred in materials with the highest clay content.

38

Page 69: Determination of effective porosity of soil materials

~

Page 70: Determination of effective porosity of soil materials

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Page 71: Determination of effective porosity of soil materials

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Page 72: Determination of effective porosity of soil materials

Table 5. Total porosity of soil materials before and after drying.

Compacted Undisturbed

Porosity

Relative

Porosity change from

before after initial before after

Relative

change from

initial

drying drying porosity drying drying porosity

-cm3jcm3 -cm3jcm3 -- % -- -cm3jcm3 -cm3jcm3 -- %-

Nicollet .29 .36

freeze dried .25 14 .28 22

acetone dr-ied .23 21 .29 19

oven dried .19 35 .22 39

Fayette .40 .48

freeze dried .39 3 .40 17

acetone dried .37 8 .33 31

oven dried .30 20 .30 38

Clarinda .46 .41

freeze dried .38 17 .32 22

acetone dried .31 30 .29 29 ,/

oven dried .25 46 .19 52

Undisturbed samples also had less total porosity after drying than

before (Table 5). Oven-dried samples of all three soil materials showed

the greatest absolute and relative losses of total porosity compared

with the initial total porosity. The le~st losses of total porosity

occurred in the freeze-dried samples of Fayette and Clarinda soil

materials and in the acetone-dried samples of Nicollet soil materials.I

It is unlikely that the total porosities of undisturbed Nicollet samples

after freeze drying and acetone drying are significantly different. As

42

Page 73: Determination of effective porosity of soil materials

in the compacted samples, there appeared to be no clear relationship

between particle size distribution and shrinkage.

Each of the drying techniques caused Bome change in total

porosity. Oven drying caused the greatest loss of total porosity, and

acetone drying generally caused an intermediate loss. Freeze dry~ng

caused minimal loss of total porosity, confirming what other workers

have reported (e.g., Zimmie and Almaleh, 1976). Although the lower

changes in total porosity by freeze drying may suggest that this

technique alters soil pores the least, pore size distribution analysis

provides additional insight concerning the three approaches to drying.

Figures 7-12 display size distributions for pores with equivalent

pore radii (epr) greater than 0.002 ~ in the soil materi~ls

investigated. The data are given as absolute porosities attributed to

pores in a logarithmic epr range. Each number in the bar graph

represents the mean of the replicates determined. Cumulative porosity

curves are shown in Figs. 13-18.

In the compacted soil samples, there were marked differences in

pore size distributions among the drying treatments. For example, most

of the porosity in freeze-dried, compacted Nicollet soil materials was

derived from pores in the 0.2-2 ~ epr range (Fig. 7). In acetone-dried

samples, however, porosity was more evenly distributed in the 0.02-

0.2 urn and 0.2-2 ~ epr ranges. In oven-dried samples, pores with epr

between 2 and 20 urn contributed most to porosity.

Freeze drying of compacted Fayette soil materials resulted in

porosity of nearly 0.27 cm3/cm3 contributed by pores in the 0.2-2 urn epr

range (Fig. 8). Acetone-dried and oven-dried Fayette samples had

essentially identical pore size distributions, except in the 0.02-2 urn

epr range. In that range, acetone-dried samples had about 0.11 cm3/cm3 ,

whereas oven-dried samples had about 0.05 cm3lcm3• The difference of

0.06 cm3/cm3 is comparable to the 0.07 cm3/cm3 difference in ~otal

porosity between the drying treatments (Table 5).J

In compacted Clarinda materials, freeze drying also resulted in a

significant volume of pores in the 0.2-2 urn epr range (Fig. 9). In both

acetone-dried and oven-dried samples, pores in the 0.002-0.02 urn epr

range contributed most to porosity. Acetone-dried samples had more

43

Page 74: Determination of effective porosity of soil materials

-Compacted .Nicollet.. .80-----......;:.-....;,.----..;....---------,D,' aCetone dry.

lEI' freeze dry

• OVen dry

.24+------------------1

.08+-----1

'...2-2 2-20 .20-70

Figure 7. Mercury intrusion porosimetry determined pore size distri­butions for till samples using three drying techniques.

44

Page 75: Determination of effective porosity of soil materials

Compacted Fayette. AD ..,.....----.....--------------

"---.....1--- ..18

!r ,,.12

I toe

0: ·acetone*,

I§I' freeze dIj

• even dry

2-20 '20-10

Figure 8. Mercury intrusion porosimetry determined pore size distri­butions for compacted)oess samples using three dryingtechniques.

45

Page 76: Determination of effective porosity of soil materials

• ·oven dryo.acetone drY.

~ ... freeZe drY

·.

Compacted Clarinda

.24+-------------------1

·.12

.06

20-70

Figure 9. Mercury intrusion porosimetry determined pore size distri­butions for compacted'paleosol samples using threedrying techniques.

46

Page 77: Determination of effective porosity of soil materials

U"ndisturbed· Nicollet.25.~·,.....----------------.....,

o I acetone.drY"

E§I" ireezedry

".. .....,.. oven-7

.20 +-------------------1--1'- ..151"I

--- --- --

.10

J~5

2-20 20-70

Figure 10. Mercury intrusion porosimetry de~ermined pore size distri­butions for undisturned till samples using three dryingtechniques.

47

Page 78: Determination of effective porosity of soil materials

/

~ndisturbed Fayette.2~:,.....------------~-----.....

o acetone dry

I§I freeze· dry

'-_. oven c*y

2-20 20-70

Figure 11. Mercury intrusion porosimetry determined pore size distri­butions for undisturbed loess samples using three dryingtechniques.

48

Page 79: Determination of effective porosity of soil materials

;.2-2· 2-20 20-70

Figure 12. Mercury intrusion determined pore size distributions forundisturbed paleosol samples using three drying techniques.

49

Page 80: Determination of effective porosity of soil materials

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Page 81: Determination of effective porosity of soil materials

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Page 82: Determination of effective porosity of soil materials

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Page 83: Determination of effective porosity of soil materials

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Page 84: Determination of effective porosity of soil materials

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Page 85: Determination of effective porosity of soil materials

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Page 86: Determination of effective porosity of soil materials

porosity than oven-dried samples in each epr range except the 20-70 umepr range.

Pore size distributions of undisturbed samples showed basically the

same effects of drying treatments as did those of compacted samples

(Figs. 10-12). Specifically, freeze drying consistently resulted ~n

high pore volumes coming from pores in the 0.2-2 um epr range. In

contrast, pores in the 0.02-0.2um epr range contributed significantly

to porosity in the acetone-dried, undisturbed samples •.In oven-dried,

undisturbed samples porosity was greatest In the 2-20 um epr range for

Nicollet, in the 0.2-2 um epr range for Fayette, and in the 0.002-

0.02 lJIIl epr range for Clarinda. In this regard, oven-dried, 'undisturbed

samples were directly comparable to oven-dried, compacted samples.

The consistent dominance of pores in the 0.2-2 ~ epr range in

freeze-dried samples of all soils, both disturbed and compacted, is

striking. A similar peak in pore size distribution of freeze-dried soil

materials has been reported by Lawrence et ale (1979), Murray and Quirk

(1980), and Delage and Pellerin (1984) for samples initially frozen"in

liquid nitrogen, Freon, or 2-methyl butane. We hoped that significant

changes in porosity by growth of ice crystals might be prevented by

freezing samples so quickly that large ice crystals could not form. We

used samples on the order of 1 cm in diameter, for example, to ensure

that heat could be withdrawn rapidly from the sample interior. Although

we froze the samples in liquid N2 at 77 K, we were only careful to keep

the samples at temperatures less than 273 K before sublimation. During

sublimation, temperature of the freeze dryer's condenser was ~248 K.

Even if water in the samples had frozen quickly into small crystals upon

initial submersion in liquid N2' there may have been recrystallization

of ice at temperature greater than 77 K yet less than 273 K. Burton and

Oliver (1935), for example, found that even at low temperature ice could

recrystallize and suggested that, at atmospheric pressure, ice crystals

are stable only at temperatures less than 163 K. Meryman (1957)-'

observed recrystallization at 203 K; crystals of 1umdiameter formed in

only 30 s. In other-words, under the conditions employed in our study,

recrystallization of ice may have increased the volume of pores in the.

0.2-2 lJIIl epr range compared to the original porosity before drying.

56

Page 87: Determination of effective porosity of soil materials

The effects of acetone drying on pore size distribution are

difficult to ascertain. The similarity of porosity in the 0.002-0.02 ~

epr range for acetone-dried and oven-dried soil samples suggests that

either the techniques do not alter very small pores much or that pores

are altered similarly by both techniques. The data further suggest

that, in acetone drying, pores with epr in the 0.02-0.2 ~ range are

favored--for either preservation or production--compared to the other

drying techniques. Finally, porosity due to pores in the 0.2-2 um epr

range of acetone-dried samples was generally intermediate between the

porosities of oven-dried and freeze-dried samples in that range. There

was no discernible pattern for pores >2 um epr.

We note that direct comparison of our results with those of acetone

exchange before resin impregnation is not possible because in the latter

instance acetone does not need to be completely removed from the samples

(i.e., polyester resins are miscible with acetone). Before mercury

intrusion, however, acetone in the samples had to be evaporated. Total

porosity values (Table 5) indicate that some shrinkage did occur, and it

may h~ve happened at the evaporation step.

Water Desorption

Porosity determined by oven drying, freeze drying, and acetone

exchange of compacted samples may be compared with porosity calculated

from soil water contents of compacted samples equilibrated at several

pressures (Table 6). Pores filled with water at 0.05 MPa actually

constituted a volume greater than or equal to the initial porosity

calculated for the compacted samples. This is because some swelling of

the samples occurred at saturation. At the other end of the pressure

range, porosity determined by water content was comparable to that

obtained by oven drying and acetone exchange for two of.the soil

materials. For example, pressures of 2.0 MPa and 1.5 MPa correspond to

equivalent pore radii of 0.1 and 0.75 um, respectively. For Nicollet

and Clarinda soil materials, pores .of that size range contributed about3 3 -'

0.03 cm /cm. This may be compared with porosities of 0.02 to 0.07

cm3/cm3 in the 0.2-2 um epr range of Nicollet and Clarinda, as

determined by oven drying and acetone ~xchange (Fig. 7 and 9). Porosity

determined by water content of Fayette compacted materials was about

57

Page 88: Determination of effective porosity of soil materials

"

0.06 cm3/cm3 in the 0.1-0.75 ~ epr range. This is not very similar to

porosity in the 0.2-2 ~ epr range determined by the three methods of

this study for compacted Fayette materials (Fig. 8). In all cases,

freeze drying resulted in more porosity in the 0.2-2 ~ epr range than

did any other drying methods or the water content method.

Table 6. Volumetric soil water content at four tensions for compacted

soil samples.

Volumetric soil water content

Soil 0.05 MPa 0~1 MPa 2.0 MPa 1.5 MPa

Nicollet .31 .28 .24 .21

Fayette .40 .36 .35 .29

Clarinda .48 .45 .42 .39

W~~er desorption curves for compacted and undisturbed samples are

presented in Figs. 19-21.

Permeability

Table 7 presents the permeabilities of three replicates of each

subsoil material compacted in Proctor molds. The mean permeability of

each subsoil material was less than 10-9 mIs, the value currently used

by the USEPA as the criterion for a material's suitability as a liner

material. Fayette materials had the highest permeability of the three

subsoil materials, although Clarinda materials had more porosity.

Fayette materials must have had larger openings or better connections in

the pore space than did Clarinda materials.

:"

58

Page 89: Determination of effective porosity of soil materials

e.6

+I C

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leo

so

l+

Q)

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ess

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)+

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Page 90: Determination of effective porosity of soil materials

0.4

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Page 91: Determination of effective porosity of soil materials

0.5

+oJ C Q)

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Page 92: Determination of effective porosity of soil materials

Table 7. Permeability of three replicates of each Proctor-type

compacted subsoil material.

Permeabili ty (m/s)

Soil I II III Mean

Nicollet 5.47 x 10-11 6.58 x 10-11 1.22 x 10-10 8.08 x 10-11

Fayette 2.84 x 10-10 2.67 x 10-10 2.61 x 10-10 2.71 x 10-10

Clarinda 4.18 x 10-11 2.97 x 10~11 5.05 x 10-11 4.07 x 10-11

Soil permeability as a function of time is shown in Figs. 22-24.

The permeability of all three soil materials held somewhat constant

during the periods of measurement.

Table 8 presents permeabilities of the smaller compressed and

extruded soil samples. Larger variation was found in measuring

permeability of these samples. The average permeabilities of the

compressed soil samples were greater than those for the larger,

compacted samples.

Table 8. Permeabilities of compressed and extruded subsoil materials.

Permeability (m/s)

Soil Average Standard deviation

Nicollet 6.4 x 10-9 7.9 x 10-9

Fayette 2.8 x 10-8 8.9 x 10-9

Clarinda 7.9 x 10-9 1.3 x 10-8

:'Table 9 presents permeabilities of the undisturbed soil samples.

Both average and variance for the undisturbed samples are greater than

for disturbed samples.

62

Page 93: Determination of effective porosity of soil materials

8

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Page 94: Determination of effective porosity of soil materials

5

- fIJ "4r

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Page 95: Determination of effective porosity of soil materials

- (i) "EC

tT

CS) - '-'

0-

>..

1JI

+oJ .- - .- ..c m Q) E L Q)

a..

5 4J-

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Page 96: Determination of effective porosity of soil materials

Table 9. Permeabilities of undisturbed soil samples.

Permeability (m/s)

Soil Average Standard deviation

Nicollet 2.9 x 10-6 2.4 x 10-6

Fayette 2.2 x 10-5 3.0 x 10-5

Clarinda 9.8 x 10-:7 1.0 x 10-6

Solute Breakthrough Curves

Figures 25-30 present the solute breakthrough curves from the three

replicates of each compacted soil material. The plots are relative

concentration versus relative pore volume. One pore volume is equal to

the total porosity of the bulk soil volume. In all cases, chloride

appeared in the effluents when about 0.2 - 0.25 of one pore volume of

solution had leached through the sample. With the same hydraulic

gradient, the first appearance of chloride under liners,of equal

thickness of the compacted subsoil materials would occur first with

Fayette, then Nicollet, and lastly Clarinda materials. All curves are

somewhat symmetrical, implying that no l~rgepores (not a bimodal pore

size distribution) were contributing significantly to flow. The solid

curves shown in the figures represent "best fit" values obtained from a

solution of the convective-dispersive equation (Van Genuchten and

Wierenga, 1986).

Figures 31-33 present solute breakthrough curves for undisturbed

soil samples. All of the figures display asymmetrical shapes. The

asymmetrical shapes are characteristic of a bimodal pore size

distribution. A few large cracks or channels must have been responsible

for most of the flow in the undisturbed sores. Thus, early breakthrough

occurred with tailing toward CICo = 1.

The breakthrough curves for the disturbed and undisturbed samples

are distinctly different. All three soil materials as they occur in

nature must be mixed and compacted in order to remove the presence of

66

Page 97: Determination of effective porosity of soil materials

1•B

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Page 98: Determination of effective porosity of soil materials

~B

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Page 99: Determination of effective porosity of soil materials

U t: 0 U ~ t: ClJ :J - ~0

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Page 100: Determination of effective porosity of soil materials

I.etJc:0 e.Bu...c:III e.6::l

......w e.'!III>... e.2III

IIIQ::

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Re Iat ive Pere Volume

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e.e e.5 1.0 1.5 2.e

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IIIQ:: e.e

B.a B.5 I.e I.S 2.0

Relative Pere Velume

Figure 28. Three replicates of measured and fitted (solution to con­vective-dispersive equation) Cl- breakthrough data forcompacted till materials.

70

Page 101: Determination of effective porosity of soil materials

I.e(,J

c:0 1l.8U

+'c:III B.6::l

~

~

w B.'!III>~ B.201

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Relative Pore Volume

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B.BB.a B.S I.e 1.5 2.0

Relative Pore Volume

Figure 29. Three replicates for measured andvective-dispersive equation) Clcompacted loess materials.

71

fitted (solution to con­breakthrough data for

Page 102: Determination of effective porosity of soil materials

I. iii

uc:0 B.Bu...c:Gl IiI.S~......w B.4Gl>... B.2'"III

Cl::

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La

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Relative Pore Volume

figure 30. Three replicates of measured and fitted (solution to con­vective-dispersive equation) Cl- breakthrough data forcompacted paleosol materials.

72

Page 103: Determination of effective porosity of soil materials

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Page 104: Determination of effective porosity of soil materials

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Page 105: Determination of effective porosity of soil materials

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Page 106: Determination of effective porosity of soil materials

cracks before they would be useful as hazardous-waste-disposal liners.

Effective Porosities

Our method of determining effective porosity depends on both the

cumulative pore size distribution and the total porosity. Yet, to

determine pore size distribution by mercury porosimetry, all water,must

be removed from the sample. Some of the total porosity in the samples

was lost when water was removed by freeze drying (Table 10). Some lo/ss

of poro~ity occurred in the Nicollet and Clarinda samples during freeze

drying. The greatest decrease in porosity was with Clarinda soil

materials, the materials highest in clay content. Total porosity in

Fayette soil materials was not diminished by freeze drying.

Table 10. Total porosities of compacted soil materials before and after

freeze drying.

Soil material Before drying After drying

Nicollet 0.29 0.28

Fayette 0.40 0.40

Clarinda 0.46 0.40

The function used to describe the cumulative porosity curve (Eq. 8)

has two empirical parameters, a and n. Only n is required to describe

the unsaturated permeability. Figure 34 presents a family of curves

over a range in n from 1.1 to 5. The curves show that the spread on a

log scale of pore sizes decreases as n increases. Thus, the theory

provided for calculating unsaturated permeability considers the spread

in pore size distribution as the predominant factor.

Figures 35, 36, and 37 show the cumulative porosities for Nicollet,

Fayette, and Clarinda soil samples, resp~ctively. The discrete, plotted

symbols represent values determined by mercury porosimetry. ',The solid

curves represent the least-squares, nonlinear regression fit of Eq. (8)

to the measured data. In all cases the model does a reasonable job of·

matching the measured data. The a, n, Sr' and Ss parameters for each

76

Page 107: Determination of effective porosity of soil materials

",

1

· 8

• 6

• 4

• 2

o.001 .01 .1 1 10

·PORE RADIUS (}Jm)100

Figure 34. Theoretical cumulative porosity curves as influencedby the n-parameter (a = 1.0, S = a/a).

s

77

Page 108: Determination of effective porosity of soil materials

.45

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Page 109: Determination of effective porosity of soil materials

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Page 110: Determination of effective porosity of soil materials

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Page 111: Determination of effective porosity of soil materials

soil are presented in Table 11.

Table 11. Parameters used with equation (8) to describe the cumulative

porosity of the soil materials.

Soil Material a 1 n1 a 1 a 2r s

Nicollet 4.08 1.52 0.00 0.28

Fayette 0.88 2.11 0.05 0.40

Clarinda 1.22 1.98 0.08 0.40

1/ a, n, and 8r were determined by least squares nonlinear regression

of mercury intrusion porosimetry data and Eq. (8).

2/ as was specified as the total porosity of the soil samples after

freeze drying.

Equation (6) describes the unsaturated permeability of soil once

the n-parameter is known. Figure 38 presents a family of curves

displaying the influence of the n-parameter on unsaturated

permeability. As n increases, the relative permeability tends to

decrease more gradually as the soil begins to desaturate. This

indicates that, the larger the n-parameter, the larger is the fraction

of porosity with relative importance for conducting fluids. As n

increases, one can expect the effective porosity to represent a larger

portion of the total liner porosity.

Figure 2 presents a family of curves, over a range in 8s from 0.3

to 0.5, displaying the influence of n on the effective porosity when aris constant at 0.05. If similar sets of curves were drawn for ar = 0.0

and 8r = 0.10, only small differences frgm Fig. 2 would be observed;

i.e., the maximum difference in E would be 0.007. Thus, Fig. 2 can be

used to obtain estimates of effective porosity of compacted clay liners

with as between 0.3 and 0.5, 8r between 0.0 and 0.1, and n between 0.1

and 3.0.

81

Page 112: Determination of effective porosity of soil materials

1

.8

· 6

en• 4

· 2

1211 • E-5 • 12112101 • 121 1 • 1 1

Figure 38. Theoretical relative permeability (K r ) curves asinfluenced by the n-parameter (5 = a/as)·

82

Page 113: Determination of effective porosity of soil materials

The method developed in this paper for estimating the effective

porosity of compacted clay liners depends only on parameters describing

liner pore structure; i.e., Ss. Sr' and the n-parameter. Cumulative

porosity measurements provide the basis for the determination of the

appropriate parameters. By using the pore structure parameters

presented in Table 11. effective porosities for the Nicollet. Fayette.

and Clarinda soil materials are estimated from Fig. 2 as 0.04. 0.08, and

0.08. respectively. Because the total porosity of the Clarinda sample

decreased as a result of drying from 0.46 to 0.40. E was recalculated

for Ss = 0.46. Thus, E was 0.09 for the Clarinda soil material. Once

effective porosity is estimated, pore-fluid velocity and noninteracting

pollutant travel time can be calculated for a compacted liner with a

known permeability, hydraulic gradient. and thickness.

Table 12 presents measured values of permeability and times of

first chloride breakthrough (relative effluent concentration equal to

0.01), estimated effective porosities, and predicted times of first

breakthrough of noninteracting pollutants for compacted Nicollet.

Fayette, and Clarinda samples. Each compacted soil material had, -9 3 2

permeability less than the EPA-preferred value of 1 x 10 m 1m Is for

hazardous wastes disposal liners. The estimated effective porosities

were between 10 and 20% of the total porosities of the compacted

samples. The predicted breakthrough time was. calculated based on the

mean permeability. The measured chloride breakthrough time was adjusted

to correspond to the breakthrough time of a permeameter with the mean

permeability.

83

Page 114: Determination of effective porosity of soil materials

Table 12. Measured permeabi1ities and time of first chloride

breakthrough and predicted effective porosities and non­

interacting pollutant breakthrough times for the compacted

soil materials (permeameters were 11.64 cm long).

Soil

Material Permeability3 2(m 1m Is)

Measured C1­

breakthrough

time

(d)

Effective

porosity

Predicted

breakthrough

time

(d)

Nicollet

Rep 1 5.47 x 10-11 3.0 0.04 2.6

Rep 2 6.58 x 10-11 4.2

Rep 3 1.22 x 10-10 4.6

Mean 8.08 x 10-11 3.9

Fayette

Rep 1 2.84 x 10-10 1.7 0.08 1.6

Rep 2 2.67 x 10-10 1.2

Rep 3 2.61 x 10-10 1.5

Mean 2.71 x 10-10 1.5

Clarinda

Rep 1 3.38 x 10-11 4.8 0.09 5.1

Rep 2 2.17 x 10-10 4.4

Rep 3 1.11 x 10-10 3.9

Mean 1.21 x 10-10 4.4

The predicted noninteracting pollutant breakthrough times agreed

84

Page 115: Determination of effective porosity of soil materials

well with the measured chloride breakthrough times. Predicted

breakthrough values were about equal to measured values for Fayette.

Predicted breakthrough was earlier than measured for Nicollet and later

than measured for Clarinda. For one replicate of Nicollet and one

replicate for Clarinda, the measured and predicted breakthrough times

were nearly equal. Because the clay fractions of the ~ompacted samples

had a net negative charge and chloride is an anion, it is reasonable to

assume that chloride could move through the samples faster than a

noninteracting pollutant (i.e., tritiated water). Nicollet soil

material had less clay than the other materials, and thus anion

exclusion would be expected to be less.

The theory presented provides the basis for estimating effective

porosity of compacted clay liners. To predict the travel time of

noninteracting substances through a clay liner, the hydraulic gradient,

liner permeability, liner thickness, and effective porosity are

required. As an example of how the theory can be used, we will now make

such a prediction. The information that we assume is: liner thickness =

1 meter, hydraulic gradient = 1.33, liner permeability = 10-9 m3jm2js.

If we follow only the Darcy equation, Eq. (1), fluid flux density

is 1.33 x 10-9 m3jm2js. However, the fluid flux density does not

represent the fluid velocity within the liner. We know that a portion

of the total porosity is responsbile for conducting fluid at velocities

higher than the average velocity and the remaining portion of the

porosity conducts fluids at velocities lower than the average

velocity. What is important in pollutant transport is the portion of

porosity that conducts fluid at higher-than-average velocities. To

determine the average effective fluid velocity, we must first estimate

the effective porosity.

Effective porosity is determined based on theory previously

presented. By using mercury porosimetry data for the Nicollet materials

presented in Fig. 35 and Eq. (9), the n-parameter is determined as 1.5,~

ar as 0.00, and as as 0.28. By using Fig. 2 effective porosity is

estimated to be 0.04. Based upon Eq. (3) the travel time for

noninteracting solutes through a Nicollet clay liner in this example is

predicted to be 0.95 years. Therefore, under these conditions, we

85

Page 116: Determination of effective porosity of soil materials

predict that after about one year, noninteracting pollutants will reach

the bottom of the clay liner. Although the concentration of the

noninteracting pollutant may be low because of dilution and lateral

mixing by diffusion, the initial fraction is predicted to appear after

one year. In this example, if the product of liner permeability and

hydraulic gradient (i.e., fluid flux density, J) is mistakenly used as

the fluid velocity, the pollutant travel time is calculated to be 23.8

years. If the fluid velocity is mistakenly assumed to be equal in all

soil pores, the noninteracting pollutant travel time is calculated as

6.7 years. Thus, travel time for noninteracting pollutants is

significantly overestimated if effective porosity is not taken into

account. The active lifetime of hazardous waste disposal units may be

overestimated if liner effective porosity is not properly estimated and

used in the prediction of pore-fluid velocity.

IMAGE ANALYSIS

Sample preparation techniques

Direct replacement of water in large (10.4 cm3) soil samples by

acetone was successful only with samples with the lowest clay content,

i.e., Nicollet soil materials. Both Fayette and Clarinda soil samples

developed large cracks and fell apart when placed in 100% acetone. We

also experimented with a graded series of replacement fluids, increasing

the acetone content in water gradually from 10% to 100% acetone, but

these samples also shrank and disintegrated. Similar results were

obtained when we placed the samples in acetone vapor. These results

were unexpected because the acetone replacement technique has been

reported by others to be simple and successful (Murphy, 1982;

FitzPatrick, 1984). But in contrast to many soils, the clay minerals of

the three Iowa soils are largely smectitic. This means that relatively

large amounts of water can be held in clay interlayers. We believe

that, when this interlayer water was withdrawn by the polar acetone

molecules, the clay layers collapsed and~sample shrinkage occurred.

On the other hand, replacement of water by methanol proved to be

successful for large samples of Fayette and Clarinda soils. No

shrinking or swelling of the soils was observed during methanol

exchange, and the samples remained intact. Methanol was successfully.

86

Page 117: Determination of effective porosity of soil materials

exchanged with acetone, and then acetone was exchanged with the

polyester resin in which Uvitex-OB had been dissolved. After the resin

was cured, porosity images were obtained from polished blocks.

Obtaining an image

Soil porosity images obtained by using a 35-mm camera and a m~cro

lens were, in general, adequate for further analysis. Considerable

experimentation was required to adjust the light intensity, the camera's

aperature, and the time of exposure for optimum photographs. The main

advantage to this approach for porosity imagery is that it is simple and

relatively inexpensive. On the other hand, there are two reasons that

images so obtained are inherently somewhat inaccurate. First, only

pores greater than about 50-60 ~ in equivalent spherical diameter can

be adequately distinguished on the photograph. This means that, if

smaller pores are of interest, they must be imaged by a different

technique. Moreover, "total porosity" measured on the photograph is

unlikely to be as high as true total porosity of the sample because

small pores have been excluded from the analysis. Second, shallow pores

at the surface of the polished sample may not contain enough dye to show

up on the photograph. Or, alternatively, thin, transparent sand-size

grains at the surface may allow florescence from an underlying pore to

shine through. Figure 39 is an example of an image of soil porosity

produced with a 35-mm camera and a macro lens.

Porosity images obtained from thin sections viewed in circularly

polarized light also required a lot of experimentation regarding the

best film, light intensity, and time of exposure. Best results were

obtained with Kodak Ectagraphic HC film. In general, the longer the

exposure time was, the less porosity was displayed on the (positive)

photograph. In other words, just as with the macro lens technique, some

judgment was required to determine which exposure corresponded the

closest to porosity of the sample.

The advantage to obtaining soil porpsity images by using circularly

polarized light is that the thin sections can be studied in transmitted

light for other characteristics, e.g., mineralogy, cutans, peds, etc.

There are, however, several disadvantages. First, one should exclude

from analysis any pores that are smaller in diameter than the thickness

87

Page 118: Determination of effective porosity of soil materials

Figure 39. Porosity image obtained by photographing fluourescentdye in soil pores with a 35-mm camera and a macrolens. Diameter of soil sample = 5.5 cm.

Reproduced from Ibest available co·py. ,

88

Page 119: Determination of effective porosity of soil materials

of the thin section, i.e., about 30 um. This is because such pores

cannot be distinguished from grains of the same size that do not extend

through the thickness of the thin section. Second, it is difficult to

choose a representative field for analysis at this scale. Porosity may

constitute from 10% to more than 60% of a given field of view even in

the same thin section. Thus many analyses may be required to

statistically evaluate the porosity. Finally, at this scale, it is

often difficult to distinguish individual pores. Pore space can be so

interconnected that discrete pores do not exist on the image. In such

instances, methods of image analysis that are based on measuring

individual pores probably are not appropriate. Figure 40 is an example

of a porosity image obtained with circularly polarized light.

Images of soil porosity were also made by using a scanning electron

microscope in backscatter mode. This technique has the advantage of

simple preparation of samples--blocks of soil in hardened resin need

only be cut to size and finely polished. On the other hand, use of the

electron microscope is expensive. Moreover, the problem of finding

representative fields at high magnific~tion is similar to that outlined

for the circularly polarized light technique. The most severe problem

we experienced was getting the resin to fill all micropores of the

sample and to harden sufficiently. We found that even after polishing

the sample, holes remained in the surface. Figure 41, for example, is a

backscattered electron image of a compacted Clarinda sample, showing

holes in the surface. These-pits provided enough backscatter contrast

that they could be measured by an image analyzer. But the pits on the

sample may not be the original pores; thus further analysis of the

backscatter image would provide doubtful information about sample

porosity.

We used a number of variations in our laboratory procedure to cure

the plastic resin: variations in the amount of catalyst, variations in

the temperature and speed of the heat treatment, -for example. But none, /

was completely successful at the Bcale viewed with an electron

microscope. As FitzPatrick (1984) has noted, there are still many

unknown factors in the process of curing impregnated blocks of soil; it

is often impossible to predict if a technique or variation will succeed

89

Page 120: Determination of effective porosity of soil materials

Figure 40. -Example of an image of soil porosity obtained withcircularly polarized light. Undisturbed Clarindasoil materials. Frame length = 6.6 rom.

cReproduced from ----"'II-best available ,copy.

90

Page 121: Determination of effective porosity of soil materials

Figure 41. Example of a backscattered electron image of acompacted Clarinda soil sample showing holes inthe surface. Frame length = 100 ~.

Repro'd~ced-fr6nibest available copy."

91

milt

Page 122: Determination of effective porosity of soil materials

or fail, especially with very clayey soils.

Analyzing the images

Apart from reporting and discussing the actual results of the image

analysis performed on porosity images of the Nicollet, Fayette, and

Clarinda soil samples. it is appropriate to document some observations

on the use of an image analyzing computer. These observations may alert

other investigators to potential pitfalls or points of concern.

I-The "image" received by the computer depends upon the level of

light falling on the photograph. the resolution of the video camera. and

the resolution of the digitizing board. We found that it was especially

important to use a video camera of high quality. The camera we used in

conjunction with a microcomputer employed a I-inch Newvicon tube and had

BOO-line resolution. This was sufficient to send high-quality images to

the microcomputer's digitizing board. Video cameras associated with the

LeMont and Leitz image analysis systems were also adequate for obtaining

high-quality images.

2-Once the image is digitized. an adjustment of the gray level of

the pixels allows the operator to match as well as possible the

binarized image with the original porosity image. This procedure

depends a lot on incident light level and angle. camera quality. and the

patience of the operator. The gray level that is finally chosen by the

operator is a compromise between that level which fills in all pores and

adds unwanted "spots" on the image and that level which does not

completely fill in all pores.

3-00 image analyzing computers such as the Leitz TAS. it is

possible to remove selectively pixels which otherwise would be counted

as pores because they have gray levels above the set threshold. This

can be done by automatic methods (erosion and dilation) or by manual

editing with a light-pen touching the monitor or a digitizing tablet.

Such editing is very useful to optimize the image to be analyzed. But

it is also time-consuming. and it once again introduces an element of

human judgment.

4-There is a theoretical problem with making measurements of object

size on two-dimensional images. If an object touches the edge of an

image. its true size cannot be observed and measured. Weibel (1979)

92

Page 123: Determination of effective porosity of soil materials

proved that statistically accurate measurements could be obtained

nevertheless if two contiguous edges of the image (say, top edge and one

side edge) were defined as "forbidden zones". Any objects that touch

the forbidden zone, then, are to be excluded from analysis, whereas

objects touching the remaining two sides are included. Such an approach

assumes a random distribution of objects in the image and sufficient

number of images to adequately represent the subject being analyzed. In

our work, the Leitz TAS was programmed to exclude from analysis pores

that touched the forbidden zone. The LeMont image analysis system was

programmed to exclude pores that touched any of the four sides of the

image. The image analysis program used with the microcomputer accepted

all pores in the image.

S-A final observation is that in image analysis of soil porosity,

the number of pores to be measured and the number of images to be

analyzed has not been well established. We tried to obtain images of

porosity from as many replicate samples as possible when using the 3S-mm

camera and macro lens. Measurements on each image were averaged with

other replicates to produce the results discussed in the remainder of

this section.

Of the three types of image analyzers tested in this study, we

consider the Leitz TAS to be the most reliable. Data reported in Table

13 were obtained by using the Leitz TAS of the National Soil Erosion

Laboratory, West Lafayette, Indiana. For each image analyzed, the

following information is presented: number of pores counted, mean pore

area (urn) and standard deviation about the mean, and measured porosity

(%) of the image. Only pores greater than about 50 urn diameter could be

recognized consistently, so the porosity value necessarily ignores pores

smaller than that. About 11 cm2 of each image was analyzed, which

corresponds to about 3.4 cm2 of each sample after magnification of the

image is taken into account. Data for four replicate samples of

Nicollet soil material and four replicat~ ~amples of Fayette soil

material are presented. Two different images of each Fayette sample

(obtained by polishing and photographing both ends of a compacted,

impregnated sample) were analyzed. Only one image of compacted Clarinda

soil material was available for analysis because of technical problems

93

Page 124: Determination of effective porosity of soil materials

with water removal described earlier.

Table 13. Results of porosity analyses obtained by Leitz TAS image

analyzing computer.

Soil material n Mean pore area Standard deviation Porosity

and replicate 2 lJII12 %lJDl

Nicollet

A 430 236 154 1.31

B-1 1182 255 152 3.99

D 442 254 442 1.51

E 797 267 797 3.73

B-2 368 209 94 0.74

Fayette

Al 319 302 215 1.68

A2 374 260 183 1.45

Bl-17 542 246 140 1.67

B2 265 275 204 1.18

Cl 588 280 176 2.47

C2 489 282 244 2.56

D1 578 336 234 3.73

D2 182 370 261 1.43

Bl-12 701 243 145 2.16

Clarinda

A 344 322 247 2.16

Variability of the porosity measurem,ents is the most striking

aspect of the data, and it occurs at every level of analysis. For

example, the mean pore area for all analyzed samples is of the same

order of magnitude and ranges from 236 to 370 vm2 • But standard

deviations about the means are large, suggesting that the distributions

94

Page 125: Determination of effective porosity of soil materials

of pore area values are relatively spread out. Variability of results

within replicates also occurred. For example, even though mean pore

areas for the four Nicollet replicates are close to one another, the

number of pores counted ranged from 430 to 1182 and the porosity values

ranged from 1.31 to 3.99%. Even different images from the same

replicate produced different results. For example, Fayette sample D had

one end with 578 pores and 3.73% porosity, whereas the other end had 182

pores and 1.43% porosity.

As discussed in previous sections, variability in image analysis

measurements can also be due to human judgment factors. The length of

time allowed for exposure of the photograph under UV light influences

the number of pores that are detected. For example", two photographs

with different exposure times were taken of Nicollet sample B (B-1 and

B-2 in Table 13). The image analyzer noted a significant difference in

the number of pores counted and in the porosity between the two

photographs of the same polished sample face. Similarly, human judgment

is involved in setting the detection of gray levels on the image

analyzer itself. Fayette sample Bl was analyzed at two detector

settings (BI-17 and Bl-12 in Table 13). This required only slight

machine adjustment by the operator and, at the time of analysis, either

detection level was considered adequate for analysis of the image. Yet

there was again a significant difference between the analyses with

respect to number of points counted and percent porosity.

On the assumption the pores were circular in cross-section, an

equivalent radius was calculated for each pore and the results were

plotted in a frequency diagram. (This assumption was reasonable for

some pores and not for others, of course, but it allowed us to roughly

compare all pores at the same time). Percent relative frequency was

calculated to allow relative comparisons of pore ~ize distributions

because there was so much variability in the absolute pore data of the

samples. Representative histograms are ~iven in Fig. 42 and 43 for

Nicollet and Fayette samples. Most pores had equivalent radii of 50-200

urn. In general, Fayette samples had more pores larger than 300 urnequivalent pore radius than did Nicollet samples. Clarinda samples were

not included in this comparison because only one image was analyzed.

95

Page 126: Determination of effective porosity of soil materials

n

II

III

I

~I

II

IIS: ~ ~ o I ~ :sJ ~ c:w :w c:w i!l

c:>: ~ .. :sJ :sJ c:w ~ c:w :sl :slN C"1 ~ U1 ~ I'- [:l C'l c:w

60 rLi

<! 8 ft

36

lII

2 4 ~

I

r12 [

~ ['--_.....L..__..!...-__

:sJ~

U.l>

III0:::

+-'CIIIUL.III

a..

EquivaJen~ For~ Radius (micron:

Figure 42. Image analyzer determined pore size distributionhistogram for compacted till material.

96

Page 127: Determination of effective porosity of soil materials

S2l ri

>. rl:

4e lc!Il:J I

I0-

~!Il..

u..,. t!Il

>~,., i!Il 2 e ~

0:: iII

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t1 IQ..

2 [::::::

i

Ir:II

:::::: - :;) - ~

:": ~~ "" --

. III , '.= -;::. ........

Figure 43. Image analyzer determined pore size distributionhistogram for compacted loess material.

97

Page 128: Determination of effective porosity of soil materials

A cumulative area curve (analagous to cumulative relative porosity)

was also plotted for each analyzed image. Figure 44 is representative

for Nicollet and Fayette samples. (Clarinda materials are again omitted

because only one image was available). Slopes of the cumulative area

curves are similar to one another, and they are steep on a logari~hmic

scale. Each point plotted on the diagram represents ~n individual pore,

so the clustering of equivalent radius values between 50 and 200 um is

clearly demonstrated. The influence of relatively large pores on total

porosity can also be observed on these diagrams. For example, pores

larger than 300 um equivalent radius account for about 50% of the

measured porosity of the Fayette sample, but only about 30% of the

measured porosity of the Nicollet sample. This observation that large

pores influence measured porosity more in the Fayette samples than in

the Nicollet samples was consistent for nearly all the images.

In conclusion, the variability of image-analyzed porosity among

replicates and the sensitivity of the measurements to human judgment

limit what can be said about porosity in the compacted samples of this

study. Analysis of data on a relative basis, however, does suggest that

most pores in all samples were relatively small with respect to

equivalent radius and area. Moreover, the few large pores that occurred

had a significant impact on total porosity of the samples.

Markov Analysis

Twenty different patterns were analyzed using the Markov

approach. We will report a series of original and generated patterns in

order to show the strength and weaknesses of this method. It is

important to note that the algorithm does not guarantee that the

statistics for an original and its resulting generated patterns will be

the same. An obvious reason for this disparity is that the generated

image is the result of a series of random processes. Thus the generated

patterns have a range of possibilities.

For all isotropic patterns investigated, we found that a pattern~

could be easily generated such that each of its Markov parameters

matched within 10% of the values of the Markov parameters of the

original pattern (see Table 14). While each generated pattern is based

on one set of Markov parameters, these Markov parameters can correspond

98

Page 129: Determination of effective porosity of soil materials

Equivalent Pore Radius (micron)

Figure 44. Image analyzer determined cumulative porosity curvesfor (a) till materials and (b) loess materials.

99

Page 130: Determination of effective porosity of soil materials

to an infinite number of generated patterns. This is due to the random

elements of the algorithm. And because of these random elements, it is

sometimes necessary to generate several patterns before an acceptable

generated pattern is,obtained. The agreement of parameters to within

10% was obtained in three or fewer attempts in all but three case~•.

Table 14. Markov probability statistics for selected pore patterns.

The transitional probabilities are for pore to pore (P+P) ,

pore to matrix (P+M) , matrix to pore (M+P), and matrix to

matrix (M~). The corresponding patterns are shown in Figs.

45, 46, 47, 48, 53, and 54.

Pattern Transitional Probabilities Marginal Probabilities Lambda

Pore Matrix

P+P P~ M+P M~ state state

A original .740 .250 .093 .907 .266 .734 .216

A generated .740 .257 .098 .901 .276 .724 .220

* original .966 .034 .007 .993 .168 .832 .122B

horizontal

B generated .980 .020 .004 .995 .132 .868 .082

horizontal

B original .857 .143 .029 .971 .168 .832 6.421

vertical

B generated .752 .247 .039 .961 .132 .868 11.41

horizontal

C original .869 .131 .057 .943 .304 .696 .104

C generated .861 .139 .062 .938 .312 .688 .112

D original .740 .260 .024 .976 .087 .913 .165

D generated .745 .255 .023 .977 .081 .919 .165

E original .948 .052 .036 .964 .406 .594 .046

F original .948 .052 .032 .968 .378 .621 .044

* anisotropic pattern

100

Page 131: Determination of effective porosity of soil materials

The patterns that required generating more than three patterns to

obtain Markov parameter agreement within 10% consisted of bi-modal pore

size distributions. This indicates that the algorithm is inefficient in

producing patterns with a bi-modal distribution. This deficiency in the

algorithm can be predicted based on the fact that the areas of the

polygons follow a unimodal distribution (Kendall and Moran, 1963), and

that the assignment of states to adjacent polygons is random, making bi­

modal distributions in the generated patterns improbable. In addition,

it seems necessary that pores in the initial image have a random spatial

distribution. Fortunately, the pore patterns for compacted materials

are generally unimodal, with a random spatial distribution.

Figures 45-48 present examples of the original and generated pore

patterns. Visual inspection reveals that the generated "pores" lack the

rounded edges present in the original patterns. Yet the original and

generated patterns are similiar to one another. Unmistakable pairing of

original and generated patterns may not be always possible for the wide

range of soil porosity patterns possible; but these results indicate

that for the unimodal pore distributions encountered, Markov statistics

have potential as useful descriptors.

Histograms showing the frequency of various pore sizes for patterns

A, C, and D (Figs. 49-51) indicate that the algorithm produces patterns

that have pore size distributions somewhat similar to the original

patterns. Figure 51 illustrates how patterns with similar model

parameters can vary with respect to their distribution of large pores.

This indicates that the algorithm may not be sensitive enough to be used

in studies involving the prediction of hydraulic conductivity. Other

methods to model soil porosity (capillary tube models) also fail in the

prediction of hydraulic conductivity. Perhaps this Markov approach,

like previous models, will prove to be a useful descriptor of relative

hydraulic conductivity, and thus of the effective porosity.

Figure 52 displays the cumulative porosity curves for the original

and generated pore patterns shown in Fig. 48. The curves appear to be

similar in spread of pores and curve slope near their middles. This

provides further evidence that the effective porosities of the original

and generated pore patterns would be similar. The theory developed in

101

Page 132: Determination of effective porosity of soil materials

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Page 140: Determination of effective porosity of soil materials

this report uses the slope of the cumulative porosity curve in order to

estimate effective porosity. Thus, Markov statistics seem to be useful

for describing pore patterns such that effective porosity is reasonably

est~mated. This is applicable to the expected unimodal pore

distributions in compacted soil materials.

Because a wide range of patterns can be successfully modeled, one

might hope to characterize different soil patterns by using model

parameters. But Figs. 53 and 54, which have similar model parameters,

correspond to strikingly different patterns. Again the problems occur

with the bi-modal distribution. Intuitively, one might guess that

patterns with similar marginal probabilities and similar total pore

perimeters will have similar transitional probabilities. Thus, in order

for the Markov statistics to be useful in characterizing soil pore

patterns the patterns should be unimodal in pore size. Such pore size

distributions seem likely to occur in most compacted soil materials but

not for many undisturbed soil materials.

110

Page 141: Determination of effective porosity of soil materials

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Page 143: Determination of effective porosity of soil materials

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