THE COMPLEX PERMITTMTY OF COMPACTEI)

HALTON TILL

by

John W. Scholte
Department of Civil and Environmental Engineering

Submitted in partial fulfilmern

of the requirements for the degree of
Master of Engineering Science

Faculty of Graduate Studies

The University of Western Ontario
London, Ontario, Canada
September 1999

O John W. Scholte 1999

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 ABSTRACT

The complex permittivity of soil-water systems is a function of a number of physical

properties, such as density, moisture content and salinity. By understanding the

relationship between the complex permittivity of a soil-water system and these soil

properties, it is possible to detect changes in the soil-water system by measuring

changes in the complex permittivity of the soil system.

A laboratory complex permittivity measurement system was developed. consisting of

an Automatic Network Analyzer (ANA) and a modular coaxial sarnple. The

measurement system was then used to conduct a total of forty complex permittivity

measurements using soil sarnples that were prepared such that the soil moisture

content. the soil bulk density. and the mixing tluid salinity varied from one sample to

the next.

Multivariable linear regression models were developed. which relate the response of

the complex permittivity of compacted Halton till samples to changes in moisture

content. relative bulk density, and mixing fluid salinity.

Keywords: Complex pemittivity, soil moisture content. relative bulk density. soil
salinity. soil conductivity, non-destructive testing of soils, electromagnetic wave
measurernent, relaxation frequency.
 ACKNO WLEDGEMENTS

1 would like to express my appreciation to my advisors, Dr. J. Q. Shang and Dr. R.K.
Rowe for their support, encouragement and suggestions throughout the duration of
this research program. It has been a pleasure and honour to have worked with them.

Secondly, I would like to extend my appreciation to the staff and students of the
Geotechnical Research Centre. In particular, 1 would like to thank Mr. Gary Lusk
and Mr. Wilbert Logan for their assistance and suggestions. particularly during the
design phase of the sarnple holder.

1 would also like to extend my personal thanks to my parents, Joop and Rosario
Scholte, for their continuous and unconditional support, encouragement and
inspiration while 1 pursued my engineering education. They have taught me to
always strive for excellence, and above all. to believe in myself.

Finally, 1 would like to thank my fiancée Paula Vanni for her encouragement and
unwavenng support throughout the completing of my M.E.Sc. 1 am looking forward
to finally beginning our life together.
 TABLE ÜF CONTENTS

..
Certificate of Examination 11
...
Abstract 111
Acknowledgements iv
Table of Contents v
List of Tables viii
List of Figures ix
List of Symbols

Chapter 1: Introduction

Chapter 2: Literature Review

PERMITTIVITY
2.1 COMPLEX

2.1.1 Relative Pennittivity

2.1.2 Relative Loss Factor

2.5 THEMEASUREMENT PERMITTIV~

OF COMPLEX
2.5.1 Parallei Plate Capacitor
2.52 Open Ended Coaxial Probe
2.5.3 Transmission Line
Chapter 3: Measurement System and Testing Procedures

3.1 MODIFICATION
OF SAMPLE
HOLDER
3.1.1 Selection of Sample Length
3.1.2 Measurernent of Soil Conductivity
3.1.2.1 Static Conductiviîy of the Soi1 Sample

3.1 -2.2 Development o f a Staiic Conductiviv iMeasurernent $vstem

3.1 2 . 3 Lérification Testing of Soil Condzrctivity Measuremrnr

3.1.3 Compaction of Soi1 Sample
AND TESTING
3.2 SAMPLE PREPARATION PROCEDURES
3.2.1 sainpie Preparation
3 2.2 Testing Procedures
OF COMPLEX
3.3 METHODOLOGY PERMITTIVITY
ANALYSE
3.3. i Electrode Polarization
3.3 2 Measurement of cd'
3.3.3 Measurement of cd"
3.3.3.1 Extraction of Soi1 DC Conductivity

3.3.3.2 Extraction of E, "

3.5 SUMMARY
AND CONCLUSIONS

Chapter 4: Complex Permittivity of Compacted Halton Till

4.1 SELECTION
OF SO[L PROPERT~ES

4.1.1 Soi1 Water Content

4.1.2 Relative Bulk Density
4.1.3 Mixing Fluid Salinity
P E R M I ~ I V I TMEASUREMENTS
4.2 COMPLEX Y
4.2.1 Soil Properties of the Measured Samples
42.2 Complex Permittivity Measurement Results
4.3 DATA
ANALYSIS
4.3.1 Volumetric Water Content
43.2 Relative Buik Density
4.3.3 Mixing Fluid Salinity
4.4 DEVELOPMENT LINEARREGRESS[ONMODEL
OF A MULTIVARIABLE

4.41 Results of the Multivariable Linear Regressions

Chapter 5: Summary, Concfusions and Future Work

References

Appendices

A: Sample calculation of Nicolson and Ross solution for conversion of S-

parameters to complex permittivity

B: Soi1 properties of Halton till

C: Calibration of HP8753D Automatic Network Analysis

D: Complex permittivity versus fiequency graphs for ail samples tested

E: Residual plots for Eqs 4.5,4.6,4.7,4.8,4.9,4.10,4.11,4.12,4.13.4.14

vii
 LIST OF TABLES

TABLE DESCRIPTION

Chapter 4: Complex Permittivity of Compacted Halton Till

4.1 S u m m q of Sample Soi1 Properties

4.2 (a) Summary of Complex Permittivity Measurement Results

4.3 (b) Summary of Complex Perminivity Measurement Results

4.3 Summary of Complex Permittivity at the Relaxation Frequency

FIGURE DESCRIPTION
Chapter 2: Literature Review

2.1 Polarization mechanisms

3.2 Maxwell Gamet mode1 of a two phase system

2.3 Debye model

2.4 Cole-Cole plot

2.5 Open-ended coaxial line probe in contact with material under test

2.6 Reflection transmission and absorption of electromagnetic waves

2.7 Wave guide and coaxial configurations of a transmission line

Chapter 3: Measurement System and Testing Procedures

3.1 Original measurement system

3.2 Schematic of original sample holder

3.3 Original sample holder with cylindrical section split

3.4 Effect of sample length on dielectric dispersion

3S Equivalent circuit model of Debye model

3.6 Dielectric dispersion frequency versus sample length

3.7 Schematic of soi1 conductivity measurement system

3.8 Cornparison study of sample ce11 to standard ASTM method

3.9 Compaction cell

3.10 Assembly of sample holder

-
i? IGURE DESCRIPTION

3.1 1 Components of the relative loss factor

3.12 Typical dielectric measurement data plot

Chapter 4: Compler Permittivity of Compacted Halton Till

Typical plot of the data trace obtained fiom a complex permittivity

measurement

Relative complex permittivity at 200 MHz versus volumetric water

content at constant density and salinity

Relative complex permittivity at relaxation fiequency versus

volumetric water content at constant density and salinity

Characteristic c u v e for the complex permittivity versus moisture

content

Relative complex permittivity at 200 MHz versus relative bulk

density at constant water content and salinity

Relative complex permittivity at relaxation fiequency versus

relative bulk density at constant water content and salinity

Relative complex permittivity at 200 MHz versus mixing fluid

salinity at constant moisture content and density

Relative complex permittivity at relaxation frequency versus

mixing fluid salinity at constant moisture content and density

The effect of dc conductivity on the relative loss factor at relaxation

fiequency

Sensitivity of the coefficients of the multivariable linear regession

to measurement frequency
(Coefficients: Eqs 4.5,4.6.4.7.4.8.4.9.4.10.4.11.4.12)
 LIST OF SEMBGLS

Area of capacitor plates (m')

Radius of inner conductor (rn)
Radius of outer conductor (m)
Capacitance (F )
Capmitance of empty space (F)
Dissipationfbctor
Penetration depth (cm)
Electr icalfield strength ai a radial distance r (Wm)
Farad
Frequency (Hz)
Loss current (A)
Churging current (A)
Electrical current (A)

fi
Current density ( k m ' )
Electricul lrngth (ml
Length oj-sample (m)
Mass (kg)
Mass of soif (kg)
Muss of water Ikg)
Total mass (kg)
Siemens
MixingJuid salinity as concentration of NaCl (g/L)
Resistivity (Rem)
Volume (m3)
Voltage potentiul between points a and b ( V )
Total volume (m3)
Volume ofwater (m3)
Gravimetric water content (%)
Characteristic moisture content (%)
Impedance (O)
Empirical factor for Cole-Cole plot
Complex permittiviîy (Fmor (C%rn)
Relative complex permittiviîy
Real component of cornplex permittivity (F/m) or ( C " / J ~ )
Imaginary component o f COmpiex perm ittiviv (F?m) or ( ~ ' d m )
Real relative permittiviîy of dielectric material
Relative loss factor of dielectric material
Relative ioss factor from siatic condzrctivity
Real relative permittiviw@orn the electrol
Relative loss factor fiom the electrode
Effective real relative permittivity
Permittivity of host medium (Flrn) or ( c ' / J + ~ )
Relurive real rneasured permittivity
Relative measurrd loss factor
Permittiviîy of a vacuum (8.8541878 F/m or (C'LJ-m))
Relative real permittiviv
Relative loss factor
Relative real permitfivi@at rhe relaxation jrequency
Relative loss factor ut the relaxation freqltency
Static permittiviîy (F/m) or ( C ? J ~ )
Very high frequency permittivity (F/m) or (c'/J-m)
Volumefiaction (%)
Loss angle (radians)

xii
Volurnetric moisfure content (96)
Angle of inner conductor (degree)
Angle of outer conductor (degree)
Line charge density per unit length ( U m )
Pi (3.1415926)
Bulk density ( ~ ~ / m ' )
Condtrctivity (mho/m)
Relaxation rime (s)
ilngular freq uency (radiands)
Relaxution freqziency (radianris)

S..

Xlll
 Introduction

The detection and delineation of soil and water contamination at industrial and

landfill sites continue to be a challenge facing engineering professionais. Currently.

the drtection of soil or water contamination involves the collection of representative

samplrs and then subsequent analysis for targeted species. Aside tiom the potential

hazards that are associated with the handling and testing of contaminated soil or

water. sample collection and laboratory analysis have a nurnber of additional

disadvantages. Soi1 sampling for contaminant detection is time consuming and

expensive: frequently a great deal of timr and effort is expended only to demonstrate

that there has been no change in conditions or ihat contamination bas not occurred.

The integrity of a collected sample may also be compromised as samples can be

contminated during sampling, transportaiion. and analysis in the laboratory. Finally.

sampling is "destructive" when soil samples are removed and is not continuous with

tirne.

These factors al1 contribute to the need for the developmrnt of non-invasive or non-

destructive in-situ technologies that can be used to establish either the presence or

absence of contamination in a reliable and quantitative manner.

For the purposes of geoenvironmental applications such as contaminant detection and

site assessrnent and characterization, it is important to understand the physical

response of a soil to changes in environmental conditions. This research project is

based on the concept that the complex permittivity of any rnaterial is a reflection of

its physical and çhemicd properties. The interaction between an extemal electnc

field and a soil-water system can be characterized into two components. conduction

and polarization. Polarization represents the ability for a material to store rlectrical

charge. while conduction refers to the ability of electrical charge to move through a

material. The combination of these two responses is commonly refened to as the

çomplrx permittivity.

The study of the interaction between rlectromagnetic waves and water containing

materials. known as microwave aquametry (Kraszewski 1997). is an emerging field

with application in many areas including geotechnical and environmental

engineering. The complex permittivity of soil-water systems is a function of a

number of physical properties such as water content. particle sizr. density and

mineralogy. Furthemore. the complex perrnittivity of al1 water containing materials

is a Function of fiequency (Kraszewski 1997) and therefore. as the frequency of the

imposed electric field increases the response of the complex perminivity will also be

affected. tt is possible therefore to detect changes in the soil-water system by

measuring changes in the complex permittivity of the soil system.

Tnere are a number u î rnrihods currently available to measure the cornplex

permittivity of soils. The most common methods include parallel plate capacitors.

open ended coaxial probes and transmission lines. Regardless of the method. it is

essential that for the accurate measurement of the complex permittivity of a soil the

measurement system satisS a few key requirements:

1. The system must be capable of performing accurate measurements of both the real

and imaginary components of the complex permittivity in a specific tiequency

range in which the complex permittivity is sensitive to changes in soil properties

and;

1. The sample holder must be large enough so that the sarnplc under test is

representative of the h b t k and structure of the native in-situ soil.

Based on the success of prior investigators using a coaxial (transmission line) sample

holder and the previous work iilready completed and discusscd in Shang et ai. ( 1999).

a coaxial sample holder was selected for this study.

The results of the study by Shang et al. (1999) suggested that the original

measurement system provided reliabie measurements of the complex permittivity of

undisturbed clay samples (obtained kom block samples). However. in order io

reduce the effects of sample handling and to further increase the accuracy of the

measurements, a number of modifications were made to the original sample holder

and the sarnple preparation procedures.

The long-term objective of this research program is to develop a new and novel in-

situ rneasurement systern that would allow quick, reliable and non-destructive

monitoring and assessrnent of soil and groundwater contamination and to implement

this in the field. To that end. this thesis represents part of that broader study and is

directed at the development of technology. based on the interaction of

clectromagnetic waves with geomaterials, to address the need for a reliable method to

detect and delineate soi1 contamination. The first stage in the development of such

technology is to assess the range of applicability and sensitivity of the technique.

This thrsis specifically addresses the development of a laboratory complex

measurement system and measurement technique that can be used to aswss the

complex permittivity of compacted soil sarnples.

Much of the investigation surrounding the complex permittivity of soil-water systems

has been centred upon the relative permittivity at a fixed frequency. The development

of a measurement system that can measure both the real (permittivity) and imaginary

(loss factor) components of the complex permittivity over a broad frequency

spectnim provides an opportunity to use the real permittivity and the loss factor. at

various fiequencies, as additional quantities to characterize a soil-water system.

me L M . * . - - E '1.'
ul uis thesis is the charactcrization of a mil-wate: çystem ushg b&!i

components of the complex permittivity, the permittivity and the loss factor. In

addition. the effect of the frequency at which the measurements are made will be

investigated as an additional parameter that may be considered in soil-water

charactenzation.

The specific objectives of this investigation are:

To develop a laboratory measurement system for measuing the frequency

dependent complex pemittivity of a soil-water-electrolyte system. The

measurement system. based upon the system developed and detailed in Shang et

al. ( 1999). is to be modified to reduce sarnple handling and to facilitate the use of

a contaminant perrneation apparatus for a cornpanion study by Xie ( 1999);

To develop a methodology to characterize soil properties using both components

of the complex permittivity. the relative permittivity and the loss Factor:

To measure the complex permittivity of soil systems of varying moisture content.

density and rnixing Huid salinity and to establish the selectivity and sensitivity of

the cornplex permittivity and:

To study the effects of voiumetric moisture content, bulk density and mixing fluid

salinity on the complex pemittivity and develop a multivariable linear regression

mode1 that is representative of the response observed.

Chapter 3 presents a literature review of the concepts and applications involving

the measurement of the complex permittivity of materiais. specifically

-eeomateriais:

Chapter 3 presents the design of the sample holder modification and sample

preparation procedures. This section will investigate the original design criteria

for the sample holder and illustrate how the modifications made to the system

improves the accuncy of the complex permittivity measurements and allows for

the measurement of static conductivity:

Chapter 4 presrnts details of the study including the selection of soil type. sample

property variables and the analysis of the complex permittivity as varied with

frequency. The results of the study will be presented as a group of linear

regression rquations that relate specific values of the complex permittivity of

Halton till as a h c t i o n of soil moisture. bulk density and mixing fluid salinity. h

discussion of those equations and their significance will also be presented. and:

Chapter 5 presents the surnrnary. conclusion and recomrnendations for hnher

research.
1.3 ORIGINAL
CONTRIBUTIONS

The development of a coaxial sample holder and measurement system is a

continuation of previous work undertaken by Shang et al. (1999). This thesis presents

a number of modifications that were made in order to increase measurement accuracy

and reduce sample handling. The development of the compaction unit and the dc

conductivity measurement system. discussed in Chapter 3. is an important strp in the

development of a laboratory measurement system for measuring the frequency

dependent complex permittivity of a soil-water-rlectrolyte system.

The use of electromagnetic waves to characterize subsurface contamination has bern

suggested by a number of authors (Thevanayagarn 1995. Kaya and Fang 1997. Shang

et al. 1999) however. much of this previous work has been focussed upon the use of

the dielectric constant and not the comples pemittivity. Little is known about the

complex permittivity behaviour of clayey soils. This thesis looks specifically at the

response of both the real and imaginary components of the complex permittivity and

the possibility that the two components c m be used sirnultaneously to characterize a

soil-water system.

Finally, the investigation into the effect of the measurement frequency on the

complex permittivity is significant with respect to developing a methodology to

delineate sub-surface contamination. The selectivity and sensitivity of the complex

permittivity to environmental changes is investigated by measuring the complex

permittivity at a number of specific frequencies.

 Literature Review

2.1 COMPLEX
PERMI~~IVI~Y

When a material is placed into an electric field the response of the material may

involve polarization and conduction. Polarization represents the ability for a material

to store electrical charge. while conduction refers to electrical charge that remains

fiee to move through a material. The combination of these two responsrs is

commonly referred to as the complex permittivity. Polarization and conduction may

involve the following mechanisms (Flinn and Trojan 1990):

1 . Eleetronic and atornic polarization (Figure 1.1 A): The positions of the outer-

shell elrctrons (valence electrons) around atoms are affected by the

rlectromagnrtic field (Flinn and Trojan 1990). The valence electrons of an atom

are displaced in the oscillating field such that its centroid is separated from the

centroid of the nucleus. An electric dipole is then created and the molecule

brcomes polarized (Rao 1977). Loss mechanisms due to atomic and electronic

polarizations. collectively called "distortion polarization". occur at frequencies in

the infiared and visible part of the electromagnetic s p e c t m (Kraszewski 1997).

Investigations involving the use of a material subjected to electrornagnetic waves

in the microwave frequency range will not observe this polarization behaviour.

2. h i c polar&ation (Figure 2.18): Results from the separation of positive and

negative ions in a molecule formed by the transfer of electrons from one atorn to
 another in the moiecule. Ionic Polarizauon iaicrs place vrry rapidiy and oniy in

ionic solids.

3. Space Charge (M~xweIl-

Wagner) (Figure 2.K): Development of charge at the

interface of two phases (most commonly. solid and liquid). The effects of

Mawell-Wagner polarization are only prominent with very low kequencies and

again. as with electronic and atomic polarization. this polwization behaviour will

not be evident at microwave and radio Frequencies factor (Santamarina and Fm.

1997.

4. Orientation oJiMolecules (Figure 2. ID): When asymmetric (polar) molecules are

present, their orientation is changed by the field. In the frequency range

corresponding to radio and microwave frequencies ( 10' to 3x10'~) Hz.) this

phenomrnon is the most important contribution to the loss factor (Santamarina

and Fam. 1997).

The constituent molecules or dipolar species within a material require a finite time.

çalled the relavation time,~.to adjust to the changing electromagnetic field. This

process gives rise to a phase lag between the imposed field and the material's

response. The phase lag is a function of the angular frequency. o. of the

electromagnetic field. 4s a result the permittivity of the material cm described by a

complex quantity ~ ' ( , ~ l m ) :

- -WU^
-L E' is the r d part of the ~ ü m p i epzmiitttvity
~ û k represerin puiàïiraiiuii (iii

phase) .j = dl. and dt is the imaginary (out of phase) part of the cornplex
permittivity .

The complex permittivity of materials is often normalized with respect to the

permittivity of a vacuum and referred to as the relative permittivity (dimensionless)

where the permittivity of a vacuum is E, = 8.854 1 IO-" F/m. &r' is the relative

pennittivity. and E," is the relative loss tàctor.

2.1.1 Relative Permittivity

The relative permittivity. E,'. is a quantity used to evaluate the charge sronng capacity

of a material (polarkation) and represents the in-phase portion of Eq. 2.2. The value

of the relative permittivity will depend on the ability of the material to react and

orient itself in the imposed electromagnetic field (Flinn and Trojan 1990). The

greater the reaction. the greater the energy stored and therefore, the higher the relative

pemittivity ( F ~ Mand Trojan 1990). In ternis of the relative permittivity. the

behaviour of a dielectric is most affected by the orientation of the molecules in the

material ( F ~ Mand Trojan 1990). The imposed electromagnetic field changes the

orientation of asymmetric (polar) rnolecules. A greater charge can build up when a

material with a stmng dipole is placed in the field and as such will have a higher
rclativc pemittivity. Siniilar reasoning suggests thal liquids have higher relative

permittivity than solids because polarization or dipole orientation is easier (Flinn and

Trojan 1990).

2.1.2 Relative Loss Factor

With the exception of some low-loss materials such as plastics and non-polar liquids.

the dielectnc properties of most materials will Vary with the frequency of the applied

electric field (Kraszewski 1997). As described in Eq. 2.1 the Ioss factor represents

the out of phase loss of elecvical field energy in a material.

In the case of porous media. the energy loss from dipolar orientation represents one of

two major components contributing to the overall energy Ioss. The second major

component of the dielectric losses in a porous media is the electrical conductivity of

the media. o (Slm). Conductivity may be the result of both surface conduction. due

to electrical charges on the surface of the solids. and ionic conductance. due to

dissolved electrolytes in the water. For dielectnc measurements invoiving clay-

water-electro lyte systems. the double layer surrounding clay particles makes the

surface conductivity a significant component to the total dielectnc loss. The

contributions of both components of the loss factors to the relative complex

permittivity gre is given by:

Clay-water systems can be described as multi-phase systems consisting of solid.

liquid and gas phases. The clay particles constitute the solid phase while water and

the air constitute the liquid and gas phases. respectively. The cornplex permittivity

properties of a clay water system are then also a function of the dielecuic properties

of each of the constituent phases. The dielcctric constant of water is much higher

than that of the other components (80 as opposed to approximately 4 for solid and 1

for air) and thus the dielectric constant is very sensitive to the water content

(Friedman 1997).

Mixing niles drscribe quantitatively how the microscopic permittivity of a mixture

depends on the components and the microstructure of the medium (Kraszewski 1997).

Mixing models are obtained tiom analytical solutions based on global and local

electnc fields. electric circuit analogies and empirical reiations (Santamarina and Farn

1997).

There have been a nurnber of empirical equations suggested for the relationship

between the volumetric moisture content (8) and the effective relative perrnittivity of

soil-water systems as observed from experirnents. ( E ' ~ ~ ~ )The

. simplest mode1

incorporates a two-phase system in which one of the components is represented as a

guest randomly embedded in the host material of the second phase (see Figure 7.2).

The Maxwell Garnett formula for this material description cm be written as follows:
where &hm, is the permittivity of the host medium, E is the permittivity of the guest

material. q is the volume fiaction of the space filled with the background material and

cegis the effective permittivity of the material sample.

D~SPERS~ON
2.3 DIELECTRIC

The dielectric parameters described in the previous section were presented as mater

constants. This implies that the mode1 was denved at a given frequency and not 01

a range of kquencies. A material whose dielectric properties Vary with

electromagnetic wave tiequency may be described as a dispersive material.

Dielectric dispersion refers to the change in the dielectric properties of a material with

a change in the frequency of the imposed field. 4 s shown in Eq. 2.3. the dielectric

behaviour of a material depends on the fiequency of the imposed electrornagnetic

field and the charactenstics of the material. It is common for electrolyte systems to

exhibit a dielectric response that can be described using the Debye mode1 (see Figure

2.3):
where es and are the iow and high-fiequency permittivities. ana r is the relaxation

time (Kraszewski1997).

The mode1 describes a relaxation behaviour caused by the molecular orientation of a

dipolar molecule. When the motion of molecules and ions cm no longer change fast

rnough to reach equilibnum with an extemal altemating electnc field. the permittivity

(E;) will start to decrease with increasing frequency and this is associated with an

increase in the loss factor (&y) as shown in Figure 2.3. The peak loss value will occur at

the characteristic relaxation fiequency. a,.and therefore changes to intrinsic propertirs

of the clay-water system c m be characterised by changes in this peak loss value. Based

on the forepoing discussion one can use components of the complex permittivity to

characterise dielecmc properties of a clay water system.

The curves presented in Fig. 1.3 are plotted in the conventional marner by plotting E'

and E" as a function of frequency and represent a typical Debye response. A more

convenient representation of the data is obtained by plotting the data on the complex

plane in which the imaginary part of the complex permittivity (E") is plotted against

the real part (E'): rach point being characteristic of one fiequency of measurement.

This diagram may be called a complex locus diagrarn or an Argand diagrarn. but is

most cornrnonly referred to as a Cole-Cole plot. narnrd after K.S. Cole and R.H. Cole

who first applied it to dielectrics. An example of a Cole-Cole plot is presented in

Figure 2.4. The plot is characteristic of a semi-circle with its centre on the real (CO)

a i s and intercepts at c', and &'r on this a ~ i (Cole

s and Cole 1941). The equation of
the semicircle is developed From the cquations for the complcx permittivity, as

presented by Deblye (Eq. 2.5 and 2.6). The equations for the cornplelr permittivity are

the parmetric equations of a circle in the E'. E" plane, for. on eliminating the

paramter or between the two equations and rearranging. one obtains:

which is the equation of a circle (Cole and Cole. 1941). Only the semicircle over

which E" is positive has physical significance. therefore this semi-circle is the locus of

the dielectric constant as o varies î'rom zero to infinity. Many materials. particularly

long chained molecules and polymers. show a broader dispersion curve and lower

maximum loss than would be expected from the Debye relationship (Hill et al. 1969).

Cole and Cole ( 194 1) suggrsted than in the case of a lossy material the permittivity

may tollow the empirical equation:

where the parameter a represents the angle of tilt of the circula arc from the real

auis. The value of a is an empirical factor. which correctly maps small departures

fiom the serni-circular c w e generated by an ideal Debye response. The use of the

Cole-Cole plot has the disadvantage that the frequency. which is the independent

variable and the one whose value is most accurately known. is not explicitly shown

(Hill et al. 1969).

2.4 ASPECTS
PRACTICAL OF COMPLEX
PERMI~IVIN

The measurement and understanding of the principals goveming the dielectric

response of a material is a multi-disciplinary challenge. The range of applications

vary from electrical en-ineerine (the design of capacitors and microchipsh to medical

research (looking into the effects of high voltage on biological tissue). to agricultural

applications (involving the measurement of soil moisture content). For the purposes

of this study. the application is limited to those involving the mrasurement of the

dirlectric propenirs of geomaterials.

In the investigation of geomatenals, the moisture content is a fundamental physical

property. The accurate measurement of soil moisture is important for soi1 relatrd

investigations. such as the study of plant growth. water infiltration and run-off.

traffïcability and soil compaction. irrigation scheduling and yield forecasting (Morgan

et al. 1993). as well as classical applications. in soil rnechanics and foundation

engineering.

The dielectric properties of rock in the frequency range of 0.5 MHz to 1.1 GHz. have

been used to estimate the hydrocarbon content of reservoir rocks. Clay minerals

occur in sedimentary rocks of al1 ages and affect the dielectric properties of the rock.

Therefore, if the effect of the clay minerals on the measurement of the dielectric

properties of the rock is not taken into account the estimation of hydrocarbons may be

incorrect (Raythatha and Sen 1986).

The gravimetric water content and bulk density of a soil cm be used to assess how

easily a soil can be worked or tilled. Following cultivation for agricultural purposes

the bulk density of a soil will remain fairly constant during the growing season so the

parameter that becomes of particular interest is the volumetric water content (Perdok

et al. 1996). Volumetric water content. 0. can be calculated from bulk density of the

soil. p. and gravimetric water content. W. by the formula &p.assuming a specific

gravity for water of 1 g/cm3. Monitoring the long-term changes in the volumetric

water content allows for the calculation of water movement and use (Perdok et al.

1996).

Environmental engineering applications involving the measuremrnt of the dielectric

response of a soil are based on the fact that many of the environmental factors that

affect the dielectric response of a soil will also affect the b'physicochernical and

mechanical soi1 behaviour" as well (Thevanayagarn 1995). By rneasuring the

dielectric constant. one could quantitatively rvaluate the microscopie and bulk soil

behaviour under existing conditions at the site as well as identify changes in the

~eoenvironrnentthat may occur with time (Thevanayagam 1995). The reason for
C

using the dielectric constant is that the dielectric constant of soiis is almost

independent of chemical composition and particle shape. and is considerably lower

than that of most liquids (Kaya and Fang 1997).

For the purposes of geoaiwiroiunèntd applications such as contaminant deteetion or

site characterization, it is important to understand the response of a soil to changes in

environmentai conditions. Currently the most comrnon methods used to characterize

subsurface contamination involve collecting representative soil and water sarnples

and analyzing them for targeted species (Kaya and Fang 1997). Frequently a great

deal of effort is expended to demonstrate that no change in conditions or

contamination has occurred. Ln addition. sarnple collection and laboratory analysis

has the disadvantage that: (1) sampling of the soil is time consuming and expensive:

(7) sampling is "destmctive" when soil sarnples are removed: (3) sampling is not

continuous with time: and (4) samples c m be contarninated during sampling.

transportation. and analysis in the laboratory (Kaya and Fang 1997). There is a

drmonstrated need for the development of non-invasive or non-destructive in-situ

technologies that can be used to reliably and quantitatively rstablish either the

presence or absence of contamination.

2.5 THE MEASUREMENT

OF COMPLU(PERMITTIVITY.

The following section will discuss a nurnber of measurement systems that are suitable

for the measurement of the complex permittivity of geomaterials.

2.5.1 Parallel Plate Capacitor

One can measure the complex permittivity of a material using the basic physical

principals behind the design of a capacitor. The capacitance. Co. of an empty space

between two parallel plates is given by:

where A is the area of the plates, d is the separation distance, E, is the reai

permittivity of a vacuum. If a material is placed between the w o plates the

capacitance will increase to:

where E~ is the relative dirlectric constant of the material. .As discussed in a previous

section the permittivity of a material is a cornplex Function resulting fiom the cnergy

dissipation in the capacitor. This energy dissipation is expressed as a loss current I,

that lags the charging current Ic. and is separated from the charging current by a loss

angle. 4:

The tangent of the separation angle between the loss current and the charging current

is comrnonly referred to as a dissipation factor. D. and can be used to describe the

complex permittivity ternis expressed in Eq. 2.1 as follows:

Iri the sàit of lvw k q u c r i c y :izlectric masüïcncnt (< = IOMHz.) "the most

significant error associated with this two-terminal measurement system is electrode

polarization" (Klein and Santamarina 1997). In the presence of ions, the ions will

move under the externally applied field if there is enough time for them to orient

themselves in the direction of the electric field (Kaya and Fang, 1997). The ionic

conduction causes an ionic d i f i s e double layer to form at the electrode (Klein and

Santamarina 1997). Depending on the material used for the electrodes. oxidation-

reduction reactions c m occur at the electrode-material interface. Collectively these

çffects are referred to as electrode polarization and they will effect the computed

values of the complex permittivity (Klein and Santamarina. 1997).

At frequrncy above -10 MHz. additional m o r s can affect the rneasurement of the

complex permittivity. such as fnngeledge capacitance and surface conductance.

Surface conduction occurs as the soil-fluid system becomes conductive and the

charging current is reduced. resulting in an increase in the dissipation factor

according to Eq. 2.1 1. The non-uniform field near the rdges of the capacitor plates

and around the sarnple causes fnnge effects but these can be reduced by using guard

electrodes (Klein and Santamarina 1997).

2.5.2 Open Ended Coaxial Probe

An open ended coaxial probe is essentially a cut off section of a transmission line (see

Figure 2.5). By measuring the reflectivr and transmission properties of the applied

electromagnetic field between in the inside and outside wave-guides. the complex

permittivity of a material c m be obtained.

Reflection occurs when an electromagnetic wave meets a matenal of different electrîc

properties. The magnitude of the reflection depends on the difference between the

real relative perrnittivities of the medium. Any power not reflected is transmitted past

the boundary and into the medium (see Figure 2.6). Refiection and transmission

behaviour can be quantified by Iooking at the ratio between the reflrcted or

transmitted power to the applied incident power. These ratios are collectively cailed

scattering parameters and are used in the closed form Nicolson and Ross solution to

compute the complex permittivity of the material under test (Nicolson and Ross 1970)

Some of the electromagnetic energy transmitted into the buik of the material will be

absorbed and convened to heat. The heating power generated is directly related to

the E". (loss factor) of the material. If the E" is large the material will strongly absorb

the field energy and microwave heating may occur. For the dielectric measurement

of a high loss material such as soi1 this becomes important as any heating h a t does

occur could have an effect on the moisture content of the sample and therefore the

sample will not be representative of the soi1 medium.

The dielectric properties of the material are measured by placing the open-ended

coaxial line against a solid. or immersing it into a liquid. Good contact between the

specirnen and the probe is very important as any air gaps and fluid segregation will

cause error in the measurements. The complex permittivity of soil-water mixtures

has been measured by a comercially available probe (e.g. HP85070a Klein and
Santamarina 1997) designed for measuriny corripiex pcriiii~ivitiesof liquid and semi-

solids. It has been reported that when used on high loss matends such as wet soils.

the electromagnetic waves transmitted from the probe c m only reach a depth of

several millimetres and as a result this approach is not suitable for distinguishing the

structure and water content of undisturbed and compacted clay soils (Shang et al..

1999). The distance over which power decreases by a certain factor is called the

penetration depth. The expression that is commonly used to describe the distance

over which power decreases by a factor of roughly 37% (Engelder and Buffler 1991 ):

For a high loss material such as wet soi1 the penetration depth wili be very low (in the

order of millimetres) and therefore insufficient to properly characterize the rnatenal.

2.5.3 Transmission Line

The transmission line utilizes much of the sarne principles involved in the open-ended

coaxial measurement systern discussed above. This method involves placing a

sample of material inside an enclosed transmission line. The transmission line may

be either rectangular or coaxial but in either case the sample must fit precisely in the

cross section (see Figure 2.7). Coaxial measurements are a comrnon technique for

high frequency rneasurements (Huang and Shen, 1982). During the measurement an

electromagnetic wave of a given Frequency is sent propagating down the centre

conductor of the coaxial system. When the wave encounters the core sample part of
the wave is absorbed and part is transmitted through the sarnplr as d o ~ i 3 j i . ihi

section 2 . 5 2 . A computer is then used to deduce E' (energy reflection and

transmission) and E" (energy absorption). The transmission line method has been

found to be more accurate and sensitive that the open-ended dielectric probe

(Engelder and Bu ffier 199 1).

The second advantage of this method over the open ended probe is that wave

penetration is much greater than that of the open ended method and thus cm

accurately reflect the dielectric property of heterogeneous materials of larger

diameters ( Baker-Jarvis. 1990).

A previous investigation (Shang et al. 1999). presented the design and calibration of a

complex permittivity measurement system for compacted and uncompacted soils

using a specially designed coaxial sarnple holder. The measurement system

developed for that study consists of an Automatic Network Analyzer (ANA). a

coaxial sample holder. a set of coaxial cables and a PC for data processing. The ANA

measures reflection and transmission functions of linear networks through sine wave

testing. The reflection and transmission characteristics of the specimen under testing.

the S-parameten. are then converted to the complex permittivity by a closed-fom

solution (see Appendix A).

Based on the success of thar investigation and d e r cornparison with other available

methods, a coaxial transmission line sample holder was chosen for this study. Details
of the measurement system used for this stuciy as well as the niudifisations made to

improve rneasurement accuracy will be presented in Chapter 3.

2.6 THECOMPLMPERMITTIVITY
MEASUREMENT
OF GEOMATER~ALS

There is a demonstrated need for the development non-destructive in-situ

technologies that c m reliably and quantitatively predict and evaluate either the

presence or absence of contamination. A nurnber of researchers have investigated the

dielectric response of soi1 to variations in soi1 properties and have presented empirical

relationships to describe that response. The following section will present some of

the major contributions to the general understanding of dielectric response involving

geomaterials, and specifically fine soils.

Klein and Santarnarina (1997) looked at two low frequency techniques and one high

frequrncy technique for the measurement of dielectric permittivities of soil-water

mixtures in the frequency range of 5Hz to 1.3 GHz. Low kequency (4OMHz.)

measurements were completed using both a two terminal and four terminal

measurement system in conjunction with an impedance analyzer and high frequency

measurements were completed using a commercially avaiiable dielectric probe. It

was shown that low fiequency measurements of clay-water-electrolytes were difficult

to obtain when using a parallel plate capacitor system (such as the two or four

terminal methods) to make the measurernents due to electmde polarization. The

minimum fiequency at which electrode polarkation does not significantly affect the

two terminal measurements is a function of the conductivity, permittivity and length

ûf ù\c specixen. Wein and Santamarinn c~.i,cb~ded
th3t altlough cumbersome to

measure, low frequency measurements could provide some information about the

interaction between phases in a multiphase system and double layer phenornena.

The high frequency measurements where made using a comrnercially available

dielectric measurement system that utilized an open-ended coaxial probe. Klein and

Santamarina concluded that the use of the dielectric probe allowed for easy

measurements of the complex permittivity and that is could be used to characterize

sorne properties of soil-water mixtures such as moisture content. It was shown that

both the effective conductivity and the permittivity of the soil-water mixture

increased as the water content increased towards saturation. This conclusion is

consistent with the conclusions presented by other authors throughout the literature.

However. the use of the open-ended dielectric probe for the measurement of the

complex permittivity of high loss materials has been s h o w to be inaccurate. As

discussed previously it has been found that the electromagnetic waves transmitted

tiom the probe can only reach a depth of çeveral millimetres and hance this approach

is not suitable for distinguishing the structure and water content of undisturbed and

compacted clay soils (Shang et al.. 1999).

Perdok et al. (1996) investigated the influence of gravirnetric water content and bulk

density on the dielectric properties of soil. Using a frequency domain sensor

operating at a fixed frequency of 20 MHz, the authors attempted to obtain a consistent

set of calibration curves that expressed the permittivity, E', as a h c t i o n of

gravirnetxic xtter content, w , d bulk dcfisity, p. The mcasuremerit system cûiisisted

of three 2-mm diameter stainless steel rods, 60 mm long, spaced 10 mm apart. The

sensor measured the complex impedance of the soil. which in tum was used to

calculate the pemittivity and electrical conductivity . The authors found that the

relationship between E' and w can be described as a power Function while the relation

between permittivity and bulk density appeared to be linear. The tests were carried

out using three soil types. a sand, a sandy loam. and a clay. The authors îùrther found

that differences in the soil texture influenced the magnitude of the relative

pemittivity, particdarly as a result of changes in bulk density. The authors

concluded that for sandy soils under drier conditions and clayey. aggregated soils. E'

is governed not only by water content but also by bulk density.

The influence of bulk density on the relative permittivity of a soil is interesting. It

has been established that the conductivity of a soil will influence the complex

pemittivity (Kraszewski. 1997) of that soi] and in tum. that the conductivity is a

function of the bulk density. Now. the conductivity affects the loss term of Eq. 2.3

and this may suggest that changes in the bulk density of a soil may be reflected in

changes in the relative loss factor of a soil. The majority of work involving the

dielectric properties and soil property charactenzation has been done with the real

part of the complex permittivity with little emphasis placed on the relative loss factor.

Thevanayagarn (1995) investigated the tiequency-domain analysis of the electrical

dispersion of soil. The concept of dispersion has been discussed previously in this
 27

chapter. In summary, dielectric dispersion refers to the change in the diclcctnc

properties of a material with a change in the fiequency of the imposed electric field.

Although the studies of various effects to explain the observed dispenion are too

numerous to report, lack of an dl-inclusive successful mode1 to explain the observed

anomalous dispersion is recognized in the literature (Thevanayagam 1995). The

author takes into account the effect of particle shape, frequency, soil mineralogy. pore

Huid type. porosity. solid-Huid interaction. anisotropy. and direction of rneasurement.

Thevanayagam found that permittivity and conductivity of soils are affected by

particle shape. particle orientation. and the ratio of the effective permittivities and

conductivitties of the solid particles and pore fluid. These results indicate that

frequency-domain interpretation of the dispersion data c m be used to predict soil

microstructure. soil and pore fluid type and interaction. porosity. particle

characteristics. anisotropy, and geoenvironmental conditions at a site (Thevanayagam

l'he research done by Thevanayagarn is important as it provides evidence hat soil

properties and characteristics can be predicted by studying the dielectnc response of

soil. Thevanayagam catagorized the dielectric response by cornparhg the occurrence

of E' and o (conductivity) dispenion. Again. most of the attention was placed on real

part of complex pennittivity and the response of the relative loss factor was

represented only by one of its components, i.e. conductivity.

 + Aoolied
b I

Electron Polarization lonic Polarization

......
+
O-:..
O +

Space Charge (Maxwell-Wagner' Orientation of Molecules

Figure 2.1 :Polarization Mechanisms (adapted from Santamarina and Fam 1997)
Figure 2.2: Maxwell Gamet model of a two-phase system, (Kraszewski 1997)

0-
Figure 2.3: Debye model

O 2 4 6 8 10 12 14 16
E ID

Figure 2.4: Cole-Cole plot

 7 Material
under test

. -

Fringing
electric field

Figure 2.5: Open-ended coaxial line probe in contact with matenal under test

lncident Material

Incident

Figure 2.6: Reflection, transmission and absorption of electromagnetic waves

 Waveguide

Coaxial

..:.:.:.:.:.:.:..
,*:.:::.:..

O
*:;{!.
iil(+'J ..:.:.:.:.:.
.:
.::::::::::::::::.:.:::::::::::::::.
s.:.:.:.:.. ;$y$!;

- ; ..::ig;;$i
:..........................
.........................
:::...................
................
:::::::::::::::::::'
.............
.......
D
C------+

Figure 2.7: Waveguide and Coaxial configurations of a transmission line

 Measurement System and Testing Procedures

The measurement system used for this thesis is based on the system developed by

Shang et al. (1999). The system consists of an Automatic Network Analyzer (ANA).

a sample holder. a set of coaxial cables and a PC for data processing, as shown in

Figure 3.1. The ANA measures the reflection and transmission characteristics of the

specimen under test. and using a closed-form solution (Nicolson and Ross 1970) the

complex permittivity of the sample is calculated using a PC.

The results of the study by Shang et al. (1999) suggest that the original measurement

system provided reliable measurements of the complex permittivity of undisturbed

clay samples (obtained from block sarnples). However. in order to reduce the rffects

of sample handling and to further increase the accuracy of the measurements. a

nurnber of modifications were made to the original sample holder and the sample

preparation procedures.

This chapter presrnts the design of the modified sarnple holder and sarnple

preparation procedures. This chapter will investigate the original design criteria for

the sample holder and illustrate how the modifications made to the system improve

the accuracy of the complex permittivity measurements and. in addition. allow for the
measuremenr of sraiic conductivity. Finally, the methodology used in the subsrquent

analysis of soil-water systems will be presented.

Consideration was made durine redesign to use as much of the original sample holder

as possible in order to reduce cost and fabrication tirne. The main sources of error

that can be attributed to the design of a coaxial sample holder are as follows (Bakrr-

Jarvis 1990):

1. Lins losses and connecter mismatc h:

2. Gaps between the specimen and sarnple holder:

3. Specimen location in the holder. and

4. Specimen dimensions.

Item 1 is a systematic error that can be reduced or compensated by measuring the S-

parameters using a high quality ANA and matching coaxial cables. in addition to

following a standard calibration procedure. The calibration procedure reduces or

eliminates any unwanted reflections or losses From either the ANA or the network

cables. Using the calibration procedure described as a "Full two-port calibration?' in

the Hewlett Packard HP8753D user's manual (Hewlett Packard. 1995) the system is

calibrated with the extension cable c o ~ e c t e dto the ANA thereby moving the

calibration and measurement plane to the point of connection of the sarnple holder.
Items 2. 3 and 4 penain ro specific errors associaied with sample prepwdtion m d

handling. Although these errors could be reduced with careful preparation using the

original sample holder, it was felt that modifications could be made to the sample

holder that would prornote more accurate measurements and easier sample

preparation.

Prior to the modifications it was necessary to investigate the design criteria used for

the original sample holder in order to access the areas where improvements could be

made. The design criteria for the original sarnple included the following constraints

(Shang et al. 1999):

1. The annula. cavity between i ~ e and

r outer conductors needed to be large enough

to represent the fabric and structure of undisturbed and/or compacted soi1

sarnples. The 14.2mm spacing between inner and outer conductors can

accommodate a soi1 specimen consisting of sand. silt and clay sized particles.

2. The HP8753D network analyzer operates at an impedance of 50 $2 and therefore.

to minimize any unwanted retlections the sample holder was designed to this

impedance. To achieve the required irnpedance when the sample holder is empty.

the ratio of the outside to inside conductor for the straight section of the coaxial

sample holder is caiculated by (Shaw et al. 1993):

where Z, is rhe impedancr of sampic: hoidcr, b is the dianeter of üuter condustüi. ü is

the diameter of inner conductor. is the relative permittivity of air. as shown in

Figure 3.2 (Section A-A').

3. The cylindncal section of the sample holder of is c o ~ e c t e dto the ANA through

standard coaxial cables of about lOmrn diameter. To prevent unwanted

reflections at the interface of the cables and holder. the c o ~ e c t i o nwas made by

two conical sections with a shallow angle of taper. These sections also have 50

Cl impedance. based on the following equation (Rudge et al. 1983).

Z,, = 60 ln( A
7
tan 8,
( = 50Q

where 19, = 15.5". angle of i ~ e conductor

r and = 6.8 O. angle of outer conductor.

measured Frorn the centrai line. as s h o w in Figure 3.2.

4. The cylindrical section is of sufficient length to reduce the effect of distonion of

the electromagnetic waves at the interfaces of conical and cylindrical sections. It

was reported that a distance of approximately 30rnm between the sample and

conical section would be suscient (Shaw et al. 1993). In addition. it is important

that the undisturbed and cornpacted soi1 samples can be easily installed at the

centre of the cylindncal section with minimal disturbance.

The placement of the sample at the centre of the cylindrical section as well as

minimizing sample disturbance becarne the essential consideration in the

modifications. In earlier investigations (Shang et al. 1999) the sample was squeezed

into the cylindrical section and located in the centre by measurement from both sides.

'This method had a tendency to cause some disturbance of the sarnple along both the

outer and inner edges of the annular soil sample as well as an increased possibility

that the sample was not properly located in the centre of the cylinder.

To reduce the effect of sarnple handling, the original sample holder was cut along the

transverse centreline. The two halves were threaded and a rniddle section was

fabricated so that the entire assembly could be screwed together to form a completed

sample holder that is of the sarne dimensions as the original sample holder (Figure

5.3). This middle section is then used to prepare the compacted sample as outlined in

the sample preparation section. The advantage of using the rnodular design is that the

size and location of the sample in the holder can be strictly controlled and disturbance

of the sample through handling is reduced as a result of the soil sarnple being

compacted in the sarnple ring.

3.1.1 Selection of Sample Length

Dielectric dispersion is associated with ail complex permittivity measurements. The

dipolar polarization of bound water to the soil solids will typically cause dielectric

dispersion to occur in a fiequency range of 200 - 400 MHz. It was s h o w in a

previous irivesûgauon (Shaiiy ei al. 19%) Uiiii tir Jieiectric disp~rsionwill occur ai a

higher frequency in shorter soi1 samples (see Figure 3.4). This observation suggests

that the dielectric relaxation frequency is dependent on the length of the sample in the

rneasurement system. However, from dielectric theory it is known that dielectric

dispersion will occur at a characteristic Frequency that is intnnsic to the soil-water

system and therefore. the observations made by Shang et ai. ( 1999) may be anributed

to a property of the measurement system.

The possible mechanism that leads to the sarnple length dependence of the relaxation

time as observed in this study can be rxplained as follows. For a material that

demonstrates a single relaxation time. the dielectric response can be eapressed as the

complex fonn of the Debye equation:

The above Debye mode1 is analogous to a simple equivalent elrctrical circuit

consisting of two capacitors and a resistor (see Figure 3.5). The real and imaginary

parts of the complex capacitance is given by (Daniel 1967):

where r (s). is the relaxation time of the branch containing C 2 and RI in series. By

cornparing Eqs. 3.3 and 3.4 to Eqs. 3.5 and 3.6 the following relationships are

O bserved:

For an ideal coaxial capacitor. the electrical field lines are represented by radial lines

that run between one conductor and the other. The capacitance per unit length. (Fim).

can be expressed as (Rao 1977):

where b is the diameter of the outer conductor, a is the diameter of the inner conductor.

The resistance value per unit length, (am). is expressed as (Rao 1977'):

where a is the conductivity (Strn).

Refemng back to Eq. 3.7 for the relaxation h i e , r. ifle fall~ivingespicssion cm bc

derived fiom the combination of Eqs. 3.8 and 3.9:

The relaxation time in the above equation is independent of al1 specimen dimensions

(a. b and 0 For the sample under test. This suggests that the relaxation time is an
intrinsic property of the material if the electric field is radial between the inside and

outside conductors.

The situation that aises fiom placing a solid material inside the coaxial linr is

analogous to connecting together two coaxial lines containing differing dielectrics.

i.e. air and soil. For Eq. 3.10 to be valid the electric field lines must remain radial to

the centre conductor and therefore, the boundary condition aises that the clectric

field at the material interface (air to soil or soil to air) must remain tangential to the

dielectric materiai. For an ideal coaxial capacitor. it is reasonable to assume that the

boundary conditions are met and therefore the relaxation tirne will be an intrinsic

material property as implied by in Eq. 3.10. This idealization is not the case in

practical applications. As a result of fringe effects at the soil-air interface the

electrical field becomes a function of the soil sample length, which in turn causes the

relaxation time of the system to become a Function of samplr length. as expressed in

Shang et al. (1999).

The dielectric relaxation time is inversely proportional to the frequency at which

dielectric dispersion occurs, a higher relaxation time represents a lower fiequency at

which dispersion will occur:

where t is the relaxation time and o,is the relaxation frequency.

This is of particular importance in the design of the sample holder. For accurate

rneasurement of the complex permittivity it is important that dispersion occurs at the

highest possible frequency thereby ensuring a sufficient frequency range ovrr which

to record reliable measurements.

To study the effect of sample length on the dieiectnc dispersion a number of complex

permittivity measurements were made to undisturbed soil specimens of various

lengths using the original sample holder. The sarnples were trirnrned from the same

soil block to reduced variations in the soi1 fabric. Figure 3.6 presents the dispersion

frequencies versus the specimen lengths. showing that dispersion occurs at higher

tiequencies in shorter soil specimens (Shang et al. 1999). Based on these results it

was found that a sample length of 35mm would provide a reliable range of

frequencies in which to determine a value for the complex penninivity and loss factor

and still adequately represent the soil structure and grain size distribution of the
sz*~?p!etested. The s~?iplering wss rnachined to a total l e n o of 3 5 m and ai1

compacted sarnples were trimmed following compaction to this length.

3.1.2 Measurement of Soi1 Conductivity

3. I .2.1 Static Conductivig of the Suil Samplr

As discussed in Chapter 2. the measurement of the static conductivity is important in

evaluating the contribution of each of the two components comprising the total loss

làctor.

The static conductivity (dc conductivity) of the soil media is not only a function of

the soil and pore fluid characteristics but is also a function of the type of soil

minerals. temperature. density and the concentration of ionic species within the soil

pore-water. In order to isolate the rffect of dc conductivity in the relative loss factor

of a soil. it is necessary to measure the static conductivity of the soil sample under the

same conditions that the dielectric measurement was made. Changes in the soil

sample's bulk density. moisture content and temperature will alter the conductivity

measured and therefore a procedure was developed to make conductivity

measurements using the same soi1 sarnple used for the complex pennittivity

measurements.
3.1.2.2 Developrnent of a Static Conductivity Measurement System

Ushg an AC voltage source, a potential difference is imposed between the inside and

outside conductors of the sarnple cell. The current and voltage is then measured

across the inside and outside of the annula soi1 sample as illustrated in Figure 3.7.

The applied AC voltage was set a frequency of 97-Hertz (ASTM G57-95a). Research

has shown that higher frequencies and DC equipment introduces addition electrical

circuit elements and a polarkation resistance resulting in inaccurate data (Chalker

1996).

When a uniform charge is placed across the sample ce11 the electric field c m be

represented as a charged cylinder of radius r. The magnitude of the electric field as a

Function of the radius is represented as (Tipler 199 1 ):

where Er is the electnc field strength at a radial distance r. and h is the charge density

per unit length (Clm). The voltage potential between two points c m thrn be

calculated as:
Solving for in Eq. 3.12, we obtain an expression for the charge density in tcrms of

the applied voltage and the geometry of the sarnple:

The current density, j, (~m'),is a function of the material conductivity and electrical

field strength as expressed in a form of Ohm's law as follows:

the cunent density can dso be rxpressed as:

where i is the current (A). By equating Eqs. 3.1 1. 3.14 and 3.15 the following

expression is O btained:

Isolating the material conductivity, o. and substituting in the expression for the

charge density (Eq. 3.13) the conductivity of material is expressed as:

where o is the conductivity (Sim),i is the current (A), V is the voltage (V), b (mj is

the radius of outer conductor. a (m) is the radius of imer conductor and 1 (m)is the

length of the soil sample in contact with the conductors. Eq. 3.18 is used to calculate

the static conductivity of a material as a function of the samples geometry and the

measured voltage and current.

3.1.2.3 Verifcation Testing of Soi! Conductivity Measurement

Once modifications were made to the sample ce11 to permit the application and

measurement of voltage and current between the outer and imer conductors a

cornparison study was undertaken in order to lien& that the conductivity value

obtained using the modified ce11 was in agreement with the value obtain using the

standard ASTM method at a given soil moisture content and bulk density. The

verification procedure involved obtaining two sets of resistivity measurements: one

using the modified sample holder and the second using the standard ASTM procedure

(ASTM (357-95a).

The ASTM procedure G57-95a utilizes the Werner four-clectrode method. which

requires that four metal electrodes be placed with qua1 separation in a srraight line in

the surface of a soil sample. A voltage is applied between the outer electrodes

inducing an electric curent to flow. and the voltage drop between the inner electrodes

is measured [ASTM G57-95a]. The measured current flow and voltage drop are used

to caiculate the soil's conductivity.

The results of the compmti\.e study are presented in Figure 1.8. The plotted data for

both the sample ce11 data and the soil box data (ASTM method) follow a similar

linear trend. The small fluctuations in the measured conductivity values between the

two methods at a given moisture content may be attributed to variations in the soil

density between the two types of tests. The linear regression equations for the soi!

box data and the sarnple data are as follows:

Soil Box Data (ASTM method)

0 = 0 . 5 4 ~ ~ + 8 . 7 1 ~ 1 0+p-0.163
+'
with an R' value of 0.95

Sample Ceil Method

0 = 0 . 5 8 - w + 6 . 7 6 x [O-' .p-0.132
with an R' value of 0.94

where o is the dc conductivity (Slm). w is the water content (%) and p is the density

(blg/rnJ).The similarity between the IWO regression equations suggrsts that the

conductivity measurements made using the modified sarnple ce11 are comparable with

the standard measwement pmcedures as outlined by the ASTM. Conductivity

rnrasurements will be made imrnediately prior to al1 complex permittivity

measurements thereby reducing variation in the measured conductivity value with the

actual conductivity value that contributes to the total loss factor.

3.1.3 Compaction of Soil Sample

As discussed in the literature review (see Chapter 2) variations in the soil bulk density

will cause a change in the measured soil complex permittivity. In order to investigate
culle c ~ î t SOf uivac ..-An+:--n
+LA-- raiiuriviia piib;Jc
i..rrrn.nci ~ û ~ i t i =~f
! x i 1 compaction is required to

produce controlled bu& densities. In addition, many of the errors associated with

sample handling and the insertion of the centre conductor into the soil sample c m be

reduced by utilizing a compaction system that incorporates the measurement sample

ce11 in the compaction procedure. The compaction system designed specifically for

this investigation is detailed in the following section.

Controlled compaction of the soil sample is achieved using a specifically designed

compaction apparatus as show in Figure 3.9. The compaction apparatus consists of a

top and bottom plate held together by connecting bolts. The bottom plate has an inset

ring on which the base of the outer conductor of the sample holder is located. In the

centre of the inset ring is another ring and threaded rod ont0 which the centre

conductor is secured. The bottom plate ensures that the centre conductor is located

precisely in the centre of the outside conductor and that it is held in place during

compaction. The top plate has been machined with a circular opening and inset ring

the same size as the inside diameter of the outer conductor (5Omm.) and is used to

hold the outside conductor in place during compaction.

Compactive energy is provided through the use of a standard proctor drop hammer

(24.3- load at a faIl height of 0.305m)and translated to the soil by an annular ram

that has the same cross-sectional dimensions as the sample holder. An extension

added to the inside conductor is used as a guide for the ram (Figure 3.9). The base of
The samples are compacted in two layers ensuring that the final layer does not have

more than about jrnm of excess soil above the top edge of the sarnple cell. Following

compaction the excess soil is shaved off, using the top edge of the outer conductor as

a guide. so that the sample length is precisely 35rnm. By varying either the moisture

content or the compactive energy. specific bulk densities can be achieved.

3.2 SAMPLEPREPARA PROCEDURES

TION AND TESTMG

The following section will discuss the sample preparation techniques used throughout

the investigation as well as the dielectric testing procedures followed for the

measurements. A clayey till From the Halton Ontario region was used for ail

cornpacted sarnples tested in this investigation. Soi1 index tests for the Halton till are

presented in Appendix B.

3.2.1 Sample Preparation

Al1 compacted samples were prepared in a soils laboratory with a nominal air

temperature of 23 "C to avoid temperature affects on complex permittivity.

The following procedure was used in the preparation of al1 compacted soil sarnples.

1. Place a batch of Halton till to oven dry (1 05 O C ) for 24 hours;

2. Pulverize the dried sarnple to a size that passes a number 4 sieve (4.75mm)
3. Combiriç a iuiown weight of soi1 with a sprcific weight of either de-ionized water

or a solution of NaCl and water to achieve a desired gravimetric moisnire content

and salinity;

4. Mix soil and water solution in a closed container until the sample reaches a

uniform colour and consistency. Allow the sample to equilibrate for 24 hrs;

5. Weigh the empty sample ce11 and record its mas;

6. Compact a volume of soil in the sample ce11 using the compaction method

described above in Section 3.1.3. Variations in the bulk density is achieved by

varying the moisture content of the sarnple and in a few cases by varying the

number blows per layer that was delivered by the compaction hammer:

7. Weigh the sample ce11 and compacted soil sample and record its mass.

3.2.2 Testing Procedures

Once the soil sample has been prepared as described in the above section. the

following procedures were followed io complrte the dielectric measurements.

Measwe the static conductivity of the soil sample as outlined in section 3.1.2.1 :

Calibrate the HP8753D ANA in accordance to the rnethod described in the user's

manual (Hewlett Packard 1995) and as outlined in Appendix C:

Comect the conical section and inner conductor to the prepared sample ce11 (see

Figure 3.10);

t sample holder to the ANA using the low loss coaxial cables used in
C o ~ e c the

the calibration procedure;

5. Measure the S-parameters over the fiequency range cf Q.3 MHz. Tu 1300 MHz.

Discomect the sample holder fiom the ANA to prevent the effect of microwave

heating;

6. Transfer the S-parameters data in ASCII format to a personal computer (PC) for

data analysis as descnbed in a subsequent section;

7. Extrude the annula cylinder of soil from the sample cell, split the sarnple;

8. Complete a water content determination as outline by ASTM procedure ASTM D

2216-90 (ASTM Standards vol. 4.08)

The data analysis of the S-parameters is complrted in the sarne manner as outlined in

Shang et al. (1999) using the Nicolson and Ross solution (Nicolson and Ross 1970).

Appendix A presents the Nicolson and Ross equations and a sarnple cdculation. Al1

calculations of the complex permittivity were done using an Excel 97 spreadsheet.

The data obtained following the processing of the S-parameters are then analyzed and

the real and imaginary components of the complex permittivity are used to

characterize a soil water system. The following section will discuss the methodology

used to analyze the soil-water system.

3.3 METHODOLOGY
OF COMPLEX
~ERMI~~/V~NANALYS/S

The measured complex permittivity can be expressed in a similar manner to that

which was previously expressed for the theoretical complex permittivity, namely:
where E, ' is the reai part of the measured complex permittivity that represents

polarization (in phase) ,j = 41,and E," is the measured imaginary (out of phase)

part of the rneasured complex permittivity.

The real and imaginary components of the measured complex permittivity contain

several components that reflect various effects as discussed in the following sections.

3.3.1 Electrode Polarization

Electrode polarization is the result of charge accumulation at the electrode and

specimen interface and affects the measured values of the complex permittivity

(Klein and Santamarina 1997).

The measured relative permittivity E',, c m be expressed as the surn of the

polarization of the material and the polarization caused by the electrode:

where E ' ~is the relative permittivity induced by electrode polarization and E ' is
~ the

relative permittivity induced by the material under test.

Similady, the measured loss factor. E", can be expressed as the total relative loss

factor presented in Eq. 2.3 and the losses associated with electrode polarization:
To charactenze a soil-water system with respect to changes in the relative permittivity

and loss factor of a soil it is necessary to subtract the electrode polxization effect

from the relative permittivity and both the electrode polarization loss and dc

conductivity effects from the relative loss factor. The value of the relative

permittivity and loss factor for the material would then be expressed as:

The values cornputed as E ' and

~ E ' represent
~ the real and imaginary responses of the

complex permittivity of the soil in the sample holder. The methodology to measure

rach of the above parameters is discussed in the following sections.

3.3.2 Measurement of s ' ~

The effect of electrode polarization on the real permittivity measurements is a

function of the fiequency at which the dielectric measurements are made. Klein and

Santamarina (1997) showed that at low frequencies (100 Hz to 10 MHz.) electrode

polarization affects the measured value of the real permittivity by increasing the

measured value of the reai permittivity with decreasing fiequency. For measwments

made at frequencies greater than 100 MHz the effect of electrode polarization on the

real relative permittivity is considered negligible. For the purposes of this

investigation, al1 real relative permittivity measurements w
i!! he made a frpquency nf

200 MHz. or greater to reduce the effects of electrode polarization:

E, = E, (at f 2 200 MHz.)

3.3.3 Measurement of sd"

The measurement of involves the extraction of the components attributable to

both electrode polarization and dc conductivity as expressed in Eq. 3.25.

R3.R 1 Extraction of Soi1 DC Conductivi@

The electrical conductivity of the media, o (Slrn), may be the result of both surface

conduction. due to electrical charges on the surface of the solids. and ionic

conductance, due to dissolved electrolytes in the water. For dielectric measurements

involving clay-water-electrolyte systems. the double layer surrounding clay particles

makes the surface conductivity a significant component to the total dielectric loss.

The measurement of the static conductivity is discussed previously in Section 3.1.2

and its contribution to the relative loss factor is expressed as:

The value of smd,is subtracted from the rneasured value of the relative loss factor and

is plotted as a function of fiequency in Figure 3.11.

3.3.3.2 Eximc!ion cf

The method by which the value of E'; is estimated is developed fiom dielectric

theory. #en the motion of molecules and ions can no longer change fast enough to

reach equilibrium with an extemal altemating electric field, the pcrmittivity (E;) will

start to decrease with increasing tiequency and this is associated with an increase in the

loss factor (EJ as show in Figure 2.3 (see Section 2.3). This suggests that theoretically

the value of E''~ is approximately zero before the onset of dielectric dispersion.

Accordingly, the value of E'; may be determined by inspection of Figure 3.1 1. The

dielectric loss factor value at Frequencies lower than that at which dielectric

dispersion occurs is representative of the value of E", as indicated on Figure 3.1 1.

The solid thick line on Figure 3.1 1 represents the value of E'; and was calculated by

subtracting the value of E", and the value of the loss due to soil conductivity from the

measured value of the relative loss factor.

3.4 CHARACTEMTION OF A SOIL-WATER SYSTEM

The results of a typical dielectric measurernent plotted as a function of fiequency are

presented in Figure 3.12. Dielectric characteristics such as the E', and E', (the low

and high fiequency permittivities) and the peak loss value, E", are indicated on the

plot. These parameters are descnbed in Chapter 2 of this thesis and form the b a i s by

which a soil- water system is characterized using the dielectric properties presented in
this study. In addition, the complex permittivity 3 specific frequency may also be

used as a characteristic of the matenal.

The Cole-Cole plot presented in Chapter 2 is a cornmon and convenient method by

which to evaluate the dielectric properties of a material. By plotting the measured

data on the complex plane the resulting plot is characteristic of a semi-circle with its

centre on the real (E?) axis and intercepts at and E', on this axis (Cole and Cole

1941). Although these characteristics are intrinsic to a material and could provide

some basis by which to make a cornparison between soil samples. they were not

selected to be used in this study. The two intercepts. E', and E',, represent the value

of the real relative permittivity at a Frequency of zero and infinity respectively. In a

practical sense. these values are theoretical in nature as the rneasurement system. and

more specifically the ANA is not capable of accurate rneasurements at these

frequencies. The fiequency range at which this thesis is focussed upon is from 200

MHz. to 500 MHz.,which represents the range in which a soil-water system will

undergo dielectric dispersion. The cornplex permittivity therefore will be measured at

specific frequencies within this range and will be represented as a matenal constant at

that given frequency. Trends between the complex permittivity of a soil sample and

variation in the soil properties of the sample will be investigated. By selecting a

number of frequencies at which to evaiuate the complex permittivity, it is possible to

investigate the sensitivity of complex permittivity to variations in a soil property (for

example. is E ' ~more sensitive to variations in bulk density at 200 MHz. than at 300

MHz).
To study the effect of changes in soil properties on the components of complex

permittivity the dielectric response of a number of sarnples of varying soil properties

are measured and their results compared. The results of the comparisons and

discussion are presented in chapter 4.

The design of a system for the measurement of the cornplex permittivity of

compacted soi1 has been presented. The rneasurement system used for this thesis is

based on the measurement system developed and tested in a previous investigation as

described by Shang et al. (1999). The system consists of an Automatic Network

Analyzer (ANA). a sarnple holder. a set of coaxial cables and a PC for data

processing. Modifications were made to the original sarnple holder in order to reduce

the effects of sample handling and to facilitate the rneasurement of the static dc

conductivity of the soil in the testing cell. These modifications include designing a

unique sample ce11 that is used as a compaction mold for the soil sarnple which, is

then connected to the ANA via the two hdves of a coaxial sample holder. The use of

a moduiar design allows for the size and location of the sample in the holder to be

suictly controlled and disturbance of the sample through handling reduced as a result

of the soil sample being compacted in the sample ring.

A procedure was developed for measuring the static dc conductivity of the soil

sample after it has been compacted in the sample cell. This procedure allows one to
measure a soil sample's dc conductivity under the same soi1 conditions at which the

complex permittivity measurements will be made. A cornparison was done between

the new procedure and the standard ASTM method G57-95A and the new procedure

was found to produce comparable conductivity values under similar soil conditions.

The sample preparation and dielectric testing procedures described in section 3 .Z

provides a methodology that will be used in obtaining al1 complex permittivity

measurements presented in this thesis.

Section 3.3 presented the analysis procedure that will be utilized for al1 complex

permittivity measurements. Electrode polarization was discussed and the method for

its extraction fiom the complex permittivity measurements was presented. A

procedure was outlined for the analysis of the real and imaginary components of the

complex permittivity.

Finally. a discussion was presented regarding the characterization of a soil-water

system using the complex permittivity values obtained through the measurement

system. To study the effect of changes in soil properties on the components of

complex permittivity the complex permittivity response of a number of samples of

varying soil properties will be measured and their results compared in Chapter 4.
 Log Magnitude HP 87530 ANA
Reflection / Transmission
and Phase Angle
1

Calculation of Cornplex
Permittivity
50Q Coaxial Cable

Sample Holder

Figure 3.1 : Original rneasurement system (Shang et al. 1 999)

 Original Sample Holder

>~iddle Section

Figure 3.3: Original sample holder with cylindncal section split

 x Sombra clay
Orleans clay
-Data Trend Line

Figure 3.6: Dielectric dispersion frequency vs. sample lengtli

 AC Vohi~gcSourcc
(4 Volts. 97 Hz.1

Figure 3.7: Schematic of soi1 conductivity measurement system

Figure 3.10: Assembly of Smple Holder
 69

CHAPTER 4

Complex Permittivity of Compacted Halton Till

The characterization of a soil-water system using the components of complex

permittivity involves cornparhg one of the components of the complex permittivity to

one or more soil properties, such as moisture content, bulk density, or mixing fluid

salinity. By observing how a change in one of the soi1 properties will cause a change

in the measured value of the component of the complex equations can be developed

to model the response. As the number of independent variables (soil properties)

increases. the number of equations needed to model its response will also increase.

Perdok et al. (1996) developed an equation that relates the real relative permittivity.

E ~ ' .to the gravimetric water content and the bulk density of a soil. In this situation.

one of the variables would have to be measured independently and substituted into

the model in order to measure the other independent variable. By developing

additionai equations that relate to the measured complex perrnittivity. the number of

independent variables that can be deduced will increase.

In this chapter, the response of both the real and imaginary components of the

complex permittivity to variation in sarnple soi1 properties will be investigated for

compacted Halton till. Observations will be made regarding the complex permittivity

response to variations in the soil water content. soil relative bulk density and the

salinity of the water used in the compaction of the soil. A brief discussion of each of
these variables is presented in the next section. The results of the smdy are presented

as a group of multiple linear regression equations that relate specific values of the

complex permittivity of Halton till as a function of soil moisture content, bulk density

and mixing fluid salinity (s). A discussion of those equations and their significance

are presented based on the results of the investigation.

4.1.1 Soi1 Moisture Content

As presented in Chapter 2. the soil moisture content is a fundamental physical

property in the investigation of geomaterials. The accurate measurernent of soil

moisnire is important for soil related investigations, such as the study of plant growth.

water infiltration and run-off. as well as classical applications in soil mechanics and

toundation engineering.

Within the field of geotechnical engineering, soil moisture content is commonly

expressed in gravimetric units as the ratio of the mass of water to the mass of solids in

the soil, namely:

where w is the gravimetric m o i m e content. LM, is the mass of water and iCI, is the

mass of solids in the soil. However for the study of the elecuical and dielectric

behaviour of soils, it is more convenient to express the soil moisture content in

volurnrlriç units, because the permittivity of a porous material is related to the

volume of solids, air, and water per unit volume. The volumetric moisture content is

the ratio of the volume of water to the volume of the total soi1 mass and is calculated

as:

where 8 is the voiumetric moisture content, V , is the volume of water and VT is the

total volume.

4.1.2 Relative Bulk Density

The bulk density of a soi1 has been identified throughout the literature as one of the

soil properties that will affect the complex permittivity (Perdok et al. 1996.

Kraszewski 1997). Most moisture senson utilizing microwave technology to

measure soil moisture content rely on a cdibration procedure to measure the soil's

bulk density and then assume that the bulk density of the soi1 will remain constant

throughout the measurement. In addition, these sensors use only the real components

of the cornplex permittivity (the dielectric constant) to calculate the soil moisture

content and therefore only use one of the components of the complex permittivity.

For the rnajority of applications it is reasonable to assume that the soil's bulk density

does remain constant throughout the measurement period. However, for the situation

of long term in-situ monitoring this assumption may no longer be vaiid. Physical or

environmental conditions at the monitoring site may change with time, thereby
altering the bulk density of the mil amund t'iS sensm. By dvelopifig relationsliips

that include bulk density and additionai components of the complex permittivity, it

may be possible to accommodate changes in the bulk density without requiring

additional calibrations.

The bulk density of a soil is calculated as a ratio of the total mass of a soil to the total

volume that contained that rnass, as expressed by:

where p is the bulk density, MT is the total mass of the soil and VT is the totd volume

of the soil.

The bulk density can be expressed as the dimensionless relative bulk density. p,. by

dividing the bulk density of the soil by the density of water. pw( 0 . 9 9 8 ~ ~ / at
r n20°C
~

4 l~~/rn'):

The relative bulk density. p, will be used to represent the bulk density of a soil

sarnple throughout this investigation.

4.1.3 Mixing Fluid Salinity

Mixing fluid salinity refes to the fluid used to hydrate the oven-dried soil (described

in Section 3.2.1) and does not represent the pore fluid saiinity of the soi1 samples.
The chad H a h n til1 soil saniples contaiii sdts (ser Appendix B), whiçh will dissolve

when water is added prior to compaction. The investigation into the effect of mixing

fluid salinity on the complex permittivity is focused on the trends of the measured

data and thus the difference between the pore fluid salinity and the mixing fluid will

not effect those trends.

The salinity of the mixing fluid will affect the Static dc conductivity of a soil sarnple.

which is one of the two factors contnbuting to the total loss factor in the fiequency

range investigated in this thesis. The mixing fluid was prepared by adding a mass of

dry NaCl crystds to a volume of deionized water (MegaPure water). The salinity of

the solution was then measured with a salinity meter to confirm its value.

4.2.1 Soi1 Properties of the Measured Samples

Using the procedures outlined in Chapter 3 for the preparation of the soil sarnples and

the measurement of the complex permittivity, a total of 40 complex permittivity

rneasurements were made. The soi1 samples were prepared such that the soil moisture

content or the soi1 bulk density or the mixing fluid salinity varied fiom one sample to

the next. The physical soil properties for each of the sarnples are summarized in Table

4.1.

The soil wmples were prepared to the desired gravimetric moisture content by
v~,rykg the mount cf mixing fluid added to ?!e dry seil. ne gmixetric rnoisture

content of the soil samples. as defined by Eq. 4.1. ranged between a minimum value

of 6% to a maximum of 22%. The optimum rnoisture content for Halton till is

estimated to be approximately 14%.

rhe bulk density for the soil samples was measured to be between 1.98 ~ ~ / r and
n'

2.3 1 ~ g / r n corresponding
~, to a range of dry density values of 1.6 ~ g / r n ' to 2.1

~ ~ / r n ' . The optimum dry density for the Halton till was estimated to be

approximately 1.8 ~ ~ l r (see

n ' Appendix B).

The mixing fluid salinity ranged between Og/L for the MegaPure water to a salinity of

15g/L (measured as a concentration of NaCl). This range was selected to Vary

between pure water to a salinity that rnay correspond to that of the leachate From a

municipal solid waste landfill.

4.2.2 Cornplex Permittivity Measurement Results

The complex permittivity of the Halton till was measured over the frequency range of

0.3 MHz to 1300 MHz. This Frequency range was selected to ensure that a complete

dielectric dispersion profile was obtained. The data traces for both the real and

imaginary components of the complex permittivity are ploned on a single figure for

each sample tested (see Appendix D). Figure 4.1 presents a typical plot of the data

trace obtained from a complex permittivity measurement.

n i e heavy solid line on each of the plots (Fig. 4.1 and Appendix D) represents the

trace of the reai component of the complex permittivity. The hi& values in the low

-
frequency range (fk 100 200 MHz) are attributed to the polarization of the electrical

double layer (Shang et al. 1999). The onset of dielecûic dispersion generally

occurred within the frequency range of 700 MHz to 400 MHz and is indicated by a

decrease in the real relative permittivity with increasing frequency. Dielectric

dispersion occurs when the motion of molecules and ions can no longer change fast

enough to reach equilibrium with an external altemating electric field. As the

Frequency continues to increase. the real relative permittivity will decrertse until it

reaches a low steady state value.

Longitudinal resonance occurs in sorne of the sarnples and is characterized as a

sudden jump in the real permittivity accompanied by a sudden drop in the irnaginary

permittivity. The Nicolson-Ross solution. which is used to calculate the complex

permittivity from the scattenng parameters, assumes a single mode of propagation in

the sarnple. With the increase of fiequency, higher modes will be generated. resulting

in resonance (,Shanget al. 1999). The scatter or "noise" observed on the data plots is

likely a result of circumferential resonance (Shang et al. 1999).

The light solid line on each of the plots (Fig. 4.1 and Appendix D) represents the trace

of the irnaginary component of the complex permittivity. Dielectric dispersion is

observed in the irnaginary component as an increase in the relative loss factor with
increasing fiequency mil it reachcs a peak value, after which it begins îo dernase

until it reaches a low steady state value.

As discussed in Chapter 3 , this thesis focuses on the fiequency range from 200 MHz

to 500 MHz. since this represents the range in which a soil-water system will undergo

dielectric dispersion. The cornpler permittivity values of the sample are reported at

four specific frequencies namely, 200 M H z 225 MHz. 250 MHz and 275 MHz. In

order to reduce the effect of the noise as a result of circumferential resonance in the

sample holder. the magnitude of the complex permittivity at these frequencies is

calculated as the average value of the complex permittivity measured within a

fiequency range of t 6 MHz. These Frequencies lie within the range in which

dielectric dispersion was observed to begin for the soil samples tested and are used to

develop the relationships that will be presented in a subsequent section.

The imaginary component of the complex permittivity is reported as the loss factor

with the dc conductivity component removed. The effect of electrode polarization on

the measurement of the complex permittivity is treated as a systematic error of the

measurement system and therefore not considered in this thesis. Further research is

required in order to understand how the electrode polarization is afl'ected by soil type

of pore water chemistry. The results of the complex permittivity measurements are

presented in Table 4.2 and Table 4.3.

This section will consider the effects of moisture content, relative bulk density and

mixing fluid salinity on the magnitude of the real relative permittivity (E,'), the

relative loss factor (CG') and the complex perminivity at the relaxation frequency

E,"). Each variable was investigated individually by ensuring that the other two

variables were held constant. For example, in order to investigate the effect of

moisture content on the reai relative permittivity. the relative bulk density and the

rnixing tluid salinity was held at a constant value.

4.3.1 Volumetric Moisture Content

To investigate the effect of changes in the volumetric moisture content on the

complex permittivity, a number of samples were prepared at a constant relative bulk

density and salinity and the complex permittivity of the samples was measured. The

results of the measurements are presented in Figure 4.2 (at a frequency of ZOOMHz)

and Figure 4.3 (at the relaxation frequency). The linear regression equations and the

R' value are indicated on the figures.

Figures 4.2 and 4.3 show an increasing trend in the measured values of the E,', E," and

ç'. E," with an increase in the volumetric moisture content of the sarnple. In

addition, the measured values of E,' (Fig. 4.2 (a)) and the complex permittivity values

at the relaxation tirne (Fig. 4.3) for the samples prepared at a relative bulk density of

2.2 are slightly higher than those prepared at a lower relative bulk density of 2.1.
This indicates that E,' and %' rnay be sensitive to changes in the buik density. in the

case of the relative loss factor, E;' as s h o w in Fig. 42(b), both sets of data exhibited

a very similar trend in the magnitude and slope, with no distinguishable differences

caused by a variation in the bulk density.

To quanti@ the sensitivity of a complex permittivity component to a change in the

independent variable (moisture content. density, or salinity) the magnitude of the

dope of the single variable trend line is investigated. In Fig. 4.2. the magnitude of the

slope of the trend line For E,' versus volumetric moisture content is in the range of 60

to 70. where as the dope of the trend line for E'; versus volumetric moisture content

is approximately 28. In Fig. 4.3 the magnitude of the dope for E,' versus volurnetric

moisture content is approximate 36 and for E," it is in the range of 65 to 80. The

slope of the trend lines for the E; (at p z 0 0 MHz) and the complex permittivity at

relaxation frequency (E,'. E,") suggests that. for the samples tested. these components

are more sensitive to changes in the volumetric moisture content than is the relative

Ioss factor. The wide use of commercial permittivity probes, which detect the relative

permittivity of a material, for the evaluation of soi1 moisture content would support

this observation.

The effect of volumetnc moisture content on the relative permittivity of a materid is

well documented in the 1iterahu-e and the data presented in Fig. 4.2 (a) is

representative of a typicd response. The relative permittivity, E;, is a quantity used

to evaluate the charge storing capacity of a matenal (polarkation). The value of the
relativ~permittivi~wiii drpenci on Lht: abiliiy of ht: material tu react and orient itself

in the imposed electromagnetic field. The greater the reaction, the greater the energy

stored and therefore, the higher the relative permittivity ( F l i ~and Trojan 1990).

Water is contained in a material in two fonns, bound and free. Bound water is the

most cornmon and refers to water that has been chemically combined with other

molecules or absorbed to the surface of the material, while free water remains

unattached. Because water molecules attached to another material (such as a soi1

particle) require more energy to rotate itself in the electric field soil-water system

exhibits a lower capacity to store energy and thus a lower value of real relative

permittivity. As the moisture content increases and the space for additional water

molecules to bind to soi1 particles decreases, the amount of energy required to rotate

in the imposed electric field will also decrease. This will cause an increase in the

ability for the material to store energy.

The response of the relative loss factor to an increase in the volurnetric moisture

content is similar to that discussed previously with respect to E,'. The relative loss

factor is the out of phase portion of the complex permittivity response and represents

the dissipation of the energy from the applied electric field. With the increase in the

volurnetric moisture content, there is an accompanied increase in the loss factor due

to the higher conductivity of the soil-water system. The effect of the volumetric

moisture content dominates the response of the relative loss factor and variations in

the bulk density do not appear to be easily observed. The effect of bulk density will

be discussed in the next section.

The response of the complex pennittivity to increases in the volumetnc moisture

content is not linear through the entire range of possible moisture content. Because

water molecules attached to those of dry material exhibit much lower rotational

mobility than molecules of liquid water. the dielectric properties of most materials

differ significantly from what would be expected from the fractionai contribution of

liquid water (Kraszewski 1997). A characteristic curve for the complex permittivity

versus moisture content would consist of an upward sloping curve with two distinct

dopes. one at lower rnoisture content and the second at higher moisture contents (see

Figure 4.4). The lower moisture contents correspond to the region of the curve where

the slope is very shallow. as a result of the water molecules being very tightly bound

to the soi1 particles. "As the moisture content increasrs. the slope of the characteristic

curve increases due to the presence of less tightly bound water molecules and

eventually free water molecules. The change of dope occurs at a certain moisture

content which is characteristic for a given matenal. w,, and most oRen may be related

to an equilibrium moisture content reached at ambient conditions'' (Kraszewski

1997). The moisture content range used in this investigation lies in the upper

moisture content range and therefore the complex permittivity response to moisture

content can be considered linear.

4.3.2 Relative Bulk Density

The effect of changes in the relative bulk density of a soi1 sample on the complex

pemiittivity were hvestigated by comparing the response of six soi1 samples of

varying reiative bulk densities. Each of the six soi1 sarnples was prepared using

MegaPure water at a gravimebic moisture content of 1 1.8 % k 0.5%. The results of

these measurements are presented in Figure 4.5 and Figure 4.6. The linear regression

equations and the R~ value are indicated on the figures.

Figures 1.5 and Fig. 4.6 show an increasing trend in the measured value of the E,'. E,"

and ~ ~ ' ( 2 0MHz).

0 E," (200 MHz) with an increase in the relative bulk density of the

sample. The influence of bulk density on the complex permittivity is due io the

dependence of a dielectric material upon the arnount of mass interacting with the

electromagnetic field. Figure 4.5 shows the response of the complex permittivity at a

Frequency of 200 MHz to increases in the relative bulk density of the sarnples tested.

The magnitude of the slope of E,' and E," is 17.9 and 5.2 respectively. As with the

volumevic moisture content, the slope of the trend lines for the data suggests that E,'

is more sensitivity to variations in the relative bulk density than is the relative loss

frictor.

The data ploaed in Fig. 4.5 (b) suggest that under a constant moisture condition, an

increase in the relative bulk density of a sarnple will be reflected as an increase in the

measured value of the relative loss factor. However, as discussed in the analysis of

the volumetric moisture content, the sensitivity of the relative loss factor to variations

in the relative bulk density is overshadowed by the volumetric moisture content. The

slope of E;' versus volumetric moisture content is approximately 28 whereas the slope

of E'; versus relative bulk density is approximately 5. This would suggest that the
relative ioss factor is ineffective at differentiating changes in bulk density unless

another parameter or method is used to hold the moisture content constant.

Consistent with observations made concerning the volumetric rnoisture content the

complex permittivity at the relaxation frequency plotted in Figure 4.6 exhibits a

similar trend to that shown by the real relativity permittivity.

4.3.3 Mixing Fluid Salinity

Samples were prepared with five different solutions of NaCl and MegaPure water; 0.5

g/L, 1 .O g/L. 5.0 g/L. 10.0 g/L and 15.0 g/L. and then prepared at a constant moisture

content and relative bulk density. The results of the measurements are presented in

Figure 4.7 and Figure 4.8. The linear regression equations and the R~ value are

indicated on the figures.

The effect of mixing fluid salinity on the real relative permittivity is illustrated in

Figure 4.7 (a). The slope of the trend line for the data is less than 0.08. which

suggests that the real relative permittivity is insensitive to changes in the mixing fluid

salinity. The slight decrease in the magnitude of E,' with increase in mixing tluid

salinity may be explained in the context of a simple three phased mixing model.

consisting of soil. water and air. As discussed in Chapter 2, a mixing model can be

used to explain the response of the complex permittivity of a soi1 system by equating

the volume fraction of each constituent with their respective dielectric constant. For

the samples tested, the volume fiaction of the air. water and soil components is held
cons*^.?, cf tL.r ;vater that is chmging ~ 5 t hsalkij.
and it is the dielectnc cor,s+~~t

As the salinity increases, the dielectric constant of the water will decrease and as a

result, the dielectric constant of the three phased system will also decrease.

Figure 4.7 (b) presents the effect on the relative loss factor by an increase in the

salinity of the mixing tluid. It is observed that. for the samples tested. as the salinity

of the mixing fluid increases the magnitude of the relative loss factor also increases.

The increase in the measured value of the relative loss factor that occurs with an

increase in the salinity of the mixing fluid may be the result of the addition of free

ions to the water. The relative loss factor presented in Fig 4.7 (b) represents the value

of the relative loss factor with the dc conductivity losses removed (see Chapter 3).

The increase in energy loss may be due to the reduced polarizability of the sample at

higher ionic concentrations. The principal loss mechanism. which is not associated to

losses due to dc conductivity at this frequency. is due to the reonentation of the

molecules in the electric field (see Chapter 2). As free ions in the mixing fluid bond

to the polar water molecules it becomes more difficult for the molecules to orient

themselves in the electric field and therefore there is an increase in the arnount of

energy lost. This increase is obsewed as an increase in the relative loss factor. The

data presented in Fig. 4.7 (b) suggests that the relative loss factor is sensitive to the

salinity of the mixing fluid.

The coiqdéx perii&.tivity at the reiaxation iiequency as a funcrion of mixing Ruid

salinity is presented in Figure 4.8. The data presented for both c,', G" venus mixing

fluid salinity shows a trend line which has a slope that is an order of magnitude less

than that of E,', ETversus volurnetric moisture content (Fig. 4.3) and versus relative

bulk density (Fig. 4.6).

The relatively flat trend line of E," may be the result of the conductivity losses

dorninating the response at the relaxation frequency. As the salinity of the mixing

fluid increased. the peak of the relative loss factor occurred at a progressively lower

frequency. This is a result of the onset of dielectnc dispersion occming at a lower

frequency, due to the mechanisms described previously. and thus the loss factor

reached its peak value at a lower frequency. The value of the dc conductivity

component subtracted from the relative loss factor is inversely proportional to the

frequency (Eq. 3.27), therefore as the frequency decreases the magnitude of the

component that is subtracted increases.

Figure 4.9 presents a plot of cT" versus rnixing fluid salinity for one of the data series

(0 = 19.3%. p, = 2.094) piotted in Fig. 4.8. Of the two series ploned on the graph,

one represents the peak loss value, G",with the dc conductivity component removed

and the other represents the same data, but without subtracting the dc conductivity

losses. It is observed fiom Fig. 4.8 that the data series. which represents a peak loss

component that included dc conductivity losses, exhibits a trend line that increases in

magnitude with increasing salinity. This suggests that the losses due to dc
conductivity dominate the relative loss factor in the fiequency range at which the

peak loss occurs. In addition, the data suggests that the value of E.;' with the dc

conductivity losses subtracted, may not be sensitive to variations as a result of

changes in the mixing fluid salinity.

The observations made conceming the complex permittivity at the relaxation and

presented on Figures 4.3. 4.6 and 4.8 suggests that E,' and E," are functions of

volumetric moisture content and bulk density but do not appear to be affected by

changes in the mixing fluid salinity.

The preceding sections have discussed various factors that will affect the complex

pennittivity of a soil sarnple. Volurnetnc moisture content, relative bulk density and

the salinity of the mixing fluid have al1 been s h o w to affect one or more of the

components of the complex permittivity, narnely. the real relative permittivity, E,'. the

relative loss factor. gr". and the cornplex permittivity at relaxation fiequency, G". By

developing an empirical mode1 that encompasses these variables, the measurement of

the complex permittivity of a soil-water system provides the opportunity to

characterize the system. The following section will present one such empirical

mode!. Using the data obtained From complex permittivity measurements and

presented in Table 4.1,4.2 and 4.3 a number of equations will be developed based on

a linear regression of al1 the data. These regression equations are valid for the range

of materiai properties presented in Section 4.2.1 and for the Halton till soil tested.
4.4.1 Results of the Multivariable Linear Regressions

The discussion on the real relative permittivity presented in the preceding section

suggested that E, is sensitive to variations in the volurnetric moisture content and the

relative bulk density. The relative loss factor was also observed to be sensitive to

volurnetric moisture content and bulk density and, in addition, exhibited an increasing

trend line to an increase in mixing fluid salinity. Findly. the complex permittivity at

the relavation fiequency was observed to be independent of changes in the mixing

fluid salinity and was found to be only a function of' the volumetric moisture content

and relative bulk density.

Using the forty measurements presented in Table 4.1 and 4.2 the following linear

regressions were obtained:

At 200 MHz

= 42.894-0+ 7.155 P, - 0.362-s - 7.627

E;(~OOMHZ) (4.5)

with an R' value of 0.83 and 0.78 and a standard error of 1.73 and 1.43 for E,' and E,"

respectively;
with an R' value of 0.81 and 0.83 and a standard error of 1.94and 1.27 for E,' and E,"

respectively;

with an R' value of 0.80 and 0.86 and a standard error of 2.05 and 1.15 for E,' and 8,"

respectively and ;

' value of 0.80 and 0.87 and a standard error of 2.1 8 and 1.1 1 for E,' and E;'
with an R

respective1y.
It was suggested in the Section 1.3 that thc compler permittivity at the relaxation

fiequency was independent of the saiinity and therefore, the linear regression for &*,

included only the volumetric moisture content and the relative bulk density as

independent variables. Again, using the data presented in Table 4.3 the following

regression equation was found:

with an R~ value of 0.82 and 0.95 and a standard error of 0.95 and 1 .O5 for E,' and E,"

respectively.

For al1 of the regression equations presented above. the value of the volumetric

moisture content. 8. is expressed in decimal format. the relative bulk drnsity is

dimensionless and the salinity of the rnixing fluid. S. is expressed as a concentration

of NaCl (g/L).

The difference between the predicted value generated by the above equations and the

measured value for the data point is known as a residual. The residuals should be

scattered randomly about the zero mis, indicating that they have no relationship to the

value of the independent variable. Plots of the residuais for each of the above
quationç are presented in Appendix E and they exhibit no discemible trend relating

them to the independent variable.

n i e regression equations for the real relative permittivity reflect the trends that were

described in Section 4.3. The predicted values generated fiom the four equations are

dominated by the volumetric moisture content and to a lesser degree. by the relative

bulk density. The variable coefficient for the mixing fluid salinity is negative and

small in cornparison to the other two coefficients. This reflects the slight downward

trend in the magnitude of the real relative permittivity descnbed previously.

The volurnetric moisture content and the relative bulk density also dominate the

regression equations for the relative loss factor. However. as discussed in Section

4.3. the relative bulk density appears to have a stronger influence on the magnitude of

the relative loss factor than it does on the real relative permittivity. By examining the

magnitude of the coefficients for the relative bulk density. it is observed that. under a

constant moisture and salinity, an increase in the relative bulk density will cause a

greater increase in the relative loss factor than in the real relative permittivity. The

coeficient for the mixing fluid salinity is positive, which supports the previous

observation that and increase in the mixing fluid salinity will cause an increase in the

magnitude of the relative loss factor.

The regression equations for G* exhibit a strong correlation with the measured data,

particularly as indicated in the high R~ value. The R~ value measures the

proportion of the variation in the data points, which is explainecl by iiic regession

model. A value of R' = 1.O means that the curve passes through every point, while a

value of R' = 0.0 indicates that the regression model does not describe the data any

better than a horizontal line passing through the average of the data points. The

regression equation for the peak loss supports the observation made in Section 4.3.

namely that complex permittivity at the relaxation fiequency can be represented

without the consideration to the salinity of the mixing fluid.

The frequency at which the measurements are made appears to have a slight influence

on the R' value and the standard error. The regression equations generated for the

real relative permittivity had the highest value for R' and the lowest standard error at

a frequency of 200 MHz. In contrat, the relative loss factor had it highest R' value

and lowest standard emor and a hequency of275 MHz. This may be the result of the

mechanisms present at the measurement frequency. With respect to the red relative

permittivity, the accuracy of the model was increased when the measurements were

obtained a lower fiequency, presumably at a Frequency much lower than that at which

dielectric dispersion would occur. The relative loss factor however. was best

measured at a higher frequency, closer to the fiequency at which dielectric dispersion

occurs and coinciding with an increase in the loss mechanisms. This would suggest

that the accuracy of the model wodd be increased if the real relative permittivity

were measured at a different fiequency than the relative loss factor.

The sensitiviy of E,' and gr7'to the volumetric moisture content, relative buik density,

and the mixing fluid salinity, appeared to Vary with the fiequency at which the

quantity was measured. Figure 4.10 plots the sensitivity of the dope coefficients

From the multivariable regression to the fiequency of measurement. A siope of a

higher magnitude indicates that the variable is more sensitive to change than a slope

of a lower magnitude. Consistent with the observations made concerning the

standard error of the regression equations. E,' appears to be more sensitive to changes

in the volumetric moisture content and relative bulk density at a lower frequency than

at a higher frequency. The opposite can be said for E,"; which is more sensitive to

changes in volumetric moisture content and equally sensitive to changes in the

relative bulk density at higher frequencies. Both the E,' and E," showed slightly

greater sensitivity to changes in the mixing fluid salinity at a lower frequency. These

observations may be important in the design of a multivariable contaminant sensor. as

they suggest that varying the fiequency at which the components of the complex

permittivity is measured could control the sensitivity of the sensor.

The application of the regression equations presented in the previous section is

limited to use on samples of Halton till with a moisture content. bulk density and

salinity within the ranges specified in Section 4.2. The application of the information

gained from the investigation however, is not Limited to such a small data set. The

following section will discuss several of the observations made in this chapter, and

how these observations may be applied to other soi1 systems and applications.
The trends identified and discussed in Section 4.3 are used as a basis to characterize a

soil-water system. It is well documented that the moisture content and buik density

of a soil influences the real permittivity. The comrnercially available moisnire

sensors, that utilize microwave technology to rneasure the soil moisture content,

assume that the buik density of the soil is a constant and therefore only relate the real

permittivity to the moisture content. If however, the bulk density of the soil was not a

constant. additional calibration measurements would have to be made to adjust for the

change in bulk density. The observations made conceming the relative loss factor

and the relative peak loss suggest that if these quantities were measured along with

the real relative permittivity. the bulk density of the soil could be treated as an

additional variable. Increasing the number of equations that can be used to

characterize a response also increases the nurnber of independent variables that can be

considered in that response. This observation is particularly applicable to long term,

in-situ monitoring applications. in which doing additional calibration measurement to

account for a change in bulk density could be difficult or impossible. A system.

which used the real relative permittivity and the relative loss factor. would be able to

mode1 both the volumetric moisture content and the relative bulk density

simultaneously .

For the purposes of geoenvironrnental applications such as contaminant detection or

site characterization, it is important to understand the response of a soi1 to changes in

environmental conditions. Current methods of contaminant detection involving

sample collection are expensive and frequently a great deal of effort is expended to
demonstrate that no change in conditions or contaïnation bas occmed. T k r z is a

demonstrated need for the development of in-situ technologies that can be used

reliably and quantitatively to establish either the presence or absence of

contamination or changes in the level of contamination.

In-situ electronic conductivity measurements are commonly used to qualitatively

detect subsurface contamination. Conductivity however, is not only a h c t i o n of the

electricai conductivity of the pore fluid, but is also effected by properties of the soil,

such as moisture content. density, porosity and properties of the soil particle, such as

grain size and shape (Kaya and Fang 1997). An additional method is needed to

quantitative detect contamination which isn't affected by other factors of the soil-

fluid system.

The investigation into the effect of changes in the mixing fluid salinity on the

complex permittivity is a first step in meeting this need. The physical changes in the

soil system, such as moisture content, bulk density and by computation, the porosity.

can be modelled by the measurement of the complex permittivity. The trends

indicated by the investigation into relative loss factor indicate that an increase in the

salinity of mixing tluid can be detected. By using multiple components of the

complex permittivity simultaneously, individual mechanisms in a soil system can be

charactenzed. In addition, this approach will allow one to monitor a soil system on a

time continuous basis. As the soil system changes due to non-contamination related

events, the effects of the changes cm be compensated for in the anaiysis of the
cornplex pzrmittivity measuremtnts by ren-iüving its predictecl effect on thé

measurement. For example, a predicted increase in the bulk density and moisture

content of a soil can be compensated for in the complex permittivity measurements

and therefore any additional changes in the complex permittivity can be attributed to

a change in the soil system, possibly from contamination.

Based on the observations made conceming the complrx permittivity at the relaxation

tiequency. it was suggested that E,' and ';E are funftions of volurnetric moisture

content and bulk density but do not appear to be affected by changes in the mixing

fluid salinity. For agricultural applications such as soil moisture monitoring this may

be significant. As discussed in Chapter 2. it is of interest to be able to monitor the

moisture content and density of a soi1 for Ming and irrigation purposes. It has been

suggested previously that using two components of the complex permittivity

sirnultaneously would allow one to mode1 both parameters without need for

additionai calibrations caused by variations in the soil's bulk density. Presurnably.

the real relative pemittivity and the relative loss factor could be used. as they are

both sensitive to moisture content and bulk density. Assuming that the salinity of the

soi1 remains a constant. this may be effective. However, the application of fertilizers

during the growing season may change the salinity of soil, thereby affecting the

complex permittivity and thus the monitoring. By using the complex permittivity at

the relaxation frequency to mode1 changes in a soils moisture and bullc density,

changes in the salinity of the soil will not affect the monitoring and additional

calibrations wouid not be required.

Though the examination of the mechanisms that affect each component of the

complex pemittivity, the sensitivity of detection systems utilizing microwave

technology rnay be increased. The dispersive nature of a soil fluid system for the

rneasurement of the complex permittivity rnay contribute an additional point of

cornparison by which to characterize a soil. As noted in Section 4.4, measuring the

real relative permittivity and the relative loss factor at different fiequencies may

increase the accuracy of a complex permittivity model. It was suggested that this was

due to the different polarization mechanisms that affect each component at the

different frequencies. Contaminant rnay also affect the complex permittivity

differently at different fiequencies. It was observed that the real relative permittivity

decreased slightly with increasing salinity. due possibly to ions binding with the

water molecules and thereby reducing their ability to orient themselves in the

imposed electrical field. Based on this observation, it rnay be possible to delineate

contaminant based on their interaction with the pore fluid. or in the case of clay soil.

the double layer. by comparing the response at different frequencies.

The investigation on the Halton till presented in this chapter has shown that the use of

the complex permittivity for the characterization of soils rnay be accomplished by

using both of the components of the complex permittivity simultaneously. By

identifjmg the trends that affect each of the variables, multivariable models can be

developed, which in turn rnay be used to monitor changes in the soil-fluid system.
Table 4.1: Summary of Sample Soü Properties

Static dc
Sample # Conductivity
(Wm)

- "
HTMP9
HTMP 1 O
HTMPI I
HTMP I 2
H -T- M-- -
P~~
-
HTMP 14
HTMP 1 5
HTMP I 6-
--. - --
HTMP 1 7
HT-15- 1
~ ~ 1 5 - j -
.'
HT- 15-3
HT-154
HT-15-5
HT-15-6
HT- 15-7
HT-15-8
- - - -
HT-1 5-9
HT- I 5- 1 O
HT-I- I
- HT-1-2
HT-1-3
HT-1-4
HT-1-5
HT- 1-6
- - - -- -- - -
HT-5- 1
- - - -

- --
HT-5-2 -
HT-05- I
HT-05-2
HT-10-1
HT- 1 0-2
HT-10-3
Table 1.2 (a): Summary of Complex Permittivity Memurement Results

Sample # E', Cr gr Cr
HTMP 1 25.0 7.8 24.9 8.7
HTMP2 15.7 7.7 15.4 7.8
HTMP3 21.8 9.2 21.5 9.7
HTMP4 19.2 8.4 18.9 8.7

HTMP IO 15.3 7.2 15.0 7.2

HTMP I 1 15.4 7.7 15.1 7.8
HTMP 12 16.2 8.1 15.8 8.2
HTMP 13 22.0 10.5 71.8 10.9
HTMP 14 22.6 10.3 22.4 10.7
HTMP 15 21.7 IO. 1 2 1.J 10.6
HTMP 16 22 .O 10.0 21.7 10.4
HTMP 17 22.3 10.5 22.0 11.1
HT-15-1 12.4 14.2 10.9 14. I
HT- 15-2 15.3 13.6 13.9 14.0
HT- 15-3 13.6 12.11 13.2 12.19
HT- 15-4 15.0 14.2 13.4 14.5
HT- 15-5 12.9 15.4 î 1.3 15.7
HT- 15-6 13.2 12.8 12.5 12.8
HT- 15-7 13.9 14.3 13.1 14.1

HT-15-9 13.2 15.2 11.7 15.6

HT-15-10 11.1 8.0 10.7 7.9
-
HT- I 1 9.1 6.6 8.8 6.6
HT- 1-2 12.5 8.0 12.2 8.0
HT- 1-3 16.9 11.7 16.5 11.9
HT- 14 17.9 11.4 17.5 1 11.7
HT- 1-5 13.7 7.4 14.4 7.5
FIT- 1-6 11.7 6.1 11.4 6.1
HT-5 - I 13.8 8.9 13.4 8.8
HT-5-2 11.4 6.8 11.1 6.7
HT-OS- 1 15.0 7.7 14.7 7.8
HT-05-2 11.7 5.8 i 11.4 5.7
HT-1O- 1 13.8 10.0 13.3 9.8
HT- 10-2 11.3 7.8 10.9 7.7
HT- 10-3 13.6 10.2 12.9 10.0
Table 1.2 (b): Surnmary of Cornplex Permittivity Measurement Results

Frequency = 250 MHz Frequency = 275 MHz

I I
Sample # Er E", E; gr
HTMP 1 25 .O 9.7 25.1 11.0

HTMPJ 18.6 9.0 18.6 I 9.4

HTMPS --.-
73 7
11.4 --.-
')? ?
12.1
HTMP6 14.9 6.5 14.8 6.8
HTMP7 18.6 9.3 i 18.5 9.6
HTMP8 20.5 1
10.7 20.4 11.1
HTMP9 14.6 7.3 14.6 7.4
HTMP10 14.8 7.2 14.7 7.2
HTMP 1 I 14.8 7.8 14.8 8.0
HTMP 12 15.6 8.2 15.5 8.3
HTMP 13 21.6 11.3 21.4 12.1
HTMP14 22.3 11.3 32.2 12.2
HTMP 15 21.2 11.2 21.0 12.1
HTMP 16 21.4 11.0 3 1.3 11.9
HTMP 17 21.9 11.7 2 1.7 12.6
HT- 15- 1 9.7 13.7 8.8 13.5
HT- I 5-2 12.8 14.1 11.8 14.5
HT- 15-3 12.5 12-26 11.8 12.18
HT- 15-4 12.2 14.6 11.0 14.8
HT- 15-5 10.3 15.7 9.1 15.8
HT- 1 5-6 11.8 12.8 10.9 12.8
HT- 1 5-7 11.9 14.0 10.4 14.2
HT- I 5-8 10.2 16.7 8.9 16.6
HT- I 5-9 10.4 15.8 9.4 16.0
HT-15-10 10.2 7.8 9.9 7.9
HT-1- 1 8.6 6.4 8.3 6.4
HT- 1-2 11.9 8.0 11.6 8.2
HT- 1-3 16.2 12.1 15.6 12.6
HT- 14 17.2 12.1 16.6 12.7
HT- 1-5 14.2 7.5 13.0 7.9
HT- 1-6 11.2 6.0 11.0 6.1
HT-5- 1 13.1 8.8 12.9 9.0

HT- 10- 1 12.8 9.7 12.3 9.8

1

HT- 10-2 10.6 7.7 10.3 7.8

HT- 10-3 12.3 10.0 11.8 10.3
 Sample # Frequency Er' Er "
(MHz)
HTMP1 480.0 1 14.2 23 -5

HTMP8 48 1.9 12.2

HTMP IO 596.4

HTMP12 563.1 9 .O 13.4

HTMP 13 469.0 12.1 20.7
HTMP 14 462.8 12.2 13 .O
HTMP 15 460.2 12. I 20.3
WTMP 16 463.7 I 12.0 20J
HTMP 17 459.8 12.6 21.3
HT- 15-1 480.00 5.6 14.2
HT- 15-2 3 19.30 9.3 15.7
HT- 15-3 4 12.22 8.6 9.9
HT- 15-4 297.00 10.1 15.0 - -

HT- 15-5 304.2 I 8.6 16.4

HT- 15-6 336.61 8.7 12.9
HT- 1 5-7 330.00 8 .O 14.6
HT- 15-8 265.O0
HT- 1 5-9 285.00 16.2
HT-15-10 50 1.36
HT-1-1 402.32 7.2 6.7
1 HT-1-2 523.32 6.2 ' 11.1
HT- 1-3 434.65 9.7 15.4
HT- 14 440.84 9.8 t 6.2
HT- I-5 540.13 9.4 11.7
HT- 1-6 57 1.74 6.9 8.5
HT-5- I 507.02 8.3 11.4
HT-5-2 552.85 6.8 8.6
HT-OS- 1 534.60 8.5 12.4
HT-05-2 587.94 7.2 8.7
HT- 1O- 1 469.67 7.5 11.2
HT- 10-2 508.73 7.3 8.5
HT- 10-3 456.23 7.3 1 I.6
 Volumetric Moisture Content, 0

Figure 4.2: &;(200 MHz) versus volurnetnc moisture content at constant density and
saiinity (deionized water) (a) ~,'(200MHz)(b) ~;'(200MHz)
 Volumetric Moisture Content, 8

Volumetric Moisture Content, 0

Figure 4.3: €;venus volurnetrîc moisture content at constant density and salinity
(deionized water) (a) G' (b) G"
 Moisture Content. tv

Figure 44: Characteristic curve for the complex perminivity versus moisture content
 Relative Bulk Density, p,

2.00 2.05 2-10 2.15 2.20 2.25 2.30

Relative Bulk Density, p,
(b)

Figure 4.5: &,'(200 MHz) versus relative bulk density at constant moisture content
and salinity (deionized water) (a) ~,'(200MHz)(b) &,"(200MHz)
 5 j
2.00 2.05 2-10 2.15 2.20 235 2.30
Relative h i k Density, p,

10
300 205 3 10 3 15 320 325 130
Relative Wilk Density, p,

Figure 4.6: E,' versus relative bulk density at constant moisture content and salinity
(deionized water) (a) G'(b) E;'
 O Z 4 6 8 10 12 14 16
Mixing Fluid Salinity ,s, (g/L)

O 2. 4 6 8 10 12 14 16
Mixing Fluid Salinity ,s, (g/L)

Figure 4.7: ~ ~ ' ( 2 0MHz)

0 versus mixing fluid salinity at constant moisture content
and relative bulk density (a) E ~(200MHz)
? (b) $'(200MHz)
 4 '
O 2 4 6 8 1O 13 14 16
Mixing Fluid Salinity, s, (g/L)

6
4
O -'7 4 6 8 1O 13 14 16
Mixing Fluid Salinity, s, (g/L)

Figure 4.8: E; versus mking fluid salinity at constant moisture content and relative
bulk density (a) G'(b) E;'
 Relative loss factor wiih dc conductivity cornponcnt rcmoved at the relaxation
frequency.

a Relative loss factor without dc conductivity component removed at the

relaxation fiequency.

6 8 1O

Mixing Fluid Salinity, s, (g/L)

Figure 4.9: The effect of dc conductivity on the relative loss factor at the relaxation frequency.
 -
.-c
JO-

;
w
3s -

Figure 4.10: Sensitivity of the coefficients of the multivariable linear regession to

measurernent fiequency.
(Coefficients: Eqs. 4.5,4.6,4.7,4.8,4.9,4.10,4.11.4.12)
 Summary, Conclusions and Future Work

This thesis is focused on the development of technology. based on the interaction of

electromagnetic waves with geomaterials, to address the need for a reliable method to

detect and delineate soil contamination. The complex permittivity of soil-water

systrms is a tùnction of a nurnber of physical properties such as density. moisture

content and salinity. By understanding the relationship between the compiex

permittivity of a soil-water and these soil properties. it is possible to detect changes in

the soil-water system by measuring changes in the complex permittivity of the soil

system.

With the recent development of microwave measurement, it is conceivable that an in-

situ complex permittivity sensor could be developed to quantitatively evaluate the

microscopic and bulk soil behaviour under existing conditions at a site. as well as

identiQ changes in the geoenvironment that may occur with time. However, before

one cari do this, it is necessary to establish the range of applicability and sensitivity of

the technique. This thesis investigated the characterization of a soil-water system

using both components of the complex permittivity, the permittivity and the loss

factor. In addition, the effect of the fiequency at which the measurements are made is
investigatcd as an additionid pxzîîeter that cm be consideitd iii suil-watzr

characterization.

The coaxial sample holder used for this investigation is based on a previously

designed coaxial sarnple holder (Shang et al. 1999). In order to reduce samplr

handling and to increase the accuracy of the system, a nurnber of modifications were

made to the original sample holder. ïhese modifications include. developing a

modular sample holder that is used with a specially designed soil compaction system.

and incorporating a procedure to rneasure the static conductivity of the soil sample.

The modified sample holder c m accornrnodate 35mm long compacted soil sarnples of

varying moisture contents. bulk densities and mixing fluid salinity.

A total of forty complex penittivity measurements were made using soil samples

that were prepared such that the soi1 moisture content. the soil bulk density. and the

mixing fluid salinity were varied in ranges comparable to in-situ conditions. The

gravimetric moisture content of the soil samplrs ranged between a minimum value of

6% to a maximum of 22% and the bulk density was measured to be between 1.98

' 2.31 ~ ~ / r n The

~ ~ / r nand ) . range of rnixing fluid salinity was selected to vary

between pure water to a salinity that corresponds to that of the leachate fiom a

municipal solid waste landfill, namely, up to 15g/L (measured as a concentration of

NaCl).
The results of the study were presented as a group of multivariable linear regression

equations that related the complex permittivities of Halton till as a function of soil

moisture. bulk density and mixing Buid salinity. Finally, a discussion of those

equations and their significance was presented. The volumetric moisture content,

relative bulk density and the salinity of the mixing fluid were shown to affect one or

more of the components of the complex permittivity of the soil-water system.

usrorvs
5.2 CONCL

Based upon the investigation presented in this thesis the following are made.

The complex permittivity measurement system can be used to accurately measure

the real and imaginary complex permittivity components of compacted soi1

samples of varying moisture content, relative bulk density, and salinity.

The results of the measurement of the static dc conductivity using the modified

sample holder are consistent with the ASTM standard method. This procedure

allows one to measure a soil sample's dc conductivity under the same soi1

conditions at which the complex permittivity measurements are made.

Multivarîable linear regression models have been developed, which relate the

response of the complex permittivity of compacted Halton till samples to changes

in moisture content, relative bulk density, and mixing fluid salinity. The response

of the real relative permittivity is dominated by the volumetric moisture content

and exhibits a low sensitivity to variations in the relative bulk density. The
 relative loss factor however, shows a snonger sensitivity to variations in the

relative bulk density than the real relative permittivity. Finally, the complex

permittivity measured at the relaxation frequency exhibited a very low sensitivity

to changes in the pore fluid salinity suggesting that E,* may be independent of

salinity.

The fiequency at which the complex permittivity measurements are taken affects

the sensitivity of complex permittivity to changes in soil water content. relative

bulk density and pore fluid salinity. This observation suggests that varying the

frequency at which the components of the complex permittivity is measured could

control the sensitivity of the measurement.

The investigation on the Halton till has s h o w that the characterization of soils

can be accomplished by using both the real and the imaginary components of the

complex permittivity simdtaneously. By understanding the relationship between

the complex permittivity of a soil-water system and these soil properties, changes

in the soil-water system can be detected by measuring changes in the cornplex

perminivity of the soil system.

5.3 RECOMMENDA
TION FOR FUTURE WORK

m s thesis represents part of a broader study and is direcred at the development of

technology to address the need for a reliable method to detect and delineate soil
contamination. The long-term objective of this research program is to develop a new

and novel in-situ measurement system that would allow quick, reliable and non-

destructive monitoring and assessrnent of soil and groundwater contamination and to

implement this in the field. Based on the understanding obtained through the research

presented in this thesis. the following recommendations for m e r research are aiso

made:

An investigation into the effect of soil type on the complex permittivity should be

conducted. The type of soil particle present in the soil-water system will a f k t

the conductivity of the soil sarnple and therefore will affect the loss factor of the

system. Samples of varying clay content fiom cohesionless sand to stiff clay

should be tested.

Continued research is suggested to assess the effect of heavy metals and organic

contarninants in the soil-water system.

. The effect of the fiequency of the complex penninivity measurement should be

investigated m e r . It may be possible to delineate contaminant based on their

interaction with the pore fluid, or in the case of clay soil, the double layer. by

comparing the response at different Frequencies.

. The multivariable regression mode1 should be expanded to include variables that

wouid describe the soil fabric. This would expand the range in which the linear

regression mode1 is applicable.

 The residual plots for the rnultivariabie linear regression equations presented in

Chapter 4 exhibit a wide scatter about t l e zero a i s . suggesting that addition work

is required to remove some of the variability in the results. Increasing the number

of data points measured within the fiequency range may help to increase the

acc-xacy of the measurements and in turn increase the accuracy of the regression

model.

The research presented in this thesis represents an important first step in achieving the

long-term objective of the research program. The measurement system.

characterization methodology and multivariable linear regression model represent a

solid basis on which to continue with the research program. The development of an

in-situ probe using the complrx permittivity for contaminant detection is an

achievable goal.
 116

REFERENCES

ASTM, (1995), Standard Method for Field Measurement of Soil Resistivity Using the
Wenner Four-Electrode Method. ASTM Designaiion: G57-95%pp. 1 1 1-215 .

ASTM. (1 990). Water Content Detemination. ASTM Designaiion: 22 16-90. Vol.

4.08

Baker-Jarvis, J., Vanzura, E. J., Kissick, W. A., (1990), Improved Technique for
Determining Complex Permittivity with the Transmission/Reflection Method.
IEEE Transactions on Microwave Theory and Techniques. Vol. 38. No. 8, pp.
1096-1 103.

Chaker, V.. (1996), Measuring Soil Resistivity. '4STiZ.I Stundardiialion News. April.
pp. 30-33.

Daniel, V. V.. (1967), Dielectric Relaxation, Academic Press, London

Engelder, D. S., Buffler, C. R.. (1 99 1). Measuring Dielectric Properties of Food

Products at Microwave Frequencies, Microwave World, Vol. 12. No. 2. pp. 2- 1 1 .

Flinn, R A., Trojan, P.K.,(1990). Engineering Materials and Their Application.

Ho ughton ibliflin Company, Boston .

Friedman, S. P.. (1997). Statisticai Mixing Mode1 for the Apparent Dielectric
Constant of Unsaturated Porous Media, Soil Science Sociey ofAmerica Journal.
6 1 , pp. 742-745.

Hewlett Packard, (1995), User's Guide HP 8753D Network Analyser. Hewlett

Packard, USA, HP Part No. 08753-9025.

Hill, N.A., Vaughan, W.E., Price, A.H., Davies, M., (1969), Dielectric Properties
and Molecular Behaviour. Van Nosirand Reinhold Company. London

Huang, F. S. C., Shen, L. C., (1982), Analysis of Error Due to Presence of Gaps in
the Measurement of Rock Sarnples in a Coaxial Line. Journal of Physics. Vol. 48.
No. 2. pp. 206-21 2.

Kaya, A., Fang, H.. (1997), Identification of Contaminated Soils by Dielectric

Constant and Electrical Conductivity, ASCE Journal of Environmental
Engineering, Vol. 123, No. 2, pp. 169-177.
Klein, IC, Santamarina, J. C., (1997), Methods For Broad-Band Dielectric
Permittivity Measurements (Soil-Water Mixtures, 5 Hz to 1.3 GHz), ASTM
Geotechnical Testing Journal. Vol. 20, No. 2, pp. 168-178.

Kraszewski, A. (Editor), (1 997), Microwave Aquametry, IEEE Press, New York

Morgan, M. T., Wood, R K., Holmes, R G., (1993), Dielectric Moisture

Measurement of Soil Cores, American Society of .4gricultural Engineers, Vol. 36,
NO. 1. pp. 17-22.

Nicolson, A.M. and Ross, G.F..(1970). Measurement of the intrinsic properties of

materials by time-domain techniques. IEEE Transactions on Instrumenration and
iMeasuremenr. Vol. IM-19, No. 4. pp. 377-382.

Perdok, U. D., Kroesbergen B., Hilhont, M. A., (1 996). Influence of Gravimetric

Water Content and Bulk Density on the Dielectric Properties of Soil. European
Journal of Soil Science, Vol. 47. pp. 367-371.

Rao, N. N.,(1977), Elements of Engineering Electromagnetics. Prentice-Hal[. Inc..

New Jersey.

Raythatha, R, Sen, P. N., (1986), Dielectric Properties of Clay Suspensions in MHz

to GHz Range, Journal of Colloid and Interface Science, Vol. 109. No. 2. pp. 301-
309.

Rudge, A. W., Milne, K., Oiver, A. D., Knight, O., ( 1983). The Handbook of
h t e ~ Design,
a Peler Peregreneus Ltd.

Santamarina, J. C.,Fam, F.. (1997), Dieiectric Permittivity of Soils Mixed with

Organic and Inorganic Fluids. Journal oj'Environmental and Engineering
Geophysics, Vol. 2, issue 1, pp. 37-5 1.

Shang, J. Q., Rowe, R. K., Umana, J. A., Scholte, J. W., (1999), A Complex
Permittivity Measurement System for UndisiurbedfCompacted Soil. .4STAl
Geotechnical Tesring Journal, Vol. 22, No. 2, pp 165- 174

Shaw, M. R, Miiiard, S. G., Houlden, M. A. Austin, B. A., Bungey, J. H., (1993),

A large diameter transmission line for the measurement of the relative pemittivity
of construction material, British Journal of Non-destractive Testing,Vo1.35, No.
12, pp. 696-704.

Thevanayagam, S., (1995), Frequency Domain h a l y s i s of Electrical Dispersion of

Soils, ASCE Journal of Geotechnical Engineering, Vol. 121, No. 8,6 18-627.
Xie, Y.,( 19991, Complex Permittivity of A Clayey Till Permeated By Aqueous Ionic
Solutions, iM.E.Sc. Thesis, The University of Western Ontario,submittedfor
examinat ion
 Appendix A

Appendix A contains a sampie calculation of the Nicolson and Ross solution (Nicolson

and Ross 1970) for conversion of S-parameters to complex perrnittivity (from Shang et

al. 1999)
 After the S-parameters are measured and adjusted, the following equations

can be used to solve the complex pemiittivity of a material filled in a coaxial sample

holder:

v,'= SI, + s;,

The reflection. T'. can be obtained from the scattering coefficients

The correct root in Eq. A2 is calculated by requiring (rl5 1.

The transmission, z*, is determined using:

 Finally, the complex relative permittivity E,' is calculated as:

and

Sample calculation

The S-parameters used for this sarnple calculation were obtained by

connecting the empty coaxial sample holder to the calibrated ports. Since the material

under test is air filled in the holder, the measured S-parameters do not need the phase

adjustment and c m be used directly in the N-R equations.

Frequency: 104.57 MHz

s*, 1 (measured by HP8753D ANA): - 2 . 8 2 1~03-7.37~

10"j

s ' (measured
~ ~ by HP8753D ANA): 0.815-0.578j
 Appendix B

Appendix B contains information regarding the soi1 properties of the Halton till.
 Sumrnary of Soil Properties for Halton Till

Maximum dry density ( ~ ~ / r n ' ) 1.8

Optimum water content (%) 15

Plastic Limit (%) 19.1

Liquid Limit (%) 30.0

Plasticity Index (%) 10.9

Specific Gravity 2.79

Non-clay Minerals (Xie 1999) Clay Minerals (Xie 1999)

Quartz Illite

Carbonate C hlorite

Feldspar Srnectite (trace)

- - - - - - - -

Soil pore fluid chernistry (from Xie 1999)

Sulphate (rng/L) 3641

Sodium (mg/L) 29 1

Potassium (mg/L) 58
 Water Content

Density and Unit Wejght

b F L

8mpl.r S 2 3 4 6 6

&- -y 6086 50 6132.80 6207 50 6227 20 6247 70 6213 20

km :. 4135 40 4135 40 4135 40 4135 40 4135.40 4135 40

1887 40 2072.10 2091 80 21 12.30 2077 80

1 9511 1 9974 2.0721 2.0918 2.1123 2.0778

.. -.. .
b-!*&::
:. 1.753 1.766 1.807 1.796 1.787 1.741

:&hk~ilg~it 17 188 17 321 17 722 17 610 17 530 17 073

O 56 O 60

Pol#iiv O 37 0.37 O 35 O 36 O 36 O 38
- P A - - - -

mor~~vnsr 2.5kg
Na. Blovvsnayer 26
NO. ~ a y m 3
v o m a of MOI^ 1ooo cm3
Max. ParW. Sua #4

8 1O 12 14 16 18 20 M ~~
L y ~ ~ n i l h 1.81
/ ~glm"
Water Content W O opl Water Carnint (n) 15%
 Liquid Limit, Plastic Limit and Plasticity Index of Soils
I
ASTM D 4318-93

-- -

TYPE OF TEST LL LL LL LL Wh Nat.

CONTAINER NUMBER 278 6B 100 258
NUMBER OF BLOWS 42 26 21 16
MASS WET SOlL + TARE 21.37 18.50 18.73 20.56
MASS DRY SOlL + TARE 19.22 16.83 16.86 17.99
MASS OF WATER 2.15 1.67 1.87 2.57
MASS OF CONTAINER 11.60 11.O4 10.66 10.07
MASS OF DRY SOlL 7.62 5.79 6.20 7.92
WATER CONTENT W (%) 28.2 28.8 30.2 32.4
ITYPE
OF TEST I PL l PL I
IBOREHOLENO.
CONTAINER NUMBER -- -- -- --

MASS WET SOL + TARE 22.86 21.96 DEPTH

MASS DRY SOlL + TARE 20.96 20.18 LIQUID UMlT (%)
MASS OF WATER 1 .90 1.78 PLASTIC LIMIT (%)
MASS OF CONTAINER 10.92 10.91 P U S ~ C I T VINDEX (%)
MASS OF DRY SOIL
WATER CONTENT W (%)
- 10.04 9.27 Wh Natural I%)

10
Number of Blows

-
I SAMPLE DESCRIPTION : CL Clay of Low plasticity
close to the A-Line (ML)
Geotechnical Research Centre
The University of Western Ontario

t :
~ r o j c e NO. j Client : 1 BH :
Date : 1 9t9/99 Project : i Sample : 1 ce114
LabWork: Location: 1 Depth : : t .5 - 2.0m

HO0 21.38 30.91 1 9.53 2.52 0.1 49 85.70

#?40 22.45 29.22 6.77 1.79 0.1 06 83.91
a00 23.78 30.19 6.41 1.70 0.074 82.21
Pan 310.5 82.21
 Appendix C

Appendix C contains a copy of the calibration procedure for the HP 8753D ANA taken

f?om:

Hewlett Packard, (1995), User's Guide HP 8753D Network Analyser, Hewlerr

Packard, USA, HP Part No. 08753-

Full Two-Port Error-Correction
rernoves directivity m o r s of the test setup in fornard and reverse directions
i removes source match errors of the test setup in forward and reverse directions
i removes load match enors of the test setup in forward and reverse directions
m removes isolation enors of the test setup in forward and reverse directions (optional)
m removes frequency response of the test setup in forward and reverse directions

Note This is the most accurate error-correction procedure Sice the anaiyzer takes
both forward and reverse sweeps, this procedure takes more time than the
other correction procedures

1. Set any measurement parameters that you want for the device measurement: power,
format, number of points, IF bandwidth.
2. To access the measurement correction menus, press:

3. If your calibration kit is not the 7 mm default, press:

CAL KIT and select your type of kit
IlEruw
tf your type of calibration kit is not Iisted in the displayed menu, refer to the 'Modifying
Calibration Kit Standards" procedure, located later in this chapter.
4. Tb select the correction type, press:

5. Connect a shielded open circuit to PORT 1.

. - - - - --

Note Indude imy adapters that you wiU have in the device measurement. That is
mnnect the standard ro the particular connecter where you wiU connect your
device under test.

aq676a

Figure 5-6. Standard Connections for Full Two port Error-Correction

6. 'Ib measure the standard, when the displayed trace has settled, press:

-
The analyzer displays UAIT IiEâSURINC CAL STANDARD dwing the standard measurernent.
The anaiyzer underünes the OPEN softkey after it rneasures the standard.
7. Disconnect the open, and connect a short circuit to PORT 1.
8. Tb measure the device, when the displayed trace has settled, press:

The analyzer measures the short circuit and underlines the S O R T softkey.
9. Disconnect the shon, and connect an impedance-matched load to PORT 1.
10. To mesure the standard, when the displayed trace has settled, press:
FURWARD: LOAD
The analyzer measures the Ioad and underlines the L O U softkey.
11. Repeat the open-short-load rneasurements describeci above, but connect the devices in t u n
to PORT 2, and use the REVERSE : OPEN , REVERSE: SfIORT , and REVERSE: LOAD softkeys
lnclude any adapters that you wouid indude in your device measwement.
12. To corn pute the reflection correction coe ftkients, press:

13. Tb s m the transmission portion of the correction, press: TRPUSMZSSZOB

14. Press ISOLATION and select from the foiiowing two options:
iIf you will be measunng devices with a dynamic range l e s than 90 dB, press:

r If you will be rneasuring devices with a dynamic range greater than 90 dB, follow chese
steps:
a Connect impedance-matched loads to PORT I and PORT S. Include the adapters that
you would include for your device measurement.

Note If you will be measuring highly reflective devices, such as fllters, use the test
device, connecred to the reference plane and terrninated with a load, for the
isolation standard.

b. Activate at least four times more avenges than desired dunng the device
measurernent.
c. Press a FEWME CAL S E Q U ' C E FWD ISOL'K ISOL > A STD
MV ISOL 'l? ZSOL 'M STD ISOLâTIOM DUNE .
d. Return the averaging ro the ongininal state of the measurement. and press
REsUME CAL SEqUENCE .
15. Make a 'thmmconnecrion between the points where you wiil connect your device under
test as shown in Figure 5-6.
16. Ib measure the standard, when the trace has settled, press:

The anaiyzer underiines the softkey label after it makes each measurement.
17. To compute the transmission coefiicients, press:
STANDARDS D O E

18. To compute the enor coefncients, press:

DONE 2-PORT CAL
The analyzer displays the corrected measurement trace The analyzer &O shows the
notation Cor at the left of the screen, ùidicathg that error correction is on.
- - .-

Note You can save or store the measurement correction to use for larer
measurements Refer to the 'Printing, Plotting, and Saving Mesurernent
ResuIts" chapter for procedures

19. This completes the full two-port correction procedure. You can mnnect and measure your
device under Lest.
 Appendix D

Appendix D contains the complex permittivity versus frequency graphs for al1

samples tested.
2
--
3
3i0
Cr,
Appendix E contains the multivariable linear regression residual plots for Eqs 4.5,

4.6.4.7,4.8,4.9.4.10,4.11,4.12,4.13,4.14
Figure El: Residud plots for muitivariable linear regression Equation 4.5
Figure E2: Residual plots for multivariable linear regression Equation 4.6
Figure E3: Residual plots for muitivariable linear regression Equation 4.7
 Vdunietric iVbistm Content, 8

1.9 7
-. 2.1 2.2 23 2.4
Relative Wilk h s i t y , pr

Figure E4: Residual plots for multivariable linear regression Equation 4.8
Figure E5: Residud plots for multivariable linear regression Equation 4.9
 Vdumetric Wstm Content, 8

1.9 2 2.1 22 2.3 2.4

Reiative I3uik Density, p,

Figure E6: Residual plots for mdtivariable linear regression Equation 4.10
Figure E7: Residual plots for multivarîable linear regression Equation 4.1 1
Figure ES: Residual plots for multivariable linear regression Equation 4.12
 1.9 2 2.1 22 2.3 2.4
Relative BuikDeasay, &

Figure E9: Residual plots for multivariable linear regression Equation 4.13
 Volumetric Moisture Content, 0

Relative Bulk Density, p

Figure E10: Residual plots for multivariable linear regression Equation 4.14