Mälardalen University Press Dissertations

No. 90

THE DIELECTRIC PROPERTIES OF SOLID BIOFUELS

Ana Marta Paz

2010

School of Sustainable Development of Society and Technology

Copyright © Ana Marta Paz,2010
ISBN 978-91-86135-94-2
ISSN 1651-4238
Printed by Mälardalen University, Västerås, Sweden
 Mälardalen University Press Dissertations
No. 90

THE DIELECTRIC PROPERTIES OF SOLID BIOFUELS

Ana Marta Paz

Akademisk avhandling

som för avläggande av teknologie doktorsexamen i energi- och miljöteknik vid

Akademin för hållbar samhälls- och teknikutveckling kommer att offentligen försvaras
fredagen 26 november 2010, 10.00 i Lambda, Mälardalens högskola, Västerås.

Fakultetsopponent: Dr Ebbe Nyfors, Roxar, Norway

Akademin för hållbar samhälls- och teknikutveckling

Abstract
The use of bioenergy has been increasing due to efforts in fossil fuels replacement. Modern bioenergy
technologies aim for high efficiency and low pollution levels, which increases the need for methods for
the on-line characterization of biofuels.
Dielectric methods have been identified as useful for the sensing of solid biofuels because they allow
for rapid, nonhazardous, nondestructive, and bulk determination of material properties. The dielectric
properties describe the interaction between the material and the electromagnetic waves. Dielectric
properties are intrinsic of the materials and can therefore be used for the development of prediction
models that can be applied regardless of the measurement technique. The study of the dielectric
properties is also important as it improves the understanding of the dielectric behavior of the materials.
This thesis focuses on the dielectric properties of solid biofuels and their use in the characterization
of these materials. The work presented includes the development of new methods permitting the
determination of the dielectric properties of solid biofuels with large particle size (waveguide method),
broadband measurement of the dielectric properties (coaxial-line probe), and the use of a previously
developed method for the accurate determination of the dielectric properties (free-space method). The
results includes the dielectric properties of solid biofuels and their dependence on parameters such as
frequency, moisture, density, and temperature.
This thesis also presents semi-theoretical models for the determination of moisture content, which
obtained a RMSEP of 4% for moisture contents between 34 and 67%, and an empirical model that resulted
in a RMSEC of 0.3% for moisture contents between 4 and 13%.
Finally, this thesis includes measurements of the influence of salt content on the dielectric properties
and a discussion of its use for estimation of the ash content of solid biofuels.

ISBN 978-91-86135-94-2
ISSN 1651-4238
Acknowledgments

I would like to express my gratitude to all those who gave me support during
my research studies and made this thesis possible:
- My main supervisor and school research director Professor Erik Dahlquist
for giving me the opportunity to become a research student at Mälardalen
University, and for his support and confidence during these years.
- Dr. Eva Thorin for supervision, guidance and tireless support, and for being
co-author in several papers.
- Dr. Jenny Nyström for supervision, for being co-author in several papers,
and for her warm friendship.
- Dr. Samir Trabelsi with special gratitude for the enthusiasm, ideas, co-
authoring in several papers, and inspiring discussions during my intense
internship in his research group.
- Dr. Stuart Nelson for the ideas, inspiring research life, and for his dedicated
work as co-author of several papers.
- Dr. Clarke Topp for interesting discussions, ideas, and for his work as co-
author.
- Värmeforsk for financing projects included in my research studies, and the
heat and power plants Eskilstuna Energi och Miljö and Mälarenergi for the
support with the measurements and biofuel samples.
- The colleagues at the Russell Research Center, and the Nelson and Trabelsi
families for welcoming me and making me feel at home in Athens (GA).
- My colleagues at Mälardalen University for the companionship, help with
experiments, and other things such as the ping-pong games.
- My friends and family for their affectionate support.
Abstract

The use of bioenergy has been increasing due to efforts in fossil fuels re-
placement. Modern bioenergy technologies aim for high efficiency and low
pollution levels, which increases the need for methods for the on-line charac-
terization of biofuels.
Dielectric methods have been identified as useful for the sensing of solid
biofuels because they allow for rapid, nonhazardous, nondestructive, and bulk
determination of material properties. The dielectric properties describe the
interaction between the material and the electromagnetic waves. Dielectric
properties are intrinsic of the materials and can therefore be used for the de-
velopment of prediction models that can be applied regardless of the measure-
ment technique. The study of the dielectric properties is also important as it
improves the understanding of the dielectric behavior of the materials.
This thesis focuses on the dielectric properties of solid biofuels and their
use in the characterization of these materials. The work presented includes
the development of new methods permitting the determination of the dielec-
tric properties of solid biofuels with large particle size (waveguide method),
broadband measurement of the dielectric properties (coaxial-line probe), and
the use of a previously developed method for the accurate determination of
the dielectric properties (free-space method). The results includes the dielec-
tric properties of solid biofuels and their dependence on parameters such as
frequency, moisture, density, and temperature.
This thesis also presents semi-theoretical models for the determination of
moisture content, which obtained a RMSEP of 4% for moisture contents be-
tween 34 and 67%, and an empirical model that resulted in a RMSEC of 0.3%
for moisture contents between 4 and 13%.
Finally, this thesis includes measurements of the influence of salt content
on the dielectric properties and a discussion of its use for estimation of the ash
content of solid biofuels.
The results presented in this thesis contribute to the development and im-
provement of methods for determination of important characteristics in solid
biofuels such as moisture content, density, and salt content using dielectric
measurement techniques.
Sammanfattning

Bioenergianvändningen har ökat tack vare insatser för att byta ut fossila
bränslen. Modern bioenergiteknik strävar efter hög effektivitet och låga emis-
sioner. Detta har lett till ett behov av metoder för online-karakteriseringen av
biobränslen.
Dielektriska metoder har identifierats som fördelaktiga for mätning av
biobränslen, eftersom de kan ge en snabb, ofarlig och icke-förstörande
bestämnig av stora volym av material. De dielektriska egenskaperna beskriver
samverkan mellan material och elektromagnetiska vågor. Dielektriska
egenskaper är specifika egenskap hos ett material och kan användas för
utvecklingen av prediktionsmodeller som kan tillämpas oavsett mätteknik.
Undersäkningen av dielektriska egenskaper är också viktiga för att de
förbättrar förståelsen av materialen.
Denna avhandling fokuserar på dielektriska egenskaper hos fasta
biobränslen och deras användning för karakteriseringen av dessa material.
Det arbete som presenteras här innefattar utvecklingen av nya metoder
som tillåter bestämningen av dielektriska egenskaper hos fasta biobränslen
med stor partikelstorlek, bredbandmätning och användning av en tidigare
utvecklad metod för noggrann bestämning av dielektriska egenskaper.
Resultaten inkluderar de dielektriska egenskaperna för fasta biobränslen och
deras beroende av parametrar som frekvens, densitet, temperatur och fukt.
Denna avhandling presenterar även semiteoretiska modeller för bestämnin-
gen av fukthalten, som gav en RMSEP på 4% för fukthalter mellan 34 och
67%, och en empirisk modell som gav en RMSEC på 0.3% för fukthalter
mellan 4 och 13%.
I avhandlingen ingår också mätningar av påverkan av salthalten på dielek-
triska egenskaper och en diskussion om deras användning för skattningen av
askinnehållet i fasta biobränslen.
De resultat som presenteras bidrar till utveckling och förbättring av dielek-
triska metoder för bestämning av viktiga egenskaper hos fasta biobränslen
som fukthalt, densitet och salhalt.
List of Papers

This thesis is a comprehensive summary of the following papers, numbered

in reverse chronological order of their writing. In the thesis, the papers are
refered to by Roman numerals.

I Ana Paz, Samir Trabelsi, Stuart Nelson, and Eva Thorin. Measurement
of the 0.5- to 15-GHz dielectric properties of sawdust, submitted to
IEEE Transactions on Instrumentation and Measurement, 2010.

II Ana Paz, Samir Trabelsi, Stuart Nelson, and Eva Thorin. Influence of
sodium chloride on sawdust dielectric properties, submitted to IEEE
Transactions on Instrumentation and Measurement, 2010.

III Samir Trabelsi, Ana Paz, and Stuart Nelson. Dielectric-based method
for determining moisture content and bulk density of peanut-hull
pellets, IMPI2010, International Microwave Power Symposium
Conference Proceedings, pages 190-195, Denver (CO), USA, 2010.

IV Ana Paz, Samir Trabelsi, and Stuart Nelson. Dielectric properties of

peanut-hull pellets, IMTC2010 Instrumentation and Measurement
Conference Proceeding, pages 62-66, Austin (TX), USA, 2010.

V Ana Paz, Eva Thorin, Jenny Nyström, and Erik Dahlquist. Complex
Permittivity of woody biomass at radio frequencies, submitted to
Measurement Science and Technology, 2009.

VI Ana Paz, Eva Thorin, and Clarke Topp. Dielectric mixing formulas for
water content measurement in woody biomass, Wood Science and Tech-
nology, DOI 10.1007/s00226-010-0316-8, 2010.

Ana Paz contributed with idea, method, and experimental work to all papers
except the following:

Paper I: initial idea by Samir Trabelsi and Stuart Nelson.

Paper III: idea and method by Samir Trabelsi and Stuart Nelson.
Paper VI: initial idea by Clarke Topp.
Other papers by the author
Ana Paz. Moisture content determination from dielectric properties of
solid biofuels, Aquametry 2010, First European Conference on Moisture
Measurement Conference Proceedings, pages 318-325, Weimar, Germany,
2010.

Ana Paz, Eva Thorin, and Jenny Nyström. Dielectric properties of

woody biomass at radio frequencies, ISEMA 09, Electromagnetic Wave
Interaction with Water and Moist Substances Conference Proceedings,
pages 249-268, Helsinki, Finland, 2009.

Ana Paz, Jenny Nyström, Eva Thorin, and Erik Dahlquist. Measuring
water content in woody biomass directly in transport containers, submitted
to journal 2009.

Ana Paz, Eva Thorin, and Erik Dahlquist. A new method for bulk
measurement of water content in woody biomass, Ecowood 2008, Third
Conference on Environmental Compatible Forest Materials Proceedings,
Porto, Portugal, 2008.

Ana Paz, Jenny Nyström, and Eva Thorin. Influence of temperature in

moisture content measurement of biofuel, IMTC2006, Instrumentation and
Measurement Technology Conference Proceedings, pages 175-179, Sor-
rento, Italy, 2006.

Reprints were made with permission from the publishers.

Symbols

ε relative complex permittivity

ε′ the dielectric constant
ε ′′ the dielectric loss factor
ε0 permittivity of the free space (F·m−1 )
ε∞′ permittivity at infinite hight frequencies
εe permittivity of the host phase in a mixture
εi relative dielectric constant of the component i in a mixture
εst′ static permittivity
εrd
′′ loss factor due to dielectric losses
θi volumetric content of the component i of a mixture (vol·vol−1 )
θ volumetric moisture content (vol·vol−1 )
µ permeability (H·m−1 )
ρw water density
ρ density (or bulk density)
ρd dry bulk density
σ conductivity (S·m−1 )
τ relaxation time (s)
ω angular frequency (rad·s−1 )
ψ density-independent function
B magnetic flux density (T)
D electrical flux density (C·m−1 )
Di depolarization factor for the component i in a mixture
E electrical field strength (V·m−1 )
J current density (A·m−2 )
H magnetic field strength (A·m−1 )
j square root of -1
ms mass of dry phase
mt total mass
mw mass of total water phase
MC gravimetric moisture content (% mass·mass−1 )
v total volume
vs volume of the solids
vw volume of the total water phase
Abbreviations

CEN European committee for standardization

GPR ground penetrating radar
MG Maxwell-Garnett dielectric mixing model
RMSEC root mean square error of calibration
RMSEP root mean square error of prediction
RF radio frequency
TDR time domain reflectometry
VNA vector network analyzer
Contents

Part I: Comprehensive summary

1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
1.1 Characterization of solid biofuels . . . . . . . . . . . . . . . . . . . . . . . 17
1.2 Dielectric measurements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19
1.3 Problem description and research questions . . . . . . . . . . . . . . . 20
1.4 Contributions of this thesis . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20
2 The interaction of electromagnetic waves with materials . . . . . . . . . 23
2.1 Dielectric properties . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24
2.2 Polarization phenomena . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24
2.3 The dielectric properties of water . . . . . . . . . . . . . . . . . . . . . . . 26
2.4 The dielectric properties of wood . . . . . . . . . . . . . . . . . . . . . . . 27
3 Solid biofuels . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
3.1 Definitions of solid biofuels properties . . . . . . . . . . . . . . . . . . . 31
4 Measurement of the dielectric properties . . . . . . . . . . . . . . . . . . . . 35
4.1 Waveguide method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35
4.2 Free-space method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37
4.3 Coaxial-line method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37
5 Determination of moisture content . . . . . . . . . . . . . . . . . . . . . . . . . 39
5.1 Dielectric mixing models . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39
5.2 Density-independent functions . . . . . . . . . . . . . . . . . . . . . . . . . 40
5.3 Statistics for the performance of the models . . . . . . . . . . . . . . . 41
6 Results and discussion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 43
6.1 Dielectric behavior . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 43
6.2 Determination of moisture content . . . . . . . . . . . . . . . . . . . . . . 47
6.3 The influence of the salt content . . . . . . . . . . . . . . . . . . . . . . . . 50
7 Conclusions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 53
Bibliography . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55

Part II: Papers

List of Figures

2.1 The dielectric properties of free water at 0, 20 and 60°C. . . . . 26

2.2 The dielectric properties of wood cell wall substance. . . . . . . . 28

3.1 From biomass to bioenergy. . . . . . . . . . . . . . . . . . . . . . . . . . . 29

3.2 Sawdust. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30
3.3 Tops and needles. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30
3.4 Residual woodchips. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31
3.5 Shelled peanuts and peanut-hull pellets. . . . . . . . . . . . . . . . . . 31
3.6 Classification of the biofuels included in this thesis. . . . . . . . . 32

4.1 Waveguide method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 36

4.2 Free-space method. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37
4.3 Coaxial-line probe. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38

6.1 The permittivity of sawdust versus frequency. . . . . . . . . . . . . . 43

6.2 The permittivity of sawdust versus density. . . . . . . . . . . . . . . . 44
6.3 The permittivity of sawdust versus temperature. . . . . . . . . . . . 45
6.4 The permittivity of sawdust versus MC. . . . . . . . . . . . . . . . . . 46
6.5 The permittivity of sawdust versus θ . . . . . . . . . . . . . . . . . . . . 47
6.6 The complex MG mixing model. . . . . . . . . . . . . . . . . . . . . . . 48
6.7 Prediction results with the complex MG model. . . . . . . . . . . . 48
6.8 The Argand-diagram of the permittivity divided by density. . . 49
6.9 The density-independent function versus MC. . . . . . . . . . . . . . 49
6.10 The influence of salt content on the dielectric properties. . . . . . 51
6.11 The permittivity of sawdust with varying salt versus θ . . . . . . . 52
Part I:
Comprehensive summary
1. Introduction

Humans have for a long time used biomass as a fuel, but about 150 years ago,
it was fossil fuels that propelled the industrial revolution. Today, a major part
of energy, chemicals, and materials has fossil origins. Fossil fuels have higher
energy density than biofuels (about 30 MJ·kg−1 for coal and about 19 MJ·kg−1
for dry woodchips), but fossil fuels have important drawbacks such as nega-
tive environmental consequences, the uneven distribution of reserves, and the
foreseeable exhaustion of those reserves. While the estimates on how long
the fossil reserves will last are not consensual, it is known that the as yet
unexplored reserves will require higher exploration costs, increasing the fuel
price [1]. The current interest in renewable energy is related to attempts to
secure energy supply and reduce the emission of greenhouse gases. The In-
tergovernmental Panel on Climate Change estimates that 56.6% of the global
warming capacity derived from anthropogenic emissions has its origin in the
use of fossil fuels [2].
The European Union has set a goal of 20% of the energy use to be from
renewable sources by 2020 [3]. Bioenergy is responsible for two thirds of
the renewable energy in the European Union and was identified as having
the largest growth potential among renewable sources because of relatively
low costs, low life cycle emissions, less dependence on short-term weather
changes, and development of the agro-forestry sector [4].
Solid biofuels are products and by-products of agriculture, forestry, and
their associated processing industries. Some examples of solid biofuels are
woodchips, sawdust, and straw. Direct combustion of solid biofuels at com-
bined heat and power plants is a mature and highly efficient conversion tech-
nique. This technique has been implemented in Sweden on a large scale, where
bioenergy accounted for 20% of the total energy supply in 2008 [5], and is un-
dergoing worldwide expansion.

1.1 Characterization of solid biofuels

Unlike those of fossil fuels, the properties of biofuels vary widely. These vari-
ations are due to different factors such as the origin of the biomass, the time
of harvest and collection, storage, and handling procedures [6]. The use of
solid biofuels at an industrial level increased the need for the rapid and non-
destructive sensing of their properties. Moisture content is the parameter with

17
the largest variation in solid biofuels. The typical moisture content for non-
processed solid biofuels varies between 20% and 60%, while for pelletized
biofuels the moisture content can vary between about 5% and 12% [7].
The determination of the moisture content of solid biofuels is important for
pricing, quality control, and the control of the conversion process. The price
of biofuel is dependent on its moisture content because it directly affects the
heating value. The possibility of correct pricing is one of the largest economic
benefits of rapid moisture sensors [8]. The moisture content can also be deci-
sive for the quality of a biofuel, for instance before a densification process [9],
or at plants where moisture content determines the acceptance or rejection
of biofuels. Moisture can also decrease the overall process efficiency and in-
crease the emission of pollutants due to incomplete combustion [7]. When the
moisture content is known, biofuels can be mixed in order to achieve a certain
average moisture content (a common practice at heat and power plants), and
process parameters such as input flows can be controlled.
Presently, the moisture content of solid biofuels used in heat and power
plants is determined with the standard oven method, which consists of dry-
ing samples in an oven and registering the mass difference before and after
drying [10]. This method is very accurate for solid biofuels [11], but it is
labor-consuming and requires a long waiting time for drying. Furthermore, it
demands sampling of the solid biomass material, delivered to power plants in
large truck containers. Samples are taken from surface layers of the biofuel in
the containers, leading to a moisture value that is not representative of entire
the biofuel load.
Due to the increasing interest in the rapid measurement of moisture con-
tent of solid biofuels, some methods have recently been developed for that
purpose. A comparative study of commercially available methods was per-
formed by Jensen et al. [12], who studied dielectric methods for at-line de-
termination of moisture content in solid biofuels, either by placing biofuel in
a sample holder or by using a probe. There are also instruments using near
infrared spectroscopy, with a penetration depth in a range of a few the mil-
limeters, which are suitable for on-line measurements of biofuels in conveyor
belts [13].
Nyström [8] reviewed the methods that could be used for measuring mois-
ture content of biofuel for power plants. The study compared methods such
as the dual X-ray, the indirect plant efficiency method, near-infrared spec-
troscopy, radio and microwave methods, and nuclear magnetic resonance. Di-
electric methods using radio frequency were considered the only ones suitable
for measuring a representative bulk of material, due to the large penetration
depth of radio waves. Nyström [14] developed a reflection method using radio
frequencies, with the vision of its further development into an application for
on-line moisture measurement of the biofuel directly in the truck containers.

18
1.2 Dielectric measurements
The expression ”dielectric measurements” is used to describe the measure-
ment of the interaction between dielectric materials and electromagnetic fields
at radio and microwave frequencies. The phenomena occurring during the in-
teraction between electromagnetic waves and materials are brieflly presented
in chapter 2.
Dielectric measurements have multiple advantages when compared with
other measurement methods. Besides permitting the rapid and nondestructive
determination of the properties of materials, dielectric measurements are non-
hazardous, due to the use of low power levels, and have large penetration depth
which provides subsurface sensing [15, 16].
Electromagnetic fields can be coupled to the materials under test using
structures such as coaxial lines, hollow waveguides, and air-coupled antennas,
measuring transmitted and/or reflected waves [16]. The parameters measured
can be attenuation, phase shift, and scattering coefficients, from which the
dielectric properties, characterized by the complex permittivity, can be calcu-
lated.
Some applications determine the properties of interest in the material di-
rectly from the parameters measured. An example is the method presented
by Kraszewski [17] for the determination of moisture using attenuation and
phase-shift. Also Nyström [14] used multivariate data analysis to determine
the moisture content in biofuels using a range of reflection coefficients in the
time domain.
It is also possible to retrieve the dielectric properties from measured pa-
rameters and thereafter determine the physical properties of the material. The
dielectric properties are intrinsic of the material and therefore independent of
the measurement method and setup. The study of dielectric properties allows
for the development of prediction models that can be applied regardless of
the measurement method, as was also noted by Trabelsi et al [18]. Studying
the dielectric properties also contributes to the understanding of the dielectric
behavior of the material, which can lead to improved sensing technology.
Many applications make use of the dielectric properties for the characteriza-
tion of materials. An example is time-domain reflectometry (TDR), in which
the dielectric constant is obtained from the travel time measured. The volumet-
ric moisture content is determined from the dielectric constant using empiri-
cal polynomials or dielectric mixing formulas [19, 20]. The method has been
widely used for soils but also for other porous materials such as snow [21,22].
Topp’s calibration polynomial found application in a variety of soils and also
with measurement techniques such as ground penetration radar (GPR) [23].
Another interesting example is the work by Trabelsi et al [24] who devel-
oped a model for the determination of density and moisture from the dielectric
properties and which showed very good results in a variety of particulate ma-
terials such as grain, seeds, shelled and unshelled peanuts, and pellets [18,25].

19
Multivariate analysis was also used by Kent [26] for the determination of the
composition and quality of foodstuffs from frequency spectra of dielectric
properties.
There are several applications of dielectric measurements for the on-line
characterization of materials, as reviewed and compiled in different works
[15,16,27–29]. Some examples of on-line applications are the free-space mea-
surements for moisture determination in green tea in conveyor belts [27], and
the resonant sensors for measuring the compositions of materials under flow
in pipelines [15].
Solid biofuels are mixtures of woody and herbaceous materials. There are
several studies on the dielectric properties of wood [30–32], but studies on
the dielectric properties of solid biofuels have not been previously published.
As resumed by Kraszewski [33], the development of new sensors requires not
only adequate technology but also specific knowledge concerning the material
of interest. Therefore, the focus of the work presented in this thesis was on the
study of the dielectric properties of solid biofuels.

1.3 Problem description and research questions

As previously mentioned, knowledge of dielectric properties is very important
for the development of new applications for material characterization. The
study of the dielectric properties of materials such as wood, soil, and grain
allows us to get an indication of the dielectric behavior of solid biofuels and
to analyze the possibility of measuring such properties with dielectric mea-
surements. However, the dielectric properties of solid biofuels are unknown.
This is the problem underlying the work in this thesis, and from which the
following three main questions are drawn:
1. What is the dielectric behavior of solid biofuels and what is the influence
of parameters such as wave frequency, density, temperature, and moisture
content?
2. How can moisture content be determined from the dielectric properties?
3. Which other characteristics of biofuels can be determined from the dielec-
tric properties?

1.4 Contributions of this thesis

The main contributions of the present thesis can be summarized as follows:
- The determination of the dielectric properties of solid biofuels (sawdust,
tops and needles, residual woodchips, and peanut-hull pellets), and their
dependence on frequency, temperature, density, and moisture.
- The development of new methods for the determination of the dielectric
properties of solid biofuels with large particle size (waveguide-reflection

20
 method), broadband measurements (coaxial-line probe), and the applica-
tion of a previously developed method for accurate measurements (free-
space reflection method).
- The development and application of semi-theoretical and empirical models
for moisture and density determination from the dielectric properties of
solid biofuels.
- The study of the influence of salt content on the dielectric properties and a
discussion on their use for the estimation of the ash content of solid biofu-
els.
The main contributions of the papers included in this thesis can be summed
up according to the research questions they are most related to:

Question 1 - The dielectric behavior of solid biofuels and the

influence of wave frequency, density, temperature, and moisture

Paper VI presents the apparent dielectric constant determined from measure-

ments with the waveguide reflection method, for different types of solid
biofuels (sawdust, tops and needles, and residual woodchips) for a sin-
gle frequency of 0.5 GHz. It is the first published estimate of a dielectric
property of solid biofuels.

Paper V describes a method for the determination of the complex

permittivity from measurements performed with the waveguide
reflection method. The complex permittivity is presented for different
types of solid biofuels (sawdust, tops and needles, and residual
woodchips) for a single frequency of 0.5 GHz. The fraction of loss
factor due to conductivity is also estimated using a dielectric mixing
formula.

Paper IV presents the complex permittivity of peanut-hull pellets at

microwaves (5 to 15 GHz) and its variation with frequency, moisture,
temperature, and density.

Paper I presents the complex permittivity of sawdust over a wide frequency

range (0.5 - 15 GHz) for different moisture contents. The papers also
presents a method for the determination of actual sample density in
measurements with the coaxial-line method.

Question 2 - The determination of moisture content determination from

the dielectric properties

Paper VI models the dielectric constant with dielectric mixing models and
evaluates their use for the determination of moisture content.

Paper V models the complex permittivity with a dielectric mixing model

and verifies its use for the determination of moisture content.

21
Paper III uses a density-independent function for determination of moisture
content from the complex permittivity.
Question 3 - The determination of other properties than moisture content
Paper II presents a study on the influence of salt content on the broadband
dielectric properties of sawdust.
Paper III uses a density-independent function for the determination of the
density of peanut-hull pellets.

22
2. The interaction of electromagnetic
waves with materials

James Maxwell worked out a theory of electromagnetism in 1864, supported

by twenty equations describing the behavior of electric and magnetic fields
[34]. These equations were later combined and simplified into four elegant
equations, known as Maxwell’s equations. Three constitutive equations (2.1),
(2.2), and (2.3) describing the relationship between electromagnetic fields and
materials, can be derived from Maxwell’s equations:

D = εE (2.1)

B = µH (2.2)

J = σE (2.3)

where E is the electrical field strength, D the electrical flux density, H the
magnetic field strength, B the magnetic flux density, and J the current density.
Permittivity ε , permeability µ , and conductivity σ are the electromagnetic
constitutive parameters of materials. The constitutive parameters are intrin-
sic properties of the materials and are also called the electromagnetic proper-
ties [35, 36].
Permittivity describes the interaction of a material with an electric field and
is a measure of how much the electric charge distribution in the material is
changed by the application of an electric field. Permeability describes the in-
teraction of a material with a magnetic field. It is a measure of the magnetiza-
tion or occurrence of magnetic moments in a material under the influence of a
magnetic field. All materials respond to magnetic fields to a certain degree, but
it is only for ferromagnetic materials that the permeability varies significantly
from the permeability of free space. Other materials are therefore generally
assumed to be non-magnetic [36].
Conductivity is a measure of how easily electrons can travel through the ma-
terial under the influence of an external electric field. Depending on their con-
ductivity, materials can be classified as insulators, semi-conductors, and con-
ductors. Conductors have a large number of loose electrons that migrate from
one atom to another when an electrical field is applied. In semi-conductors,
there is smaller number of free charges. Insulators have very low conductiv-
ity, usually in the range 10 to 20 σ ·m−1 [36].

23
2.1 Dielectric properties
In works on the electromagnetic characterization of materials, the term "di-
electric" is used to describe materials with high polarizability. The perme-
ability of dielectrics is comparable to that of free space and is therefore not
considered in dielectric measurements. The conductivity of dielectrics is low,
but its effects can be present the measurement of the complex permittivity. In
other words, the electromagnetic properties of dielectrics are characterized by
the complex permittivity, whose components are the dielectric properties.
Permittivity is expressed as a complex number, as shown in (2.4), in order to
represent the energy storage and energy dissipation phenomena that occur in
the material under the influence of an electric field. The real part of permittiv-
ity, ε ′ , is called the dielectric constant and describes the energy storage. The
imaginary part, ε ′′ , is the dielectric loss factor and describes energy losses.
The permittivity of a material is expressed in relation to the permittivity of
free space, which is why it is a relative parameter with no units.

ε = ε ′ − jε ′′ (2.4)

Power loss occurs due to differences between the alignment of the charges
and the electric field (dielectric losses) and due to conductivity. Permittivity
can therefore be expressed as in (2.5), where εrd ′′ , is the loss factor due to

dielectric losses, ε0 is the permittivity of free space, and ω is the angular

frequency.
σ
ε = ε ′ − j(εrd
′′
+ ) (2.5)
ωε0

The dielectric constant, ε ′ , affects the speed of propagation and the wave-
length of electromagnetic waves. The loss factor, ε ′′ represents the power that
is absorbed by the material, and, has only minor influence on the velocity of a
propagating wave [28].

2.2 Polarization phenomena

Permittivity can be understood as measure of the polarization that occurs in
a medium when submitted to an electric field. Polarization is a process of
distortion of the electric charges in a material, which tend to align with the
electric field. The period required for the charges to align with the electric
field, is the relaxation time, τ . The frequency corresponding to the relaxation
time is called the relaxation frequency, and is calculated according to (2.6):
1
frelaxation = (2.6)
2πτ

24
 At frequencies under the relaxation frequency, the charges in the material
are able to align with the field, but as the frequency approaches the relaxation
frequency, a phase lag between the charges and the field arises, resulting in
energy dissipation [37].
The different phenomena contributing to polarization are discussed in the
next sections.

Electronic and atomic polarization

Electronic polarization occurs in neutral atoms when the electron cloud is
distorted by an external electric field. Atomic polarization occurs due to dis-
tortion in the molecules without a permanent dipole but with regions that have
positive and negative charges. For many dry solids these are the dominant
polarization mechanisms, which determine their permittivity at radio and mi-
crowave frequencies. Because electronic and atomic inertia are small, the re-
laxation time is very small, and the resonant frequency is above the microwave
region. If only these polarization mechanisms are present in a material, its di-
electric constant is rather low and it is nearly lossless [35].

Orientation or dipole polarization

Dipole polarization occurs in molecules with a permanent dipole. Because the
inertia of the molecule is higher than that of an electron or an atom, this type
of polarization requires longer periods to develop and the relaxation frequency
is lower than for electronic and atomic polarization. Materials with permanent
dipole moments are characterized by high dielectric constants at frequencies
below the resonant frequency of the molecules, as well as a peak in the loss
factor at the relaxation frequency [28, 35].

Ionic conductivity and the Maxwell-Wagner effect

Conductivity is the movement of unbound charge carriers under an electro-
magnetic field. In moist materials, dissolved ions may contribute to conduc-
tivity, which dominates the loss factor, ε ′′ , at low frequencies, according to
(2.5).
In heterogeneous dielectrics, ionic conduction can also affect the dielectric
constant, ε ′ . As the ions move under the influence of the electric field, they
accumulate in interfaces, creating regions in the material with higher con-
ductivity. This results in space-charges with a relatively long relaxation time,
which contribute both to conduction and polarization. This type of polariza-
tion, called the Maxwell-Wagner effect, was noted in moist wood [31, 32].

25
2.3 The dielectric properties of water
The arrangement of the H2 O molecule is responsible for the unusual proper-
ties of water and its multiple functions in nature. The electric charges are not
uniformly distributed over the water molecule, which results in a permanent
electric dipole moment [38]. Apart from the polarizability due to electronic
and atomic displacement, the water molecule can develop dipole polarization.
Figure 2.1 shows the complex permittivity of water at radio and microwave
frequencies. Figure 2.1 was obtained with relaxation times, τ , for water at
different temperatures, published by Kaatze [38] and with the Debye equation
for polar substances, according to (2.7),

εst′ − ε∞′
ε = ε∞′ + (2.7)
1 + jωτ

where ε∞′ is the permittivity at infinitely high frequencies for which dipole
polarization has no time to develop, εst′ is the static permittivity correspond-
ing to the permittivity at low frequencies, where dipole polarization develops
fully, and ω is the angular frequency.

ε’ 0°C
80 ε’’ 0°C
70 ε’ 20°C
ε’’ 20°C
60 ε’ 60°C
Permittivity, ε

ε’’ 60°C
50

40

30

20

10

8 9 10 11
10 10 10 10
Frequency (Hz)

Figure 2.1: The dielectric properties of free water at 0, 20 and 60 °C as a function of

frequency. The complex permittivity was calculated using the Debye equation with
parameter values published by [38].

Looking at the behavior of water at 20°C, it can be noted that the relaxation
frequency is at about 17 GHz. At frequencies below the relaxation frequency,
ε ′ is high due to the alignment of the water molecules with the field; as the
frequency approaches the relaxation frequency, the ability of the molecules to
align with the field decreases, a lag between the phase of the field and that of
the molecules grows and peaks at the relaxation frequency, where ε ′′ is maxi-
mal. At frequencies higher than the relaxation frequency of water molecules,
both ε ′ and ε ′ are very low.

26
 Figure 2.1 also shows that the complex permittivity varies not only with
frequency but also with temperature. The relaxation frequency decreases with
temperature. This is because the relaxation time, τ , is inversely proportional
to temperature, as molecular movement is faster at higher temperatures [28],
and according to equation (2.6), the relaxation frequency decreases when τ in-
creases. Temperature also influences εst′ , which decreases with rising temper-
ature. This is because a higher temperature leads to an increase in molecular
disorder and makes dipole polarization difficult even at lower frequency [28].

Ice
The molecular structure of ice differs from that of liquid water, which influ-
ences its dielectric properties. Water molecules form hydrogen bonds with
the oxygen atom of neighboring molecules. In their regular structure, ice
molecules form three hydrogen bonds, which makes them unable to rotate in
the direction of an external electric field at microwave frequencies [39]. The
relaxation frequency is shifted far down to the kHz region, and at microwave
frequencies the ε ′ of ice is about 3.5 and losses are very low [28].

2.4 The dielectric properties of wood

Wood is the dry constituent of many solid biofuels. The dielectric properties of
wood can also exemplify how the characteristics of dry materials differ from
those of water.
Figure 2.2 shows the complex permittivity of wood cell wall substance as
a function of frequency. The figure was obtained with data from Torgovnikov
[31] for an electric field oriented perpendicularly to the tubular cells of the
wood. The dielectric behavior of the wood cell wall substance is typical of a
polar substance, with ε ′ decreasing with frequency, and a small peak in ε ′′ .
This behavior indicates the presence of some polar molecules in wood cell
wall substance, but the importance of dipole polarization in dry wood is very
small compared with its effect in water. Electronic and atomic polarization are
dominant phenomena, which also implies a minimal influence of temperature
[31].
Figure 2.2 refers to the complex permittivity of wood cell wall substance
that has a density of 1.53 g·cm−3 . Dry wood is a mixture of wood cell wall
substance and air, with typical densities between 0.4 and 0.8 g·cm−3 , and con-
sequently a lower permittivity than wood cell wall substance.

Moist wood and bound water

With the addition of water, the dielectric properties of wood change dras-
tically. Because of the polar nature of water, its dielectric properties at radio
and microwave frequencies dominate those of the materials where it is present.

27
 7
ε’
6 ε’’

Permittivity, ε
4

0 2 4 6 8 10
10 10 10 10 10
Frequency (Hz)

Figure 2.2: The ε of the wood cell wall substance at temperatures of 20-25 °C as a
function of frequency. Values are for an electric field perpendicular to the tubular cells
of the wood and as published by Torgovnikov [31].

However, the resultant dielectric properties of the moist material are not a sim-
ple combination of the dielectric properties of the dry matter and water.
Water in solid materials has different thermodynamic properties than free
water. Water in wood is primarily held by chemical bonds. These are hydrogen
bonds formed by the hydroxyl groups in the wood cell walls. As moisture
increases, water occupies the cell cavities and pores, held only by mechanical
forces. The chemically bound water is generally called bound water, and the
fraction up to which water is chemically bound in wood is called the fiber
saturation point. This point can generally be assumed to be 30% of the mass
of dry material [40].
The properties of bound water are complex and inseparable from those of
the dry phase. There can be different degrees of binding, and different fiber
saturation points, depending on the constitution of the dry phase. Therefore a
phase known as solid solution, composed of the dry-matter and bound-water
fractions in wood, is often used in studies [40].

28
3. Solid biofuels

Biofuels are solid, liquid, or gaseous products derived from organic raw ma-
terials [6]. Some biofuels are obtained directly from biomass without any pro-
cessing or conversion, as is the case with some logging residues. In other
cases, biomass undergoes some form of processing such as chopping in order
to obtain woodchips, or drying and densification to produce pellets and bri-
quettes. Some biofuels are obtained through a conversion process, as is the
case with ethanol, biogas, and bio-oil. Ultimately, all fuels are combusted for
the production of electricity, heat, or mechanical work. Figure 3.1 illustrates
the relationships between biomass, biofuels and bioenergy services.

Biofuel

Solid biofuels

Bioenergy
(Electricity
Biomass Liquid and
Heat
gaseous
Work)
biofuels

Non-fuels

Figure 3.1: From biomass to bioenergy. Adapted from CEN [41].

The biofuels studied in this thesis were:

Sawdust: residue from sawmills, rather homogeneous with particle size

smaller than 5 mm, mainly from spruce and pine.
Tops and needles: residue from forest operations such as cleaning and prun-
ing, a mixture of small woody parts and more or less green tops, mainly
from spruce and pine.
Residual woodchips: residue from the demolition of objects made of un-
treated wood, such as pallets, with large and rather heterogeneous par-
ticle size that can vary between 10 and 150 mm.

29
Peanut-hull pellets: residues from the peanut processing industry that un-
dergo a pelletization process for increasing their density, homogeneous
cylindrical particles with a diameter of about 8 mm and a length of 9
mm.

Figures 3.2 to 3 show examples of sawdust, tops and needles, residual

woodchips, and peanut-hull pellets.

Figure 3.2: Sawdust.

Figure 3.3: Tops and needles.

Biofuels can be classified according to different criteria such as biomass

production system (energy crops, by-products), economic sector (forest
biomass, agricultural biomass, municipal waste), and class of material
(woody biomass, herbaceous biomass, fruit biomass). The European

30
 Figure 3.4: Residual woodchips.

Figure 3.5: Shelled peanuts and peanut-hull pellets.

Committee for Standardization (CEN), defines solid biofuels as products

and wastes from forestry and agriculture, and wastes from their associated
transformation industries. The CEN also presented a classification for solid
biofuels according to origin and source, with the aim of facilitating the
communication between sellers, buyers, equipment manufacturers, and
authorities [41]. Figure 3.6 shows the classification of the solid biofuels
studied in this thesis according to CEN.

3.1 Definitions of solid biofuels properties

As mentioned in section 1.1, the properties of biofuels are highly variable.
They vary primarily with the type of biomass and growing conditions such
as soil type and climate. Harvest, handling, and storage procedures, as well

31
 Forest plantation Bleands and Tops and
Logging residues
wood mixtures needles

Wood processing
Chemically untreated
Woody biomass industry by-products Without bark Sawdust
wood residues
and residues

Chemically untreated Residual

Used wood Withour bark
wood woodchips

Fruit processing
Fruit biomass Chemically untreated Peanut-hull
industry by-products Nuts
fruit residues pellets
and residues

Figure 3.6: The solid biofuels in this thesis according to the CEN classification of
origin and sources [41].

as treatment such as drying, grading, and densification, will also affect the
final characteristics of the biofuels. Important physical characteristics of bio-
fuels are moisture content, bulk density, and ash content [14,42]. The moisture
content is important for pricing and quality control, and also for controlling
the conversion process. The bulk density affects the flow dynamics of mate-
rials and can also be important for the determination of quality. Ash content
affects the heating value, and may contribute to increased concentrations of
pollutants in the flue gases, as well as to several equipment-related problems
such as slagging, fouling, and corrosion, thus causing a decrease in the over-
all efficiency of the plant, equipment wear and failure, and unscheduled and
costly shut-downs [43, 44]. Chlorine has been mentioned as the most impor-
tant element causing ash-related problems, since it is responsible for making
alkali available in a corrosive form [42, 43, 45].

Density
The density, also termed bulk density, of a material is defined as the total mass
of the material, which is the mass of water mw and the mass of solids ms ,
divided by the total volume, v, according to equation (3.1):
mw + ms
ρ= (3.1)
v
Other definitions of density are also mentioned in this thesis. The dry bulk
density, ρd , is used in Paper VI, defined as the mass of solids divided by the
total volume, according to equation (3.2):
ms
ρd = (3.2)
v
Paper VI also used the definition of density of dry solids, ρs , which is de-
fined as the mass of solids divided by the volume of the solids, vs , according
to equation (3.3). In the case of wood the density of the dry solids is that of
the wood cell wall, which properties are shown in figure 2.2.

32
 ms
ρs = (3.3)
vs

Moisture content
The gravimetric moisture content, MC, is the quotient between the mass of
water mw and the total mass of the sample mt , according to (3.4).
mw
MC = · 100 (% mass·mass−1 ) (3.4)
mt

Moisture content can also be defined on a volumetric basis. The volumetric

moisture content, θ , is the quotient between the volume of water, vw and the
total volume of the sample, v, according to (3.5). The volumetric moisture
content, θ , refers to the water volume fraction, independent of the material
density. In materials with high moisture content, whose dielectric properties
are dominated by those of water, the permittivity shows a better correlation
with θ than with MC [46].
vw
θ= (vol·vol−1 ) (3.5)
v
The reference moisture content of the biofuels considered in this work was
determined with the gravimetric oven method, which meant weighing the bio-
fuel samples before and after drying at 105°C for at least 12 hours. The ref-
erence method for moisture determination yields results in gravimetric units,
and it is possible to calculate θ from MC using (3.6), where ρw is the water
density.
MC ρ
θ= (vol·vol−1 ) (3.6)
100 ρw

Ash content
The ash content of a biofuel is the amount of inorganic matter in the fuel that
is left unburned after combustion. Ashes can be present in the flue gas phase
or be left in the bottom part of the furnace.
Ash content is defined on a gravimetric dry basis, as the mass of ash, mash ,
divided by the mass of solids, ms , according to equation 3.7.
mash
Ash = · 100 (% mass·mass−1 ) (3.7)
ms

33
4. Measurement of the dielectric
properties

As discussed in section 1.2, there are different methods for measuring dielec-
tric phenomena. In this thesis, three different measurement systems were used:
the waveguide method, the free-space method, and the coaxial-line method.
The measurement methods are useful in different measurement situations and
have different characteristics such as measurement frequency, setup, and vol-
ume of the sample. Table 4.1 gives an overview of some characteristics and
principal advantages of each of the three measurement methods. They are fur-
ther described in the next sections.

Table 4.1: Overview of some characteristics of the methods for measurement of the
dielectric properties used in this thesis.
Measurement system Waveguide Free-space Coaxial-line

Frequency (GHz) 0.56 5 - 15 0.5 - 15

Sample volume (m3 ) 1 0.01 0.001

Particle size (mm) <150 <9 <1.2

Principal advantages measurement of large vol- accurate measurement of broadband

ume; reflection concept low-loss materials measurements
that can be applied on-line
Used in papers
V and VI I, III, and IV I and II

4.1 Waveguide method

The method was developed by Nyström [14] for measuring the moisture con-
tent of biofuels. It was developed as a laboratory-scale system, using an ap-
proach meant to be further developed to measure an entire depth of biofuel di-
rectly in lorries where only one side of the biofuel is accessible, requiring the
use of a reflection method. Nyström achieved good results with the waveguide
reflection system using multivariate data analysis to correlate time-domain
data with moisture content [14].
Figure 4.1 shows a diagram of the method. The system consists of two steel
drums; the upper drum shields the antenna and the other drum contains the

35
sample. The two drums are connected during the measurements, and act as a
cylindrical waveguide. The lower drum is the sample holder and the antenna
hangs in the upper drum. The antenna is connected to a vector network an-
alyzer (VNA). The measured complex reflection coefficient is corrected for
systematic errors due to directivity, source matching, and reflection tracking
in the coaxial cables and in the waveguide. This calibration uses three stan-
dard measurements: short, offset short, and load. Afterwards, a Kaiser win-
dow is applied to the frequency-domain data, resulting in a dominant centre
frequency of 555 MHz. The windowed frequency-domain data is transformed
into the time domain with the inverse Fourier transform and, from the time-
domain data, the surface and bottom reflection peaks are identified.

Figure 4.1: The waveguide measurement system. The upper drum shields the antenna,
which is connected to a VNA, and the other drum contains the sample. Figure from
Nyström and Franzon [47].

This measurement system was used in studies presented in Paper V and

Paper VI for measurements of sawdust, tops and needles, and residual wood-
chips. In Paper VI, the apparent dielectric constant was calculated using the
velocity of the electromagnetic waves, obtained from the travel times between
surface and bottom reflection peaks, and the depth of the material. In Paper
V, a more complete method was applied for the extraction of the complex di-
electric permittivity from measurements with this system. The method used
the velocity of the electromagnetic waves and the attenuation of the waves at
the bottom of the sample holder.

36
4.2 Free-space method
This measurement system was developed by Trabelsi et al. [25] and has been
shown to provide very accurate determination of the bulk dielectric properties
of low-loss materials. It consists of a free-space transmission measurement
method, as shown in Figure 4.2. Two linearly polarized horn-lens antennas are
connected to a VNA. The system is calibrated in the frequency range from 2
to 18 GHz, but the frequency range for the measurements depends on whether
the attenuation obtained is within the dynamic range of the system [25]. The
sample holder was a box with a rectangular cross section, made of Styrofoam,
a material with a dielectric constant close to that of air. The dielectric prop-
erties, ε ′ and ε ′′ , are determined from measurements of the attenuation and
phase shift of waves traversing a layer of material, according to a procedure
described in Paper IV.
This method was used in studies presented in Paper III, Paper I and Paper
IV for the measurement of sawdust and peanut-hull pellets.

Figure 4.2: Diagram of the free-space system. The transmitter and receiver horn an-
tennas on each side of the sample holder are connected to a VNA. Figure from Trabelsi
and Nelson [18]

4.3 Coaxial-line method

This is a commercial system for measuring the dielectric properties of liquids,
solids with a flat surface, and fine granular materials. It consists of an Agilent
Technologies 85070E open-ended coaxial-line probe and a Hewlett-Packard
8510C network analyzer with associated software. The probe used for the
measurements was the high-temperature probe with 3 mm-diameter coaxial
line and a 19 mm-diameter ground-plane. Measurement calibration was done

37
with the inbuilt calibration correction using a short, open air, and distilled
water at 25°C as standards. An Agilent Technologies Ecal module was also
used with the probe providing automatic correction for possible displacements
of the coaxial cable connecting the probe to the network analyzer. A stainless-
steel cup with an inside diameter of 19 mm and a depth of 19 mm, designed
for use with the high-temperature probe [48], was used as the sample holder.
Figure 4.3 shows the coaxial-line probe and the sample holder.

Figure 4.3: The sample holder and the high-temperature dielectric probe.

The coaxial-line probe is a very advantageous instrument in dielectric char-

acterization because it allows measurements within a wide frequency range,
but its utilization in granular materials is challenging due to the difficulty of
controlling the density of the measured samples. The repeatability of the mea-
surements of granular materials with the dielectric probe is dependent on the
contact between the probe and the sample, and the density of the sample in
the region around the open end of the coaxial line. The effective density of the
measured samples is likely to differ from the average density of the total sam-
ple [48]. A method for determining the effective density of sawdust samples
measured with this probe was presented in Paper I.
This measurement system was used in studies presented in Paper I and Pa-
per II for the measurement of sawdust.

38
5. Determination of moisture content

In order to determine the moisture content from the dielectric properties, a

model is necessary describing the relationships between those parameters.
Models relating the dielectric properties to the physical properties can have
a theoretical, semi-theoretical, or empirical basis. The advantage of theoret-
ical models is their contribution to improved understanding of the dielectric
behavior of the materials and of water binding modes [49]. Empirical param-
eters are often included in theoretical models in order to improve their ability
to fit empirical data. Empirical models are useful in practical applications as
they are often simpler than theoretical models and can provide good prediction
results.
In this thesis semi-theoretical approaches using dielectric mixing models
and an empirical approach based on a density-independent function were used.
A general presentation of these approaches is given in the next sections.

5.1 Dielectric mixing models

Dielectric mixing models relate the permittivity of a mixture to the permittiv-
ity of all the individual components of the mixture, their fractional volumes,
and the polarization effects, which are dependent on the shape of the compo-
nents.
Dielectric mixing models can have a pure theoretical basis, or can incor-
porate empirical parameters. The parameter describing the shape of the con-
stituents is often obtained empirically in order to improve the performance of
mixing models in practical applications, but also because it is very difficult to
define the shape of the constituents on a theoretic basis.
Mixing models have been used to describe the dielectric behavior of differ-
ent materials such as soil [50], granular materials [51], as well as snow and
ice [52]. Practical applications privilege the use of simple mixing equations
such as the power law model, shown in equation (5.1):
n
β
ε β = ∑ (εi · θi ) (5.1)
i=1

where εi and θi are the permittivity and the volumetric content, respectively,
of the constituent i, and β is the geometric factor.

39
 The power law model does not account for interactions between the dif-
ferent constituents in the mixture. This interaction is accounted for in other
mixing models, with expressions derived from the Maxwell equations (2.1)-
(2.3) and based on different mixing assumptions. An example is the Maxwell-
Garnett model (MG). This model is most adequate for sparse mixtures with in-
clusions of a determined geometry distributed in a host phase [52]. The model
is shown in equation (5.2):
n
γ
ε = εe + εe ∑ (5.2)
i=1 1 − γ

where
θi εi − εe
γ= ∑ εe + Di,k (εi − εe )
3 k=x,y,z
(5.3)

εe is the permittivity of the host phase, which in this case is air. Di,k is the
depolarization factor of the inclusion i in the direction k, being the geometry of
the inclusions defined by the semi-axes in the orthogonal directions x, y, and z.
The depolarization factor can be calculated according to equations presented
in [52].
The determination of the moisture content from dielectric mixing models
may not be applicable in many practical cases because values have to be as-
signed to several parameters such as permittivity of the dry solids and bulk
density.
The Maxwell-Garnett model was used to predict the volumetric moisture
content of solid biofuels in Paper V and Paper VI.

5.2 Density-independent functions

Studies have also been developed in order to determine the gravimetric mois-
ture content, MC, from the dielectric properties. An approach that has been
used by some authors consists of developing a function of the dielectric prop-
erties that, for a determined temperature, is only dependent on the moisture
content.
Trabelsi and Nelson [53] developed such a density-independent function
which has been tested with good results in several types of grains and seeds
[18]. The function is based on the Argand-diagram of the complex permittivity
divided by the density of the materials. From this diagram, obtained from data
at a given frequency and temperature, a linear regression equation is obtained,
according to equation (5.4):

ε ′′ ε′
= a f [ − k] (5.4)
ρ ρ

40
 where a f is the slope and k is the x-axis intercept of the regression line.
Equation (5.4) can also be used for the determination of density. a f is a cal-
ibration parameter used in the density-independent function, ψ , according to
equation (5.5):

ε ′′
ψ= (5.5)
ε (a f ε ′ − ε ′′ )
′

The relation between ψ and MC is linear, and from the linear regression
equation, the slope a and the x-intercept b are obtained, and MC is determined
according to equation (5.6):
ψ −b
MC = (5.6)
a

5.3 Statistics for the performance of the models

The analysis of the methods for moisture content determination was made
using the root mean square error, according to (5.7):

(ymeas − ycalc )2
RMSE = (5.7)
n−1

where ymeas is the empirical moisture content, ycalc is the moisture content
calculated with the model, and n is the number of samples.
In experiments with large data sets, the data was divided into a calibration
and a validation set. The calibration set was used to develop the calibration
model and the validation set to measure the prediction performance by using
the root mean square error of prediction (RMSEP). When the data set did
not allow a validation with an independent set, the performance was analyzed
using the root mean square error of calibration (RMSEC), also referred to as
SEC in Paper III.

41
6. Results and discussion

6.1 Dielectric behavior

Frequency dependence
Figure 6.1 shows the variation of ε ′ and ε ′′ with frequency for sawdust at five
moisture levels. These results were obtained with the coaxial-line probe and
were published in Paper I. Figure 6.1 (a) shows that ε ′ decreases with fre-
quency for all moisture levels, but samples with MC larger than 27% have an
inflection point at about 9 GHz after which the decrease of ε ′ with frequency
is steeper. Figure 6.1 (b) shows a peak in ε ′′ for the high moisture samples at
the same frequency. The inflection point in ε ′ and the peak in ε ′′ evidence the
relaxation of the free water molecules in the sawdust samples. The relaxation
of free water at 20°C occurs at 17 GHz, as shown in figure 2.1, but it is known
that a shift of the relaxation to lower frequencies occurs when the water is
bound [38]. Even in samples with water above the fiber saturation point, the
total water-phase has a lower energy level than free water, which explains the
lower relaxation frequency. The fact that ε ′ of sawdust decreases also before
the relaxation at 9 GHz can be attributed to the presence of bound water in the
sample with a relaxation frequency occuring under the measured frequency
range.

6 1.4
MC=45%
1.2
5
1
Dielectric constant, ε´

Loss factor, ε´´

4
0.8 37%
MC=45%

0.6
3
27%
37%
0.4
2 27%
21%
21% 0.2
13% 13%

1 9 10
0 9 10
10 10 10 10
Frequency (Hz) Frequency (Hz)
(a) (b)

Figure 6.1: The complex permittivity of sawdust with MC between 13 and 45% and
temperature of 20°C in the frequency range 0.5 − 15 GHz.

43
Density dependence
The study presented in Paper IV is here used to show the effects of density and
temperature on the dielectric properties. The measurements were performed
with the free-space method which provides very accurate estimates for low-
loss materials. All measurements refer to the dielectric properties of peanut-
hull pellets, at a frequency of 5 GHz.
Figure 6.2 shows how ε ′ and ε ′′ vary with density for peanut-hull pellets
at four moisture levels and a temperature of 20°C . Figure 6.2 (a) shows that
the dielectric constant, ε ′ , increases linearly with density for the entire MC
range. The influence of density on the loss factor, ε ′′ , shown in figure 6.2 (b)
is smaller than for ε ′ , and is visible only at higher moisture contents. The
increase of the dielectric properties with density was to be expected, because
an increase in ρ with constant MC and volume, means an increase of both dry
matter and water in the sample, according to equations (3.1) and (3.4).

2.6 0.35
MC= 4%
2.5 MC= 6%
0.3
MC= 10%
2.4 MC= 13%
0.25
Dielectric constant, ε´

Loss factor, ε´´

2.3
0.2
2.2
0.15
2.1
0.1
2

1.9 0.05

1.8 0
0.5 0.55 0.6 0.65 0.7 0.5 0.55 0.6 0.65 0.7
Density, ρ (g ⋅ cm−3) Density, ρ (g ⋅ cm−3)
(a) (b)
Figure 6.2: The complex permittivity as a function of density for peanut-hull pellets
at 20°C and 5 GHz.

Temperature dependence
In order to analyze the variation of the dielectric properties with temperature,
the effect of density was minimized by dividing the dielectric properties by the
density [18]. Figure 6.3 shows how the dielectric properties divided by den-
sity vary with temperature varying between -20°C and 40°C. Both ε ′ /ρ and
ε ′′ /ρ increase linearly with temperature, which contrasts with the behavior of
free water. As discussed in section 2.3, ε ′ and ε ′′ of free water decrease with
temperature (see Figure 2.1). But part of the water in the sawdust samples is
bound to the solid phase. Jones and Or [54] studied the effects of temperature

44
on the dielectric properties of granular material, concluding that an increase
in temperature is accompanied by two concurrent phenomena: the release of
some of the bound water, which increases the overall permittivity of the ma-
terial, and a decrease in the permittivity of the free water. The authors suggest
that one of the phenomena dominates the changes of the overall permittivity
of the mixture until a certain point where both phenomena would have equal
influence. In the case of the peanut-hull pellets in figure 6.3, the increase in
permittivity resulting from the release of bound water dominates the variation
of the permittivity of the mixture.
Figure 6.3 also shows that the effect of temperature is greater for higher
moisture contents. This is to be expected because temperature mainly affects
the phenomena of dipole polarization, which occurs in water.
The linear behavior of the dielectric properties within the temperature range
shown in figure 6.3 indicates that the water in the sample is unfrozen. This
nonfreezing condition can be explained because the water is bound to the dry
matter and requires lower temperatures to break those bounds and freeze. In
grain the freezing point has been identified at -20°C, where an inflection in
the relation bewteen the dielectric properties and temperature occurs [55].

4.5 0.7
MC=4%
MC=6% 0.6
MC=10%
4 MC=13%
0.5

0.4
ε´´/ρ
ε´/ρ

3.5
0.3

0.2
3

0.1

2.5 0
−20 0 20 40 −20 0 20 40
Temperature, (°C) Temperature, (°C)
(a) (b)

Figure 6.3: The complex permittivity divided by density as a function of temperature

for peanut-hull pellets at 5 GHz.

Moisture content dependence

According to the theory discussed in sections 2.3 and 2.4, moisture content
is expected to strongly influence the dielectric properties of biofuels. In this
section, the variation of the dielectric properties of both peanut-hull pellets

45
and sawdust is presented. The results are based on the studies published in
Paper I and Paper IV, and were obtained with the free-space method.
Figure 6.4 shows how ε ′ and ε ′′ vary with the gravimetric moisture content,
MC. The dielectric properties increase with MC for both biofuel types, but
are much higher for the peanut-hull pellets than for sawdust at a given MC.
This is due to the higher density of the peanut-hull pellets. For a MC of about
13%, ρ is 0.6 g·cm−3 for peanut-hull pellets and 0.2 g·cm−3 for sawdust. This
difference means that the sample of peanut-hull pellets has both more dry-
matter and more water per volume than the sawdust samples.

3.5 0.6

sawdust
peanut−hull pellets 0.5
3
Dielectric constant, ε´

Loss factor, ε´´ 0.4

2.5

0.3
2
0.2

1.5
0.1

1 0
0 20 40 60 0 20 40 60
Gravimetric moisture content, MC (%) Gravimetric moisture content, MC (%)
(a) (b)

Figure 6.4: The dielectric properties as a function of the gravimetric moisture content
for sawdust and peanut-hull pellets at 20°C and 5 GHz.

The volumetric water content, θ , can be used to analyze the dielectric prop-
erties of both biofuel types for similar water volumes. Samples with similar θ
have a similar volumetric fraction of water, and density influences only the rel-
ative fractions of solids and air. Because the dielectric properties of water are
higher than those of dry-matter, the dielectric properties of moist substances
are expected to be mostly influenced by the water fraction. Figure 6.5 shows
the variation of ε ′ and ε ′′ with θ for sawdust and peanut-hull pellets. Fig-
ure 6.5 (a) shows that ε ′ of peanut-hull pellets is higher than that of sawdust,
but the difference decreases as θ increases. On the other hand, figure 6.5 (b)
shows that ε ′′ of peanut-hull pellets is smaller than that of sawdust for lower
θ levels, while both tend to converge for θ of about 0.1.
The difference in the dielectric properties of both biofuel types may be due
to differences in the dry bulk density of the samples, which represents the
fraction of dry-matter, to differences in the water-binding forces of the bio-
fuel types, and to differences in the granular structure of the particles in the
mixtures, which affects the depolarization of the waves. The dry bulk density,

46
ρd , is also about four times higher for the peanut-hull pellets than for sawdust,
which can explain that peanut-hull pellets have a higher ε ′ than sawdust for
the same θ . It is likely that the fraction of dry-matter contributes to ε ′ due
to electronic and atomic polarization, but these polarization types do not con-
tribute to ε ′′ (see section 2.2). The higher dry-matter fraction can result in a
decrease in ε ′′ , as seen in figure 6.5 (b), due to greater water binding forces.

3.5 0.6
sawdust
peanut−hull pellets
0.5
3
Dielectric constant, ε´

0.4

Loss factor, ε´´

2.5

0.3

2
0.2

1.5
0.1

1 0
0 0.05 0.1 0.15 0 0.05 0.1 0.15
Volumetric moisture, θ (vol ⋅ vol−1) Volumetric moisture, θ (vol ⋅ vol−1)
(a) (b)

Figure 6.5: The dielectric properties as a function of the volumetric moisture content
for sawdust and peanut-hull pellets at 20°C and 5 GHz.

6.2 Determination of moisture content

Dielectric mixing models
Paper VI studied the applicability of three dielectric mixing models to the
dielectric constant of solid biofuels measured with the waveguide method. The
Maxwell-Garnett mixing model (presented in equation (5.2)), provided the
best fit of the data, using empirical parameters for the depolarization factors.
The model was also used for the prediction of moisture content. The prediction
of an independent test set resulted in a RMSEP of 0.03 vol·vol−1 .
In Paper V, the Maxwell-Garnett mixing model was used to model both ε ′
and ε ′ measured with the waveguide method. This model resulted in a RM-
SEP of 0.018 vol·vol−1 , which is significantly lower than the prediction error
obtained when predicting θ from ε ′ only.
Figure 6.6 shows the complex permittivity as a function of θ , for the mea-
sured data and the data modeled with the Maxwell-Garnett model, developed
in Paper V. The variation of ε ′ for a determined θ is not explained by the
dielectric mixing model, which indicates that this variation is not due to the

47
influence of density but to inaccuracies in the measurement of the dielectric
properties with the waveguide method. Figure 6.7 shows the prediction results
obtained with the Maxwell-Garnett model in Paper V.

8 ε’ empirical
ε’’ empirical
7 MG model
6
Permittivity, ε

0
0.05 0.1 0.15 0.2 0.25 0.3
Volumetric water content, θ (vol⋅vol−1)

Figure 6.6: Empirical and modeled data with the complex dielectric mixing model.

0.3

0.25
Predicted θ (vol⋅ vol−1)

0.2

0.15

0.1

0.05
0.05 0.1 0.15 0.2 0.25 0.3
Measured θ (vol⋅ vol−1)

Figure 6.7: Measured and predicted θ with the complex MG mixing model.

Density-independent function
In Paper III, the density-independent function by Trabelsi et al. [24] was used
in the development of a calibration equation for peanut-hull pellets. The fre-
quency that yielded the best results was 5 GHz. Figure 6.8 shows the Argand-
diagram of the complex permittivity divided by the density of the peanut-hull
pellets, measured at 5 GHz and 20 °C. The relation between ε ′′ /ρ and ε ′ /ρ is
linear, and was used to determine the bulk density, ρ , according to equation
presented in (5.4), which results in equation (6.1).

48
 0.6

0.5

0.4

ε’’/ρ
0.3

0.2

0.1

0
2.8 3 3.2 3.4 3.6 3.8 4 4.2
ε’/ρ

Figure 6.8: The Argand-diagram of the dielectric properties divided by density for
peanut-hull pellets at 20°C and 5 GHz.

0.419ε ′ − ε ′′
ρ= (6.1)
1.2
The density-independent equation, ψ , calculated according to (5.5), was
plotted as a function of MC, as shown in figure 6.9. From the linear relation
between ψ and MC, the slope a and x-intercept b used in equation (5.6) are
obtained and finally, MC can be determined according to equation (6.2). The
RMSEC was of 0.3%. This value is in the range of those obtained for other
granular materials such as grain and seeds [18].

0.45

0.4

0.35

0.3
ψ

0.25

0.2

0.15
3 4 5 6 7 8 9 10 11 12 13 14
Gravimetric moisture content, MC (%)

Figure 6.9: The ψ function as a function of MC for peanut-hull pellets.

ψ − 0.064
MC = (6.2)
0.027

49
Overview of moisture prediction
Table 6.1 presents an overview of the methods used for the determination of
moisture content. It shows that the use of dielectric mixing models as predic-
tion models is more complex than that of empirical models. This is because
the calculation of the volumetric fractions of the inclusions requires the den-
sity, ρ , as well as the permittivities of the inclusions. The RMSEP obtained
for the complex mixing model, shown in Table 6.1, was re-calculated in gravi-
metric units, resulting in a RMSEP of about 4 % mass·mass−1 . The density-
independent equation yielded a much lower RMSEC of calibration of 0.3%.
Even if this is a value for calibration, it is likely that the prediction ability
with an independent test-set would also be rather low. However, it should be
noted that the frequency range covered by the density-independent function is
also much smaller that the range used in the other methods. The applicability
of the density-independent function to samples with a wide range of moisture
content has to be tested in future studies.
Jensen et al. [12] compared several commercial methods for moisture mea-
surement in solid biofuels. The best results for bulk measurements were ob-
tained with a dielectric method using a volume of about 0.06 m3 , which gave
a standard error of prediction between 2.5 and 22.9%. The range covered
refers to results of different laboratories that measured different solid biofuels
with MC ranges between 0 and 55%. Compared with the results published by
Jensen et al. [12], the RMSEC obtained with the density-independent func-
tion are promising and show that it can be possible to get improved prediction
results.

Table 6.1: Results overview with the different models for moisture determination.
Method Response Predictors Calibration RMSE Moisture range
parameters
θ MC
(vol·vol−1 ) (% mass·mass−1 )
MG model θ ε ′, ρ εi′ , εh′ , Di 0.03 vol·vol−1 0.07-0.29 31-63

Complex MG model θ ε ′, ε ′, ρ εi′ , εh′ , Di 0.02 vol·vol−1 0.08-0.30 34-67

(4 %)
Density-independent MC ε ′, ε ′ af 3% 0.03-0.08 4-13
function (RMSEC)

6.3 The influence of the salt content

The coaxial-line probe method was used to perform measurements on the in-
fluence of the salt content in the dielectric properties of sawdust, because it
can provide the measurement of the dielectric properties at low frequencies,
where ionic effects are dominant. The results of this study were published in
Paper II. Figure 6.10 shows the dielectric properties of sawdust samples with

50
no added NaCl, with 1%, and with 3% added NaCl, for the five MC levels.
Figures 6.10 (b) and (d) show that the addition of NaCl results in a strong
increase of ε ′′ towards lower frequencies. The increase is larger in samples
with 3% NaCl than in samples with 1% NaCl. For the lowest MC, 13%, the
increase of ε ′′ at lower frequencies in samples with added salt is difficult to
detect. In Figure 6.10 (c), there is also an increase in ε ′ at lower frequencies
in samples with added salt as compared to samples with no added salt. The
increase is also larger for samples with 3% NaCl than for samples with 1%
NaCl. This suggests the occurrence of interfacial polarization due to hetero-
geneous structures formed by regions with different conductivity, as discussed
in section 2.2.
3 0.8
no salt added
2.8 1% salt 0.7
3% salt
2.6
0.6
Dielectric constant, ε´

2.4 Loss factor, ε´´

0.5
2.2
0.4
2
21%
0.3
1.8
21%
0.2
1.6 17%
17%

1.4 0.1
13% 13%

1.2 9 10
0 9 10
10 10 10 10
Frequency (Hz) Frequency (Hz)
(a) (b)

6 4

5.5 3.5

3
Dielectric constant, ε´

5
Loss factor, ε´´

2.5
4.5
2
4
1.5
45%
3.5
1 37%
45%
3 0.5
37%
2.5 9 10
0 9 10
10 10 10 10
Frequency (Hz) Frequency (Hz)
(c) (d)

Figure 6.10: The complex permittivity of sawdust samples with no salt added, 1%,
and 3% of added salt.

51
 Figure 6.11 shows the dielectric properties as functions of θ for samples
with no added salt, and with 1% and 3% added salt at 0.5 GHz and 10 GHz.
θ was calculated according to the method for density determination presented
in Paper I. Figure 6.11 (a) shows that ε ′ is larger for samples with higher salt
content. A very large difference between different salt contents can be seen for
ε ′′ in figure 6.11 (b). Figures 6.11 (c) and (d) show that samples with different
salt contents have very similar dielectric properties at 10 GHz. These results
indicate that it may be possible to determine the salt content from the ionic
conductivity of sawdust samples, by measurements at two frequencies, one
where conductivity is not detectable and another one where it is dominant.

6 4
0.5 GHz
no NaCl added 3.5
5 1% NaCl
3% NaCl
3
Dielectric constant, ε´

Loss factor, ε´´

4 2.5

2
3
1.5

1
2
0.5

1 0
0 0.05 0.1 0.15 0.2 0 0.05 0.1 0.15 0.2
Volumetric water content, θ (vol/vol) Volumetric water content, θ (vol/vol)
(a) (b)

6 4
10 GHz
3.5
5
3
Dilectric constant, ε´

2.5
Loss factorε´´

4
2
3 1.5

1
2
0.5

1 0
0 0.05 0.1 0.15 0.2 0 0.05 0.1 0.15 0.2
Volumetric water content, θ (vol/vol) Volumetric water content, θ (vol/vol)
(c) (d)

Figure 6.11: The complex permittivity as a function of θ for sawdust samples at five
MC levels with no added salt, with 1%, and with 3% added salt, at 0.5 and 10 GHz.

52
7. Conclusions

The aim of this thesis was to study the dielectric properties of solid biofuels
and their utilization for the characterization of such fuels. Three main research
questions were posed at the beginning of this thesis. The first question con-
cerned the influence of parameters such as the wave frequency, temperature,
bulk density, and moisture.
The study of the frequency dependence of the dielectric properties of saw-
dust between 5 and 15 GHz showed that sawdust samples with moisture con-
tent above the fiber saturation point evidence a relaxation at about 9 GHz at-
tributed to the free water in the samples. The measurements also evidence
the existence of bound water with a relaxation frequency under the measured
frequency range.
Temperature was shown to affect the dielectric properties of peanut-hull
pellets measured with the highly accurate free-space method. Both ε ′ and ε ′′
increase linearly as the temperature rises from -20°C to 40°C. This behaviour
evidences the existence of nonfreezing water due to its bound condition.
Density affects the dielectric properties because it changes the dry-matter
and water fractions in the materials. In peanut-hull pellets with similar gravi-
metric moisture contents, the dielectric properties increase linearly with den-
sity. Density mainly affects the dielectric constant.
As expected, the dielectric properties of solid biofuels are strongly affected
by moisture content. Besides moisture content, temperature, density and fre-
quency, other parameters such as water binding modes and granule structure
can affect the dielectric properties of different types of biofuels. This indicates
that specific calibration might be necessary for different biofuel types.
The second question posed at the beginning of the thesis concerned to the
determination of the moisture content of solid biofuels from their dielectric
properties.
Dielectric mixing models were used for modeling the dielectric behavior of
solid biofuels. The Maxwell-Garnett model was found to be capable of fitting
apparent dielectric constant and complex permittivity data, using empirically
determined parameters as depolarization factors. The models were used for
the prediction of moisture content in solid biofuels. The mixing model us-
ing the complex permittivity showed a considerablely better prediction result
than the mixing model using only the apparent dielectric constant, yielding
a RMSEP of 0.018 vol · vol−1 , or 4% mass·mass−1 . Dielectric mixing models
are important tools in the study of the dielectric behavior of granular materi-

53
als, but their use as prediction models is more complex than that of empirical
models. Furthermore, the Maxwell-Garnett model cannot be solved explicitly
for the volumetric moisture content, which has to be calculated by iterations.
The density-independent equation by Trabelsi et al. for the determination
of the gravimetric moisture content was also tested with microwave frequency
data for peanut-hull pellets with MC between 4 and 13%. The RMSEC was
of 0.3 %, which is a very promising result. However, the application of this
method should be tested for larger moisture ranges.
The third research question concerned the determination of other character-
istics than moisture content from the dielectric properties.
The density-independent equation by Trabelsi et al. was also used with good
results for the determination of the bulk density of peanut-hull pellets.
Another parameter of interest in the characterization of solid biofuels is ash
content. Part of the ash content in solid biofuels has its origin in free ions in
the material. The influence of free ions on the dielectric properties was tested
in sawdust with varying salt content. Salt content was shown to affect both
ε ′ and ε ′′ at low frequencies. The influence is dominant at frequencies below
4 GHz. This results can be used to determine the salt content from the ionic
conductivity with measurements at two frequencies, one where conductivity
is not detectable and another one where conductivity is dominant.
The results presented in this thesis contribute to the development and im-
provement of methods for determination of important characteristics in solid
biofuels such as moisture content, density, and salt content using dielectric
measurement techniques.

54
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