MASTER'S THESIS

Sensus Aquae in Ferrum ac Air

Characterization of Electrical Properties of a Moisture Measurement System

Christian A. M. Karlsson

Master of Science in Engineering Technology Space Engineering

Lule University of Technology Department of Computer Science, Electrical and Space Engineering

Sensus Aquae in Ferrum ac Air

Characterization of Electrical Properties of a Moisture Measurement System

Christian A.M. Karlsson

Lule University of Technology Department of Computer Science, Electrical & Space Engineering Division of EISLAB

2011-08-24

Cover illustration:
Images from left to right

LKAB Kiruna aerial picture (2008), photo taken by LKAB LKAB mine Kirunavaara, cross-section of mine, image produced by LKAB Iron ore from Kirunavaara mine (2010), photo by C. Karlsson The first CEO of Kirunavaara and Loussavaara mine, Hjalmar Lundbohm, drawing published by LKAB A pile of magnetite concentrate (2010), photo taken by C. Karlsson (assisted by Rolf Schrter) LKAB KK4 lightened, photo by LKAB Pellets in a gloved hand, photo by LKAB

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ABSTRACT Fast precise moisture measurement in mineral process plants, has long been a difficult problem. In this master thesis a foundation for a new way of measurement using transmission line theory, is laid out. Macroscopic electro-magnetic properties of the measured sample can be linked to those of the individual constituents of the sample. Thus one is believed to be able to do a precise estimate of the amount of moisture in a sample. In our case the samples are moist magnetite concentrate. The characterization of sample macroscopic electro-magnetic properties is done by using a coaxial cell, performing frequency spectra measurement. In this master thesis, the electrical behavior that links the measured data to the macroscopic electro-magnetic properties is examined. It exists two setups, one inductive and one capacitive. The DC resistivity of the moist magnetite concentrate is determined and some interesting phenomena, suggested to be self potential were discovered. This phenomenon is in general known from geochemistry of mineral rich clays. This made the measurements of resistivity tricky to perform, some measurements were achieved and a new relation between moisture of the moist magnetite concentrate and resistivity is presented. Studies have been performed on the history of attempts of solving this problem, as well as current relevant research. Reference samples have been prepared in a geotechnical laboratory. Impedance frequency behavior of the measurement equipment is measured and presented, with different curves for different moisture content. From these measurements it is obvious that the moisture affects the impedance of the measurement equipment and thus it is possible to use this method to measure moisture content, if one can determine the electrical model which describes the measurement system. A few equivalent circuits of transmission lines have been discussed, and one was chosen to represent the purely coaxial part of the coaxial cell. Other parts have been modeled with other elements of AC theory. A new electrical model for the coaxial probe is proposed, based on LC resonances. Some Comsol FEM simulations have been performed on the coaxial cell, as well as on electric property sensors. Ideas to designs of electrical sensors are discussed. It is mainly the geometry which has been investigated. First it was proposed that a phenomenon of resonance occurs at the interface of the bottom and coaxial part of the cell, LC resonance. The resonance effect has later been investigated and identified as quarter wavelength resonance, due to the length of the measurement cell and change of wave velocity due to wave propagation in MUT. Simulations of proposed circuit equivalents in Orcad with PSpice have given some correlation with measured data for dry and non-conducting samples. There is still work to be done, to complete an accurate mathematical model of the system.

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PREFACE This master thesis covers some of the first trembling steps toward the solution of measuring moisture content in the magnetic granular media, moist magnetite concentrate, also containing some different minerals which add further complexity to the problem of electrical measurements. This problem has engaged engineers and scientists for a few decades. The recipient of the result is the mining company LKAB which is interested in the technique for the refinement of their pelletization process. Also some electronic companies have shown some interest to future developments for a wider production of measurement units. The reason for high precision moisture measurements at LKAB is the effect it puts on the formation of pellets. Pellets are round balls with a certain prerequisites of roundness and diameter. When shaping the pellets, the moisture content of the moist magnetite concentrate affect the quality and the shaping of the pellets. Thus having the ability to easily monitor the moisture content of moist magnetite concentrate, would increase productivity and improve quality of pellets. The idea is to find the moisture content by using one or two electric property mixing formulas, the Maxwell-Garnet formula and / or the Bruggeman formula. These two formulas describe the relation between electric properties and constituent volume fractions, thus one can deduce the different volume fractions by measuring the electric properties. In this master thesis we will not go into calculations with mixing formulas, but focusing on the measurements of the electric properties of the material under test (MUT). The electric properties which describe the media are electric permittivity [F/m], magnetic permeability [H/m] and resistivity [m]. Later these properties can be used together with the already known properties of each separate component which then allows us to extract the moisture content from one or both of the mixing formulas. Christian Karlsson

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ACKNOWLEDGEMENT I would like to thank my supervisor Torbjrn Lfqvist for his support, inspiration and devotion to the project. Again Torbjrn Lfqvist and Johan Borg for extremely important laboratory assistance without which the project would have been far more time consuming. Lars-Gran Westerberg (TFMM) for his discussion around Comsol Multiphysics modelling and Sverker Fredriksson (TFMM) for refinement of my report writing technique, through a few courses. Many people at EISLAB LTU has brought understanding to the problem and given valuable help in theoretical issues. The following peoples are appreciated for these contributions Torbjrn Lfqvist, Johan Borg, ke Wisten, Johan Carlsson and Kalevi Hyypp. Mikael Larsmark provided help by constructing electrode plates for the resistivity measurement equipment. Dr. Per-Erik Martinsson (Project Manager for Process IT) for his interest and support for the project SAFA. Thanks to Dr. Bertil Plsson (TKG) for access to the geotechnical laboratory. Magnus Westerstrand (TKG) for discussions on process water characteristics and self potential. For test samples and introduction to the refining process by LKAB and sa Partapuoli. Discussions of details on the process between grinding iron ore and the pellets formation, as well as the characteristics of the magnetite concentrate and pellets by Seija Forsmo. Also many thanks to the people who have supported me throughout my master studies, those who have made me determined to finish my master and my family for their support.

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TERMS, DEFINITIONS AND ABBREVIATED TERMS AC B BUW CCPL Concentrate DC Dry Case E EISLAB E-M GPR Green Pellet HUT LTU M M-G MUT PEEC SAFA SDSP TDEM TKG VNA Wet Case WikiUN Alternating Current Bruggeman Bauhaus-University Weimar Creative Commons Public License Concentrated mineral powder Direct Current Material measurement where the Rp parameter is high enough to be neglected in the model Electric Embedded Internet System Laboratory Electro-Magnetic Ground Penetrating Radar Non-Sintered Pellet Helsinki University of Technology Lule University of Technology Magnetic Maxwell-Garnett Material Under Test Partial Element Equivalent Circuit (method) Sensus Aquae en Ferrum ac Air (project name) Soil Dielectrics Spectroscopy Probe Time Domain Electro Magnetic Measurement Department of Chemical Engineering and Geosciences Vector Network Analyzer Material measurement where the Rp parameter is low enough to be considered a part of the circuit. Wiki User Name

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CONTENTS Abstract .................................................................................................................................... IV Preface ...................................................................................................................................... VI Acknowledgement ................................................................................................................. VIII Terms, Definitions and Abbreviated Terms .............................................................................. X Contents ...................................................................................................................................XII Figures ................................................................................................................................... XIII 1 Introduction ......................................................................................................................... 1 1.1 1.2 2 2.1 2.2 2.3 2.4 2.5 2.6 2.7 2.8 3 3.1 3.2 3.3 4 4.1 4.2 5 5.1 5.2 5.3 5.4 5.5 5.6 6 7 8 The Objective of the Project ........................................................................................ 1 The Objective of this Master Thesis ............................................................................ 1 A Short Introduction to the LKAB Process of Interest ............................................... 2 General Properties of Magnetite Concentrate and Pellet............................................. 3 A Short Introduction to the Measurement Environment ............................................. 4 Summary of LKABs Earlier Tested Measurement Techniques ................................. 4 Other Research Groups ................................................................................................ 6 Possible Measurement Techniques .............................................................................. 7 Suitable Setups for Magnetic and Conductive Materials ............................................ 9 Electric Equivalent Models ......................................................................................... 9 Preparation of Moist Magnetite Concentrate Samples .............................................. 11 Resistivity (DC) ......................................................................................................... 12 Permittivity, Permeability and Parasitic Resistance (AC) ......................................... 15 Coaxial Cell Inductive and Capacitive Setup ......................................................... 20 Capacitive Surface Sensors ....................................................................................... 22 Evaluation of Models and Motivation for Chosen Model ......................................... 25 Improvements in Calculation after A. Saremi Work ................................................. 30 Calculations Using the Saremi Circuit Model - Inductive Setup .............................. 31 Simple Model Analyses ............................................................................................. 35 Calculation Using Electric Circuit Proposed by C. Karlsson .................................... 41 Resonance Analysis ................................................................................................... 48

Literature Study ................................................................................................................... 2

Lab Work and Measurements ............................................................................................ 11

Why Comsol Modeling ..................................................................................................... 20

Calculations and Electric Modeling .................................................................................. 25

Discussion of Results and Final Conclusions .................................................................... 50 Discussion of Future Work ................................................................................................ 51 References ......................................................................................................................... 53

Appendix A Geometric and Material Constants ................................................................... 55 XII

Appendix B Preparation of Moist Magnetite Concentrate .................................................... 56 Appendix C Resistivity Measurements ................................................................................. 57 Appendix D Mathematical System - Saremi Model ............................................................. 58 Appendix E Inductive Mathematical System - Karlsson Model ........................................... 59 Appendix F Capacitive Mathematical System - Karlsson Model ......................................... 61 Appendix G Matlab Functions - Cost and Zload Functions.................................................. 62 Appendix H Matlab Script Inductive Optimizer ................................................................ 63 Appendix I Matlab Script PLOT Results ........................................................................... 66 Appendix J Matlab Script Constants .................................................................................. 68 Appendix K Matlab Script Data Loader ............................................................................ 69

FIGURES Figure 1: A flow diagram of a part of the LKAB process. ......................................................... 2 Figure 2: A picture of a sandcastle, illustrating the properties that granular material gains from moisture. This picture has been released in to the public domain, at pdphoto.org. ................... 3 Figure 3: A pile of dry magnetite (left) and a pile of 11 % wet sample pile (right). .................. 4 Figure 4: Schematic picture of linking coaxial elements, licensed use under CCPL (CC BYSA 3.0) by WikiUN Qianchq [30; 31]. .................................................................................... 10 Figure 5: Industrial mixer, photo by T. Lfqvist ...................................................................... 11 Figure 6: Table of ideal moisture content and actual moisture content. .................................. 12 Figure 7: In the back there is a white bucket with moist sample of magnetite concentrate. In the front there is a resistivity measurement setup, consisting of a plastic pipe, with outside covered in aluminium foil. In the bottom of the pipe, there is a circular copper surface. The surface constituting an electrode connected to a wire exiting the bottom of the setup. A similar circular surface can be thread into the pipe from above, thus connecting through the sample put in beforehand to the surface in the bottom and finally constitute a connected system. One can do measurements between the two cables exiting the setup. The wooden plate in the bottom is for stability of measurement setup. To the left, an abandoned measurement device, a general resistance meter. .......................................................................................................... 13 Figure 8: Schematic picture illustrating the geometric dependence of the resistivity measurement setup, licensed use under CCPL by WikiUN Omegatron [30]. ......................... 14 Figure 9: DC resistivity versus actual moisture content. The red arrow indicates that the value at zero percent moisture, most probably can be considered infinite, as the measurement equipment reached its limit. The actual characteristic is believed to be of the type one over fraction, according to this diagram though, from two percent to eleven percent an almost linear behaviour. ....................................................................................................................... 15 Figure 10: Measurement setup with coaxial cell and VNA. The coaxial cell is connected only through one VNA port. The wooden box contains a calibration set for calibration of the VNA. .................................................................................................................................................. 16 Figure 11: Real part impedance spectra for inductive setup translated from the measured S11 parameters. ............................................................................................................................... 18 XIII

Figure 12: Imaginary part impedance spectra for inductive setup determined from the measured S11 parameters. ........................................................................................................ 18 Figure 13: Real part impedance spectra for capacitive setup determined from the measured S11 parameters. ........................................................................................................................ 19 Figure 14: Imaginary part impedance spectra for capacitive setup determined from the measured S11 parameters. ........................................................................................................ 19 Figure 15: Cross-Section of coaxial cell. ................................................................................. 20 Figure 16: 3D Model of Inductive Coaxial Cell. ..................................................................... 21 Figure 17: 3D Model of Capacitive Coaxial Cell. ................................................................... 21 Figure 18: Geometry of Capsense1. ......................................................................................... 22 Figure 19: Graphical E-Field Representation of Capsense1. ................................................... 22 Figure 20: Graphical E-Field Representation of Capsense2. ................................................... 23 Figure 21: Graphical E-Field Representation of Capsense3. ................................................... 24 Figure 22: Graphical E-Field Representation of Capsense4. ................................................... 24 Figure 23: L-type equivalent circuit with correction equivalent. ............................................. 27 Figure 24: T-type equivalent circuit with correction equivalent. ............................................. 27 Figure 25: PI-type equivalent circuit with correction equivalent. ............................................ 28 Figure 26: Saremi equivalent circuit with correction equivalent. ............................................ 28 Figure 27: Semi-lumped semi-distributed equivalent model with split correction lid and bottom....................................................................................................................................... 29 Figure 28: Karlsson proposed inductive equivalent circuit with correction equivalent. .......... 29 Figure 29: C. Karlsson proposed capacitive equivalent circuit with correction equivalent. .... 30 Figure 30: Real r provided by optimization of Saremi model for different water content. ... 33 Figure 31: Imaginary r provided by optimization of Saremi model for different water content. ..................................................................................................................................... 33 Figure 32: Conductivity provided by optimization of Saremi model for different water content. ..................................................................................................................................... 34 Figure 33: Error surface representing the impedance error for the optimized Saremi model compared to the measured impedance...................................................................................... 34 Figure 34: r provided by simple inductive model for air. ...................................................... 36 Figure 35: r provided by simple inductive model for water. ................................................. 36 Figure 36: r provided by simple inductive model for dry magnetite concentrate. ................. 38 Figure 37: r provided by simple inductive model for 2% moisture. ...................................... 38 Figure 38: r provided by simple inductive model for 4% moisture. ...................................... 39 Figure 39: r provided by simple inductive model for 6% moisture. ...................................... 39 Figure 40: r provided by simple inductive model for 7% moisture. ...................................... 40 Figure 41: r provided by simple inductive model for 8% moisture. ...................................... 40 Figure 42: Measured equivalent impedance for air (theoretical value by simple model), Matlab Calculated Impedance Using C. Karlsson Circuit. ...................................................... 42 XIV

Figure 43: Measured equivalent impedance for de-ionized water (mQ).................................. 42 Figure 44: Measured equivalent impedance for dry magnetite concentrate. ........................... 43 Figure 45: Orcad air equivalent with constant maximum magnitude resistance. .................... 44 Figure 46: Orcad plot of equivalent impedance for air. ........................................................... 44 Figure 47: Orcad water equivalent with constant maximum magnitude resistance. ................ 45 Figure 48: Orcad plot of equivalent impedance for water........................................................ 45 Figure 49: Matlab calculation of the air case. .......................................................................... 46 Figure 50: Matlab calculation of the water case. ..................................................................... 47 Figure 51: Matlab calculation of the dry case. ......................................................................... 47

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INTRODUCTION

This master thesis covers measurement of E-M properties of magnetic and conductive granular material, moist iron ore concentrate. The reason to measure E-M properties is that it forms the foundation for determining moisture content.

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The Objective of the Project

The objective of the project is to do precise moisture measurement of moist iron ore concentrate. Having the ability to easily monitor the moisture content of moist iron concentrate, would increase productivity, improve the quality of iron ore pellets and make production cheaper. The vision of this project is to develop an in-line moisture sensor unit, capable of accurate precise measurement of moisture down to 0.1 % precision. To achieve this, it is necessary to know the density and temperature of the MUT, if the sample is not in a controlled environment. Hence for characterization of measurement equipment and MUT, we stay in a controlled environment, the laboratory. Later when field measurements are performed, the effect of temperature and density deviations has to be incorporated.

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The Objective of this Master Thesis

The objective of this master thesis is to develop models for determination of E-M properties, which constitutes a basis for a new measurement technique for determining moisture content. The master thesis shall also work as documentation for further research and development, as well as describe the work performed during the master thesis period. The E-M properties which describe the characteristics of material under test (MUT) are the electric permittivity, r [F/m], magnetic permeability, r [H/m], and resistivity [m]. Later these properties can be used to find the moisture content of the MUT. For the extraction of the E-M properties r and r, the intention is to use a single or two different near-field antennas / sensors. Probably one electric and one magnetic sensor, needs to be designed, if a combination is not possible. The E-M properties can be retrieved from the expressions of capacitance and inductance. Then the value of r and r can be determined due to the following relationship [1], in equation 1.1: (1.1) Where C [F] is the capacitance obtained from the equivalent models when the model has been applied to the moisture measurement values of impedance. C0 [F], the capacitance according to the model when air (or preferably vacuum) constitute the MUT. The work is based on an earlier attempt to determine moisture content, from which the results brought some doubt. It was preferable to find a better lumped electrical equivalent model for the measurement cell and make new measurements to verify the model. This cell is supposed to be evaluated by reflection measurements which could be related to impedance and at the end to capacitance and inductance, through the electrical equivalent model. Further literature studies and discussions have brought a deeper understanding and have resulted in some ideas, which will be presented throughout this master thesis. 1

LITERATURE STUDY

Studies have focused on different techniques to measure moisture or E-M properties. The analyses have covered what the physical and chemical properties are of the magnetite concentrate used in the moist filter cake at LKAB? Other tested methods for measuring moisture in moist magnetite concentrate for LKAB? Which other research groups exists? Which apparatus has been used for E-M measurements on materials? Which setups can be used for measurements on magnetic and conductive materials? Which electric models are there? What work has earlier been performed within the project at LTU?

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A Short Introduction to the LKAB Process of Interest

The LKAB process that is of interest for the understanding of the problem is the balling process and the preparation of the moist magnetite concentrate to become a green pellet, the wet process. Magnetite is a specific type of iron ore, below these terms will come in context. For the balling process it is very important to control the moisture content of the moist magnetite concentrate. First the iron ore is ground to suitable size for pelletizing, cleaned by magnetic separation and flotation. The resulting slurry is mixed with different additives and put through press filters to reduce water content, resulting in a moist filter cake suitable for balling. The moist filter cake is stored in a storage silo, where it is further transported from and mixed with a binder and again put in a storage silo. From there portioned to a balling drum, where seeds starts the balling process and the balls slowly grows, exemplified by rolling a snowball. The described part of the process can be seen in Figure 1.

Figure 1: A flow diagram of a part of the LKAB process.

If one wish to understand the reasons behind the interest of moisture content of the moist filter cake (or our lab equivalent, moist magnetite concentrate) one could think of the properties of sand castles depending of sand moisture content (Figure 2), sand being another granular material. Also magnetic effects operate in this material, causing attraction and repulsion between particles.

Figure 2: A picture of a sandcastle, illustrating the properties that granular material gains from moisture. This picture has been released in to the public domain, at pdphoto.org.

A selection is made by screening the green pellets to correct size [2]. Green pellets that has exceeded the determined size, goes to a new grounding station and are inserted into the balling drum as seeds again. Smaller green pellets also go back to the drum as seeds. Those green pellets that have passed screening are loaded to the pelletizing machine for drying and sintering, at about 250 C and 1250 C respectively. It is of course during the wet process which LKAB would like to perform online moisture measurements and more specifically between the filters and balling drum (red square in Figure 1). Today these measurements are performed manually once per work shift; a sample is taken, weighed, dried and weighed again, this will provide the amount of moisture as percent mass [3].

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General Properties of Magnetite Concentrate and Pellet

Magnetite is an iron oxide containing, FeOFe2O3 (Fe3O4). The magnetite concentrate are finely ground iron ore. The fineness of the magnetite concentrate is roughly 80% - 45 m in diameter (meaning that 80% of the magnetite granules are 45 m or less in diameter), controlled by screening. Pelletizing is done using external binders, where the most common one is bentonite clay, commonly sodium activated bentonite clay. Typical composition of magnetite concentrate is 71 % Fe, 23 % Fe2+ and 0.6 % SiO2. Additives are about 0.5 % bentonite binder and grounded olivine, (Mg,Fe)2SiO4. Our laboratory equivalent however contains as close to pure dry magnetite concentrate as it ever becomes in the LKAB process. For mathematical modeling our approach is to assume a clean matrix of magnetite based on spherical particles. The water mass concentration of the moist filter cakes used today is around 8 - 9 %. At this concentration it provides a suitable base for the agglomeration process. Too low water content 3

will have a to slow growth or none at all, too high will either grow too fast and / or collapse due to insufficient binding properties. In modeling the moist magnetite concentrate will be modeled as a fixed matrix of magnetite with fixed inclusions. The accepted green pellets have a diameter around 10 mm with some small margin.

Figure 3: A pile of dry magnetite (left) and a pile of 11 % wet sample pile (right).

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A Short Introduction to the Measurement Environment

The MUT (moist magnetic concentrate) is due to its fineness and magnetic properties a dirty material and thus tends to smear down most things in its environment. The following characteristic phenomena occur in the moist magnetite concentrate; conduction, galvanic corrosion, self potential and it acts abrasively. When looking at the moist filter cake, one can add seasonal change of the salinity of the process water (as well as the moisture abundant in the MUT.)

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Summary of LKABs Earlier Tested Measurement Techniques

Throughout the years many methods of measuring moisture content have been tested [3], the currently used measurement technique is the manual weigh-dry-weigh test, which provides an accurate result. This process is time consuming, why LKAB would wish to have an in-line and real-time measurement technique. Tested methods which are not related to the measurement technique we try to introduce will be mentioned. Methods related to our measurement technique will be deeper discussed with emphasize on their implications for our measurement technique. Unrelated Techniques Tested First the weigh-dry-weigh method has been the target for development and refinement, but still this method suffers from difference in sample collection, heating may induce chemical reactions changing mass relations, the method is time consuming and does not allow in-line or real-time measurements. Different general commercial moisture measurements units have been tested without any stable results, mainly due to the complex nature of the moist magnetite concentrate. Chemical analysis of moisture dependence of chemical reactions resulting in a pressure proportional to the moisture contents has been tested; the pitfall of this test seems to have been its minor sample volume.

Multivariate analysis has been tested; but has been considered in minor further interest to this project. The problems with the technique are the stability of the method when it is exerted to external disturbance and that it is a system that needs training by estimating moisture from pre-known moisture samples. Radiometric measurement technique has been tested where the observation only could be done for long term variation over the period of a day. Therefore has been considered being a non sufficient measurement technique. Related Techniques Tested Within the microwave area, an instrument called Hydro-Probe II has been tested, by submersing it into the moist magnetite concentrate. The general opinion then was that the equipment did not work as the moist magnetite concentrate was absorbing around 90 % of the signal. The signal used was 300 MHz to 1.2 GHz, either this experiment shows that the commercial techniques for moisture measurement does not work for moist magnetite concentrate, due to its complex nature (if the instrument was not developed having the complex nature in mind) or it shows that EM waves has trouble of penetrating the MUT, especially in the microwave range. At a seminar of moisture measurements with microwaves in subject [3] it was stated that microwaves could not be used as a measurement technique as moist magnetite concentrate absorbs the microwaves. Also commercial companies have stated that this is the case, that microwaves cannot be used as measurement technique due to the major absorption of signal power. Measurements of optical reflection have been tested. Optical techniques in general require massive maintenance, calibration and are very sensitive to external disturbance. Only if a method can find some frequency where all disturbances are extremely low compared to the response of the variable representing the moisture content this method has usability. Electric conductivity has been investigated as an interesting method, by measuring the conductivity between two electrodes; one could determine the moisture content. In the process industry this method is not believed to be of sufficient stability due to the many parameters from which the moisture measurement depends on. The measurement depends on the grain size, process water salinity, moist magnetite concentrate temperature, geometry, compression and moisture content. Another experiment confirms that the resistivity is heavily dependent of moisture content [4]. Resistivity is the reciprocal of conductivity. Short on the Apparent Demands of the Measurement Equipment When analyzing earlier evaluated measurements it is apparent that Accuracy - The accuracy should be around 0.1% Tolerant - The measurement should be stable towards environmental changes / process disturbance Instant - Preferred to be real-time measurements Independent - Should have minimal maintenance Representative - Propose a value representing a whole batch

These are quite tough demands under the circumstances for in-line measurements. However the method presented in this master thesis is believed to cope with them. Untested Techniques and Our Role in the Continuation From studies of earlier tested techniques it obvious that one will need to utilize a multivariable solution as all methods suffer from other environmental effects. The author 5

believes that either submerged measurements with sample contact will have the most controllable and/or measurable environment or a macro sized capacitance and/or inductance and/or resistivity measurement module. Examples of non tested methods (2005) are heat conduction, density, measurements with ultrasound and infrasound, pressure posed to static obstacles, nucleus spin resonance (Proposed by the company Omicron) and other chemical or heating related methods. There are also many untried measurement techniques related to electromagnetic and/or frequency spectra measurement. These methods are mentioned as radio waves (transmission), dielectric property measurements, electromagnetic AC measurements, inductive methods, capacitive methods; at this point it seem a bit messy as all these seems to be different parts of the same kind of measurement technique, just that they are mathematically- and model-wise separated. Some short conclusions when it comes to electromagnetic measurements. One has tested transmission of microwaves submerged, optical surface reflections of microwaves (outside media) and electrical resistivity measurements submerged. Where the transmission and optical reflection techniques has been discarded due to lack of quality. The resistivity has shown to be sensitive to moisture content, but faces uncertainties due to large number of dependent parameters. The method proposed by T. Lfqvist and C. Karlsson is to utilize a model which measures the AC spectra of capacitive, inductive and conductive behavior of the moist magnetite concentrate. By large means it is reasonable to believe that a commercial product must also be able to measure the temperature and resistivity of process water and dry magnetite or utilize some kind of calibration at least month wise. At first the ambition would be to prove the legality of this method. A big strength is that this method utilizes many parameters which by themselves are moisture dependent. If one could determine these parameters, there would be many parameters to use in moisture estimation. Only one of the parameters is sensitive for all constituents, that is capacitance and one parameter is sensitive for the magnetite that is inductance, the actual material dependent variables are the electric permittivity (dielectric constant) and magnetic permeability (magnetization constant). Together these two will allow us to determine the amount of magnetic particles (magnetite grains) from air and water, with that as input we can determine the amount of particles with higher dielectric constant from those that have less. That is water from air that in the end allows us to estimate the water content. This estimation is done using a two phase mixing formula causing an input to a three phase mixing formula, allowing the water content to be determined. Another interesting property we might find from knowing the permeability is the dry density or mass volume of a moist powder.

2.5

Other Research Groups

A book containing an overview of theory and techniques in the field of E-M aquametry have been written by K. Kupfer at BUW [5]. One co-writer of the book is A. Sihvola at HUT whose research is focused to the area of material characterization of matter with high dielectric loss. An Italian group involved in planetary research and sub soil measurements has performed measurements with a toroidal probe. This was a step in the direction of building an instrument intended for a mission to Mars to perform moisture / ice content measurements in Martian soil. The Martian soil connects with our experiments due to its rich iron content. 6

There are also many other people around the world which has brought contributions to and been working on the problems of moisture measurements, as well as measuring other material properties using the electromagnetic properties. Short information of A. Sihvolas Work and Concerning M-G and B A. Sihvola has been working with aquametry [6; 7], with the main target of building model systems for material with high dielectric losses. In his work he has studied the geometry effects of host and inclusions, where the host is the main constituent and inclusions are secondary constituents. Mainly it is the formulas by M-G and B, which have resulted in more knowledge for the effects in using mixing formulas. He is the author of the book, Electromagnetic Mixing Formulas and Applications [7]. A. Sihvola together with L. Jylh has also developed a differential formula for effective permittivity [8] which combines the effects of the M-G and B [7] formulas, thus they have achieved a formula that are valid for quite high permittivity contrasts which seems to be the case of these measurements. Initially the ambition will be to prove the electric behavior of the measurement equipment. Short Information on the Work Performed by the Italian Group The group consists of many members of different disciplines; astrophysics, electronics, geology, computer and system engineering. They have been working with several techniques to discover the E-M parameters of the sand of Mars, as SDSP, GPR and TDEM. The reason why they use the many techniques is that the environment at Mars is varied and they have no knowledge of any parameter in advance. On earth one knows some parameters and can calibrate for them in calculations.

2.6

Possible Measurement Techniques

Studies were performed on summarizing documents and articles evaluating different instruments; Venkatesh and Raghavan (2005) [9], the NIST standard document [10] by Baker-Jarvis et al. (2005) and the two ASTM standard documents D 7449 (2008) [11] and D 5568 (2009) [12]. The NIST document is the most valuable of the documents. Literature studies and discussions have come up with a few different ideas to setups using capacitance and inductance to determine the E-M constants. The different methods are based on reflection measurements or reflection-transmission measurements. The reflection methods will be discussed further in subchapters to identify problems or advantages of each method, using facts from article studies. Reflection Measurements Open-ended coaxial measurements Toroidal probe Open and closed coaxial cell Micro-strip sensor Reflection-Transmission Measurements 2-port coaxial cell 2-port transformer Earlier unsuccessful experiments on plate capacitors, N. rlander, and a technique developed in an earlier report by A. Saremi, a version of reflection measurements of an inductive 7

(closed) / capacitive (open) coaxial cell. This open/closed technique will be further developed by the author later in this master thesis. Open-Ended Coaxial Measurements This measurement technique is based on the change of fringing field capacitance due to change of material measured, in example compared to air. The simplest interpretation is this by Jaspard and Nadi [13], in equation 2.2. First the interpretation of measurement as admittance, in equation 2.1: (2.1) Where Y11 [1/ or S] correspond to the admittance of the system using only one port of the VNA. Y0 [1/ or S], is the characteristic admittance of the VNA cable, in our case (1/50) S . The S11 parameter is a scattering parameter which says something of the reflection caused in the macroscopic measurement equipment. The indexes in all cases refer to the first element of a matrix, where the index represents a port number; in this case only port one. Thus looking at the admittance due to the reflection of a pulse sent at port one, observed at port one. (2.2) G [1/ or S] is the conductance (inverted impedance) due to leak currents between the center conductor and the outer cylinder. The angular frequency [rad/s], Cfc [F] capacitance regarding the full length of coaxial cable, from the VNA cable connector to the cut surface used as sensor and Cfm [F] being the full material dependent fringing field capacitance. Simulations in Comsol have not been able to confirm the validity of these, which could have been caused by bad conditions for boundary values in the simulation or that the model is insufficient. Most probably this is due to adaptations of the model, which has not been implemented, dependency of other geometrical factors. There is also a more advanced model for determining the complex r, described in the book Microwave Electronics: Measurement and Materials Characterization [14]. Even though the title of the book refers to microwaves, this is somewhat applicable for RF as well. This technique / theory might be needed for the construction of a surface sensor for the measurement module, but probably cannot be used to characterize the material properties in our case, as the response of the fringing field capacitance should be quite small and it will only measure the capacitive property within the measured volume. This was realized from Comsol FEM simulations and reading articles. Also from simulations and articles it seems to be most sensitive at the core, where current are injected and there are a certain area of the flange shield which gives optimal fringing field response. Also letting the core penetrate deeper and letting the flange stay at the surface may have a good impact on the fringing field capacitance. Important contributions to this area which the author has studied follows; Zheng and Smith (1991) [15], Moreau and Aziz (1993) [16], Gasvenor (1993) [17], Baker-Jarvis (1994) [18], Aimoto and Matsumoto (1996) [19], Folger and Tjomsland (1996) [20], Jaspard and Nadi (2001) [13], Hagl et al (2003) [21], Cheng et al. (2006) [22], Ellison and Moreau (2006,2008) [23; 24], MacLaughlin and Robertsson (2007) [25] and Oppel et al (2008) [26].

Toroidal Probe As described above this has been tested earlier by an Italian group. The toroidal probe seems to be a good measurement technique, but the trick is to get the material into the toroid. The solution of the Italian group is to use an air winded toroid, which would allow the toroid to be pressed down into the moist magnetite concentrate. Then the toroid is filled with moist magnetite concentrate and as the inductance is only dependent of the material characteristics of the material inside the toroid windings, it is easy to determine the measured volume. The group used a constant volume of Martian soil and the sensitivity should be really good due to the concentrated fields. This geometry may be a good geometry for the magnetic sensor to be used for in-line measurements. No experiments, modeling or deeper literature studies have been done yet, on this method. Open and Closed Coaxial Cell An earlier report by A. Saremi [27] has been written on the coaxial cell, but some of the modeling is questionable. Some new measurements, analysis and simulations will bring further light on the subject. The general overview sources contained the best written material found for this measurement technique, as well as previous measurements performed at EISLAB [27] and newly acquired knowledge from new measurements and modeling. See chapter 5 for further information. Micro-Strip Sensor A micro-strip sensor is believed to be one of the sensors to be used for an in-line solution. Together with the magnetic toroid / loop / transformer it would constitute a full laboratory solution for the measurement of r and r. The drawback associated with this type of sensor is its surface sensitivity and that it will not represent a whole batch properly. To solve these issues, one solution could be to have a lot of measurement units well distributed and submersed in the moist magnetite concentrate. This would allow a mean value representation of the moist magnetite concentrate moisture content and decrease the risk of moist concentrate surface anomalies. Interesting articles discussing this type of sensor are published by Avitabile et al. (2001) [28], interdigital dielectrometry by Guggenberg and Zaretsky (1995) [29] and Sonnet Application Note, SAN-206A (2006) [30], for design of RFID sensors. RFID sensors are probably useful sensors to use for material measurements in the radio frequency spectra, even though the measurement in itself has nothing to do with RFID.

2.7

Suitable Setups for Magnetic and Conductive Materials

When determining moisture in magnetic and conductive media, it is important to use both inductive and capacitive technique. For the material characterization it seems to be suitable to use the open and closed coaxial cell. This will allow measurement of a constant volume, which will simplify the verification of the measurement. When measuring in-line, the pair of a micro-strip sensor (mainly capacitive) and a magnetic sensor (mainly inductive) will probably constitute the laboratory measurement setup.

2.8

Electric Equivalent Models

There are two types of electrical equivalent models which can be used to model a transmission line [1]. It is the lumped parameter model and the distributed parameter model. In this sense we either see the transmission line as a RLC circuit or that the element is made 9

up of infinitesimal elements of RLC circuits. The modeling which has been performed on the coaxial cell is of the lumped parameter type. When it comes to distributed parameters, there is a common model for the impedance of an element of a transmission line [1] (characteristic impedance). There is a special formula to relate the characteristic impedance to the impedance seen by a VNA, through different segments of different lengths for lossy lines. A schematic sketch in Figure 4 describe the different variables in equation 2.3.

Figure 4: Schematic picture of linking coaxial elements, licensed use under CCPL (CC BY-SA 3.0) by WikiUN Qianchq [30; 31].

(2.3)

(2.4) Here the Zi+1 [] the complex impedance at any point on the line, looking towards the load. The Zi [] are the complex impedance at the distance li [m] towards the load. Z0,i [] the characteristic impedance of the coaxial line, linking point (i+1) with (i). i [1/m] is the propagation constant (segment i), i [dB/m] the attenuation constant (segment i) and i [rad/m] the phase constant (segment i). The expressions for matched, short and open refers to special conditions regarding the impedance of the load, where one can see the impedance at Z2 by using Z0 = Z0,1 and = 1. However in our case using the coaxial cell, the aluminum bottom will not be represented by the short condition as resistance and inductance exists. Using the plastic lid we might be able to use the condition, open, provided that one consider that the plastic lid constitute another coaxial element and the fringing field capacitance are small enough. The fringing field capacitance is the capacitance due to the escaping field in the open or semi-open case. The continued work within this master thesis will be with the lumped parameter model. Lumped parameter models for two conductor transmission lines can be modeled in three different ways according to literature; L-type, T-type and PI-Type [1] p.477 and 533. The variation of these makes it plausible that other combinations of the components could be used as well. The lumped parameter model proposed by A. Saremi is another one [27], see chapter 5.3.

10

3
3.1

LAB WORK AND MEASUREMENTS

Preparation of Moist Magnetite Concentrate Samples

Purpose The sample preparation of moist magnetite concentrate was performed in the laboratory of the TKG department. The samples will provide both a basis for calibration and test. For full liability these measurements should be repeated a few times with newly prepared moisture samples. Equipment The equipment used was 9 plastic buckets with lid, scale, an industrial mixer (depicted in Figure 5), measuring cylinder, de-ionized water and bags with dry magnetite concentrate. Execution Weighing empty bucket with lid, weighing half-filled bucket with lid and calculating the amount of dry magnetite and the amount of water that should be added to give each moistened sample its right moisture content 0, 2, 4, 6, 7, 8, 9, 10, 11 mass percent. Due to inaccuracy of the amount of water added to the samples (equation 3.1), also actual percentage has been calculated (equation 3.2). (3.1)

(3.2) Where mm is the mass of magnetite, mw is the mass of water, fw is the mass fraction of water and the mass fraction of magnetite are of course fm=1-fw.

Figure 5: Industrial mixer, photo by T. Lfqvist

11

Results and Conclusions The resulting moisture contents deviates quite a bit from the intended, thus using separate buckets measuring dry magnetite and water, will make the percentage more precise and constitute a better testing frame. The actual moisture contents are presented in the table in Figure 6 below.
Moisture %m Real %m 2 2,044 4 3,054 6 6,061 7 7,278 8 8,311 9 9,373 10 10,43 11 11,44
Figure 6: Table of ideal moisture content and actual moisture content.

3.2

Resistivity (DC)

Purpose The purpose of determining resistivity was to model parasitic resistance in the model of the impedance for calculation of permittivity / permeability dependence. Equipment The setup (depicted in Figure 7) consisted of a cylindrical plastic pipe with a circular plate in the bottom and a height adjustable circular plate in the top. Both plates connected to wires. The measurement apparatus were a regular resistance measurement unit and a fine tunable DC voltage measurement unit with programmable current.

12

Execution

Figure 7: In the back there is a white bucket with moist sample of magnetite concentrate. In the front there is a resistivity measurement setup, consisting of a plastic pipe, with outside covered in aluminium foil. In the bottom of the pipe, there is a circular copper surface. The surface constituting an electrode connected to a wire exiting the bottom of the setup. A similar circular surface can be thread into the pipe from above, thus connecting through the sample put in beforehand to the surface in the bottom and finally constitute a connected system. One can do measurements between the two cables exiting the setup. The wooden plate in the bottom is for stability of measurement setup. To the left, an abandoned measurement device, a general resistance meter.

The measurement equipment was connected to the wires of the measurement apparatus. First DC Resistance was measured with a resistance meter, it was noticed that the DC resistance was changing rapidly, this seemed strange. Second voltage was measured with the same equipment and no voltage source attached, still the measure equipment showed a voltage across the plates. Decision to use constant current measurement equipment instead was made, and then one could make measurements of voltage for positive and negative current. Followed by calculation of resistance and taking the mean value of them to find the most accurate resistance. For each sample measurement, also the height of the cylindrical bulk mass sample was noted. The resistance was then converted to resistivity and conductivity by a geometric dependence [1] p.166 using equation 3.3. A schematic picture in Figure 8 depicts the different variables. (3.3)

13

Figure 8: Schematic picture illustrating the geometric dependence of the resistivity measurement setup, licensed use under CCPL by WikiUN Omegatron [30].

Where [m] is the resistivity, R [] the resistance measured on the sample length l [m] and using electrodes of area A [m2]. Results and Conclusions The measurement data and results can be found in appendix C and results in the following figure, Figure 9. The effect of generating a voltage, suggested to be self potential, is very interesting and will certainly affect electrical measurements on the moist magnetite concentrate. At least for DC measurements and could be another interesting phenomenon of study further for other reasons or maybe for measurement of moisture with DC levels. This is a problem which mainly occurs during DC measurements, should not interfere too much in the AC model. Analysis of the measured data show that resistivity is approximately reversely proportional to the moisture content expressed as a fraction, at least within the interval 0-12 % moisture. Only doubts would be around 2-4 %, but as our area of interest is mainly around 8 % the results can be considered sufficient. The bad results around 2-4 % could also somehow be related to the measurements, as the voltage was fluctuating. The recording of values was done when the fluctuations slowed down a bit. One could issue that it should be done after a certain time, but satisfactory results could be presented with the current method.

14

Figure 9: DC resistivity versus actual moisture content. The red arrow indicates that the value at zero percent moisture, most probably can be considered infinite, as the measurement equipment reached its limit. The actual characteristic is believed to be of the type one over fraction, according to this diagram though, from two percent to eleven percent an almost linear behaviour. The measurements have been performed in a laboratory environment where the temperature has been at room temperature and the packing density of the MUT has been as low as possible but still so that the amount of macroscopic air pockets are at a minimum. Measuring higher moisture percentage gets more troublesome as air pockets are unavoidable due to the agglomeration process. Despite this effect it is obvious from the measurement data that the conductivity is very high, around 10 % moisture. The measurement of dry magnetite concentrate gave the same voltage value as it did when the two electrodes were in free space. This indicates that if moisture content goes towards zero, the resistivity goes toward infinity. This implies that there are two models needed to model each setup of equipment one with parasitic resistance and one without, if it is not possible to use a combined model which satisfies both cases.

3.3

Permittivity, Permeability and Parasitic Resistance (AC)

Purpose By determining the E-M properties of the moist magnetite concentrate it is possible to determine moisture content through the mixing formulas Maxwell-Garnett and Bruggeman. Thus this measurement is the core of this project to accurately determine the E-M properties. For accuracy it is also very important that we understand the effects in the MUT and the measurement cell. Which covers the most of the time spent in this master thesis work. The first objective is to measure the complex and frequency dependent S11 parameters. From there one can calculate the E-M properties.

15

Equipment Equipment used was a VNA and the measurements cell, depicted in Figure 10. The measurement cell drawing, dimensions and more pictures are to be found in appendix A. The measurement cell can be used in two setups, inductive (for magnetic properties) using metallic bottom and capacitive (for electric properties) using plastic bottom. Thus we end up with two equations and two unknowns for each measurement. The cables to the VNA were 50 cables.

Figure 10: Measurement setup with coaxial cell and VNA. The coaxial cell is connected only through one VNA port. The wooden box contains a calibration set for calibration of the VNA.

Execution Scripts for GPIB communication were used to make ten measurements for each sample, and a statistical analysis is possible to determine the variance and other statistical measures, when a satisfactory model has been found. The script acquires the frequency used and the complex S11 parameters from the VNA as a matrix of the size of frequency times ten. The matrices are stored in Matlab files (.mat). The S11 parameter could be translated to the impedance seen at the connection between 50 VNA cable and the connector-lid system of the measurement cell. According to equation 3.4 below: (3.4) Zeq is the impedance seen by the VNA and correspondingly the impedance matched with the equivalent circuit discussed in chapter 5, at the time of publishing believed to be best described by the model proposed by C. Karlsson. represents the reflection coefficient [1] 16

p.442. In our case Z0 is 50 (characteristic impedance of VNA cable) and reflection is equal to the S11 scattering parameter (one VNA port measurement). Measurements were done on various moisture contents 0 %, 2 %, 6 %, 7 %, 8 %, 9 %, 10 % and 11 %. Where the intervals are shorter around 8 % to give better accuracy at the interval where it is intended to determine the moisture content in the end. Data from moistening process could be found in appendix B. Some measurements have been done on regular water, de-ionized water and air. Results, Modifications and Conclusions The values from initial measurements on air had a low correlation with model values; this was believed to be caused by the VNA, that it measures impedance best around 50 . Then air measurements are supposed to be badly represented by measurement data. By physical means, this was believed to be caused by lack of parasitic current (associated to the parasitic resistance). For example, air has very low conductivity, as well as it causes a rather low inductance, compared to water of a factor of approximately 80. These conditions would result in a loss of the parasitic resistance in the model by A. Saremi as the resistance gets very high and thereby can be neglected. This case also occurs when measuring de-ionized water or dry magnetite concentrate, which also has a high resistivity (low conductivity). Later analysis has disproved this idea, the bad correlation were probably caused by bad data treatment and/or insufficient modeling. For further analysis, see chapter 5.5. Some modifications to the measurement device have been done. The connection between connector and center rod was first a coiled spring, as it was feared that this spring somehow would affect the impedance behavior of the circuit, it was replaced by a needle-hole connection, where the needle has a bow of feather material to tighten the connection (commercial component). It seem like the effects on the impedance was minor, but the connection between the conductors was greatly enhanced, which allows measurements to be performed with ease. Also the center rod has been polished. Measurements on samples of moist magnetite concentrate clearly show that the system cannot only be modeled by an inductance or a capacitance alone. In the case with metal bottom (inductive), first we will assume that all current goes through the conductor and therefore the capacitance is not part of the model. Then if there is no capacitance behavior, it is clear that the interaction between the leak current associated with the parasitic resistance and the current that passes through the material dependent inductor interact to form a non-linear inductive behavior. This will be discussed further in the discussion of chapter 5, Calculation and Electrical Modeling. New model proposes that there should be capacitance in the inductive model as well. The first peak of the curves is probably the peak of the quarter wave resonance, which has a decreasing frequency and magnitude, for increasing moisture content. In the imaginary inductive case (Figure 12) the quarter wave resonance is more dominant than the other effects and hence the nice asymptote. There is some confusion of the curve corresponding to 6 and 7 % in all graphs. The effects in the capacitive setup are still not identified, but are believed to follow the theory as strictly as the inductive case.

17

Figure 11: Real part impedance spectra for inductive setup translated from the measured S11 parameters.

Figure 12: Imaginary part impedance spectra for inductive setup determined from the measured S11 parameters.

18

Figure 13: Real part impedance spectra for capacitive setup determined from the measured S11 parameters.

Figure 14: Imaginary part impedance spectra for capacitive setup determined from the measured S11 parameters.

19

WHY COMSOL MODELING

To get a greater understanding of capacitance and inductance contributions, as well as having a geometrical view of the fields allows us to develop better instruments or make our equivalent models better. The equivalent models might need correction from fringing field effects resonance phenomenon or similar. Several Comsol models have been developed, some models of the inductive and capacitive setup. A few versions of microstrip capacitive sensors have been evaluated. There has been no breakthrough with any sensor so far, but one can see that the fringing field capacitance of the capacitive coaxial set up should be negligible, if the surrounding media are air. This depends on the length of the coaxial cell, combined with the spread and extended field in the media air (outside the coaxial cell), which has a fairly lower permittivity than does the magnetite concentrate and water. If one would immerse it into the moist magnetite concentrate this would probably not be the case, concerning open ended probing.

4.1

Coaxial Cell Inductive and Capacitive Setup

A graphical representation of the coaxial cell presented in Figure 15 below:

Figure 15: Cross-Section of coaxial cell.

For the inductive cell in Figure 16, we can see that the electric field is strongest along the strictly coaxial part; the measurement cell excluded the lid and bottom. The electric field weakens when approaching the edges of the coaxial cell. The edges in this case are the inductive short (metal bottom) and the lid with connection to coaxial cable and eventually the VNA. Especially magneto static or quasi static simulation of this setup could be of further value to understand such things as end effects. The end effects observed, means that the capacitance calculated in the inductive case according to the latest equivalent model would be slightly larger than the actual one. For the capacitive setup in Figure 17 the capacitance of the last part, the coaxial segment where the plastic lid constitute dielectric will have an increased capacitance in reality. First due to the fringing field effects and second due to the plastic layer attached outside the cylinder (part of the plastic bottom) which further will increase effects of the fringing field. Due to the length 20

of the coaxial part we will assume that the irregularities are negligible. Thus we will neglect fringing field effects and loss of capacitance due to the inductive short. Later these effects might need more study, when one considers more accuracy and sensitivity for measurements.

Figure 16: 3D Model of Inductive Coaxial Cell.

Figure 17: 3D Model of Capacitive Coaxial Cell.

21

In Figure 17 the outer discs (blue), tell that there is no electric potential outside the measurement cell (as expected). The dotted lines (red) show the electric field and the arrows, pointy structure (red), show the orientation of the field inside the cylinder. The internal disk, rainbow colored, shows the magnitude of the electric potential. At this point the models does not offer more than further geometrical understanding of the problem, the models must be more sophisticated to give more information. The further need off modeling will rather be towards the in-line measuring sensors, than on the coaxial probe.

4.2

Capacitive Surface Sensors

Some different surface sensor geometries have been simulated, offering some insight to the distribution of electric field and electric energy density. The geometries simulated are of a 2D symmetrical one, that means that the view should be rotated 360 around the left edge or r=0. After this the sensor becomes somewhat of a circular disc.

Figure 18: Geometry of Capsense1.

Figure 19: Graphical E-Field Representation of Capsense1.

During these simulations it was discovered that long grounding planes will enhance the sensitivity of the sensor, an approximate of twice the diameter of the centre electrode seems to be a good dimension. In the picture above there are two smaller rings as grounding plane, this is not efficient. Instead if one could use the second ring as a guard, meaning putting the same voltage as to the centre electrode, but without direct connection. Thus the electric fields that generate the capacitance will not bulge at the ends. This will give a more centre aligned field.

22

Figure 20: Graphical E-Field Representation of Capsense2.

Another thing to address could be the length of the electric field lines; it is generally known that capacitance is proportional to electrode area and reversely proportional to the distance between the electrode areas. What this really means is that the distance between the electrode areas causes the field lines to travel a further distance before decoupling in ground. Thus short field lines are field lines with a great impact on capacitance. If one sticks with the surface sensor, one would like to have a maximal area of the centre electrode, because this is where the sensitivity is at its highest. A maximal area would be achieved by a sphere, where one could experiment with different radius. When area are increased one will need higher power to maintain the energy density, as the current are more spread out on the surface. The authors recommendation is to use some kind of parallel or semi parallel electrode solution, this to maximize the capacitance measurability and thereby accuracy of measurements. One possibility would be to use geometry similar to an old thread roll or timeglass with an extended waist, thus one might avoid problems with the moist magnetite concentrate not entering the cavity of measurements. This kind of geometry would belong with the parallel plate type, be of cylindrical symmetry and possibly have conical plates. The plates would also have a hole in the middle to allow cables to the outer electrode.

23

Figure 21: Graphical E-Field Representation of Capsense3.

Another interesting thing was discovered, maybe not too surprising, when using multiple circles with increasing radius. Fed with the same feed (voltage), it has a superposition effect (Figure 22). This means it has a very good electric energy density; however the capacitive system also becomes very complex. If one would utilize this system one would need some advanced algorithm calculating the capacitance seen by each electrode ring, thus using the different capacitances for as good value as possible.

Figure 22: Graphical E-Field Representation of Capsense4.

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5
5.1

CALCULATIONS AND ELECTRIC MODELING

Evaluation of Models and Motivation for Chosen Model

The first electrically equivalent models investigated consist of two parts, the first part are the correction part for correction between the coaxial theory (the material dependent part) and the VNA. The second and most important part is the coaxial theory determined part [1]. The coaxial part is the part which allows extraction of the E-M material characteristics. The first part of the circuit analysis has been inspired by A. Saremis work. The latest models consist of the material dependent part and the modeling of the bottom part; it seems that any resistance or inductance of the lid causes no larger effects of overall impedance. In the end it could off course affect the accuracy of the E-M parameters; this is a question for the accuracy analysis once the method has been verified in general. The behavior of these E-M characteristics is not known, thus to generally validate the model it is necessary to first of all well know the different characteristics and the models counterpart, the parameters. If modeling is not fully correct these extracted E-M parameters will be wrong. This however does not imply that the moisture content from mixing formulas would be wrong, as the E-M properties are determined the same way for all measurements, the relation between composite parameter (containing different properties) still could cause accurate results for moisture. The formulas are valid for different parameters, why not a composite parameter, but this would require further investigation. However the main idea still is to try to find the actual E-M parameters, as these might also be useful for other purposes. First of all, one can analyze the impedance of the whole setup, to see which characteristics there are. It is also important to keep correct physical measures of the device in equations; even though one might have better equation correlation with slight offset, otherwise the model may compensate for formula errors and thereby give wrong answers. This when considering accurate determination of the individual E-M parameters. To characterize the connector-lid system (VNA-coaxial cell) we can measure the short circuited simple system, namely lid and bottom connected. However this cannot directly be used as a modeling correction for the connector-lid system as there are also the characteristics of the bottom included. Here we need to separate the effects of the connector-lid and bottom system. Also it is important to notice that the areas of these surface current spread on the bottom will be different connecting directly to the lid instead of through the coaxial cylindrical part, the area is bigger for the latter. Due to area dependence of the surface current, the parameters Rc and Lc cannot be directly split into lid and bottom, without knowing anything about the area dependence. Theoretical studies of the bottom phenomena was not been successful using the Saremi circuit, it is also suggested that this bottom dependence as part of the single-loop coil would be material dependent. If so, this would cause a dependence of frequency and moisture. It would certainly be good to find such a theoretical dependence; probably one can see the effects of the surface current stream of this connection between the middle conductor and the bottom as end effects when a conducting rod is connected to a circular disc.

25

The newest idea is to determine the geometrical dependence from measurements on water and air, then modeling the inductance as rLG. If that is valid our problem simplifies. Similar calibrations have been done by others for similar setups. When choosing an equivalent circuit for moisture determination; it is necessary to combine the behavior of leakage (G or Rp) with the material dependent inductive behavior. Later it has been understood that also the capacitance of the coaxial part must be a part of the circuit as well as the bottom impedance. The Parameters of Equivalent Circuits for Coaxial Cell For any two conductor transmission line one can represent the impedance by a lumped parameter model where the parameters are calculated according to equations 5.1 to 5.4. Where skin resistance, Rs [], inductance, L [H] (most models) / LM [H] (latest models), conductance, G [S or 1/], and capacitance C [F] (most models) / CM [F] (latest models). These parameters however are dependent of the transmission line geometry; hence for coaxial elements they are as follows [1] (geometrical properties can be found in appendix A):

(5.1)

(5.2)

(5.3)

(5.4) These parameters were also derived by A. Saremi in [27]. [F/m] is the permittivity, [H/m] is the permeability, [1/(m)] is the conductivity, a [m] is the core conductor radius, b [m] the inner radius of the cylinder wall, [rad/s] the angular frequency and l [m] is the length of the cylindrical symmetric coaxial segment. The subscripts c and d stands for conductor and dielectric respectively. Other parameters are described along with the corresponding models and their development. In the latest model the bottom resistance, R [], is calculated using the skin-depth, [m], by: (5.5)

(5.6)

26

Where [Hz] is the frequency and the other variables are the same as described for the equation above. If one uses LC resonance theory to model the bottom impedance, the theoretical skinresistance of the bottom needs an adjustment multiplying with a coefficient to get the right magnitude for the damping of resonances. The bottom inductance might be modeled as follows in equation 5.7: (5.7) Where [H] is the geometrically dependent inductance and can be determined for the case when the coaxial cell is empty, containing air or preferably vacuum, we can find the parameter inductance of the bottom based on multiplying with the magnetic permeability. L-type Circuit

Figure 23: L-type equivalent circuit with correction equivalent.

In the L-type equivalent circuit in Figure 23 it is easy to see that if we short-circuit the capacitor the leakage would be short-circuited as well, thus we would get a purely inductive behavior. One should be aware that the characteristics of the material properties also might interfere with our model, why it is important to model by care and keep addressing the pitfalls of this problem. Minding this, this model does not seem to be the one we are looking for. T-type Circuit

Figure 24: T-type equivalent circuit with correction equivalent.

If the capacitor is shorted here in Figure 24, the same happen, except the skin resistance and inductance will be halved. Again this will result in a circuit with only resistance and inductance. Another way of seeing this case would be to accept C here and realize that the impedance could also be affected by a capacitance along the coaxial even if it is shorted by the end. However as the model does not take the opening capacitance into account, so that 27

something can be short-circuited, after all it seems to be a bad model. Keeping these ideas in mind, continue with the next type of model PI-type circuit in Figure 25. PI-type Circuit

Figure 25: PI-type equivalent circuit with correction equivalent.

Here the leakage and capacitance divided in two halves, and then if the right capacitor is short-circuited the effect of half of the capacitance and leakage (G or Rp) will stay in the model. When starting this analysis one should be aware that this is a step in the direction of making a semi-lumped semi-distributed model. Because if one appreciate the fact that capacitance is split in two, it could as well be split in more parts. A distributed model is built by infinitesimal elements of these equivalent circuits, preferably by the L-type. Somewhere between the two models we will have a number of lumped models where each parameter value is divided by the number of the lumped models used, and then we can only short circuit the last capacitor. The parameters otherwise has the same properties as when only one lumped model is used. This type of modeling maybe would better reflect the behavior of the measurement cell. When this interpretation is used, the mathematical system will become large and bring time consuming analysis. Thus it is a good idea to analyze the system where we completely can ignore the capacitance, but still keep the effects of leakage (G or Rp). Thus we will continue working with the Saremi model when considering optimization, discussed below. If it considered being insufficient for modeling purpose, we will continue with building a semi-lumped semi-distributed equivalent circuit. For ease we will build this system by matrices, so that the increase of the number of lumped models is practically simple. Saremi Circuit

Figure 26: Saremi equivalent circuit with correction equivalent.

This is the model used in the optimization calculation with somewhat of a success (Figure 26). By previous analysis, this model seemed to be the best model to predict the behavior of 28

the measurement cell. If the analysis is not enhanced using a chain of lumped models by matrices. Further analysis and earlier knowledge of model simplification suggest that this model should be replaced by another model. Thus we will make a jump in the modeling and continue working with an expanded L-type model. The semi-lumped semi-distributed model are still of interest, maybe for future analyses. Semi-Lumped Semi-Distributed Circuit System Analysis of such a rather complex system is very time consuming, to simplify the work with the equations and the modeling; it is convenient to choose a matrix approach to the problem. It exist several sets of parameters to relate the output to the input of a two-port circuit system, not to be mixed with the ports of the VNA. In this case we would have seen our system as a two-port system and it will be illustrated in figure 27 below, this if correction parameters for the lid would be used.

Figure 27: Semi-lumped semi-distributed equivalent model with split correction lid and bottom.

For microwaves the S parameters are good as voltage and current values are not well defined. One can transform one two port matrix to another for other parameter such as Z, T or G [31]. New Electrical Model Proposed by Karlsson

Figure 28: Karlsson proposed inductive equivalent circuit with correction equivalent.

When analyzing the complex impedance regarding the effects of the correction parameters Rc and Lc, one could see that subtracting the modeled impedance of the combination of the lid and bottom from any measured impedance did not change the magnitude of impedance by much, thus we neglect these effects at the lid position (first) and instead modeling only the bottom resistance and impedance (last). The bottom skin-resistance is very small, but according to the LC resonance theory it would affect the impedance much, due to damping effects of the LC resonance peak which would occur as a result of the parallel connection between bottom inductance and coaxial capacitance of the coaxial part. 29

In general when considering AC current one would model a conductor as a serially coupled resistance and inductance. Simple analyses done for dry systems, eg no conduction; air, deionized water and dry magnetite concentrate, resulted in the choice of this model, as by theory one could build the actual impedance curves and this was done in Orcad with PSpice. The bottom resistance causes a resonance peak at the real part of impedance as well, more about this analysis in chapter 5.5. New in this model are also that the whole material dependent capacitance is kept, this is the effect of a non ideal system, the inductance and along the coaxial part as well as that of the lid. Also the capacitance is distributed throughout the system and cannot be short-circuited; by an ideal coaxial cell it could neither be short-circuited due to the resistance and inductance of the bottom. Only for a completely ideal conductor case one could totally short the capacitance, but in such a case probably none of the material parameters we are interested in would be present. For the capacitive measurement setup one probably just connects a new segment of coaxial cell to the inductive version without bottom (in model without bottom inductance). Initially the plastic bottom effects will be neglected and left for later analysis of model quality.

Figure 29: C. Karlsson proposed capacitive equivalent circuit with correction equivalent.

General for the two models are that the parasitic resistance vanish for the dry case, corresponding to a case where there are no conductance.

5.2

Improvements in Calculation after A. Saremi Work

A better characterization of the DC behavior of the moist magnetite concentrate was performed; this provides the model with better guesses or values of the parameter Rp, depending on which model are in use and if Rp are considered to be frequency dependent or not. Here it was also discovered that the resistivity of dry magnetite concentrate respond equally to the resistivity of air which can be considered infinite or at least very large. This was shown in the experiment by having same values unconnected as connected to the dry sample. The Saremi circuit optimization modeling was modified to model the magnetic permeability as a complex unit, according to theory, and guessing both the real and imaginary part together with the conductivity presents a more valid characterization of the material. The accuracy of this modeling is highly dependent of the structure and order of segments in the model, the model needs more work to present accurate results. Representation of modeling error is turned into a graphical presentation allowing the error to be viewed as a surface spanned by frequency vector and moisture vector. The data loading is now done from within the folder easily allowing the whole measurement calculation folder to be copied or moved, still executable without any modifications. 30

In the new model proposed by C. Karlsson we bring in capacitance into the inductive model and in general takes full use of the coaxial ac theory. Capacitances also are modeled as a complex frequency dependent vector which will add further unknowns to the problem. However in one way this also simplifies our problem a bit, by using this model we exclude many parts which were not fully correct, as bottom impedance and capacitance of inductive model. Some initial verification that this model is justified will be discussed in chapter 5.5.

5.3

Calculations Using the Saremi Circuit Model - Inductive Setup

Purpose The intention with the calculations performed so far is to perform a material model to describe a spectrum of permeability as separate curves for each moisture sample measured. Also there could be a frequency dependent conductivity; this will together form a magnetic material model for the moist magnetite concentrate. Data The input data to the mathematical model are the frequency dependent and complex S11 parameters (VNA output) from connector lid bottom measurement (correction data). Performing the same type of measurement on the inductive setup for each moisture sample, together with the DC resistivity data this provides the data to be used for material modeling. DC resistivity data based on resistivity from measurements providing guesses for Rp, guesses are the same for each frequency but changes with the moisture content. S11 parameters are early transformed into impedance by equation 3.4. In the modeling case used in this master thesis for this method, even numbered moisture contents from 2 to 10 % are evaluated in the model. This choice has been done to be able to compare the output between the measurements made by A. Saremi (even 0-12%) and those made by C. Karlsson (0, 2, 4, 6, 7, 8, 9, 10 and 11 %). Then our available data are two correction vectors Rc [] and Lc [H] (determined from measurement), both of length omega (2000). A vector of parasitic resistance Rp [] (from measurement in DC and estimated in AC) and a vector Rs [] (theoretical) skin resistance of length omega. The moisture data are represented by a complex value impedance matrix (2000 x 5). Mathematical Tools Calculations are performed in Matlab, full code in appendix G-K. The main mathematical tool used is the optimization function fminsearch [32; 33; 34]. fminsearch minimizes J the value its input function, in this case the mean square error of the model. The input function / cost function is the following: (5.8) The cost function provided with, theta = [re, im, Rp], the guess parameter and other data determined from measurements. Other data span correction resistance, correction inductance, measured impedance and corresponding discrete frequency vector. (5.9) 31

E [] the actual error of the guessed impedance, Zm [] measured impedance and Zhat [] modeled impedance. (5.10) With included impedance model, where Zc [] is correction, Zp [] parasitic and Zm [] measured impedances. The measured impedance also holds some theoretical information, as well as the parasitic impedance which probably also would be determined from measurements, as it is believed to vary with frequency.

(5.11)

The impedances Ztx [] and Znx [], are only substitutions to make the system more easily overview able and manageable.

(5.12)

Here Zeq,real [] and Zeq,imag [], are the real part and the imaginary part of the modeled equivalent impedance. Preparation and Optimization of Material Properties (r, Rp) By equation 3.4 and 5.13 the moisture impedance matrix are transformed into guesses of r, based on the much simpler equivalent circuit of only an inductor, having a complex r resulting in an equivalent impedance according to equation below: (5.13) Then a matrix of size 2000x10, five columns of re [H/m] real permeability and five columns of im [H/m] imaginary permeability is used, value by value together with the corresponding value from matrix of Rp [] 2000 x 5. Once for each frequency the fminsearch evaluates the optimal r and Rp. The error is once again calculated for the optimal values and a surface plot of the error is made, results of the optimized parameters will be presented next.

32

Presentation of the Results

Figure 30: Real r provided by optimization of Saremi model for different water content.

Figure 31: Imaginary r provided by optimization of Saremi model for different water content.

33

Figure 32: Conductivity provided by optimization of Saremi model for different water content.

Figure 33: Error surface representing the impedance error for the optimized Saremi model compared to the measured impedance.

34

Discussion of the Results One can see from the data acquired from the optimization of the material parameters that this optimization suffers from disturbances, most probably from the calculation of the parameters in the optimization function fminsearch. Strange jumps and non-expected discontinuous behaviors occur in the parameter spectra. This is probably an effect of many things. First of all it is believed that the electrical model of the measurement system still is badly characterized, especially the bottom, which could cause these discontinuities. Second the small noise on the parameter curves could be related to function-minimum triangulation and that the number of guesses (or unknowns) makes the system instable. This model turned out to be of insufficient nature, mathematically weak as non deterministic model; we know our system shall be deterministic. A decision to analyze the circuit from a fairly easier point of view, only as a purely inductive component was made, still with frequency and complex behavior, more of this in chapter 5.4. This decision was made after identifying that the estimated r according to this model looks good, compared to the optimized version.

5.4

Simple Model Analyses

The optimization breakdown, due to mathematical insufficiency, instead a more simple study was carried out. Then observation of behaviors can be done, even though the actual magnitudes and numbers will not be applicable in any way. Starting by analyzing the inductive setup as purely inductive, the division of the complex inductance to a full complex number, where the real and imaginary parts switch place due to multiplication by J, that is: (5.14) Remember the definition of r (equation 5.13), so that the parts of Zeq [] (here the impedance of the simple inductive model), will become positive in the impedance equation. Purpose, data and Mathematical Tools The purpose of this analysis is to look for special characteristics of the r curves, which could guide our design of the equivalent circuit model. The data sets are those of measurement 10 and 11, which are those containing samples of moist magnetite concentrate. In general the data are of the same kind as those used in optimization explained in chapter 5.3. The mathematical tool used is Matlab. Calculations, Results and Discussion The impedance was converted to inductance, using equation 5.14, further to r by relations between inductance and r, in equation 5.2. The results of the plots performed on r for different conditions measured are presented below:

35

Figure 34: r provided by simple inductive model for air.

Figure 35: r provided by simple inductive model for water.

36

The air sample measurement provides us with a reasonable r, however there are some deviations for low frequency and a little more on the higher frequency, this indicates that especially the model concerning the reactance are too simple. It is possible to subtract complex impedance from the measured impedance to make this permeability equal to one as was expected. However this information is not enough to determine which components there really are, as they could interact to cause this impedance. If we only know this, one would suggest that it is the adding of lid inductance which causes this increased of r, primarily at high frequencies. The imaginary part is with noise subtracted zero, all according to theory of air having a real characteristic permeability. Still there are some modeling issues to solve. Observing the results from water measurements in Figure 35, a strong resonance appears. From discussions and calculations, one can see that it is caused by the equivalence of the electrical length and the quarter wave length. Recalling the inductive model of Saremi equivalent circuit, where there is no capacitance. Recalling the coaxial theory and if one reanalyzing the equivalent circuit. All parameters except the unknown lid inductance are per unit length parameters, but by using the equivalent circuit with a shorted capacitance we automatically assumes the capacitance not to be a per unit length parameter, which allows us to short it. However the short (or the metal bottom) actually does not affect the impedance of the coaxial model, this depends on the inductance and other impedance elements along the coaxial part. Thus we would have a LC parallel connection at the end of the equivalent circuit, which could have been causing this LC resonance. This phenomenon and its consequences for the measurements will be further investigated in chapter 5.5. Otherwise the real part of r is close to one, as expected, as well as that the imaginary part keeps to zero. If one can assume that the resonance is of the LC type, we could from the resonance frequency of this graph and the theory behind the LC resonance frequency, determine the value of inductance for the bottom. This model is fairly simple, as permeability and permittivity are real. When dealing with complex permeability and permittivity, one could expect more problems, if they also are frequency dependent, the system tends to become more theoretically complex. For the dry magnetite case, we have the same linear / constant basic behavior. Also the resonance which occurs for all dense media, here it seems to be the same frequency for both real and imaginary permeability. Same frequency for resonance should imply approximately the same values of real part and imaginary part. Possibly a leaning real part resonance indicates a frequency dependent real part. The guess based on the permeability of pure magnetite are r=2-3j, which may be bad. This could change when we have made our model more theoretically complex. The resonance frequency decrease by increasing moisture content and separation between real part and imaginary part occurs. The slope of the resonance decreases due to increasing moisture content. Also some more theoretically complex effects are hidden in the graphs. This is subject for more study.

37

Figure 36: r provided by simple inductive model for dry magnetite concentrate.

Figure 37: r provided by simple inductive model for 2% moisture.

38

Figure 38: r provided by simple inductive model for 4% moisture.

Figure 39: r provided by simple inductive model for 6% moisture.

39

Figure 40: r provided by simple inductive model for 7% moisture.

Figure 41: r provided by simple inductive model for 8% moisture.

40

The steep slope of the curve is believed to be the effect of a very low parasitic resistance and could also be affected by changes in relaxation due to increased charge transport. However no valid conclusions can be drawn from these graphs.

5.5

Calculation Using Electric Circuit Proposed by C. Karlsson

Purpose and Data In large the purpose of these calculations is the same as for those with the optimization using the Saremi circuit model. Thus our calculation should first verify the electrical models put up for the measurement cell. For this purpose one will start by analyzing the dry case due to the simplicity, and then further complicate the case until the models are thoroughly understood. When the system is fully known one could start estimating moisture content. Before this one must fully characterize dry cases and also measurements of wet frequency dependent cases, that is regular water and moist magnetite concentrate filtering water (process water), either directly from the mine or laboratory filtered water to make an approximated lab equivalent. At this point it is possible to use measurements of moisture samples of known moisture content, using one or two mixing formulas to determine the properties that would be prescribed by the theory for the moisture samples; if we have too many unknowns we could also use this data to determine parameters not covered by number of equations. For the latter case, however one could only verify the model by estimating moisture contents in new samples. It would be preferred if the model could be completely mathematically proofed. Measurements 10 and 11, was used for this purpose as they are the most complete sets of data existing. Mathematical Tools and Simulation Tools The S11 parameters have been converted to impedance curves in Matlab and then these are compared to the curves plotted by Orcad, when the equivalent circuit was built there. The circuits are designed according to theory from LC resonances. Measured Data For air in the coaxial cell, we find that the resonance is outside of our spectra, but we can see some of the effects of the resonance in the end of our spectra as the imaginary impedance deflect from its otherwise linear behavior. The de-ionized water spectra, as seen before in Figure 43, have a very sharp resonance. While the measurements on dry magnetite concentrate has a slightly more spread resonance.

41

Figure 42: Measured equivalent impedance for air (theoretical value by simple model), Matlab Calculated Impedance Using C. Karlsson Circuit.

Figure 43: Measured equivalent impedance for de-ionized water (mQ).

42

Figure 44: Measured equivalent impedance for dry magnetite concentrate.

43

Orcad Equivalents and Their Spectra

Figure 45: Orcad air equivalent with constant maximum magnitude resistance.

Figure 46: Orcad plot of equivalent impedance for air.

So far using frequency dependent resistors has failed, thus the frequency dependent resistors have been replaced by maximum resistance for each resistor. The resistance is really small

Orcad Real and Imaginary Impedance [ ]

44

and is assumed to have a small impact on our graph. The behavior of the Comsol model looks similar to the measurement data.

Figure 47: Orcad water equivalent with constant maximum magnitude resistance.

Orcad Real ] Imaginary Impedance [ ] [ and Orcad Real and Imaginary Impedance

Frequency [ MHz ]

Figure 48: Orcad plot of equivalent impedance for water.

Same with water graph, we have similar impedance behavior as for our measurement.

45

Matlab Calculated Impedance Using C. Karlsson Circuit The latest models for equivalent circuits have been evaluated in Matlab, for comparison with earlier presented measured data. The following equivalent circuit equation 5.15 has been used; (5.15)

Figure 49: Matlab calculation of the air case.

This impedance graph for our theoretical Matlab model for air (Figure 49) well correlate to the one from Orcad model and less with the simple theoretical model, by comparison with the actual measurement data (Figure 42) one can see a missing deflection (in upper part of spectra) of the theoretical data to correlate with measurement data. This missing deflection might be a sign of missing modeling of lid. The water (mQ) impedance resonance peak (Figure 50) well correspond to measured data, but the basic behavior under the resonance might still badly represent the actual circuit. This data is of course biased as it was used for the modeling; one certainly needs to confirm these resonant elements towards other MUT.

46

Figure 50: Matlab calculation of the water case.

Figure 51: Matlab calculation of the dry case.

The material values for permittivity and permeability for the dry concentrate, is not yet determined, thus for our guesses and for the C. Karlsson model do not have a good correlation or actually none at all (Figure 51). Here more work is needed. Possibly the resonance of the

47

lid will change this behavior or we need to look for other explanations. By pursuing the capacitive models, we might enhance our chance of understanding the system.

5.6

Resonance Analysis

The frequency spectra of impedance from measurements suggests that the measurement catches up some resonances, the resonance phenomena analyzed are the LC - resonance and quarter wavelength resonance. Thus using different models for modeling of LC resonances and theory for quarter wave resonance, the results show that the most likely resonance to occur is the quarter wave resonance. Looking at graphs of LC - resonance models, one can observe that the phenomena observed does not fully explain those observed at the measurement spectra. To overcome these problems with resonances, the most appropriate way, would be to go towards lower frequencies and/or distributed parameter analyses. Another idea would be some redesign, where one would risk stepping into another resonance phenomena. In subchapters each resonance phenomena and its analysis is described in detail. RLC Resonances in Coaxial Cell An approach to the modeling problem is to consider the coaxial cell to be a RLC resonant system. This means that the electrical equivalent circuit of the coaxial cell has parallel and serially connected inductors and capacitors which might cause resonances. The resistance of the circuits damp and broadens the base of the resonance peaks. Generally a simple LC resonator, parallel or serial has a resonant frequency matching equation 5.16 below: (5.16) For more complex systems, one might assume a more complex description of the resonant frequency or as multiple LC resonance contributions to the resonant frequency If one considers the coaxial cell behavior to be approximated by an RLC system, one resonance believed to originate from the bottom and another one suspected to come from the lid connection, the latter has not been modeled yet. Quarter Wave Length Analysis The relationship between the quarter wavelength resonance frequency (fr [Hz]) and the electrical length (l [m]) of the device is as follows: (5.17) It is also recommended to stay with a frequency, so that the below relationship will hold: (5.18) Thus avoid resonances and allow the use of lumped parameter models.

48

When calculating the quarter wavelength for the corresponding resonance frequencies for each medium air and water, one can see that the quarter wavelength almost exactly matches the length of the electrical length of the device. Even though the E-M parameters of the moist magnetite concentrate are not known, one may assume that they are larger than those for less dense matter, such as air or vacuum. There are three roads to pursue; either build smaller sensors for in-line use to "complete" the measurement with the coaxial cell, look further in the spectra towards lower frequency, go on with advanced transmission theory or build smaller coaxial cell to avoid quarter wave length resonances.

49

DISCUSSION OF RESULTS AND FINAL CONCLUSIONS

For the dry cases, the equivalent circuit follows theory. The coaxial part can be modeled using L-type equivalent circuit. The metallic bottom can be modeled as a conductor that is a resistor and inductor in series and the plastic bottom could probably be modeled as another coaxial part with plastic as dielectric, which remains to be proved. Lid effects, seem to be negligible for impedance, but might be necessary if one needs good accuracy. Based on the knowledge of the system for dry models assuming that the resonance phenomena originates from parallel LC connection a model for wet case has been proposed. One for the inductive case and one for the capacitive case, in this sense inductive and capacitive refer to the end load (bottom) of coaxial cell according to above. If one can assume that the inductive air inductance carries all geometrical properties and material dependence r can be multiplied to acquire inductance for bottom for the case of media inside coaxial cell. Then the inductive system is fully described with two unknowns, assumed known resistivity. If the capacitive setup can be modeled as assumed, one would have two equations and two unknowns for each frequency. Thus the system which is proposed will assume resistivity constant in frequency spectra but changing with moisture. For more understanding, please look at chapter 5 where these things are described in more detail. New measurements of resistivity has given a new picture of the DC resistive behavior of the moist magnetite concentrate, the dry magnetite concentrate has an almost infinite resistivity. The more water added the more conductivity and at 11% water the resistivity is very low. Also a strange behavior of self potential was discovered during the measurements. Self potential, a concept known from geophysics, caused by charge separation in clay by transport of charges through the pores of magnetic granular media or flow of mineral rich fluid through the granular media. Otherwise the calculations of r have confirmed the theories on complex r. In-line sensing using this method can be constructed in two ways, one way is to build a segment of the process line as a transmission element and another way is to use small in-line units, using small inline units will probably imply a use of large amount of units. Ensuring a representative value for a batch, where moisture content largely differs. In-line sensing using small immersed sensors will probably consist of two sensors, one sensing magnetic properties and one sensing electric properties. A few electric geometries have been analyzed, but a lot of analysis remains to be done before one can develop a complete in-line sensor.

50

DISCUSSION OF FUTURE WORK

It is possible that the possibility of publishing research result from this master thesis in an article will arise, concerning the measurements of dry samples, meaning samples without conduction. Presenting the measurement method, equivalent modeling and results from measurements. One should analyze the effects of resistivity for AC conditions, if one can use the DC resistivity or if it is frequency dependent. Using other methods as Comsol simulations and PEEC simulations one could compare electrically derived values for different components in the measurement equivalent circuit, mainly the bottom. It would be favorable to have analytic mathematical equations for these values. Research with PEEC modeling is run at LTU under J. Ekman, where a few PhD students working alongside. This PEEC modeling might be interesting as collaborative project, where modeling for the air case could be identified and then maybe one could validate bottom properties. Also this might be an interesting technique to continue working with towards sensor design of in-line sensors. The PEEC project has mainly been working with surrounding air media, however if one could confirm models of air, regularly simple modeling can be adapted to surrounding material property change. How this adaptations works with PEEC modeling is unknown to the author. Measurements of water may improve understanding of the electric model as it has a constant permeability and a frequency dependent permittivity. Determining the process water permittivity is a step towards verification of determined permittivity from moisture samples. When a complete understanding of the dry magnetite E-M properties and of the process water E-M properties have been established, one can prepare comparison data from mixing formulas. Combining determined permeability of dry magnetite and determined permeability of process water in mixing formulas. This should be done for the different actual mass fractions of moisture, using the prepared moisture samples. This produced set of reference data will allow evaluation of the validity for our E-M model. Using a correct resistivity and finely calibrated equipment to eliminate noise, one can have improved measurements of characteristic impedance. Small noise could appear due to the damages inside the measurement cylinder (part of coaxial cell), therefore one might reproduce that cylinder and get it internally polished. One may also again evaluate if some connection with the bottom could cause any noise or contribution, maybe studying the effect of screw thread. For this study one may produce extra coaxial cells without these screw threads, using only frictional connection. Then one can study the effects of geometrical changes and general stability of model, causing changes in impedance. When the measurement equipment is improved, the E-M model fully accepted, one can start to determine the E-M properties of the different moisture samples and compare to the prepared sample comparison data. If the modeling is correct this should match very well. When the E-M properties have been fully justified it can be used as a reference for choice of 51

suitable measurement frequency and provide reference values for this frequency. At this point the project has reached the point of instrumental design for in-line measurements, as well as presenting a full material model. When a full material model has been acquired, one can write an article on the material properties of LKABs moist magnetite concentrates. Here one should present a thorough analysis of the E-M properties with a stabile foundation in the electric equivalent as well as the impedance relations and the mixing formulas. Another topic which needs to be attached to verify the legality of using mixing formulas for identifying the permeability and permittivity is the E-M analysis with Comsol for the effective E-M parameters based on mixing of grains and water filled and air filled cavities. The later analysis has been assessed by T. Lfqvist. When the knowledge of E-M properties has been accumulated one can start to develop an embedded solution. Two different communication modules have been proposed, RFID technology suggested by Electrotech in Kalix and the LTU product Mulle (acting as a node for Bluetooth sensor networks). Contact at electro tech is J. Rajala and for Mulle at LTU it is J. Eliasson. The end product must have a measurement of temperature, resistivity (DC or AC), impedance and maybe total measurement / sensing volume must be known a priori. Permittivity and permeability could be determined from an equivalent electrical circuit.

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[19] Aimoto, A., & Matsumoto, T. (1996). Noninvasive Method for Measuring the Electrical Properties of Deep Tissues Using an Open-Ended Coaxial Probe. Med.Eng.Phys. , vol.18 (no.8), p.641-646. [20] Folger, K., & Tjomsland, T. (1996). Permittivity measurement of thin liquid layers using open-ended coaxial probes. Meas. Sci. Technol. , vol.7, p.11641173. [21] Hagl et al. (2003). Sensing Volume of Open-Ended Coaxial Probes for Dielectric Characterization of Breast Tissue at Microwave Frequencies. IEEE TRANSACTIONS ON MICROWAVE THEORY AND TECHNIQUES , vol.51 (no.4), p.1194-1206. [22] Cheng et al. (2006). Evanescent microwave probe study on dielectric properties of materials. Journal of the European Ceramic Society , Vol.26, p.18011805. [23] Ellison, W.; Moreau, J-M. ;. (2006). Open-Ended Coaxial Probe: Model Limitations (Not published). [24] Ellison, W. J.; Moreau, J-M. (2008). Open-Ended Coaxial Probe: Model Limitations. IEEE TRANSACTIONS ON INSTRUMENTATION AND MEASUREMENT , Vol. 57 (no.9). [25] McLaughlin, B. L., & Robertson, P. A. (2007). Miniature open-ended coaxial probes for dielectric spectroscopy applications. J. Phys. D: Appl. Phys. , vol.40, p.45-53. [26] Oppel et al. (2008). Broadband Measurement of Complex Permittivity Using Reflection Method and Coaxial Probes. RADIOENGINEERING , vol.17 (no.1), p.14-19. [27] Saremi, A. (2008). Sensus Aquae en Ferrum ac Air - A Prestudy: Electro-Magnetic Moisture Metering of Magnetite Ore Concentrate (Not published). Eislab. Lule: Lule University of Technology. [28] Avitabile et al. (2001). A Rugged Active Sensor for Microwave Aquametry. IEEE MTTS Digest , p.2259-2262. [29] Guggenberg, P. A., & Zaretsky, M. C. (1995). Estimation of one-dimensional complexpermittivity profiles: a feasibility study. Journal of Electrostatics , vol.34, p.263-277. [30] Sonnet Software Inc. (2006). Using Electromagnetic Analysis for RFID Antenna Design. Sonnet Application Note (SAN-206A). [31] Wedelin, B. (1988). KOMPENDIUM - ELKRETSTEORI DEL C - LEDNINGAR och FILTER. Gteborg, Sweden: Teknologtryck - Chalmers Tekniska Hgskola. [32] Mathworks. (n.d.). fminsearch. Retrieved 2010-10-05, from Mathworks.com: http://www.mathworks.com/help/techdoc/ref/fminsearch.html [33] Lagarias et al. (1998). Convergence Properties of the Nelder-Mead Simplex Method in Low Dimensions. SIAM Journal of Optimization , Vol. 9 (no. 1), p. 112-147. [34] Mathworks. (n.d.). fminsearch Algorithm. Retrieved 2010-10-05, from Mathworks.com: http://www.mathworks.com/help/techdoc/math/bsotu2d.html#bsgpq6p-11 [35] Creative Commons. (2008-01-09). Creatice Commons - Attribution - ShareAlike 3.0 Unported. Retrieved 2010-12-28, from Wikimedia Commons - Creative Commons: http://creativecommons.org/licenses/by-sa/3.0/deed.en [36] WikiUN:Qianchq. (2010-01-16). Special:ListFiles. Retrieved 2010-12-28, from Wikipedia: http://en.wikipedia.org/wiki/File:Segments.jpg [37] Sjberg, B. (1971). Frsk med konduktiv fuktmtare. Utredning, dk nr 28/42,LKAB.

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APPENDIX A GEOMETRIC AND MATERIAL CONSTANTS Coaxial Cell Geometrical Dimensions a = 0.00495 m b = 0.027 m c = 0.03 m twall = c-b = 0.003 m ltot= 0.249 m llid-insert = 0.008 m (Top,bottom and lid-teflon) lM= ltot- 2llid-insert lM= 0.233 m (Measured length) rinner, teflon lid= a router, teflon lid= 0.0125 m (0.01235) bottom hole and rod: M8
(Metric 8 mm screw thread)

Coax-Cell, Schematic Picture

Coax-Cell, Photo by A. Saremi

rlidprobestick= (thin)~0.001m (+-0.0002) (med)0.0012 (thick)0.00165 llidprobestick= 0.021 m (from connector Teflon end) (0.022 m) hlid outside = ~ 0.012 m (+-0.0002)(Short air-line)(Length cal?) hconnector-teflon = 0.0093m coaxial connector: square side 0.025m, cylinder height 0.0218 m, screw thread M3.
(metric 3 mm)

Bottom, Aluminium and Plastic

bottom of coaxial cell can be plastic or metal. Material Constants and Speed of Light Basic constants: 0 = 8.8541910 (F/m), 0 = (H/m) | (N/A2), c = 299792458, = r 0, = r 0 Air 1.00059 1.00000037 ~0 / 10-16 PTFE ~2.1 ~1 ~0 / 10-16 Water (mQ) ~80.4 0.999992 ~0 PC ~2.9 ~1 -12

Lid and coax cell, lid-probe and core hole

Property \Medium r r (S/m)

Vacuum 1 1 0

Tap water ~80.4 (f) 0.999992 ~10-3

Salt Water ~80.4 (f) 0.999992 ~4

Aluminum ~1 1.000022 3.538107

Property \Medium r r (S/m)

Magnetite Powder > 1000 (f?) Guess 2-3j 0.00151

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APPENDIX B PREPARATION OF MOIST MAGNETITE CONCENTRATE Fraction Magnetite Powder w.Container Empty Container Magnetite Powder Water (calc.) Water (actual) Actual Fraction 0.02
2968,9

0.04
4054,4

0.06
3051,4

0.07
3911,1

0.08
3932,1

0.09
3657,3

0.10
3463

0.11
3721

94,12 2874,7 8 58,668 97959 60 0,0204 44

93,01 3961,39 165,057 9167 124,8 0,03054 2

92,98 2958,42 188,835 3191 190,87 0,06060 7

160,51 3750,59 282,302 4731 294,4 0,07278 1

160,48 3771,62 327,966 9565 341,9 0,08311 6

160,32 3496,98 345,855 1648 361,7 0,09373 7

160,29 3302,71 366,967 7778 384,7 0,10432 8

160,45 3560,55 440,067 9775 459,9 0,11439

The magnetite concentrate used in the moist samples in laboratory is originally as clean as the LKAB factories can make it.

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APPENDIX C RESISTIVITY MEASUREMENTS

Moisture Fraction 0% 2% 4% 6% 7% 7% 8% 9% 10% 11% 0 0.02 0.04 0.06 0.07 0.07 0.08 0.09 0.1 0.11 V(I=-1mA)[V] -42.11 -7.87 -5.11 -3.2 -3.18 -2.35 -2.6 -1.72 -1.17 -0.64 Moisture 0% 2% 4% 6% 7% 7% 8% 9% 10% 11% Res_M664,5389 134,6333 82,56105 47,90005 47,60067 37,96839 38,35475 29,17911 20,53302 11,23174 V(I=1mA)[V] 42.11 6.3 5.18 3.3 3.2 2.34 2.61 1.77 1.18 0.393 Res_M+ 664,5389 107,7751 83,69203 49,39692 47,90005 37,80682 38,50227 30,02734 20,70851 6,896988 l [cm] 6.5 6.0 6.3 6.8 6.8 6.3 6.9 6.0 5.8 5.8 mean_res 664,5389 121,20423 83,126542 48,648486 47,75036 37,887607 38,428508 29,603228 20,620764 9,0643615 R_M- (ohm) 42110 7870 5110 3200 3180 2350 2600 1720 1170 640 Sigma 0,001505 0,008251 0,01203 0,020556 0,020942 0,026394 0,026022 0,03378 0,048495 0,110322 R_M+ (ohm) 42110 6300 5180 3300 3200 2340 2610 1770 1180 393

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APPENDIX D MATHEMATICAL SYSTEM - SAREMI MODEL

Here Zc is correction, Zp parasitic and Zm measured impedances. The measured/optimized impedance also holds some theoretical information, as well as the parasitic impedance which also probably are a measured/optimized variable.

Conjugate multiplication and then split in real and imaginary part.

In this case Z0 = VNA-CABLE-RES = 50 and S11 are the complex frequency dependent S11 parameter measured by the VNA.

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APPENDIX E INDUCTIVE MATHEMATICAL SYSTEM - KARLSSON MODEL

59

60

APPENDIX F CAPACITIVE MATHEMATICAL SYSTEM - KARLSSON MODEL

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APPENDIX G MATLAB FUNCTIONS - COST AND ZLOAD FUNCTIONS

%************************************************************************* %**************************costfun**************************************** %************************************************************************* %Mean square function - With mean square error as output %Author: Amin Saremi %Edits by: Christian Karlsson function J = costfun(theta,R_C,L_C,f,real,img) constants; w=2*pi*f; % define some parameters for measurement cell skin_depth=1/sqrt((pi*mu_al*sigma_al)*f); % Skin depth Rs=l/(sigma_al*(2*pi*a*skin_depth))+l/(sigma_al*(2*pi*b*skin_depth)); %AC resistance (skin resistance) Z0=real+1i*(img); %putting together Zreal and Zimag to Z0, Z0 is the measured impedance mu_real=theta(1);mu_imag=theta(2);Rp=theta(3);%Picking out mu_r and Rp from theta %mu_r=mu_real-1i*mu_imag; Lreal=(l*mu_0*mu_real*log(b/a))/(2*pi); %Calculating the inductance of the cylinder Limag=(l*mu_0*mu_imag*log(b/a))/(2*pi); %Calculating the inductance of the cylinder %Components of impedance to make the system more easy overviewed Zt1=Rp*(Rs+w*Limag); Zt2=Lreal*Rp; Zn1=Rp+Rs+w*Limag; real_hat=R_C+((Zt1*Zn1+w^2*Zt2*Lreal)./(Zn1^2+w^2*Lreal^2)); %real part of Z_hat img_hat=L_C*w+((w*Zt2*Zn1-w*Zt1*Lreal)./(Zn1^2+w^2*Lreal^2));%imag part of Z_hat Z_hat=real_hat+1i*(img_hat); %Z_hat is the calculated impedance. %**********Mean Square of error******************************************* E = Z0-Z_hat; %E is the error and Z0 is the measured impedance J = conj(E)*E; %Scalar product Error squared becomes real %disp(['r = ', num2str(theta(1)),', a = ',num2str(theta(2)),' , v = ',num2str(theta(3)),', J = ',num2str(J)]); %************************************************************************* %************************************************************************* %**************************ZLOAD****************************************** %************************************************************************* %% Function for translating the S11 parameter to equivalent impedance of %Author: Christian Karlsson %% ZLOAD function [ ZL ] = zload(S11) %Zload calculates the ZLoad as a function of frequency %Zload(S11) ZL=50.*((1+S11)./(1-S11));

62

APPENDIX H MATLAB SCRIPT INDUCTIVE OPTIMIZER

% % % % Optimization of the inductive case coaxial cell using fminsearch (inductive_optimizer.m) Original Author: Amin Saremi Rewritten and edited by: Christian Karlsson

%% Formalism % clear all; clc; constants; %loadconstants loaddata;%f,w,w_m,Zs,Z2,Z4,Z6,Z8,Z10,Z12, %% Initiations % theta=zeros(3,1); mu_real=zeros(length(w),length(phi)); mu_imag=zeros(length(w),length(phi)); Rp_opt=zeros(length(w),length(phi)); j=zeros(length(w),length(phi)); %% Calculating correction parameters and well known behaviour of cell (Skinresistance) % % Directly from Eq.Circuit of lid Z=R_C+JwL_C % determine the resistance Rc and inductance Lc of the non-ideal connection % on top of the cylinder inductive equivalent model (for lid representation) disp('Warning about badly conditioned polynomial is expected!, due to modeling and canceling of unwanted noise.') L_C=imag(Zs)./w; %Inductance of lid P=polyfit(f,real(Zs),3); %Stores an 3rd order polynomial which fits P(f)=real_c R_C=polyval(P,f); %A nice approximation of serial skin resistance

%% Guessing mu_r values by assuming the circuit of an only inductive circuit % with complex mu_r that is a resistor value of wLimag and a inductor value % of Lreal assuming Rs very small. Lrguess=imag(Zmeas)./w_m; Liguess=-real(Zmeas)./w_m; %Minus sign according to definition of positive impedance and that the reactance part of mu_r will be defined negative Lguess=[Lrguess,Liguess]; % An length(w)*12 matrix containing guesses of real and imaginary inductance mur_guess=((2*pi).*Lguess)./(l*mu_0*log(b/a)); %Already adjusted for negative reactance

%% Guessing Rp based on resistivity measurements % %Fit a 10th order polynomial curve to the dataset of measurements P1=polyfit(resistivity_data(:,1),resistivity_data(:,2),10); %(moisture content,resistivity,order of polynomial)

63

%Evaluate the polynomial for the vector phi res=polyval(P1,phi); %Assumptions res_slig=repmat(res,size(w),1); %size(w) x 6 sigma_slig=1./res_slig; G=(2*pi.*sigma_slig)./log(b/a); Rp=1./G; %% Optimization %% ************** Start of optimization - Information disp **************** %************************************************************************ disp(' '); disp('Optimization just started...'); disp('Thanks for your patience!...'); disp(' ');

%% *********************** Start of optimization ************************ %*********************************************************************** %Optimization settings oldopts = optimset('fminsearch'); newopts = optimset(oldopts,'MaxIter',200); %newopts = optimset(newopts,'TolFun',1e-3); %newopts = optimset(newopts,'TolX',1e-3);

tic, %take the execution time for the below code (until instruction toc) %OPTIMIZATION LOOP for m=1:length(phi) %Moisture content (2:2:12%) for n=1:length(w) %frequency start:length(w) theta(1)=mur_guess(n,m); %real mu_r guess theta(2)=mur_guess(n,m+length(phi)); %imag mu_r guess theta(3)=Rp(n,m); theta_r= fminsearch(@(theta) costfun(theta,R_C(n),L_C(n),f(n),real(Zmeas(n,m)),imag(Zmeas(n,m))),theta,n ewopts); mu_real(n,m)=theta_r(1); %Den optimerade frekvensberoende mu_r_real mu_imag(n,m)=theta_r(2); %Den optimerade frekvensberoende mu_r_imag Rp_opt(n,m)=theta_r(3); %Den optimerade frekvensberoende Rp j(n,m)= costfun(theta_r,R_C(n),L_C(n),f(n),real(Zmeas(n,m)),imag(Zmeas(n,m))); end err=sum(j(:,m))/length(j(:,m)); disp(['mean square error at the frequency range for', num2str(2*m),'% water content' '= J = ', num2str(err)]); end; toc; %Stop the execution time and auto disp "Elapsed time" figure(1) surf(j)

64

%% Display % % mu_opt=mu_real+1i.*mu_imag; %mu_imag is negative so the condition hold for mu_opt=mu_real-1i*mu_imag (from guess) sigma_opt=log(b/a)./(Rp_opt.*(2*pi*l)); %Optimized Conductivity - Sigma %Calculating optimized impedance for different moistures and plotting skin_depth=1./sqrt((pi*mu_al*sigma_al).*f); % Skin depth Rs=l./(sigma_al*(2*pi*a*skin_depth))+l./(sigma_al*(2*pi*b*skin_depth)); %AC resistance (skin resistance) %Rbot=log(b/a)./(2*pi*skin_depth*sigma_al); %Lbot=

clear L; for m=1:length(phi) %Check so that the model does not deviate Rp=Rp_opt(:,m); Lreal=(l*mu_0.*mu_real(:,m).*log(b/a))./(2*pi); %Calculating the inductance of the cylinder Limag=(l*mu_0.*mu_imag(:,m).*log(b/a))./(2*pi); %Calculating the inductance of the cylinder(ev. stoppa in -) %Components of impedance to make the system more easy overview Zt1=Rp.*(Rs+w.*Limag); Zt2=Lreal.*Rp; Zn1=Rp+Rs+w.*Limag; real_hat=R_C+((Zt1.*Zn1+w.^2.*Zt2.*Lreal)./(Zn1.^2+w.^2.*Lreal.^2)); %real part of Z_hat img_hat=L_C.*w+((w.*Zt2.*Zn1w.*Zt1.*Lreal)./(Zn1.^2+w.^2.*Lreal.^2));%imag part of Z_hat Z_hat=real_hat+1i.*(img_hat); %Z_hat is the calculated impedance. figure(2) hold on plot(f, real_hat,'b') %Plotting optimized mu_r plot(f, real(Zmeas(:,m)),'r') figure(3) hold on plot(f, img_hat,'b') %Plotting optimized mu_r plot(f, imag(Zmeas(:,m)),'r') end hold off plot_results

65

APPENDIX I MATLAB SCRIPT PLOT RESULTS

% Result plotting function % Original Author: Amin Saremi % Editor: Christian Karlsson %************************************************************************** %* Plots of the results * %************************************************************************** threshold=ones(size(w)); %*********** Real Relative Permeability depending on watercontents (real part)*************** figure hold on plot(f, mu_real(:,1),'-b') %Plotting optimized mu_r based on 2% moisture (frequency dependent) plot(f, mu_real(:,2),'-g') %Plotting optimized mu_r based on 4% moisture (frequency dependent) plot(f, mu_real(:,3),'-y') %Plotting optimized mu_r based on 6% moisture (frequency dependent) plot(f, mu_real(:,4),'-m') %Plotting optimized mu_r based on 8% moisture (frequency dependent) plot(f, mu_real(:,5),'-c') %Plotting optimized mu_r based on 10% moisture (frequency dependent) %plot(f, mu_real(:,6),'-r') %Plotting optimized mu_r based on 12% moisture (frequency dependent) plot(f, threshold,'--k') %Plotting threshold title('Real Relative permeability of the magnetite clay for different water contents [optimized]'); xlabel('Frequency[hz]');ylabel('Mu_r_,_r_e_a_l'); %*********** Imag Relative Permeability depending on watercontents (imag part)*************** figure hold on plot(f, mu_imag(:,1),'-b') %Plotting optimized mu_r based on 2% moisture (frequency dependent) plot(f, mu_imag(:,2),'-g') %Plotting optimized mu_r based on 4% moisture (frequency dependent) plot(f, mu_imag(:,3),'-y') %Plotting optimized mu_r based on 6% moisture (frequency dependent) plot(f, mu_imag(:,4),'-m') %Plotting optimized mu_r based on 8% moisture (frequency dependent) %pinkish plot(f, mu_imag(:,5),'-c') %Plotting optimized mu_r based on 10% moisture (frequency dependent)%light bluish %plot(f, mu_imag(:,6),'-r') %Plotting optimized mu_r based on 12% moisture (frequency dependent) plot(f, threshold,'--k') %Plotting threshold title('Imag Relative permeability of the magnetite clay for different water contents [optimized]'); xlabel('Frequency[hz]');ylabel('Mu_r_,_i_m_a_g'); % %*************Real Relative permeability guesses based on moisture MUT tests****************** % figure % hold on % plot(f, mur_guess(:,1),'-b') %Plotting guess of mu_r based on 2% moisture (frequency dependent) % plot(f, mur_guess(:,2),'-g') %Plotting guess of mu_r based on 4% moisture (frequency dependent) % plot(f, mur_guess(:,3),'-y') %Plotting guess of mu_r based on 6% moisture (frequency dependent)

66

% plot(f, mur_guess(:,4),'-m') %Plotting guess of mu_r based on 8% moisture (frequency dependent) % plot(f, mur_guess(:,5),'-c') %Plotting guess of mu_r based on 10% moisture (frequency dependent) % %plot(f, mur_guess(:,6),'-r') %Plotting guess of mu_r based on 12% moisture (frequency dependent) % plot(f, threshold,'--k')%Plotting threshold % title('Real Relative Permeability Guesses of the Magnetite Clay for Different Water Contents'); % xlabel('Frequency [hz]');ylabel('Mu_r_,_g_u_e_s_s_,_r_e_a_l'); % % %*************Imag Relative permeability guesses based on moisture MUT tests****************** % figure % hold on % plot(f, mur_guess(:,1+length(phi)),'-b') %Plotting guess of mu_r based on 2% moisture (frequency dependent) % plot(f, mur_guess(:,2+length(phi)),'-g') %Plotting guess of mu_r based on 4% moisture (frequency dependent) % plot(f, mur_guess(:,3+length(phi)),'-y') %Plotting guess of mu_r based on 6% moisture (frequency dependent) % plot(f, mur_guess(:,4+length(phi)),'-m') %Plotting guess of mu_r based on 8% moisture (frequency dependent) % plot(f, mur_guess(:,5+length(phi)),'-c') %Plotting guess of mu_r based on 10% moisture (frequency dependent) % %plot(f, mur_guess(:,6+length(phi)),'-r') %Plotting guess of mu_r based on 12% moisture (frequency dependent) % plot(f, threshold,'--k')%Plotting threshold % title('Imag Relative Permeability Guesses of the Magnetite Clay for Different Water Contents'); % xlabel('Frequency [hz]');ylabel('Mu_r_,_g_u_e_s_s_,_i_m_a_g');

%*********************Sigma - Conductivity of clay************************* figure hold on plot(f, sigma_opt(:,1),'-b')%Plotting optimised conductivity for 2% water plot(f, sigma_opt(:,2),'-g')%Plotting optimised conductivity for 4% water plot(f, sigma_opt(:,3),'-y')%Plotting optimised conductivity for 6% water plot(f, sigma_opt(:,4),'-m')%Plotting optimised conductivity for 8% water plot(f, sigma_opt(:,5),'-c')%Plotting optimised conductivity for 10% water %plot(f, sigma_opt(:,6),'-r')%Plotting optimised conductivity for 12% water title('Sigma - Conductivity of Magnetite Clay'); xlabel('Frequency[hz]');ylabel('Sigma [S/m]');

67

APPENDIX J MATLAB SCRIPT CONSTANTS

% Different constants of our problem both for materials and geometry % (constants.m) % Author: Christian Karlsson % sigma_al=3.54e7; %conductivity of aluminium % mu_al=1.0141; %Permeability of aluminium global t_wall t_ptfe eps_0 mu_0 r_ptfe a b c d l eps_air eps_w mu_air mu_w mu_al sigma_air sigma_w sigma_ws sigma_al %Basic constants% eps_0=8.85419E-012; %F/m mu_0=4*pi*1E-007; %H/m | N/A^2 c=299792458; % start=15; %index makro %Geometrical constants% a=0.00495; %m b=0.027; %m d=0.03; %m %l=0.3; %m (amin value) %l=0.5; %m (experimentation value) l=0.249-(1.6e-2); %m (Ck value for inductive) Removed for bottom and lid insertion dept=0.008; %m t_wall=d-b; %m r_ptfe=0.0125; %m t_ptfe=0.00785; %m %Material Specific constants% %Permitivity eps_air=1.00059*eps_0; eps_w=80.4*eps_0; eps_ptfe=2.1*eps_0; %Permeability mu_air=1.00000037*mu_0; mu_w=0.999992*mu_0; mu_al=1.000022*mu_0;%Could be complex and frequency dependent Christians values %mu_al=1.0141*mu_0;%Could be complex and frequency dependent (Amin values) mu_ptfe=1*mu_0;

%Conductivity sigma_air=0; %S/m %Actual: ~1E(-16) sigma_ptfe=1E-16; %sigma_w=55*1E-009; %S/m sigma_w=1E-003; %S/m sigma_ws=4; %[S/m] for salt water (varies dep. Saltcontent probably ref. ocean water) sigma_al=3.538E+007; %S/m %Pure aluminium, changes with type of aluminium phi=[0.02,0.04,0.06,0.08,0.10]; %moisture content vector

68

APPENDIX K MATLAB SCRIPT DATA LOADER

% Data Loader (loaddata.m) %Author: Christian Karlsson %% % load lidind.mat %Inductive measurement of lid f=(s(1,:)).'; w=2.*pi.*f; Sli=(d(1,:)).'; Zli=ZLoad(Sli); %% % load lidcap.mat %cappacitive measurement of lid Slc=(d(1,:)).'; Zlc=ZLoad(Slc); %% % load airind.mat % Sai=(d(1,:)).'; Zai=ZLoad(Sai); %% % load aircap.mat % Sac=(d(1,:)).'; Zac=ZLoad(Sac); %% % load h2oind.mat % Swi=(d(1,:)).'; Zwi=ZLoad(Swi); %% % load h2ocap.mat % Swc=(d(1,:)).'; Zwc=ZLoad(Swc); %% % clear s d

69