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Theory and Methods 42
CHAPTER 3
THEORY AND METHODS
3.1 Elementary Discussion About Dielectric Material
In electromagnetism, materials are classified into two categories:
1) Conductors and 2) insulators or dielectrics. The dividing line between the two
categories is sharp and some media (eg. the earth) are considered as conductors in
one part of radio frequency range but as dielectrics (with losses) in other part of
frequency range. A material is categorized as a “dielectric” if it has the capacity to
store energy when external electric field is applied. The theory of dielectrics was
proposed by Faraday and then later on it was modified by Maxwell. In 1837,
Michael Faraday performed experiments to investigate the effect of filling dielectric
material in the space between the plates of capacitor. If a DC voltage is applied
across a parallel plate capacitor as shown in Fig. 3.1, it is observed that more charge
is stored in the case when a dielectric material is placed between the plates than the
case when no material (a vacuum) is placed between the plates. The dielectric
material enhances the storage capacity of the capacitor by neutralizing the charges at
the electrodes which ordinarily would contribute to the external field. This
phenomenon is dependent on the dielectric properties such as breakdown voltage.
The capacitance of the capacitor filled with the dielectric material depends on the
dielectric constant of the material.
Fig. 3.1: Application of DC voltage across the plates of a parallel plate
capacitor (Agilent, 2005)
Theory and Methods 43
From the Figure 3.1,
C0 = A / t (3.1)
C = C0 k' (3.2)
k' = ε'r = C /C0 (3.3)
where k' = ε'r is the real dielectric constant of the material
C0 = Capacitance without material (vacuum) =A / t
C = Capacitance with dielectric material = qd /V
A= area of capacitor plates
t = distance between the capacitor plates
qd = magnitude of charge stored on each plate
V = voltage applied to the plates
If an ac sinusoidal voltage Ve jωt
is applied across the same capacitor as
shown in Fig. (3.2), the resulting current is made up of a charging current Icharge and
a loss current Iloss that is related to the dielectric constant. The losses in the material
can be represented as a sum of conductance (G) in parallel with a capacitance (C).
Fig. 3.2: Application of AC voltage across the plates of a parallel plate capacitor
For the applied voltage across the capacitor, the current
I = Icharge+ Iloss (3.4)
= jωVC0k' + VG
If G =ωC0 k'' then
I = jωVC0k' +VωC0k'' (3.5)
I = jωVC0 k '+ (− j)2 VωC0k''
Theory and Methods 44
I = V jωC0 k* (3.6)
where k* = k'− jk"
The complex dielectric constant k* consists of a real part k' which represents
the storage of energy and an imaginary part k'' which represents the loss.
The complex dielectric constant k* of a material is equivalent to relative or
normalized complex permittivity given by
εr* = k* = ε'/ε0 - j ε''/ ε0 = ε'r - εr'' (3.7)
where εr*, i.e. the permittivity ε* relative to free space ε0,is called complex relative
permittivity, and ε0 = Permittivity in free space = 8.854 x 10-12
Farad/m
The real part of permittivity ε'r is a measure of the ability of dielectric
material to store electric energy from an external electric field. The imaginary part
of permittivity ε"r is called the loss factor and is a measure of how dissipative or
lossy a material is, to an external electric field. The imaginary part of permittivity ε"r
is always greater than zero. The loss factor includes the effects of both dielectric loss
and conductivity. Fig. 3.3 shows complex permittivity in the form of a simple vector
diagram .The real and imaginary components (ε'r, ε"r) are 90° out of phase. The
vector sum ε*r forms an angle δ with the real axis ε'r. The relative “lossiness” of a
material is the ratio of the energy lost to the energy stored.
Fig. 3.3: Loss factor vector diagram
Theory and Methods 45
tan δ = = (3. 8)
The product of angular frequency and loss factor is equivalent to a dielectric
conductivity.
ζ = ωε0ε''
3.2 Polarization of Dielectric Materials
The dielectrics contain bound charges which are tightly bound together in
atoms and molecules. They differ from plasma and conducting media, in as much as
they do not contain free charges like the other two states of matter. The application
of a steady external electric field causes a small but significant separation of the
bound charges so that each infinitesimal element of volume behaves as if it were an
electrostatic dipole. The induced dipole field tends to oppose the applied field. A
dielectric material which exhibits this separation of bound charges is said to be
polarized. On a microscope scale, the type of polarization is determined by the
nature of material. In most of the materials, polarization occurs only in the presence
of an applied field, although a few materials exhibit permanent polarization;
ferromagnetic crystals exhibit permanent polarization while certain other materials
called electrets become permanently polarized if allowed to solidify in a strong
electric field. On an atomic scale, charge separation can occur due to the
displacement of the negatively charged electron cloud relative to the positively
charged nucleus; this is called electronic polarization. On a molecular scale, ionic
and orientational polarization are important. Ionic polarization results from the
separation of positive and negative ions in molecules which are held together by
ionic bonds. Orientational polarization arises in materials whose molecules are
permanently polarized but randomly oriented; the application of an external electric
field causes the molecules to align themselves parallel to the applied field, thus
producing a net polarization in the material. On a still larger scale, one encounters
space charge polarization which arises when free conduction electrons are present
but are prevented from moving through large distances by the barriers such as grain
boundaries; when a field is applied,the electrons „pile up‟ against these barriers
producing the separation of charges required to polarize the material. The four types
Theory and Methods 46
of polarization described above are indistinguishable in a steady field, but in a time
varying field each type exhibits a different characteristic response time. A molecule
develops a dipole moment proportional to applied electric field for small field
magnitude. This proportionality is expressed as
p = αT Eav (3.9)
In which the total polarizability αT is the sum of polarization arising from
each of the different types of polarization viz electronic, ionic etc. Eav is the average
rms field acting on a molecule (which in general is different from the applied field).
If we multiply the equation by n0 the number of molecules per cubic meter, the
result is the dipole moment per unit volume or the polarization. P.
P = n0 p = n0αTEav (3.10)
When a material having non-polar atoms is subjected to an electric field it
gets polarized due to the displacement of the center of charge of electrons relative to
the nucleus in each atom, causing electronic polarization (Pe).and the displacement
of atoms of different polarity relative to one other induces dipole moments in the
molecules called atomic polarization (Pa). These two polarizations together
constitute a distortion polarization (Pd).
In a polar molecule, a third process also contributes to the polarizability
(provided the dipoles are free to orient /reorient) in which when an electric field is
applied there is a tendency for the permanent dipoles to align themselves parallel to
it, although, because of the thermal motion the departure from a random arrangement
is very small in the fields of the strength normally used for measurement and at
ordinary temperatures. In polar molecules, the orientation polarization is in addition
to the distortion polarization observed in non polar materials, so that polar materials
have higher permittivity than non polar ones. The relationship between permittivity
and the various types of polarization can be expressed in the following way:
ε = 1 + (3.11)
where P is the polarization produced by the applied field E in an isotropic material.
Substituting the value of P from equation (3.9), we get
Theory and Methods 47
ε = 1 + (n0αTEav) (3.12)
Each of the three types of polarizability is a function of the frequency of the
applied field. As the field alters and reverses, both the distortion of the molecules
and their average orientation must change. When the frequency is sufficiently low,
all types of polarization attain the value they would have had in a steady field equal
to the instantaneous value of alternating field, but as the frequency is raised the
polarization no longer has time to reach its steady value. The orientation polarization
is the first to be affected. This type of polarization takes a time of the order 10-12
to
10-10
seconds to reach its equilibrium value in liquids and solids with moderately
small molecules and at normal temperatures; consequently when the applied field
has a frequency in the range 1010
to 1012
cycles/sec, the orientational polarization
fails to reach its equilibrium value and contributes less and less to the polarization as
the frequency rises.
It is this fall of polarizability from αT = αe + αa + αo to αT = αe + αa, which has
associated with it related fall of permittivity and occurrence of absorption that
constitutes dielectric dispersion. In the frequency range in which the dielectric
dispersion occurs, αe and αa remain unchanged, since the distortion polarization of a
molecule takes much less time to reach equilibrium state with an applied field than
the orientational polarization does .At frequencies comparable with the natural
frequencies of vibration of the atoms in the molecules, however, αa will fail to attain
its equilibrium value and as a result of it further dispersion regions will occur. These
usually lie in the infrared region of the spectrum. The fall-off of the electronic
polarization occurs at frequencies corresponding to the electronic transitions
between different energy levels in the atom, that is, mostly at visible, ultraviolet and
X-ray frequencies. In electronic and atomic polarization, quantum effects are
predominant in all phases, but the dielectric dispersion in the liquid phase, and to
some extent also in solid phase, can be explained by classical theory.
Theory and Methods 48
3.3 Determination of Dielectric Parameters at Microwave Frequencies
Electromagnetic waves are in general observed in bounded space, confined
by various types of boundaries. The reflection and refraction of fields by matter
provide an essential mean for directing and modifying such fields, which are useful
in measurements of the dielectric properties of materials.
When the electromagnetic waves travel through a dielectric medium, its
amplitude and phase change with the distance in the medium. These changes are
governed by the complex propagation factor
γ d = αd + j βd (3.13)
where αd is the attenuation constant and βd is the phase constant, such that
βd = 2 π / λd (3.14)
λd being the wavelength of electromagnetic wave in the dielectric medium.
For rectangular wave guides, γ d for TEmn and TMmn modes is given by the relation
γ d = j √ω2 μ ε – {( ) )} (3.15)
Here ε and μ are the absolute permittivity and permeability of dielectric
medium respectively. Wavelength in free space (λ0) of the electromagnetic wave is
given by
λ0 = 2π / ω√μ0ε0 (3.16)
The absolute permittivity ε and the complex permittivity ε* of the dielectric
material are related as
ε = ε0ε* (3.17)
Since μ = μ0 (for non magnetic materials), substituting the equations (3.14)
and (3.15) in equation (3.13),we obtain
γ d = j √( )2 ε*
– {( ) } (3.18)
γ d = j ( ) √ ε* – {( ) ) } (3.19)
Cutoff wavelength (λc ) for rectangular waveguide in TEmn and TMmn modes
is given by
Theory and Methods 49
λc = (3.20)
Substituting (3.20) in equation (3.19) we obtain
γ d = j ( ) √ ε* – ( ) (3.21)
Since ε* = ε' - jε'' (3.22)
Substituting the value from equation (3.12) and (3.22) in equation (3.21) and
separating the real and imaginary parts we have
2 2 2
0 0 d
c d d
' 1
(3.23)
2
0 d
d d
" 2
(3.24)
Where βd = ( 2π / λ d),
Equations (3.23) and (3.24) may be used for determining dielectric constant
and dielectric loss factor for both low loss and high loss dielectric materials.
3.4 Methods Suitable for Investigation of The Dielectric
Properties of Food Materials at Microwave Frequencies
The dielectric properties of food materials at the microwave frequencies can
be determined by several methods using different microwave measuring sensors
(Kraszewski, 1980). According to Kraszewski (1980), measurement techniques can
be categorized as reflection or transmission types, using resonant or anti-resonant
systems, with open or closed structures for sensing of the properties of material
samples. Waveguide and coaxial line transmission measurements represent closed
structures while the free-space transmission measurements and open-ended coaxial-
line systems represent open-structure techniques, respectively. These techniques
include wave guide measurements, resistivity cell, lumped circuit, coaxial probe,
transmission line, resonant cavity, free space transmission, parallel plate capacitor,
cavity resonator, and time domain spectroscopy, each having unique advantages and
Theory and Methods 50
disadvantages (Icier and Baysal, 2004; Nyfors and Vainikainen, 1989). The use of
lumped circuit techniques is limited to low frequencies and high loss materials.
Open-ended coaxial probe method is one of the most commonly used method to
determine the dielectric properties of high loss liquid and semi-solid foods (Nelson
et al., 1994; Herve et al., 1998), and fresh fruits and vegetables (Nelson and Bartley,
2000). The measurement technique relevant for any specific application depend on
the nature of the dielectric material, physical state of the material (liquid or solid),
shape (thickness, flatness), desired range of frequency and the degree of accuracy
(Agilent,2005; Nelson 1999). The sample holder design also depends upon the
physical state of the dielectric materials to be measured. The measurement methods
that have been used to determine the dielectric properties of agri-food materials are
described here.
3.4.1. Cavity Perturbation Technique
The dielectric properties of homogeneous food materials can be measured by
cavity perturbation technique which is a preferred technique because of its simplicity,
easy data reduction, accuracy, and high temperature capability (Bengtsson and
Risman 1971; de Loor and Meijboom, 1966). This technique is well suited for
dielectric measurements of low loss materials and is also sensitive to low loss
tangents (Hewlett-Packard 1992; Kent and Kress-Rogers 1986). In the resonant
cavities, the mode of oscillation of the electromagnetic fields is the standard TM
(transverse magnetic) or TE (transverse electric) mode. This method of determination
of dielectric properties is based on the shift in resonant frequency and the change in
absorption characteristics of a tuned resonant cavity, due to insertion of a sample of
target material. The sample is placed completely inside the cavity through the centre
of the waveguide and the measurements are made by noting the changes in the
resonant frequency and the width of resonance maxima due to insertion of the
sample. The arrangement is shown in Fig. 3.4.
Theory and Methods 51
Fig. 3.4: Schematic representation of a resonant cavity method (R = reflected
power, T=transmitted power (adapted from Venkatesh and Raghvan,
2005)
The use of vector network analyzer (VNA) makes the measurement easy
since it automatically displays changes in frequency and width of resonant maxima
which can be used to compute the values of ε' and ε'' (Engelder and Buffler,1991).
The measurement details and the perturbation equations adapted for determination
of dielectric constant( ') and loss factor ( '') along with accuracy information for
network Analyzer were reported by Liao et al. (2001). With the help of the resonant
cavity systems, the dielectric measurements are limited to a single frequency.
Calibration is required to be done for each cavity but once the calibration curves are
obtained, calculations can be done rapidly. Preparation of sample is relatively easy
and measurements can be made on a large number of samples in a short span of
time. This method can be used at temperatures as high as 140°C and as low as
−20°C according to Ohlsson and Bengtsson (1975) and Risman and Bengtsson
(1971). Sharma and Prasad (2002) have used the cavity perturbation method to
measure the dielectric properties of garlic at selected levels of moisture content and
at 35°C to 75°C.
3.4.2 Transmission Line Technique
The transmission line is an ordinary method to determine the complex
permittivity for solid, particulate and liquid material. In transmission line methods, a
sample of the substance is put inside an enclosed transmission line energized by an
Theory and Methods 52
electromagnetic source and both reflection and transmission are measured. This
method is more accurate and sensitive as compared to coaxial probe method but it
has a narrower range of frequencies over which dielectric measurements can be
made. The measurements are restricted to the dominant mode and frequency range.
Preparation of the sample is difficult and time consuming since the material has to
be filled in the cross-section of the transmission line (coaxial or rectangular),
(Engelder and Buffler 1991; Hewlett-Packard 1992). Kraszewski (1996) reported
that when such methods are used for moisture content determination, the frequency
employed should be above 5 GHz to avoid the effect of ionic conductivity and
bound water relaxation. Dielectric properties of liquids and viscous-fluid type foods
can be measured by this method by using a sample holder connected through E
plane bend at the end of a transmission line. According to Nelson et al.(1974), the
dielectric properties can be easily and inexpensively obtained by this technique by
utilizing a slotted line and standing wave indicator. A more sophisticated version of
this technique uses a swept-frequency network analyzer, which measures the
impedance automatically as a function of frequency. This technique is cumbersome
when it is used for solid samples because the sample must be made into a slab or
annular geometry for being used in a waveguide or coaxial transmission line. At
2,450 MHz, the sample size is somewhat large, particularly for fats and oils
(Venkatesh and Raghavan, 2005).
3.4.3 Network Analyzers
A measurement of the reflection from and transmission through a material
along with knowledge of its physical dimensions provides the information to
characterize the permittivity and permeability of the material. Vector network
analyzers such as the PNA, PNA-L, ENA, and ENA-L make swept high frequency
stimulus-response measurements from 300 kHz to 110 GHz. A vector network
analyzer consists of a signal source, a receiver and a display as shown in Fig. 3.2.
The source generates a signal at a single frequency and make them incident on the
material under test. The receiver is tuned to that frequency to detect the reflected and
transmitted signals from the material. The measured response gives information
about that the magnitude and phase data at that frequency. The source is then
Theory and Methods 53
stepped to the next value of frequency and the measurement is repeated to display
the reflection and transmission measurement response as a function of frequency on
the screen of the detector. (Agilent, 2005)
Fig.: 3.5. Network analyzer system (Agilent,2005)
3.4.4 Open Ended Coaxial Probe Technique
The coaxial probe method is basically a improvised form of the transmission
line method. It uses a coaxial line, which has a special tip that senses the signal
reflected from the material. The tip of the probe is brought into contact with the
substance by touching the probe to a flat surface of a solid or by immersing it in a
liquid. This probe acts as the receiver of the signal reflected by the sample. The
reflected signal gives information about the dielectric properties of the substance by
measuring the phase and magnitude. The method is quite easy to use and it is
possible to measure the dielectric properties over a wide range of frequencies viz. 50
MHz to 50 GHz,500 MHz to 110 GHz by using different models of probe with
different types of Network Analyzer. It provides limited accuracy in the case of
materials with low values of absolute permittivity i.e. dielectric constant and loss
factor (Engelder and Buffler, 1991; Hewlett-Packard, 1992). According to Sheen
and Woodhead (1999); Hewlett-Packard (1992),this technique yields good results
for materials with loss factors greater than one when used for 915 and 2,450 MHz.
Typical open ended probes utilize 3.5 mm diameter coaxial line. For measurement of
Theory and Methods 54
solid samples, probes with flat flanges may be utilized (Hewlett-Packard,1992). An
open-ended coaxial probe technique was used to measure the dielectric properties in
thermal treatment for controlling insects in fruits at temperatures 20°C to 60°C over
a frequency range from 1MHz to 1,800 MHz (Wang et al., 2003). For liquid and
semi-solid materials including biological and food materials, open-ended coaxial-
line probes have been used for broadband permittivity measurements (Blackham and
Pollard,1997; Grant et al.,1989). A similar technique was used by Nelson et al.
(1994) and Ohlsson et al. (1974a) for permittivity measurements on fresh fruits and
vegetables. This technique is not free from errors because of the probability of air
gaps or air bubbles between the end of the coaxial probe and the sample. This method
has advantages that include ease of sample preparation and small size of sample. It
is non destructive and provides broadband information (Komarov et al.,2005).
3.4.5 Time Domain Spectroscopy /Reflectometry (TDR) Method
Time domain spectroscopy/reflectometry methods for determination of
dielectric properties were developed in the 1980s. The frequency range covered by
this technique from 10 MHz to 10 GHz. This method also employs the reflection
characteristic of the material under test to compute the dielectric properties. The
measurement is very rapid and accuracy is high with error within a few percent only
(Afsar et al., 1986). The material under test should be homogeneous and the size of
the sample used is very small .Although these methods are expensive, they can be
employed for advanced research on the interaction of the electromagnetic energy
with materials over a wide range of frequency (Mashimo et al., 1987; Ohlsson et al.,
1974b). The dielectric properties of honey-water mixture have been investigated by
Puranik et al. (1991) using this technique in the frequency range of 10 MHz to 10
GHz at 25°C. This technique has been used by Lahane et al. (2003) to study
dielectric relaxation of ayurvedic medicines with varying volume fractions in
ethanol.
Theory and Methods 55
3.4.6 Free Space Transmission Techniques
Fig. 3.6: Schematic of a free space transmission technique for measuring
reflection and transmission (Port 1 and 2 are connected to Vector
Network Analyzer) (Venkatesh and Raghvan, 2005)
In this method, sample is placed between a transmitting antenna and
receiving antenna and the attenuation and phase shift of the signal are measured. The
dielectric sample holders with rectangular cross-section were placed between the
horn antennas or similar radiating elements by Trabelsi et al. (1997). It is assumed
that a uniform plane wave is normally incident on the flat surface of a homogenous
material, and that the planar sample has infinite extent laterally (Venkatesh and
Raghavan,2005). This method does not require special sample preparation.
Kraszewski (1980) reported that this method can be easily implemented in industrial
applications for continuous monitoring and control, e.g., moisture content
determination and density measurement. Broadband and accurate measurement of
the permittivity can be achieved by this technique.
3.4.7 Micro Strip Transmission Line
Micro strips have long been used as microwave components, making it
suitable for use in dielectric permittivity measurement and show such properties
which overcome some of the limitations faced in other methods. It is well known
that the effective permittivity of the combination of the substrate and the material
above the line taken in form of a layer, i.e. for a micro strip transmission line with at
least thin width to height ratio is strongly dependent on the permittivity of the region
above the line (Venkatesh and Raghavan, 2005). This effect has been utilized in
Theory and Methods 56
implementing microwave circuits and to a lesser extent for investigation of dielectric
permittivity. Furthermore, the measurement of effective permittivity by this method
is relatively straightforward and well suited for testing of permittivity in industrial
equipments. Keam and Holmes (1995) suggested that permittivity of the material
can be derived by determining the effective permittivity of a micro strip line covered
with and without an unknown dielectric substance.
3.4.8 Six-Port Reflectometer (SPR) Using An Open-Ended Coaxial Probe
SPR can provide non-destructive broadband permittivity measurements with
accuracy comparable to commercial instruments as per review presented by Venkatesh
and Raghavan (2005). Non destructive broadband permittivity measurements, using
open-ended coaxial lines as impedance sensors, are of great interest in a wide variety
of biomedical applications (Ghannouchi and Bosisio 1989). The test device used in
this method is an open-ended coaxial test probe immersed in the test liquid, kept at a
constant temperature and data acquisition and reduction are fully automatic. This
effective transmission line method, used to represent the fringing fields in the test
medium, provides a good model to interpret microwave permittivity measurements
in dielectric liquids. Using such a model, the precision on relatively high-loss
dielectric liquid measurements is expected to be good. However, this method
involves a more complex mathematical procedure in order to translate the signal
characteristics into useful permittivity data (Venkatesh and Raghavan 2005).
3.5 Determination of ε' and ε'' Using Transmission Line Techniques
The transmission line methods of measurement of complex permittivity are
based on the use of a slotted line and a variable short circuit. Slotted line techniques
are well suited to complex permittivity measurements (except for very low loss
samples) at microwave frequencies. The accuracy of measurement depends to a
large extent on the accuracy with which the VSWR and the position of the voltage
minimum can be found.
3.5.1 Von Hippel’s Method:- This method is also known as shorted waveguide
method. This method essentially involves reflection of microwaves propagating
in TE10 mode, incident normally on a dielectric sample placed against a
perfectly reflecting surface.
Theory and Methods 57
When an electromagnetic wave traveling through medium 1 strikes normally
on medium 2, a part of it is reflected and the rest is either absorbed or gets
transmitted. A standing wave pattern is thus produced in medium 1. The transverse
electric field component in this partial reflection case is given by
Ey = 1 12
0 0. 1j x x
E e r e (3.25)
where γ1 is the propagation constant in medium 1.
Fig . 3.7: Standing waves in a waveguide (a) without dielectric (b) loaded with
dielectric of any length represented by ‘d’ (c) loaded with dielectric of
length λd/2
Theory and Methods 58
The reflection coefficient r0 is given by
ro = | r0 | e-2jψ
(3.26)
Where | r0 | is the magnitude and 2ψ is the phase angle of reflection
coefficient. The input impedance Z(0) at the boundary x = 0 is given by
Z(0) = 0
1
0
1
1
rZ
r (3.27)
where Z1 is the impedance of medium 1.
As attenuation in medium 1 is negligible, inverse voltage standing wave ratio
(IVSWR) in medium 1 may be written as
1 0
max min
0
1/
1
rE E
r (3.28)
Putting ro = e-2u
(3.29)
where u = θ + jψ (3.30)
We may write equation (3.27) as
00 1 1
0
1coth
1
rZ Z Z u
r (3.31)
and
2
min
2max
1tanh
1
eE
E e (3.32)
On expanding coth u in equation (3.31), we get
1
tanh cot0
1 tanh cot
jZ Z
j (3.33)
If x0 be the position of the first minimum (from the surface of the dielectric)
where the incident and reflected waves combine out of phase, i.e. at a phase
difference of π, we obtain
4 / 2o gx (3.34)
Theory and Methods 59
Thus the phase angle is obtained as
12 4
4
o
g
x (3.35)
Substituting the value of ψ from equation (3.33) in equation (3.31), we
obtain the expression for Z(0) as
1
2tan
(0)2
1 tan
o
g
o
g
xj
Z Zx
j
(3.36)
If medium (2) is terminated in a short circuit, the input impedance at the
interface x = 0 is given by
2 2tanho scZ Z d
(3.37)
Where Z2, γ2 and d are respectively the characteristic impedance,
propagation constant and the length of the medium (2). If the shorting metal plate is
placed at a distance λg /4 from medium 2 (Fig.3.6), it corresponds to an open-
circuited termination and the input impedance at the interface is
2 2cotho ocZ Z d (3.38)
For rectangular waveguides, the propagation constant (γ2) for TEmn and
TMmn modes is given by
Fig. 3.8: Standing waves in a waveguide in which short circuiting plunger is
placed at a distance λg / 4 for medium 2
Theory and Methods 60
1/22 2
2
2
m nj
a b (3.39)
Where ε and μ are the absolute permittivity and permeability of the dielectric
medium respectively. If εo and μo are the values of these quantities for free space,
then these can be related as
* o r (3.40)
and μ = μo (for non-magnetic materials) (3.41)
Where ε* is the complex permittivity of the dielectric medium given by
ε* = ' - j '' (3.42)
On using equations (3.40),(3.41) and (3.42), equation (3.39) can be expressed as
2 2 2
02 2 2
0
2*
2
m nj
a b (3.43)
or2
/ / / 0 .2 2
0
2
c
j j
(3.44)
where λo is the free space wavelength and λc is the cut-off wavelength
12 2 2
2 2
2c
m n
a b
(3.45)
If αd and βd are the attenuation constant and phase factor for the dielectric
medium, then
2 d dj
(3.46)
Separating real and imaginary parts of equation (3.44) and (3.46), we get
2 2 2
/ 12
o o d d
c d
(3.47 )
2
/ / /od d
d
(3.48)
Theory and Methods 61
Equations (3.47) & (3.48) may be used for determining dielectric constant
and loss factor for both low loss and high loss dielectric materials.
3.5.2 Yadav Gandhi Method
3.5.2.i Theory
This method is used for the samples in powder form. This method is a
combination of the method of Dube and Natrajan (1974) and the method employed
for polar liquids in dilute solutions of non – polar solvents, employing a slotted
waveguide and a short circuiting plunger used by Heston et al (1950). This method
has been successfully Srivastava and Vishwakarma(2004) for study of dielectric
properties of Bauxite, by Gupta and Jangid (2008) for dielectric properties of soil
and by Sharma et al.(2010) for determination of dielectric properties of wheat in
powder form.
When a rectangular waveguide filled with a dielectric material of complex
permittivity ε* is excited in TEmn or TMmn mode, the propagation constant γd of the
electromagnetic waves through the dielectric can be written as (Yadav and
Gandhi,1992)
1/ 22
0d d d
0 c
2j j * (3.49)
Here αd and βd are the attenuation and phase shift introduced by unit length
of the material, measured respectively in Nepers/m and radians/m; λ0 represents the
wavelength of electromagnetic waves in free space and λc is the cut off wavelength
of the waveguide.
Substituting ε* = ε ' – j ε" in Eq.(3.49) and separating real and imaginary
parts, we obtain
2 2 2
0 0 d
c d d
' 1 (3.50)
2
0 d
d d
" 2 (3.51)
Theory and Methods 62
The food grains are known to appreciably absorb electromagnetic radiation
at microwave frequencies, as evidenced from the fact that the domestic microwave
ovens operate at 2.45 GHz (Dibben, 2001). In the present investigations equations
(3.48) and (3.49) are used for finding out dielectric properties of the powder of
foodstuff. The main quantities to be measured experimentally are αd and βd for the
samples for which ε' and ε" values are to be determined.
Fig. 3.9: Experimental set up for measurement of dielectric properties of
powders by Yadav and Gandhi method
Symbolic meanings of numerals used in the Figure are as given below:
1 Power supply 9 Mica window
2 Microwave oscillator 10 Sample holder
3 Isolator 11 Movable plunger
4 Frequency meter 12 Water circulating jacket
5 E-H tuner 13 Screw gauge for plunger movement
6 Variable attenuator 14 Tuning probe
7 Slotted waveguide section 15 Crystal detector
8 E-band 16 Indicating meter
Theory and Methods 63
3.5.2.ii Measurement of λd
The experimental arrangement is shown schematically in Fig.3.6. Microwave
power obtained from a microwave source, viz. Klystron tube or Gunn Oscillator, is
allowed to form standing waves in the slotted waveguide section after being reflected
from the short circuiting plunger in the dielectric cell, which is initially kept at its
lowest position in the cell. The probe in the slotted waveguide section is accurately
adjusted at the node of the standing waves, as adjudged by the position of the minima
in the indicating meter. Now a small quantity of food grain powder is introduced in
the dielectric cell and the plunger is brought over it by moving the micrometer screw
till a proper contact is established. The height h of the powder in the dielectric cell is
determined from the difference of readings on the scale of micrometer screw taken
with and without food powder in the cell. The position of minima in the slotted
section shifts either towards the receiver or towards the generator on introducing the
powder in the cell. The shift is towards the receiver when h < (λd/4) and towards the
generator when (λd/4) < h < (λd/2). If h1 and h2 are two heights of the powder
column in the cell for which equal shift of minima position is obtained towards the
receiver and the generator respectively, then
1
d g
2 2h x (3.52)
2
d g
2 2h x (3.53)
where λg is the guide wavelength.
Combining equations (4) and (5) we obtain
1 2
d
2(h h ) (3.54)
or
d 1 22(h h ) (3.55)
Theory and Methods 64
Alternatively, we may go on adding slowly the powder in the dielectric cell
till for a height h of the powder in the cell, the position of minima in the slotted
section is the same as for the empty cell. For this position
dh2
Or d 2h (3.56)
Eq. (3.56 ) permits us to directly determine the value of λd..
3.5.2.iii Measurement of αd
Let Ei and Er be the amplitudes of the incident and reflected fields respectively
forming standing waves in the slotted guide carrying the probe. Assuming no loss in
reflection, Er = Ei with no sample in the sample holder, if the movable probe is
located at maximum position and the indicating meter gives a deflection of x1 units,
we may write
E i + E r α √x1 (3.57)
On introducing the sample of length L in the sample holder and locating the
movable probe at the resulting maximum position, the output shown by the
indicating meter will change to x2 units due to partial absorption of the e.m. waves.
The absorption takes place twice, once when the incident wave travels through the
sample and again when the reflected wave travels through it. Therefore, Er becomes
Er = Ei e-2αL
(3.58)
Again at the maximum, we have
Ei + E r = (Ei + Ei e-2αL
) α √x2 (3.59)
From equations (3.58 ) and (3.59 )
1
d
2 1
x2.303log
2h ' 2 x x (3.60)
For measuring αd we start with the empty cell, the plunger being kept at the
bottom of the cell. The probe is located at one of the maximas, i.e., at the position of
a voltage antinode in the waveguide slotted section, and reading x1 of the indicating
Theory and Methods 65
meter is noted. The powder (flour of the food stuff in the present case) is now added
slowly in the dielectric cell and position of the maxima in the slotted section is noted
every time from the indicating meter. The height of the powder column in the
dielectric cell (h') is accurately adjusted so that the probe position locating the
maxima in the slotted section is again the same as with the empty cell. The deflection
x2 of the indicating meter in this state, for such height h' of the powder column, is
noted. In this experiment the electromagnetic waves travel twice through the powder
column in the cell before they form stationary waves in the slotted waveguide
section, after being reflected from the plunger of the dielectric cell. For obtaining
appreciable absorption of the wave, height of the powder column in the cell is taken
equivalent to several λd. The value of the αd is then calculated using equation (3.60) .
3.5.3 Two Point Method Using Solid Dielectric Cell
A most widely used and simple microwave measurement technique to measure
the complex permittivity of solid materials, which could be shaped in the size of the
waveguide for preparation of samples, is the two point method which involves the
solution of a transcendental equation. The input impedance of a short circuited
waveguide is measured with and without the sample placed in the waveguide, shift
in minima position is noted for the sample and a transcendental equation is solved to
obtain dielectric properties of the material. A proper solution out of many is chosen
on the basis of approximate value of dielectric constant of the material. If the
approximate dielectric constant is not known, then two such measurements are
carried out with samples of different lengths.
Two point method (Sucher and Fox, 1963; Behari, 2005) is a technique
involving measurement of reflection coefficient of a solid material in a wave guide,
backed by a short circuiting conducting plate. This method is suitable for low and
medium loss dielectrics and can be adopted for measurement of dielectric properties
of food stuff in powder form.
3.5.3.i Theory
Figure (3.7 a) shows an empty short-circuited waveguide dielectric cell with
a probe located at a voltage minimum DR. Figure (3.7 b) shows the same waveguide,
Theory and Methods 66
containing a sample of length lε with the probe located at a new voltage minimum D.
The sample is kept adjacent to the short circuit. At the open boundary of the sample
as shown in Fig. 3.7 (b), impedance equation can be written as
Z0 tan βl = −Zε tan βε lε (3.61)
(a) (b)
Fig. 3.10: (a) Wave guide with a short circuit ;(b) wave guide loaded with a
sample and short circuit
Similarly in figure (3.7a), looking toward the left, one can write
Z0 tan β (lR + lε) = 0 (3.62)
Now, consider
tan β (DR – D + lε ) = tan β [(lR + lε) – (l + lε)+ lε ]
= tan β[(lR + lε) –l ]
=–
= - tan βl (3.63)
Since, tan β (lR + lε) = 0 from equation (3.60)
From equation (3.59), tan βl = [- tan βεlε (3.64)
tan β (DR – D + lε ) = - [- tan βεlε (3.65)
But, = which gives
Zε
Theory and Methods 67
tan β (DR – D + lε ) = tan βεlε (3.66)
Dividing both sides of this equation by βεlε, we get
Rtan (D D l tan l
l l (3.67)
In equation (3.67) all the quantities on the left hand side are measurable,
where as the right hand side term is of the form tan Z /Z,with Z = βε lε, so that once
the measurements have been carried out, the complex number, Z = βε l ε, can be
found by solving the transcendental equation, and from it, βε can be determined.
There exist infinite number of solutions of the transcendental equation for εr. To
obtain proper solution, the measurements are carried out on two samples of different
sample length lε and lε'. A solution common to the two sets of solutions will be the
proper solution for εr . The solution is given by the “intersection point” of the two
curves shown in the Fig. 3.8.
Fig. 3.11: Two sets of solutions for two samples of different lengths, point of
intersection represents the proper solution
It should be noted that the accuracy of the experimental results of complex
permittivity y using this method depends to a large extent on the smoothness of the
sample, the fitting of the sample in the waveguide, the care which should be taken to
ensure that its surfaces are made flat and properly shaped as „rectangular‟ fitting
with the dimensions of the waveguide, the accuracy of measurement of length lε of
Theory and Methods 68
the sample, the positions of minima DR and D and the accuracy in the measurement
of VSWR.
3.5.3.ii Experimental Set Up for Estimation of Complex Permittivity of Powders
Employing Two Point Method
For using this method for powders, the waveguide is bent through 90° by
means of a E-plane bend and terminated by a specially designed dielectric cell in
which powder sample is filled up. In this method, the experimental set – up for
measurement of dielectric properties of powders is shown in figure 3.9, where the
details of components used in the microwave bench are self explanatory. First with
no sample in the dielectric cell, the position of the first minimum DR in the slotted
section is noted. Now the powder sample is filled up in the dielectric cell and
compressed by using the hydraulic press and applying pressure which the dielectric
cell can withstand. The height of the compressed sample in the cell is noted, say it is
lε. Then the position of the first minimum D on the slotted line and coressponding
VSWR are measured. The VSWR is measured by a micrometer or VSWR meter.
For the measurement of VSWR using micrometer no amplitude modulation is
applied to the microwave signal but when the VSWR meter is connected, the
amplitude modulation is applied to the microwave signal, by using internal
modulation in Klystron power supply or by using a pin diode if a Gunn diode is used
as microwave source. The accuracy of measurements of dielectric constant of
powders by this method has been estimated to be of the order of 5% whereas the
accuracy for the measurement of dielectric loss is within 10%.
Fig. 3.12: Experimental setup for determination of dielectric properties of
powders by two point method
Theory and Methods 69
The transcendental equation obtained by impedance matching at the
boundary of flat surface of powder and air can be written as
Rtan (D D l tan l
l l (3.68)
Where β = ( 2π / λ g), λ g being the waveguide wavelength;
and βε = ( 2π / λ0) { εr μr – (λ0 / λ c)2}
1/2, λ0 being free space wavelength and λ c
is the cut off wavelength of the waveguide.
The propagation constant β in powder is calculated, by using
β = ( 2π / λ g) (3.69)
where, λg =2 x (distance between successive minima with empty short
circuited wave- guide sample holder)
The phase difference in the waves traveling in the guide with and without
dielectric is given by
θ = 2 β (∆ x – lε) (3.70)
where ∆ x is the shift in minima position
We determine voltage standing wave ratio for the load (food powder in this
case) and compute magnitude of the reflection coefficient (│Г│ ) by employing the
following relation:
│Г│ = (S- 1) / (S+1) (3.71)
where S is the VSWR for the sample.
In two point method, the complex dielectric constant is given by
j
j
1 e1 tan XC
j l 1 e X (3.72)
The transcendental equation provides several solutions for X θ, which can
be found by employing graphs and tables provided for solution of such equations by
Hippel (1954) or alternatively the problem may be solved by using a mathematical
tool like MATLAB. The experiment is repeated with a different length ( lε') of the
Theory and Methods 70
sample compressed to the same pressure as used in the first case. The common root
of solutions obtained for the two cases, on using samples of different lengths, is
chosen for evaluation of the admittance. Alternatively we may perform the experiment
for a given sample at two different frequencies to obtain the correct root X θ.
The admittance (Yε ) of the material of the sample is given by
XY 2( 90 ) G jS
l (3.73)
where Gε and Sε are respectively the normalized conductance and normalized
susceptance of the sample.
The values of Gε and Sε are obtained by separating Equation (3.71) in to real
and imaginary parts, from which the values of ε' and ε'' can be calculated in the
following form:
2
g
2
g
G ( / 2a)'
1 ( / 2a) (3.74)
2
g
S''
1 ( / 2a) (3.75)
A computer program in Matlab may be used to solve the transcendental
equation and obtain the values of dielectric constant (ε') and loss factor (ε''), by
using equations (3.74) and (3.75).
3.6 Dielectric Mixture Equations
Dielectric mixture equations can be used to estimate the dielectric properties
of the solid material from the properties of an air-particle mixture, made up of air
and the pulverized particles of the solid. To use such equations, one needs to know
the complex permittivity (ε*) of the pulverized sample at its bulk density, i.e., the
air- particle mixture density (ρ). If the density of solid material is ρ2, the fractional
part of the total volume of the air-particle mixture occupied by the particles (i.e., the
volume fraction occupied by the solid in the mixture), v2 is then given by ρ / ρ2.
In the present work two component dielectric mixture equations are proposed
to be used, in which ε represents the complex permittivity of the mixture, ε1 is the
Theory and Methods 71
complex permittivity of the medium (air in the present case, for which ε1 = 1 _
j0), in
which particles of the solid material having complex permittivity ε2 are dispersed, v1
and v2 being the volume fractions of the medium (i.e., the air in this case) and the
solid material (i.e. the bulk solid material of food powder) respectively, such that v1
+ v2 = 1.
The formulation of the dielectric mixture equations to be used in the present
work are as given below (Nelson,1991):
i) Complex refractive index mixture equation:
1/ 2 1/ 2 1/ 2
1 1 2 2( ) v ( ) v ( ) (3.76)
ii) Landau and Lifshitz, Looyenga equation:
1/3 1/3 1/3
1 1 2 2( ) v ( ) v ( ) (3.77)
iii) Böttcher‟s equation :
1 2 1
2
2
v3 2
(3.78)
iv) Bruggeman – Hanai equation:
1/3
2 12
1 2
1 v (3.79)
v) Rayleigh‟s equation:
1 2 1
2
1 1 2
v2 2
(3.80)
3.7 Estimation of Nutrients
The basic aim of estimation is to evaluate the nutrients in the food grains by
using the standard methods available for estimation of nutrients, viz., moisture,
protein, fat, ash, crude fiber and carbohydrate. The estimation of nutrients was carried
Theory and Methods 72
out using standard reagents and glasswares. All the analytical instruments used were
standardized and calibrated before use, as per their respective specified methods.
The nutrients analyzed, for the present study, in food grains are moisture by
oven drying, protein by Micro Kjheldal Method, fats by ether extraction method, ash
and crude fiber by acid alkali method. The carbohydrate is estimated by the
difference method. Proximate analysis for estimation of different nutrients is done as
per procedure given below:
3.8.1.i. Moisture (AOAC,2005)
Procedure – About 5 g of the prepared sample is weighed accurately in a tarred
aluminium dish with a cover, having a diameter of at least 50 mm and a depth of
about 40 mm. The dish is shaken until the content is evenly distributed. With cover
removed, the dish is placed in an air oven maintained at102 2°C and heated for
about 3-4 hours . After cooling it to the room temperature, it is weighed.The process
of heating, cooling and weighing is repeated until the difference in weight between
two successive weighing is less than one milligram.
Calculation –
Moisture, percent by mass = 1 2
1
100( )W W
W W
where,
W1 = weight in g of the dish with the material before drying,
W2 = weight in g of the dish with the material after drying, and
W = weight in gram of empty dish
3.8.1.ii Crude Protein (AOAC,2005)
Principle – The percentage of crude protein is ascertained by multiplying the
percentage of nitrogen other than ammoniacal nitrogen by a factor. The factor used
in the present case is 6.25
Apparatus – Kjeldahl flask distillation assembly: The assembly consists of a
round bottom flask of a 1000 ml capacity fitted with a rubber stopper through which
Theory and Methods 73
passes one end of the connect in bulb tube. The other end of the bulb tube is
connected to the condenser, which is attached by means of a rubber tube to a dip
tube, which dips into a known quantity of the solution of standard sulphuric acid and
boric acid, contained in a conical flask of 500 ml capacity, to which 3 to 4 drops of
methyl red indicator solution are added.
Reagents-
1. Potassium Sulphate or Anhydrous Sodium Sulphate
2. Copper Sulphate
3. Concentrated Sulphuric Acid – sp gr. 1.84( IS:266-1961)
4. Sodium Hydroxide Solution – About 450 g of sodium hydroxide is dissolved
in 1000 ml of water.
5. Standard Sulphuric Acid – 0.1 N
6. Standard Sodium Hydroxide Solution – 0.1 N
7. Methyl Red Indicator Solution – 1 g of methyl red is dissolved in 200 ml of
rectified spirit (95 percent by volume)
8. 60 g of boric acid is dissolved in 2 litre of hot water; cooled to room
temperature and allow maturing for 3 days before decanting the clear liquid.
9. Magnesium Oxide – carbonate free freshly ignited.
Procedure
Total Nitrogen - About 2 g of the prepared sample is accurately weighed and
carefully transferred to the Kjeldhal flask. About 10 g of potassium sulphate or
anhydrous sodium sulphate, about 0.5 g of copper sulphate and 25 ml or more, if
necessary, of concentrated sulphuric acid is added. The flask is placed in an inclined
position, and heated to a temperature below the boiling point of the acid, until
frothing ceases. Heating is continued until the acid boils vigorously and digested for
a time after the mixture is clear or until oxidation is completed ( about 2 hours). The
contents of the flask are cooled and transferred quantitatively to the round bottom
flask with water, the quantity of water used being about 200 ml. Few pieces of
pumice stone are added to prevent bumping. Sodium hydroxide solution is then
added carefully in quantity which is sufficient to make the solution alkaline,by the
side of the flask so that it does not mix at once with the acid solution but forms a
Theory and Methods 74
layer below the acid layer. The apparatus is assembled taking care that the tip of the
dip – tube extends below the surface of the standard sulphuric acid solution in the
receiver. The contents of the standard sulphuric acid solution is then thoroughly
mixed. Titration with standard sodium hydroxide solution is done and a blank
determination is carried out using all reagents in the same quantities but without the
material to be tested.
Alternatively, the ammonia evolved by distillation is absorbed in boric
acid.The digestion is carried out as prescribed earlier. The contents of the digestion
flask are transferred completely through the separating funnel. The separating funnel
is rinsed with water. The total volume of the liquid in the distillation flask should not
exceed half the capacity of flask otherwise frothing may occur. Excess of sodium
hydroxide solution is then added to make the solution alkaline. The round- bottom
flask is then connected immediately to steam trap and condenser. The condenser is
arranged to dip the dip-tube in 50 ml of boric acid which is kept cool in the conical
flask. 2 or 3 drops of the mixed indicator are added to the flask. About one third of
total volume of the solution is distilled in the flask. The distillation assembly is
cooled and dismantled. The tip of the condenser and the dip – tube are rinsed with
water. The washings are collected in the receiver. The ammonia present in the
distillate is titrated with sulphuric acid until the grass – green colour changes to steel
grey, an addition of one drop of acid giving the purple colour.
Calculation –
Total nitrogen ( on moisture- free basis) = –
Percent by mass
where
B = Volume in ml of the standard sodium hydroxide solution used to
neutralize the acid in blank determination.
A = Volume in ml of the standard sodium hydroxide solution used to
neutralize the excess acid in the test with the material.
N = normality of the standard sodium hydroxide solution.
m = mass in g of the material for the test.
Theory and Methods 75
M = moisture percentage.
When boric acid has been used for absorption, calculation of total nitrogen
are given below:
Total nitrogen (on moisture - free basis) =
percent by mass
where,
V = volume in ml of standard sulphuric acid used in titration.
N = normality of the standard sulphuric acid.
m = mass in g of the material taken for test and
M = moisture percentage.
3.8.1.iii.Crude Fat (AOAC,2005)
Reagents-
Petroleum ether of boiling range 40 °C to 60 °C
Hexane, food grade-conforming to IS : 3470-1966.
Procedure – About 2.5 g of the dried material is taken and weighed accurately as
described earlier and then it is extracted extracted with petroleum ether or hexane,
food grade, in a Soxhlet or other suitable extractor. The extraction period may vary
from 4 hours to 6 hours. The extract is dried on a steam – bath for 30 minutes,
cooled in a dessicator and weighed. The process of alternate drying and weighing is
repeated at intervals of 30 minutes until the difference between two successive
weighing is less than one mg. The lowest mass of the sample is noted.
Calculation –
Crude fat (on moisture free basis), Percent by mass = –
Where,
M1 = mass in g of the extraction flask with dried extract
M2 = mass in g of the extraction flask, and
M = mass in g of the dried sample taken for the test.
Theory and Methods 76
3.8.1.iv Crude Fiber (AOAC,2005)
Reagents –
Sulphuric acid – 0.255 N [1.25 per cent (m/v)], accurately prepared.
Sodium hydroxide solution – 0.313 N [1.25 percent (m/v)], accurately prepared.
Procedure – About 2 g of the dried material is taken and weighed accurately and
the fat is extracted for about 8 hours with petroleum ether or hexane, food grade,
using a Soxhlet or other suitable extractor or the residue from the crude fat
determination. The fat free dry residue is transferred to a one liter conical flask.
200 ml of dilute sulphuric acid is taken in another flask and was heated to
boil. The whole of the boiled acid is transferred to the flask containing the fat free
material and the flask is immediately connected with a reflux water condenser and
heated, so that the contents of the flask begin to boil within one minute. The flask is
rotated frequently, not permitting the material to be deposited on the sides of the
flask, out of contact with the acid. Boiling is continued for 30 minutes and then the
flask is removed and the content of the flask is filtered through fine linen (about 18
threads in the centimeter) held in a funnel and washed with boiling water until the
washings are no longer acidic to litmus. Now the filterate is mixed with some
quantity of boiled sodium hydroxide solution under a reflux condenser and boiled
again for 30 minutes. The flask is then removed and its contents are immediately
filtered through the filter cloth. The residue is thoroughly washed with boiled water
and transferred to a Gooch crucible prepared with a thin but compact layer of ignited
asbestos. The residue is washed thoroughly first with hot water and then with about
15 ml of 95 % (by volume) ethyl alcohol. The Gooch crucible and contents are dried
at 105±1ºC in the air oven till it attains constant mass. It is then cooled and weighed.
The contents of the Gooch crucible is incinerated at 600±20 ºC in a muffle furnace
until all the carbonaceous matter is burnt. The Gooch crucible containing the ash is
cooled in a dessicator and weighed.
Calculation –
Crude fiber (on moisture free basis), Percent by mass = –
where,
M1 = mass in g of Gooch crucible and contents before ashing
Theory and Methods 77
M2 = mass in g of Gooch crucible containing asbestos and ash, and
m = mass in g of the dried material taken for the test
When the residue from fat determination is used.
Crude fiber (on moisture free basis) = (M1 – M2) (100-f ) percent by mass
Where,
M1 = mass in g of Gooch crucible and contents before ashing
M2 = mass in g of Gooch crucible containing asbestos and ash
f = crude fat ( on moisture free basis),percent by mass, and
m = mass in g of the fat free material taken for the test.
3.8.1.iv Ash (AOAC, 2005)
Procedure - About 2 g of the dried material is taken and weighed accurately in a
tarred porcelain, silica or platinum dish. It is then ignited with the flame of a Meker
burner for about one hour. The ignition is completed by keeping it in a muffle
furnace at 550± 20 ºC until grey ash results. It is then cooled in a dessicator and
weighed. The dish is ignited again in the muffle furnace for 30 minutes, cooled and
weighed. This process is repeated until difference in mass between two successive
weighings is less than 1 mg. The lowest mass of the dish and its contents is noted.
Calculation -
Total ash (on moisture free basis) percent by mass = –
M2 = the lowest mass in g of the dish with the ash.
M = mass in g of the dish, and
M1= mass in g of the dish with the dried material taken for the test.
3.8.1.v. Carbohydrate (AOAC 2005)
Principle – The carbohydrate estimation method used in the present study is based
on the principle that total carbohydrates can be estimated by the difference between
total weight of the sample and sum of the estimated values of moisture, protein, fat,
ash and crude fiber present in the sample.
Theory and Methods 78
Procedure – A sum of values (g /100g) of moisture, protein, fat, ash and crude fiber
is subtracted from 100 g to get the carbohydrate content (g / 100g) of sample.
Formula –
Carbohydrate (g /100g) = 100 - [Moisture + Protein + Fat + Ash + Fiber] (g
/100g of sample)
3.8.2. Correlation Between Dielectric Properties and Food Nutrients
After practical determination of the dielectric properties and nutrients of the
food samples, attempts are made to establish a correlation between the two types of
properties by employing the SPSS software and linear and curvilinear regression
techniques.