th
THE 8 INTERNATION
NAL SYMPOSIUM ON ADVANCED TOPICS IN ELECT
May 23-25, 2013
Bucharest, Romania
Thermal Ageing Effects
E on the Dielectriic Properties
and Moisture Conntent of Vegetable and Mineral Oil
Used In
I Power Transformerss
Laurentiu Marius Dumitran1, Member
Me IEEE, Alexandra Ciuriuc1 and Petru V. Notinghher1, Member IEEE
1
University POLITTEHNICA of Bucharest, Laboratory of Electrical Mateerial,
Splaiul Inddependentei, No. 313, 060042, Bucharest, Romania
dumitran@elmaat.pub.ro, aciuriuc@elmat.pub.ro, petrunot@elmat.pubb.ro
Abstract- The operational safety of transmissiion and distribution
grids depends essentially on the power transformers’ state.
Lately, there is a tendency to replace mineral oils with vegetable
oils because vegetable oils provide a higher explosion safety
aspect for transformers due to their higher fire
f points. Further,
vegetable oils are favorable for the environ nment due to their
higher biodegradability. The focus of the present
p paper is to
study the properties of mineral and vegetablee after these oils are
exposed to accelerated thermal ageing. Veggetable and mineral
oil samples were subjected to accelerated th hermal ageing (with
and without cellulosic paper) at three diffeerent temperatures:
135 °C, 155 °C and 175 °C. The dielectricc properties of the
samples (relative permittivity, loss factor and
a resistivity) and
their water content were determined for different ageing
durations. The results show that in the case c of mineral oil
samples, there is a direct relation between n the water content
values and the dielectric properties. How wever, the obtained
results indicate that the water content does noot fully characterize
the ageing condition of vegetable oil.
Keywords: power transformers, vegetable and mineral oils,
thermal ageing, dielectric properties, water coontent
I. INTRODUCTION
N
In recent years, the use of vegetable oils instead of mineral
oil is gaining a lot of attention. Today, a majority of the
power transformers which operate in transmission and
distribution grids have mineral oil im mpregnated paper
insulation and a large volume of mineraal oil is used [1].
Although mineral oil has excellent electriic properties and a
good thermal stability that has been proven p over time,
environmental considerations in recent tiimes have always
raised a concern on their continuous usagee [2]. Conventional
mineral oil is obtained through petroleum m refining and they
are usually non-biodegradable and can harm m the environment
for many years.
From this point of view, vegetable oils (or natural esters)
appear to meet the requirements necesssary for insulation
systems of power transformers. First of all, vegetable oils that
are specially designed for electric insulatioon and heat transfer
purpose, have high biodegradability theereby causing less
harm to the environment. In addition, theyy increase the fire-
safety aspect in transformers due to theirr higher fire-point
values as compared to mineral oil and theyy have appropriate
electric properties and thermal stability [22-4]. However, the
continuous use of vegetable oils in insuulation systems of
978-1-4673-5980-1/13/$31.00 ©2013 IEEE
TRICAL ENGINEERING
power transformers requires a good knowledge of their
behavior over time. Perform mance of vegetable oils in
combination with cellulosic paaper and stability of these oils
under thermal, electric and ennvironmental stress should be
understood.
Information concerning the general
g properties of vegetable
oils (viscosity, flash and fire pooint etc.) is presented in [5-7],
and the gas content of these oils is analyzed in [2]. In a
previous study [8], it has been shown that the electric
properties of vegetable oil (thee relative permittivity εr’ and
loss factor tgδ) under accelerateed thermal stress increase with
ageing time and temperature. The moisture content and its
effect on the electric properties of vegetable oils and mixtures
of mineral and vegetable oils haave been discussed in literature
[4-7, 9-15]. Numerous studies concerning the variations of
water content, permittivity, losss factor, electric conductivity
and breakdown voltage with resspect to the ageing temperature
and duration have also been reported [4, 6-7, 12, 14-15].
Generation of acids in natural esters
e under thermal stress has
also been discussed [5, 7, 16]. Acids are known to be one of
the ageing by-products of ceellulosic paper and oils. The
autocatalytic effect of the acids accelerates the ageing process
of the oil and paper which can influence the measured
properties [16, 17]. It has been shown that paper in vegetable
oil contains fewer amounts off low molecular weight acids
compared to the case with minneral and this is an advantage
for vegetable oils because thesee acids are very dangerous for
cellulose-based products [5]. Liifetime estimation of vegetable
oil is presented in [2] and severaal comparative studies focused
on the properties of mineral, sillicone and vegetable oils [4, 6,
11-12, 15, 18].
The present paper focuses on the effect of accelerated
thermal stress on the electric prroperties (real part of complex
permittivity, loss factor and ressistivity) and moisture content
of vegetable oil. Possible correelations between the variation
of electric properties and moissture content are investigated.
Samples of vegetable oil weere subjected to accelerated
thermal ageing and the electricc properties and water content
were determined at different ageing
a durations. For a better
understanding, the obtained reesults for vegetable oil were
compared with those of mineraal oil samples aged under the
same conditions.

Fig. 1. The hydrolysis reaction of vegetable oils [20]
II. AGEING MECHANISMS OF OILS
When power transformers are in operation, their insulation
systems consisting of oil and paper are subjected to different
stresses. Amongst these stresses, thermal stress is the most
important because it causes degradation reactions, thereby
worsening the properties of the oil.
Vegetable oils used for electric insulation are based on
triglyceride chemistry with saturated and unsaturated fatty
acids attached to the glycerol backbone [8]. Due to the nature
of the chemical structure, vegetable oils are more hygroscopic
and can also undergo hydrolysis. Further, vegetable oils are
also prone to oxidation wherein, the rate of oxidation depends
on the types and concentration of fatty acids. The main
reactions that cause the degradation of the vegetable oil are
oxidation and hydrolysis, and the resulting by-products are
gases (CO, CO2), water and acids [19]. The unsaturated bonds
in the fatty acids lower the oxidation stability of the natural
ester because the oxygen molecule disrupts the fatty acid at
the carbon double bond. Therefore, for higher un-saturation
levels, the number of double bonds is higher and the oil
becomes more susceptible to oxidation [20].
Besides oil ageing, the degradation of the cellulose paper
should also be taken into account because the resulting by-
products reach the oil and change its properties. Due to the
influence of temperature, chemical reactions take place in
cellulosic paper, and several by-products like CO, CO2, H2O,
H2, CH4 and furans are generated [8].
Water, which is a by-product of oil and paper degradation
reactions, can exist in transformers in different states. Most of
the water in oil is found in the dissolved state. After it
exceeds the saturation value, free water precipitated from the
oil will be found in suspension or drops [21].
The moisture content in the oil can be characterized by the
absolute (wabs) and, relative (wrel) values. The relative
moisture content in oil is represented by the ratio of the
absolute moisture content (wabs) of oil for a given temperature
T and the saturation water content at the same temperature T
(wL(T)) [14]:
Fig. 2. Trans-esterification of cellulose [20].
CnH2n+2 → CnH2n + H2
Alkane → Alkene + Hydrogen
Cm+nH2(m+n)+2 → CmH2m + CnH2n+2.
n-Alkane → Alkene + Alkane
Fig. 3. Cracking and dehydrogenation reactions of mineral oil.
wabs . (1)
wrel =
wL (T )
At room temperature, the saturation limit of vegetable oil is
about 3000 mg/kg, compared to 60 mg/kg for mineral oil
[20]. Due to this significant difference, even though the
vegetable oil has absolute moisture content higher than
mineral oil, the relative moisture content of the vegetable oil
is much lower. This could have a positive effect on the global
insulation system because the vegetable oil absorbs the water
from the paper and in this way it keeps the paper drier.
Moreover, the hydrolysis reaction (Fig. 1) that takes place in
the oil is also beneficial for the cellulose insulation. The free
fatty acids that are formed in the vegetable oil as a result of
the hydrolysis reaction participate in a trans-esterification
reaction in the cellulose (Fig. 2). The reactive hydroxyl
groups on the cellulose molecule become esterified with fatty
acids in vegetable oil and it prevents the paper from further
degradation [20].
Concerning the degradation of the mineral oil, this topic
was much studied and is better known. The main reactions
that lead to the degradation of the mineral oil are the cracking
reaction (which leads to the C-C bonding scission and forms
alkanes and alkenes), oxidation and dehydrogenation (Fig. 3)
[8]. High temperature accelerates the mineral oil oxidation
and some metals like copper act as a catalyst. The presence of
oxygen can degrade the hydrocarbons through processes
based on free radical reactions, which generate hydro
peroxides [22, 23] which are unstable and decompose to free
radicals finally leading to the appearance of water, ketones
and other by-products [24].
III. EXPERIMENTAL SET-UPS AND SAMPLES
The experiments were performed on commercially
available natural ester and mineral oil meant for power
transformer applications. In order to perform the ageing of the
oil samples, 15 controlled clean stainless steel ageing cells
were used. The first five of these were filled with vegetable
oil, the next five cells were filled with vegetable oil and 10
samples of 0.25 mm thick Weidmann cellulose paper and the
last five cells were filled with mineral oil. Each ageing cell
contained 8.4 grams of paper, 9 grams of copper and 23
grams of iron. Further, for clarity, the investigated oil samples
will be called A – vegetable oil aged in presence of copper
and iron, B – vegetable oil aged in presence of cellulosic
paper, copper and iron and C – mineral oil aged in presence
of copper and iron.
 10.0 1.6
9.5
9.0
Real part of relative permittivty
1.4

Resistivity · 10 (ohm·m)
8.5
8.0 1.2
7.5
7.0 1

-11
6.5
6.0 0.8
5.5
5.0 0.6
4.5
4.0 0.4
3.5
3.0 0.2
2.5
2.0 0
0 200 400 600 800 1000 1200 1400 1600 0 200 400 600 800 1000 1200 1400 1600
Ageing time (h) Ageing time (h)

Fig. 4. Variation of real part of relative permittivity for A samples (|, U, Fig. 6. Variation of resistivity for A samples (|, U, †), and B samples (z,
†), and B samples (z, S, „) aged at 135 °C (|,z), 155 °C (U, ▲) and S, „) aged at 135 °C (|,z), 155 °C (U, ▲) and 175 °C (†, „) (U0 = 40
175 °C (†, „) for f = 1 mHz. V).

All ageing cells, fully sealed, were introduced in the drying

oven at three different temperatures (135 °C, 155 °C and 175
°C) for a total of 1250 h. Three ageing cells containing each
type of sample (A, B and C) were extracted every 250 h and
the following properties of the oils were determined: the real
part of the complex relative permittivity εr’, the loss factor
tgδ, the resistivity ρ and the absolute water content wabs.
The resistivity of the oil’s samples was calculated using the
values of absorption/resorption currents [8] measured with a
Keithley 6517 electrometer and an Irlab liquid measuring
cell. The value of the DC applied voltage was U0 = 40 V. In
order to determine the dielectric loss factor and the
components of the complex relative permittivity, a
Novocontrol impedance analyzer was used. The applied
voltage had the value of 1V and the electric field frequency
was in the range of 10-3 – 103 Hz. The ambient temperature
during the measurements was 28°C. The absolute water
content was measured using a Karl-Fischer coulometer.
450
400
350
300
250
Loss factor
IV. RESULTS AND DISCUSSIONS
Figs. 4-6 present the variations of electric properties of
samples A and B of vegetable oil as a function of ageing
duration, τ. It can be seen that the values of εr’ and tgδ
quantities increase with ageing time. Also, the increase in εr’
and tgδ with ageing time is more pronounced at higher
temperatures. On the other hand, the resistivity decreases with
time and this variation is faster at higher temperatures.
Obviously, for A samples, these changes in the electric
properties are exclusively due to the vegetable oil degradation
which has no contact with the environment during ageing
process. In the case of B samples, the degradation by-
products of cellulosic paper which reach the oil can also
modify the measured properties.
The increase of the real part of complex relative
permittivity (Fig. 4) may have a common reason based on the
increase in polar by-products of chemical degradation
reactions. For lower temperature (135 oC and 155 oC) and
ageing duration shorter than 1000 h, the variation of εr’ is not
significant which means that no important degradation rate
exists. However, for 175 oC, εr’ strongly increases and that
indicates an accelerated degradation process. Fig. 5 indicates
that the vegetable oil’s loss factor increases steeply with

ageing time. This shows that polarization and conduction

200 phenomena intensify in time (especially for samples
150 submitted to 175 oC). Fig. 6 shows the decrease of the oil’s
resistivity with the ageing time which is due to the increase of
100
charge carrier’s concentration as a result of degradation
50 process.
0 In the case of the tgδ and ρ properties, there are three
obvious distinct intervals (dependent on the ageing
0 200 400 600 800 1000 1200 1400 1600 temperature) in which the values of the properties for samples
Ageing time (h) B are higher or lower than those of samples A (Table 1). In
the first interval (I), the loss factor and resistivity values for
Fig. 5. Variation of the loss factor for A samples (|, U, †), and B samples vegetable oil aged in the presence of paper (respectively, tgδB
(z, S, „) aged at 135 °C (|,z), 155 °C (U, ▲) and 175 °C (†, „) for f =
1 mHz.
 5.0
5.0 4.5
4.8 4.0
Real part of relative permittivity

Resistivity·10 (ohm·m)
4.6 175 °C
3.5
4.4 155 °C
3.0 135 °C
4.2
135 °C

-11
4.0 2.5
3.8 155 °C 2.0
3.6 1.5
3.4 175 °C 1.0
3.2 0.5
3.0
0.0
2.8 0 200 400 600 800 1000 1200 1400 1600
0 200 400 600 800 1000 1200 1400 1600 Ageing time (h)
Ageing time (h)
Fig. 9. Variation of the resistivity for C samples aged at 135 oC (z), 155 oC
Fig. 7. Variation of the real part of complex relative permittivity of C („) and 175 oC (S) as a function of ageing time (U0 = 40 V).
samples aged at 135 oC (z), 155 oC („) and 175 oC (S) as a function of
ageing time (f = 1 mHz). concentration, which determines an increase of tgδ and ρ
values for the B samples compared to the A samples. This
and ρB) are higher than those corresponding to the samples model is verified completely in the case of the tests
aged in the absence of paper (tgδA and ρA). This could be due performed at 175 oC and partially for the ones performed at
to the absorption of water in paper and to the increase of the 155 oC and 135 oC.
concentration and mobility of electric dipoles and charge The variations of electric properties of mineral oil samples
carriers. aged under same conditions were investigated and are
TABLE I presented in Figs. 7 -9. As expected, the quantities εr’ and tgδ
LOSS FACTOR AND RESISTIVITY FOR A AND B OIL SAMPLES FOR DIFFERENT increase with τ while the resistivity decreases. Similar results
AGEING TIME τ
were presented in [25] and indicate that a degradation process
Ageing time [h] I II III takes place in mineral oil submitted to thermal stress. Given
o
T = 135 C 0 - 500 500 - 1200 > 1200 that the ageing of mineral oil was done in sealed cells, (like in
T = 155 oC 0 - 350 350 - 600 > 600 the case of A and B samples), the variations of mineral oil’s
T = 175 C o
0 - 300 300 - 500 > 500 electric properties are exclusively due to the by-products
which result from chemical degradation reaction of the oil.
tgδB : tgδA tgδB > tgδA tgδB < tgδA tgδB > tgδA
Figures 10-12 present the variation of absolute moisture
ρB : ρA ρB > ρA ρB < ρA ρB > ρA content as a function of ageing time in samples A, B and C
respectively. As it can be seen in Fig. 10, in the case of the
At higher ageing durations (interval II), part of the water is vegetable oil aged at 135 °C and 155 °C, the water content
consumed in the hydrolysis reaction, which leads to an increases in the first 300 hours of ageing and then decreases
increase of tgδ and ρ values for samples A compared to for the rest of the ageing time. Similar results were presented
samples B. During interval III, the paper degradation in [15]. This variation can be explained by the different
contributes more to the increase of charge carrier’s
140 330
300
120
270
100 240
Water content (ppm)

155 °C 210 135 °C

80
Loss factor

180
60 150
175 °C
40 120 155 °C
90 175 °C
20 135 °C
60
0 30
0 200 400 600 800 1000 1200 1400 1600 200 400 600 800 1000 1200 1400 1600
Ageing time (h) Ageing time (h)

Fig. 8. Variation of the loss factor of C samples aged at 135 oC (z), 155 oC Fig. 10. Variation of water content of A samples aged at 135 oC (z), 155 oC
(„) and 175 oC (S) as a function of ageing time (f = 1 mHz). („) and 175 oC (S) as a function of ageing time.
 200 60
180

Relative water content (%)

50
160
Water content (ppm)

140 155 °C 40
C
120
30
100
80 175 °C 20
A
60 B
135 °C 10
40
20 0
0 200 400 600 800 1000 1200 1400 1600 0 200 400 600 800 1000 1200 1400 1600 1800

Ageing time (h) Ageing time (h)

Fig. 13. Variation of relative water content of A („), B (z) and C (S)
Fig. 11. Variation of water content of B samples aged at 135 oC („), 155 oC
samples as a function of ageing time.
(z) and 175 oC (S) as a function of ageing time.

degradation reactions that take place in the vegetable oil: at
the beginning of the ageing process the water content
increases due to the degradation process and after this period,
the hydrolysis reaction takes place and it consumes the water
from the oil [15]. This reaction leads to the formation of free
fatty acids. Therefore it can be assumed that during the whole
ageing process the acidity of the oil increases [15], which,
taking into account that the free fatty acids are polar
compounds, could have an influence on the value of the
permittivity.
In the case of the samples aged at 175 °C, the absolute
water content is very low, and that can be probably given by
the fact that the hydrolysis reaction is more intense at a higher
temperature. As it can be seen in Fig. 11, the water content of
oil aged in presence of cellulosic paper takes lower values
compared to those obtained for A samples. This difference
can be explained by the fact that the vegetable oil was aged in
the presence of paper and the trans-esterification reaction of
the cellulose has to be taken into account. During the first 200
– 300 hours of ageing the water content increases rapidly due
40
35
Water content (ppm)
to the transfer of the water from the paper to oil (because of
the high temperature value). For the following 500 – 700
hours of ageing, the water content decreases due to the
hydrolysis reaction and for the rest of the ageing process it
increases again because more water resulted from the trans-
esterification reaction of cellulose is transferred in oil [20].
Regarding the water content in the mineral oil samples
(Fig. 12), it can be seen that for the temperatures of 135°C
and 155 °C, wabs increases with the ageing time. In the case of
T = 175 °C, it can be seen a pronounced increase of the water
content during the first 200 hours of ageing, followed by a
decrease to around 21 ppm. During the last part of the ageing
process (after 650 hours) the water content starts increasing
again and this is most probably due to the oil degradation
[18].
Examining Figs. 7 and 12, it results that in the case of
mineral oil, it can be distinguished a correlation between the
water content in oil and its real part of relative permittivity
and loss factor variations. Thereby, during the first time
interval (τ1, depending of the ageing temperature) the water
content and εr’ increase, in the following time interval τ2 they
decrease, and in the last part of ageing (τ > τ2) they increase
again. Based on this observation it results that the increases of
εr’ and tgδ in the last period of ageing time, are given, among

others factors, by the water which is present in the oil.

30
Fig. 13 presents the variation of relative water content wrel
as a function of ageing time for mineral oil and vegetable oil
25 135 °C
aged without and with paper (samples A and B) at T = 135 °C.
It results that wrel is significantly lower in the case of
20 175 °C
vegetable oil compared to the values obtained for mineral oil.
155 °C Also, it can be seen that, while the relative water content for
15 mineral oil increases in time, in the case of vegetable oil, wrel
increases during the first 350 h and then slowly decreases for
10 the rest of the ageing time. Looking at these results, it appears
0 200 400 600 800 1000 1200 1400 1600 that while in the case of mineral oil, a direct correlation is
Ageing time (h) observed between the relative water content and electric

Fig. 12. Variation of water content of C samples aged at 135 oC („), 155 oC
(z) and 175 oC (S) as a function of ageing time..
properties, but, in the case of vegetable oil such a link is not
evident.
Based on these results, it appears that the estimation of
vegetable oil ageing condition based on the relative or
absolute water content seems to be erroneous.
V. CONCLUSIONS
The results presented in this paper confirm that thermal
ageing results in a variation in the electric properties and
moisture content of vegetable and mineral oils. Also, a
correlation between the variation of absolute and relative
moisture content of mineral oil is observed on one side, and
the variation of its electric properties, on the other side.
In the case of vegetable oil, it has been observed that there
is no evident relationship between the absolute and relative
water content with the dielectric properties. It means that the
water content is not an appropriate diagnostic factor to
estimate the ageing condition of vegetable oil. A possible
explanation could be that the water content does not
contribute to a variation in the dielectric properties of the oil,
but the variation is due to the degradation products resulting
from the chemical reactions that take place between water
and oil (with or without paper).
ACKNOWLEDGMENT
This work has been supported by the Sectorial Operational
Programme Human Resources Development 2007-2013 of
the Romanian Ministry of Labour, Family and Social
Protection through the Financial Agreement
POSDRU/89/1.5/S/62557, POSDRU/107/1.5/S/76903.
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