Ageing phenomena of cellulose/oil
insulation in natural ester and mineral oil
C. Perrier*, M-L. Coulibaly, (Alstom Grid - France)
J. Lukic, V. Vasovic, (Institute Nikola Tesla - Serbia)
Abstract
Degradation of electrical insulation due to ageing by
combination of thermal, oxidative and hydrolytic processes
is one of the main factors that affect power transformer
service life. A better understanding of ageing phenomena is
of great importance for transformer condition assessment.
This enables reliable operation and affords application of
adequate mitigation action to slow down the degradation
process of insulating materials and extend transformer
service life. This issue is all the more important when
new insulating liquids as natural esters are being applied
in growing number in transformer industry. For these
reasons, this paper is focused on the ageing phenomena of
cellulosic materials (paper and pressboard) impregnated
with different insulating liquids as natural ester, inhibited
and uninhibited mineral oils.
A first part is dedicated to moisture equilibrium in
impregnated paper and pressboard systems in order to give
some guidelines on the evaluation of cellulose humidity
through the oil. Moisture equilibrium isotherms were created
for temperatures from 40 to 120°C and for water content
in paper and pressboard from 0.5 to 5%. Differences in
distribution of water within cellulose/oil insulation between
natural ester and mineral oil were observed and discussed.
Natural esters have higher water solubility and therefore, for
the same water content in cellulose, at same temperature,
water content in the oil was considerably higher in natural
ester oil than in mineral oil. It was also found that water
distribution between paper and pressboard in mineral and
ester oils is quite different. Established isotherms constitute
a useful tool for the condition assessment of green power
transformers [1].
A second part is dedicated to thermal ageing at 140°C up to
120 days in order to evaluate ageing profile and long term
stability of different oils and solids. Ageing experiments
*christophe.perrier@alstom.com
KEYWORDS
Cellulosic insulation, Mineral oil, Moisture equilibrium, Natural ester, Thermal ageing
Cigre Science & Engineering • N°1 February 2015
6
were performed using copper, paper, pressboard and
insulating oils in proportions close to real design. Hermetic
systems were used and oxygen content in the oil was
adjusted to simulate conditions of sealed transformers
(not free breathing). It was found that in conditions of
particular ageing test, thermal degradation, i.e. oil pyrolysis
was dominant degradation mechanism, while oxidation
and hydrolysis were minor processes. This was confirmed
by low to moderate rate of antioxidants depletion in
both, natural ester and inhibited mineral oil. Stability and
performance of natural ester were found to be very good,
especially regarding the impact on solid insulation. Indeed,
degradation of solid insulation was present at lowest rate, in
comparison with mineral oils, on the basis of highest degree
of polymerization values at the end of ageing.
1. Introduction
Power transformers are one of the vital and expensive
elements in the industry of electrical energy, having
essential functions in power transmission and generation.
Although transformers are very reliable devices, there
remains one inevitable type of failure called “end of life”
failure mode. Most, if not all, organic materials used within
the transformer are subject to aging processes which lead
to the gradual degradation of their physical, chemical and
electrical properties. The most important of these organic
materials is the composite insulation system, i.e. cellulosic
materials (mainly paper and pressboard) impregnated with
insulating liquid (mainly mineral and ester oils). Three
main processes drive the aging of cellulose/oil insulation
systems. First one, pyrolysis is initiated by the temperature
as the main driving force behind the chemical reactions that
cause ageing. The other processes are hydrolysis, initiated
by the presence od water and oxidation, initiated by the
presence of oxygen. Water is also recognized as the “enemy
number one” of liquid-filled transformers [2] because it
has detrimental effect to the dielectric properties of the
insulation system as well as its mechanical characteristics.
The mechanical life of the transformer insulation is halved
for each doubling in the water content [3].
Although the end of life failure is inevitable, the life of the
cellulose can be maximized through careful monitoring
and maintenance. Proper condition monitoring of ageing
parameters for evaluation of the condition of insulation
system can improve replacement planning in order to
avoid the consequences of a sudden and untimely failure of
transformer. End of life of cellulose insulation is determined
by the mechanical strength and best measurement to assess
this property is the degree of polymerization (DPv). From
literature data, end of life is reached when DPv is below 250,
this being the minimum strength considered necessary to
withstand a short circuit. Since it is not possible to monitor
DPv values of transformers in service, laboratory models
simulating ageing of paper/oil insulation in accelerated
conditions enables a feasible way to analyze the effect of
different oils and key ageing parameters: temperature,
oxygen and water on cellulose ageing kinetics.
With the growing interest to use alternative liquids as
insulating fluids, such as natural esters (vegetable oils)
instead of mineral oils, for some transformer applications,
it becomes important to evaluate the applicability of current
monitoring techniques and test methods for evaluation of
cellulosic insulation condition. For this reason, this paper
will be focused in a first part on experimental studies
related to humidity equilibrium curves and in a second part
on ageing stability of composite oil/cellulose system.
2. Moisture equilibrium
isotherms
2.1 Condition assessment
Moisture in oil/cellulose insulation can affect the life of
transformers by leading to significant reductions in both
dielectric and mechanical properties. More precisely, water
increases the ageing rate and the dielectric losses, reduces
dielectric breakdown and mechanical strength and also
can introduce the risk of bubble formation during overload
[4]. Water is one of the degradation products of cellulosic
materials, but major amount of water in cellulose materials
is present due to moisture ingress from outside and retained
water in the solid insulation after manufacturing process.
Cigre Science & Engineering • N°1 February 2015
7
Since the cellulose insulation is more hygroscopic than the
oil it contains most of the water in paper/oil system and can
constitute several percentages by weight of the total mass of
solid insulation.
In order to avoid premature degradation of the cellulosic
insulation, the water must be kept to a minimum value.
In a new transformer, the water content of the cellulose is
about 0.5% and is expected to gradually increase during
the life of the transformer. Since it is not possible to remove
paper samples from the active windings of a transformer
under operation and measure water content of the paper,
indirect measurements were developed as the assessment
through the oil humidity (chemical method), or dielectric
response measurements [5]. The chemical method is
based on moisture partitioning curves between oil and
paper under equilibrium conditions. Various researchers
had experimentally derived moisture equilibrium charts
showing moisture in cellulose insulation versus water
content in mineral oil [6, 7, 8]. It is generally not known
if the equilibrium curves were obtained from experiments
using paper and pressboard insulation in mass ratios
corresponding to actual ratios in transformers, and how
the water is distributed between the paper and pressboard
insulation. In addition, due to increased applications of
natural ester oils in transformers, moisture equilibrium
charts become necessary tool to evaluate water content
in insulation systems impregnated with natural ester
insulating liquids.
2.2 Experimental study
Moisture equilibrium charts were created for conventional
Kraft paper and pressboard immersed in mineral insulating
oil and natural ester oil. Oil, paper and pressboard
were heated in 50 ml sealed vials with butyl septa at the
specified temperature. After reaching equilibrium, direct
measurements of moisture in the oil, paper and pressboard
were performed by Karl-Fisher titration. Moisture
equilibrium isotherms were created for temperatures from
40 to 120OC and for water content in paper and pressboard
from 0.5 to 5 %.
2.2.1 Test conditions
Oil, paper, and pressboard (see table 1) were taken in
specified mass ratios (90% of oil, 4% of paper and 6% of
pressboard), corresponding to approximate mass ratios in
actual power transformers. To achieve the initial low water
content, the paper and pressboard samples were dried and
filtered under vacuum oven. This procedure was followed
 Materials Type Standard
Mineral oil Naphtenic, non inhibited IEC 60296
Natural ester Triester, inhibited IEC 62770
Paper Thickness 0.25mm, Density 1.2-1.3 g/cm3 IEC 60641-3-2
Pressboard Thickness 1mm, Density 1-1.2 g/cm3 IEC 60641-3-1

Table 1: Tested materials

by impregnation with dried and degassed oil, for 24 h, at
700C for mineral oil and 90°C for ester oil. The water content
in the mineral oil and ester oil used for impregnation was
respectively up to 5 ppm and 30 ppm, and the oxygen
level in the oils was kept below 10000 ppm. The moisture
contents of paper, pressboard, and the insulating liquids
were analyzed by the test method described in IEC 60814.
Initial water contents in the paper and pressboard at
selected moisture levels of 0.5 to 5.0 %, were achieved by
placing the impregnated specimens in a wet chamber for
certain time at specified temperature and humidity [4, 9].
Prepared oils, paper, and pressboard specimens were placed
together in 50 ml vials crimped with butyl septa, leaving
the air space above the oil level. Then, they were heated
in an oven at specified temperatures between 40 and 120
0
C and for an equilibration time that was taken from the
literature, taking into consideration the material type and
thickness, which was extended slightly to verify the state of
equilibrium [10-11]. The moisture levels were considered
as reached when last three measurements matched closely.
All preparation procedures were made in a glove box with
argon atmosphere.
Different equilibrium times obtained for each oil with paper
and pressboard, are presented on figure 1. Equilibrium was
reached at longer times for low temperatures as well as for
low moisture contents. For the same moisture level and the
same temperature, equilibration time was longer with ester
oil, taking into consideration higher viscosity of ester oil.

Figure 1: Equilibrium times as a function of temperature and water content in the paper
and pressboard samples impregnated with mineral oil and natural ester

Cigre Science & Engineering • N°1 February 2015

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2.2.2 Experimental results

The developed charts are referred to in this article as

the “Perrier-Lukic” equilibrium curves. Comparative
analyses of the moisture distribution between cellulose,
natural ester and mineral oil are presented for absolute
moisture content. Note that calculation of the total
moisture content in paper and pressboard, together, was
done using the following equation:

Figure 2: Perrier-Lukic equilibrium curves for paper/pressboard

in mineral and natural ester oils
Where Wcc is the total moisture content in the cellulose
materials (%mass), Wcpaper is the moisture content in the
paper (%mass), mpaper is the mass of the paper (g), Wcpress
is the moisture content in the pressboard (% mass) and
mpress is the mass of the pressboard (g).

Due to the higher solubility of moisture in natural ester

compared to mineral oil, the moisture equilibrium
curves are significantly moved on the right with natural
ester oil (figure 2). Therefore, for the same moisture
content in the cellulosic materials, the expected water
content in natural ester oil is significantly higher than
in mineral oil. For example, for equilibrium at 60OC,
and 3 % water in cellulosic insulation, water content
in natural ester oil is around 10 times higher than in
mineral oil.

Separate equilibrium curves for paper, pressboard,

paper and pressboard together, in both oil types are Figure 3: Perrier-Lukic equilibrium curves for paper and
presented in Figures 3 and 4. Distribution of humidity pressboard in mineral oil
between paper and pressboard in mineral oil is relatively
equivalent, whereas uneven distribution, i.e. lower water
contents in pressboard and higher water contents in the
paper were obtained in ester oil. The observed differences
with moisture distribution paper and pressboard
impregnated with natural esters can have an important
role in estimating the moisture content in transformer
insulation based on electrical measurements (FDS).
Indeed, the estimated moisture in the paper can be
underestimated. The use of equilibrium charts for paper
and pressboard together enables greater precision in
estimating the moisture content and likely closer to those
expected from electrical tests. This is why these curves
are even more important, as they can be used to evaluate
water content in the paper and pressboard separately, as
well as to evaluate cumulative moisture content in both
cellulosic materials.
Figure 4: Perrier-Lukic equilibrium curves for paper and
pressboard in natural ester

Cigre Science & Engineering • N°1 February 2015

9
3. Ageing stability
3.1 Ageing of transformer insulation
The exact life of a transformer is not a fixed period and
depends on many factors. These factors include the operating
and maintenance regime, the characteristics of the network,
and to a certain extent, the design and materials used.
Experiences show that heavily loaded transformers have a
lifespan of 20-25years, and less heavily loaded transformers
can last 40-60 years and even longer [12]. In this paper, we
are only focused on the ageing performance of insulating
materials.
Temperature, water and oxygen are three main factors
affecting the ageing of the cellulose/oil insulation system.
The critical parameter is temperature, with heat energy
being the main driving force behind the chemical reactions
that cause ageing. The presence of oxygen is particularly
detrimental to ageing of transformer oil, while the presence
of water predominately speeds up ageing of solid insulation
by causing a cleavage of cellulose macromolecule chain.
Water is also the main factor which affects the dielectric
strength of the insulation system.
The most critical aspect of the ageing process of solid
insulation is reduction of its mechanical strength. Once
the cellulose has fallen below a critical level of mechanical
strength, the transformer is at risk from the mechanical
forces arising under short circuit or even during normal
operation.
Acids produced during oil ageing can increase paper
degradation and attack metallic parts in the transformer.
Decomposition products (from cellulose and oil itself) will
increase the concentration of polar compounds and cause
the increase of dielectric dissipation factor. Sludge, as end
product of oil ageing, can be deposited on the windings and
decreases heat transfer by blocking cooling ducts.
Materials Type
Mineral oil
Naphtenic, inhibited, high grade
(MOHG)
Mineral oil (MOSG) Naphtenic, non inhibited
Natural ester (VOR) Triester, inhibited
Paper Thickness 0.25mm, Density 1.2-1.3 g/cm3
Pressboard Thickness 1mm, Density 1-1.2 g/cm3
Table 2: Tested materials
Cigre Science & Engineering • N°1 February 2015
10
With the emergence of new insulating liquids as natural
ester, a comparative ageing study versus mineral oil was done
at laboratory scale under accelerated ageing conditions.
3.2 Experimental study
Oil, copper, paper and pressboard were aged in 50 ml
headspace vials, crimped with silicone septa, and with
restricted oxygen ingress (initial oxygen content < 10
000 ppm). The aim of this test set-up is to simulate sealed
transformer conditions as it is requested for the use of natural
esters. The test temperature was chosen at 140°C (for 120
days) to simulate an accelerated ageing. Indeed, based on
Arrhenius law and IEC 60076-7 standard (loading guide),
120 days at 140°C are equivalent to around 40 years at 98°C.
3.2.1 Test conditions
Cellulose materials have been dried in deep vacuum at
60°C during 24h and immediately thereafter impregnated
with respective dried and degassed oil during 48 h at 90
°C in deep vacuum. Water content of mineral oils used for
impregnation was around 5ppm and 25ppm for natural
ester oil. Initial water content in kraft paper and pressboard
was around 0.5%. All materials (table 2) were taken in mass
and surface ratios close to real design: paper/oil mass ratio:
4 %, pressboard/oil mass ratio: 6 % and copper /oil mass
ratio: 30%. For each oil, independent vials were heated at
140°C during different periods: 10, 20, 40, 60, 100 and 120
days. For each period, duplicate vials were used for heating
oil alone (“I exp”) and for heating oil in presence of paper,
pressboard and bare copper (“II exp”).
Prior and after ageing, following measurements were
performed: water content in oil and cellulose (IEC 60814),
2-FAL content (IEC 61198), degree of polymerization (IEC
60450), viscosity at 40OC (ISO 3104), pour point (ISO 3016),
acidity (IEC 62021) and antioxidants content (IEC 60666).
Standard
IEC 60296
IEC 60296
IEC 62770
IEC 60641-3-2
IEC 60641-3-1
 Figure 5: Evolution of acidity (left) and humidity (right) in mineral oils and natural ester

3.2.2 Experimental results
Note that for all graphics, “I exp” means results on oil alone
and “II exp” means results on oil in presence of paper,
pressboard and copper. As shown on figure 5, increase
of water content in the oil was significant after 10 days
of ageing in all investigated oils, but then decrease was
observed in all ageing periods for both oils. This peak was
the consequence of water migration from cellulose materials
into the oil. Water content in the cellulose decreased over
whole ageing period in both oils. The increase and decrease
of water was more significant in ester oil VOR, (oil with
paper, pressboard and copper), due to higher rate of water
migration from cellulose materials to ester oil which has
higher water solubility. Important increase of acidity in
ester oil (figure 5) is correlated with water consumption and
can be explained by hydrolysis reaction, as shown by other
studies [13, 14]. These acids seem not to be aggressive for
solid insulation and should be of high molecular nature,
since they do not degrade cellulose insulation significantly
[15], as shown on figure 7.
Consumption of detected antioxidants (figure 6) is more
pronounced in mineral oil (MOHG) than in natural ester
(VOR). This can be explained by higher thermal stability
of ester oil and the fact that high temperature-low oxygen
testing conditions suited better for ester oil. Nevertheless,
the level of additive at the end of ageing in mineral oil
still remained acceptable (IEC 60422). Low to acceptable
decrease of inhibitor content can be explained by low
concentration of oxygen and reduced oxidation process
during ageing. These results are quite encouraging for
the use of natural ester in power transformers in sealed
applications.

Figure 6: Inhibitor consumption (left) and 2-FAL evolution (right) in mineral oils and natural ester

Cigre Science & Engineering • N°1 February 2015

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 Figure 7: Evolution of degree of polymerization (DPv) of pressboard (left) and paper (right)

Degradation of paper and pressboard aged with ester
oil (VOR) was observed to be of slightly lower rate in
comparison to mineral oils (figure 7). Higher values of
degree of polymerization can be correlated to lower 2-FAL
values (figure 6), and this was observed in other studies
[16].
However, the difference in 2-FAL values between oil seemed
to be more significant than the difference between DP
values. This may be attributed to lower solubility of furans
in ester oil than in mineral oil. It was interested to observe
that after 120 days of ageing at 140ºC, paper and pressboard
reached end of life in both mineral oils, with negligible
difference in respect to different oil quality and presence of
antioxidant in inhibited oil.
Kinematic viscosity of mineral oils did not change during
whole period of ageing whereas small increase was detected
with ester oil (figure 8). This increase remains acceptable
in comparison with previous studies under higher oxygen
concentration [17], thus confirming the possibility of using
natural ester oil in sealed units. Note that, pour point of all
three oils was not affected during whole period of ageing.
4. Conclusion
Moisture distribution between cellulose materials (paper
and pressboard) and insulating oils (mineral and natural
ester) have shown that natural ester oil has higher capacity
to dissolve water comparing to mineral oils, as chemical

Figure 8: Evolution of oil viscosity (left) and pour point (right) in mineral oil and natural ester

Cigre Science & Engineering • N°1 February 2015

12
composition of natural ester is more polar nature. Moisture
equilibrium in natural ester oil is moved towards the oil,
more water is dissolved in the oil in comparison with
mineral oil, at the same temperature and water content
in the paper. Uneven distribution of water between paper
and pressboard was observed in ester oil, lower values were
measured in pressboard and higher water contents in the
paper. This may cause underestimation of water content in
the paper when evaluation is done using electrical methods
(FDS, RVM, PDC). The use of equilibrium charts for paper
and pressboard separately and together enables greater
precision in estimating the moisture content in insulation
system, especially for natural ester.
Ageing mechanism was predominantly pyrolytic (low
oxygen, at 140ºC) and was found to have more significant
impact on degradation of solid insulation impregnated
with mineral insulating oils than on solid insulation filled
with natural ester oil. Acidity of natural ester oil increased
significantly during ageing and it seems that some amount
of water in the oil was spent in hydrolysis reactions and
formation of fatty acids. However, solid insulation was not
degraded significantly in the presence of high acid content.
It seems that chemical composition of acids is more
important than its total amount. Behavior of mineral oils
related to paper ageing was similar regardless of difference
in oil quality and presence of antioxidant in inhibited
mineral oil. Flow properties were acceptable at the end of
ageing for mineral oils and also for ester oil with acceptable
viscosity increase of 15% from the initial value.
Achieved results related to ageing of solid insulation and
natural esters are quite encouraging for the use of natural
ester in power transformers in low oxygen environment
(sealed units).

References
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[10] L. J. Zhou, “Modeling of transient moisture equilibrium in Oil-Paper Insulation”, IEEE TDEI Vol. 15, No. 3, pp. 873-878, 2008.
[11] J. A. Thompson, “Transformer paper in oil water diffusion time constant”, presented at the IEEE Insulating fluids Subcommittee, C 57.106 WG, Apr.
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[13] H. P. Gasser, C. Krause, M. Lashbrook and R. Martin, “Aging of pressboard in different insulating liquids”, ICDL conference, 26-30 June, 2011.
[14] M-L. Coulibaly, C. Perrier, M. Marugan and A. Beroual, ‘‘Aging behavior of cellulosic materials in presence of mineral oil and ester liquids under various
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[15] L. Lundgaard & al., “Aging of Kraft paper by acid catalyzed hydrolysis”, IEEE TDEI, Vol. 15, No. 2, pp. 540-546, 2008.
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Cigre Science & Engineering • N°1 February 2015

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Biographies
Christophe Perrier obtained his Ph. D degree in
insulating materials in 2005 from the Ecole Centrale de
Lyon (France). He started his career in the R&D center
of Areva T&D (Villeurbanne) on insulating liquids
to optimize power transformers reliability. In 2006,
he moved to the R&D Center on Power Transformers
(Massy) where he developed a laboratory and activities
dedicated to insulating materials. Since 2012, in Alstom
Grid, he is in charge of R&D projects on materials, acts as
technical expert on insulating liquids and is Eco-design
coordinator for Power Transformers. He is member of
CIGRE (A2, D1) & IEC (TC 10).
Mamadou-Lamine Coulibaly has joined the Technology,
Innovation and Competence Development Centre
(TICC) of Areva T&D (presently Alstom Grid) at Massy,
France after receiving the Ph.D degree in Electrical
Engineering (Dielectric Materials and High Voltage)
from the Ecole Centrale de Lyon in collaboration with
Areva T&D in 2009, France.
He is currently with Alstom Grid - TICC Massy and
works on R&D projects linked to insulating materials
involving solids and mixed solids/liquids for power
transformers. He is member of CIGRE and IEC Working
Groups.
Cigre Science & Engineering • N°1 February 2015
14
Jelena Lukic, PhD in Chemical Engineering is Head of
Laboratory for insulating oil and paper testing, department
for Electrical Measurements of Electrical Engineering
Institute Nikola Tesla. Main field of her expertise are oil
analysis, diagnostics, degradation phenomena of paper/
oil insulation, corrosion phenomena induced by corrosive
sulphur and for oil treatment processes. She is Serbia NC
representative in IEC TC 10 Committee and co-liaison of
IEC TC 10 for CIGRE SC A2. She is engaged in different
IEC TC 10 and CIGRE working groups and is a convenor
of CIGRE WG A2.40: “Copper sulphide long-term
Mitigation and Risk Assessment”.
Valentina Vasovic is working in Electrical Engineering
Institute «Nikola Tesla», in Laboratory for Testing and
Calibration, department for mineral insulating oil testing,
at the position of associate research engineer. Her main
field of work is oil analyses, High-performance liquid
chromatography, Infrared Spectrofotometry, Karl Fisher
Coulometry, determination of viscosimetric degree of
polymerization of paper for electrotechnical purposes,
etc. She is engaged in research activities in the field of
natural ester oils. In 2008. she took a university degree
B.Sc. Chemical Engineering at Faculty of Chemical
engeenering, University of Belgrade, Serbia. Currently
she is in the course of PhD studies.