Electrical Insulating Oils
Part I: Characterization and
Pre-treatment of New Transformer Oils
Andrzej Sierota and Juris Rungis
CSIRO Division of Applied Physics, Lindfield, Australia
Introduction
he first mineral insulating oil proposed for use in
T transformers was patented in the USA in 1887,
and a subsequent British patent followed in 1891.
Transformer oil was first used in 1892; the first trans-
former oil manufactured to a specification was used in
1899. The early transformer oils were paraffin-based
but, in about 1925, they were replaced with naphthenic
oils because of the high pour point of paraffinic oils. It
was soon recognized that naphthenic oils are prone to
sludging, and this resulted in the development of oil
reclamation techniques. However, reclaiming proce-
dures stripped oils of their naturally occurring oxida-
tion inhibitors, so that they deteriorated at a much faster
rate than new oils. Consequently,in the late 1950s, the
industrial application of anti-oxidants was com-
menced. However, because inhibitors are depleted dur-
ing service, their use has been restricted mainly to
distribution transformers. A predicted world shortage
of good grade naphthenic crudes has resulted in re-
newed interest in paraffinic oils (Clark [l], Wilson [2],
Myers et al. [31 Lipscomb [41).
It has been generally acknowledged that the life of
an oil in service depends primarily on its initial quality,
but service conditions need to be considered, also. The
methods for evaluating various properties of insulating
oils that guarantee their quality and long life have been
standardized. The general specifications and methods
of testing electrical insulating oils to be used in the
electrical industry are covered by ASTM D 117.The USA
standard covering new oil is ASTM D 3487, and there
are various national and international standards, such
as the IEC 422, Japanese Industrial StandardsJISC 2320,
and Australian Standard AS 1883. Nevertheless, the
question of whether the existing standards are good
enough to evaluate a new oil is still a point of conten-
tion. Oil manufacturers, equipment manufacturers, and
0883-7554/ 95/$4.0001995
8 January/February 1995-Vol.11,No.1
The most critical step in the manufacture of
insulating oils is crude oil selection.
users do not always agree in their approach (Lipscomb
[4], Erdman [5], Geiman 161, Johnson 171, Pearce 181).
Definition of Transformer Oil
In ASTM D 3487, IEC 442 and AS 1883, only the
general term ”insulating oil” has been used. The term
”transformer oil” is misleading, as some oils can be
used in electrical apparatus other than transformers.
However, transformer oil readily accommodates the
needs of manufacturers of different types of apparatus.
Thus, the term ”transformer oil” has been accepted in
practice to describe varieties of mineral insulating oil
used elsewhere (Clark [ll, Myers et al. [31, Pearce [SI).
ASTM D 2864, which defines terms relating to elec-
trical insulating liquids, recommends only two catego-
ries of mineral insulating oils, as either refined from
naphthenic or paraffinic crude. However, this classifi-
cation is not technically correct and is of limited practi-
cal significance, as both categories may have virtually
the same basic properties (Lipscomb 141, Crine et al. [91).
A more pragmatic approach is that of ASTM D 3487,
which deals with only one specification that is intended
”to define a mineral insulating oil that is functionally
interchangeable and miscible with existing oils, is com-
patible with existing apparatus and with appropriate
field maintenance, and will satisfactorily maintain its
functional characteristics in its application in electrical
equipment.” The question of whether this can be
achieved to a satisfactory level of confidenceunder the
present standards and practices is still the core of many
investigations.
IEEE Electrical Insulation Magazine
 The ASTM D 3487 definition covers new mineral
insulating oils regardless of their crude oil base and
origin prior to any processing,and it defines two types.
Type I is of normal oxidation resistance and Type 11 of
greater oxidation resistance. Some Type I oils may not
require the addition of an oxidation inhibitor as they
may already contain naturally occurring inhibitors.
Type I1 oils are inhibited artificially.
Effects of Oil Manufacturing Procedures
The most critical step in the manufacture of insulat-
ing oils is crude oil selection. The degree of distillation
and refining of the crude and the kind of processes
involved may greatly change the constituents of the
final product (Hobson and Pohl [lo], Nelson [ l l l , Gruse
and Stevens [121).
The purpose of the refining process is, (a) to select
the liquid fraction having the most desirable charac-
teristics, and (b) to remove or minimize objectionable
constituents that may affect the required oil properties.
There is no single best method for the manufacture of
good insulating oil. The choice is based on the source of
crude, manufacturing experienceand equipment avail-
able. To produce transformer oils, particular attention
must be paid to fluidity, electrical characteristics, oxida-
tion stability, gas-absorbing properties, sulphur and
nitrogen content, contaminants, and an optimal aro-
matic content (Wilson [21, Lipscomb [4], Geiman [61).
Modern mineral transformer oils are produced using
the following refining methods:
Acid and Clay Treating
This produces the best quality oil. The finished insu-
lating oil is neutral in acidity, non-corrosive, and has
good electrical properties. However, the acid treating
process, although very powerful in eliminating un-
wanted compounds, is no longer used in some coun-
tries, such the USA, where acid-treated oils require a
cancer hazard warning. Acid treating, however, is still
performed in other parts of the world.
HydrotreatinglHydrogenation
These two processes differ in the severity of the
treatment. Hydrogenation adversely affects oxidation
stability if too much aromatic content is removed.
Solvent Extraction
This improves electric properties and decreases the
gassing tendency. It must be used in combination with
other processes such as hydrotreatment and clay treat-
ment. The advantage of solvent extraction, in contrast
IEEE Electrical Insulation Magazine January/February 1995-Vol.1 1, No.1
to acid treatment, is that the extracted aromatics have
valuable uses.
De-Waxing
In general, de-waxing is not required when the crude
oil is naphthenic. It must be employed, however, when
the crude is paraffinic or if naphthenic crude has a high
paraffin content. Only the wax structures are removed,
thereby reducing the pour point of the oil.
If an oil is under-refined, it always has a higher
aromatic content and the unstable aromatics retained
will result in poor oxidation stability. However,an over-
refined oil with too low an aromacity may also have
poor oxidation and gassing properties, as the result of
too few natural aromatic inhibitors. Satisfactory insu-
lating oil should have a balance of these properties, and
this can be achieved by using a combination of proc-
esses sequentially. A combination consisting of solvent
extraction as the first stage, followed by a hydrogena-
tion, may be the best solution (Myerset al. 131, Lipscomb
141, Geiman [61).
Modern insulating oils are not the same as those once
obtained by the acid method. Some are designed to rely
on the addition of oxidation inhibitors, and without
these, they do not display good inherent stability. But
transformer oils need to have a satisfactory inherent
stability as the inhibitors are consumed during service.
Although the benefits of inhibitors have been demon-
strated in various accelerated oxidation laboratory
tests, there is some evidence that they may not be as
effective in service (Wilson [21, Griffin [131, Dominelli
[141).
Maintenance of New Oils
Experience shows that transformer oil is a product
that requires extreme care and careful maintenance to
ensure satisfactory service. However, there is only a
brief mention in the standards of the maintenance re-
quirements for the shipping, storage and handling of
new oil. The lack of complete consensus on this subject
can be gauged from the fact that for specific problems,
the standards refer to oil and equipment manufactur-
ers’ recommendations (Lipscomb [4]).
Another important factor is the sampling of oil for
testing. Many factors have to be looked at in order to
avoid contamination and/or modification of the oil
samples, thus affecting the measured properties. Stand-
ards, such as ASTM D 923, ASTM D 3613, and AS 1883,
give specifications for the preparation of oil samples
before testing. Once defined, the procedures of sam-
pling the oil for various measurements should be
strictly followed. In principle, in order to ensure the
9
integrity of the oil and equipment, the initial monitor-
ing of the oil quality should consist of sampling the new
oil as delivered and sampling the oil in the equipment
before energization. Supply authorities, but also the
users, may specify their own sampling requirements
and sample treatment procedures (Crine 1151, Griffin
and Baker 1161).
Oil Characterizationby Manufacturers and
Users
With the use of oils from new sources and the reduc-
tion in the physical size of modern high-voltage appa-
ratus, the electrical industry has become aware of the
necessity to better define its selection criteria for insu-
lating oils (Myers et al. [31, Johnson 171, Griffin [17]).
Standards and specificationsare of fundamental impor-
tance for all parties involved in the application of insu-
lating oils but their need is not always sufficiently
appreciated. The oil manufacturers, the equipment
manufacturers, and the equipment users may have dif-
ferent interpretations of the standards.
Oil Manufacturers
The primary concern of the oil manufacturers is to
meet the quality levels that are set by the standards and
specifications. The manufacturers produce their own
specifications for the evaluation of oil quality, but they
have also to satisfy the requirements of the purchasing
organizations. Oil manufacturers are interested in a
formulation that ensures high production rates and
sales. The production of insulating oils is only a small
fraction of the overall refining output. Manufacturers
do not see the need for any new process or major change
in the core manufacturing routes used to refine electri-
cal insulating oils (Lipscomb 141, Geiman [6]). The
manufacturers are mainly concerned about the source
and type of crude to be used and that the use of increas-
ing amounts of paraffinic crudes will become a feature
of future production. The manufacturers favor the
specification of well established and well understood
characteristics, such as high dielectric strength, heat
transfer capability, low temperature pour point, and
good resistance to oxidation (Myerset al. [31, Pearce [SI).
Oil manufacturers use different refining processesto
produce the same apparent product. These products,
even under the same brand name, may have different
long-term properties because the oil composition may
significantly vary from one product or batch to another.
The trend to slightly over-refine oils for better antioxi-
dant inhibitor susceptibility may result, however, in
decreasing the aromatic content, which may have a
negative effect in weakening the long-term oxidation
stability (Petrovic and Vitorovic [181, Griffin [17]). Al-
10 January/February 1995-Vol.11, No.1
though manufacturers provide certificatesof oil quality,
care has to be taken that these did not become invalid
during shipment and storage. The manufacturers ex-
pect that the current product requirements will con-
tinue without much change and that they will not have
to get involved in new developments. Within the US
market they will be guided by ASTM D 3487; elsewhere,
by other standards.
Oil Users
Oil users usually want a more comprehensive char-
acterization of a new oil than do oil manufacturers. The
users are also more amenable to the specificationof new
tests. The equipment manufacturers and users often
seem to have similar viewpoints and common interests.
The equipment manufacturer is predominantly inter-
ested in specifying characteristics that could affect his
design and short-term operating performance, while
the equipment user is focused on service and mainte-
nance problems and is most interested in the long-term
performance and ultimate equipment and oil life (Erd-
man 151, Johnson [71, Pearce [81). Users have realized
that new parameters could be used for oil charac-
terization, although they do not yet appear in
standards.
Oil performance is especially important for the elec-
tricity generating authorities. The trend has been for
equipment manufacturers to minimize the amount of
oil needed and also to reduce the basic insulation level
safety margins, with a result that tremendous reliance
has to be placed on the oil to withstand the rigors of
thermal and electrical stresses during service. The effec-
tiveness of this protection can be monitored by ensuring
that the oil properties are within acceptable levels set
by specification requirements and limits. However, oil
users should probably impose much stricter and more
explicit rules than currently used in purchase specifica-
tions. A less conservative approach to the usefulness of
more modern oil test results would be of benefit to
equipment users.
Standards and Specifications
In spite of all the differences in their standpoints, the
refiners, manufacturers and users have worked to-
gether to produce mutually acceptable standard speci-
fications for oil characteristics and test requirements.
The most comprehensive specification to date is ASTM
D 3487 in the USA. This standard discusses most but not
all of the important parameters that can be used to
characterize an oil. Table I lists the oil properties men-
tioned in American,Australian and Japanesestandards.
In the most comprehensive approach to oil testing,
the range of tests and parameters considered can be
IEEE Electrical Insulation Magazine
 Table I
Oil Properties in Various Standards
-I

1
I
I
USAASTMD3487 AUS SA 1883 JAP JIS C 2320
L
~

Physical: I
Color a n d appearance D 1500 I S 0 2049 c 2101
D 1524
1 Density/Specific gravity D 1298 IEC 296 c 2101
D 88 c2101 ~

Viscosity D 97 I S 0 3675 c 2101

Pour point D 92 c 2101
Flash point D 611 I S 0 3104 -
Aniline point D 971 -
Interfacial tension D 2285 I S 0 3016 c 2101
-
1 Specific dispersion I S 0 2719
-
I S 0 6295
-

~ Chemical:
Neutralization number (acidity) D 974 IEC 296 c 2101
, D 2440 c 2101
I Oxidation stability D 2112 IEC 1125
D 1473 -
I Inhibitor content D 2668
D 1533 IEC 666 c 2101
Water content
D 1275 c 2101
1 Corrosive s u l p h u r IEC 733
IEC 814
-
I
~ Electrical:
l Breakdown strength (ac) D 877 IEC 156 c2101
D 1816
D 3300 -
Impulse strength D 924 - c 2101
Dissipation factor - IEC 247 c 2101
Volume resistivity - c 2101
Permittivity D 2300 IEC 247 -
Gassing tendency - I -

Total gas content -

-
IEC 567

very large. In the oil evaluation program used by the
Doble Company, three phases of testing are covered:
(a) evaluation of basic oil properties in laboratory tests;
(b) continuity tests and compatibility tests and (c) ex-
tended development plant tests, including accelerated
life tests and field tests (Baker [191).
In the USA, oil users most often employ ASTM D
3487 and perform all the tests quoted for the qualifica-
tion of a new supplier of transformer oil but only repeat
some of these tests a s a criterion for acceptance. How-
ever, they may also recommend additional tests. In
general, four categories of tests have been used:
(a) qualification tests; (b) acceptance tests; (c) design
tests and (d) additional tests (Johnson [71).
Qualification testing demonstrates that the product
offered by the vendors is of suitable quality, while ac-
ceptance testing ensures that the batches of known
products retain the expected characteristics. Only these
two types of tests and one additional test (PCB content)
are covered by ASTM D 3487. Design tests include

IEEE Electrical Insulation Magazine JanuaryFebruary 1995-Vol.1 1, No.1 11

thermal conductivity measurement (ASTMD 2717) and
specific heat evaluation (ASTM D 2766). Additional
tests can be a variety of standardized tests, such as
dissolved gas analysis (ASTMD 3612), measurement of
resistivity (ASTM D 1169), foaming tendency (ASTM
D892) and PCB analysis (ASTM D 4059). Additionally,
non-standardized tests such as electrostatic charging
tendency (ECT) and electric strength of oil in motion
can also be performed (Johnson 171, Pearce [81, Griffin
[171).
The transformer oil purchase specification (TOPS)
designed by Doble uses different testing categories:
(a) functional; (b) purity; (c) compositional and (d) sta-
bility tests. It has been followed by many oil users
(Myers et al. 131, Doble [201).
Functional tests cover a limited number of oil prop-
erties and include the measurement of specific gravity,
viscosity, flash point and pour point as well as dielectric
breakdown and power factor (Myers et al. [3],Griffin
[171).
Different terminology has been employed in Austra-
lian Standard AS 1883: (a) basic tests; (b) special tests;
(c) identification tests and (d) restricted tests are used.
These tests are based on IEC and IS0 recommendations.
Users should always request certain additional infor-
mation from oil manufacturers to help to identify the
oil, although this data is not necessarily a part of any
specification. For instance, in the USA, the following
must be supplied by the oil manufacturers to the users:
(a) the generic refining process employed; (b) the type
of crude; (c) whether an inhibitor was used (if used, the
type of oxidation inhibitor has to be specified);(d)poly-
chlorinated biphenyl (PCB) contamination concentra-
tion a n d (e) any additional test requirements
(Johnson 171).
Oil Constitution
Mixtures of Hydrocarbons
Refined oils are very complex mixtures and may
consist of as many as 2900 paraffinic, naphthenic and
aromatic hydrocarbon molecule types, 25% of these
being aromatics. Thus, their properties may vary sig-
nificantly from one batch to another, even from the
same brand. Although the final products have been
analyzed by the oil manufacturers and users, up to 90%
of the compounds still remain unidentified, as the high
cost of chemical analyses make their full implementa-
tion practically impossible. Hydrocarbon analysis can
serve as a ”fingerprint” of the oil’s characteristics
(Petrovic and Vitorovic 1181, Duval and Lamarre [211).
12 January/February 1995-Vol.11, No.1
Non-Hydrocarbons
These are also present in oil and the most important
are sulphur, nitrogen, and oxygen combined with carb-
on and hydrogen. The sulphur compounds are pre-
dominantly thiophenes and sulphides, and the range of
sulphur in new oils is approximately 0.05%to 0.5%.The
range of nitrogen compounds content (quinolines and
pyroles) is 0.005%to 0.05%.Unrefined oils may contain
up to 0.5% of oxygen containing compounds (acids and
esters) but refining techniques reduce this to a very low
level, which nevertheless may affect various oil proper-
ties (Wilson [2], Jezl et al. [221).
Impurities
There are different impurities and contaminants pre-
sent in insulating oils either in solution (various gases,
moisture, ionic impurities, metals) or in non-soluble
form (solid contaminants in suspension) and they all
affect many oil properties.
Dissolved gases (hydrogen, oxygen, methane, carb-
on dioxide, and others) are present in new oil as
residues of manufacturing processes and/or be-
cause of improper handling of an oil before its use.
The maximum solubility of gases by volume in
transformer oil at atmospheric pressure and 25°C
is 10% for air, 9% for nitrogen, 16%for oxygen, 6%
for hydrogen, 9% for carbon monoxide, 30% for
methane, and even higher for other higher hydro-
carbon gases (Wilson 121, Zaky and Megahed [231,
Duval [241).
Water contamination in oil can be present in the
dissolved state or in the form of droplets or clouds
as the result of oil manufacture and improper main-
tenance. Typical values for new transformer oils are
about 15pprn to 30 ppm. It has been recognized that
moisture is ”enemy number one” for transformer
insulation. Dry oils have a water content below 10
pprn and levels as low as one pprn have been meas-
ured (Wilson 121, Dickson [25], Oommen [261).
Ionic and polar contaminants may be present in oils
as a result of refining treatments. They mainly affect
the electricalproperties as they are the major charge
carriers. Traces of sulphate, sulphonates and alkalis
can be present, and traces of solvents and phenols,
sulphur dioxide, furfural, and organo-chloro com-
pounds may also appear. The typical range of these
compounds is from 0.1 ppm to 1.0 ppm (Wilson 121,
Crine [151, Lamarre [271).
Particulate contaminants get into new oil in the
manufacturing process and in its transportation in
containers. They are predominantly metal oxides
and metal elements, mainly iron and copper but
also lead, zinc, nickel, vanadium and sodium. Non-
IEEE Electrical Insulation Magazine
 metallic fibers (cellulose) and carbon particles are
also present. Oils may contain between 0.0001%
and 0.001% of particulate matter larger than 5 pm
in size; this represents approximately 105 to 106
particles per 100 ml of oil. Smaller particles, 1 pm
and below, have only lately become of interest
because of the previous lack of appropriate meas-
uring methods (Wilson [21, Miners, [281 Oommen
and Petrie [291).
Polychlorinated biphenyls (PCBs) were used in
power transformers but have now been banned.
PCBs are treated as unwanted contaminants and
are not allowed at detectable levels in transformer
oils (ASTM D 3487, Rickley [301, Rouse [311, Manger
1321).
Additives
These are various chemicals that act as inhibitors,
passivators, or pour point depressants. Their concentra-
tion in the oil may vary significantly depending on the
additive, ranging from parts per million to several per-
cent (Belanger et al. 1331, Duval et al. [341, Zaky and
Megahed 1231).
Basic Oil Properties
Color and appearance can be used during both accep-
tance and qualification tests to eliminate substandard
oils. For new oils the maximum acceptable color value
(color number) is 0.5, and a bright and clear appearance
is required. However, slightly colored new oil does not
always indicate poor quality (Johnson [71, Pearce [SI).
Density is not very significant in determining the
quality of an oil but may be useful for type identification
and evaluation of an oil's suitability for use. Specific
gravity is important when there is a concern about
water in oil freezing and rising to float on top of the oil.
A lower limit for specific gravity would eliminate this
potential problem (Johnson [71). In cold climates, den-
sity may be pertinent in determining oil suitability
(Mulhall and Thompson [35], Mulhall [36]).Normally,
new paraffinic oils have higher densities, while the
mixed base or paraffinic oils have lower densities.
Slightly different limit values are set by different stand-
ards and specifications (Myers et al. 131).
t fication and delivery acceptance purposes. In order to
Viscosity is important for the dissipation of heat. A
comparison of naphthenic and paraffinic crude oil be-
havior at low temperatures showed that the higher
viscosity of the paraffinic oils indicated wax formation
(Langhame et al. [37]). The increase in viscosity de-
pends on the oil constitution, being most pronounced
IEEE Electrical Insulation Magazine January/February 1995-Vol.1 1, No. 1
for aromatic and least for paraffinic hydrocarbons (Wil-
son [21).
Pour point is a measure of the ability of the oil to flow
at low temperature. It is an important parameter that
always has to be considered when low ambient tem-
peratures of workmg equipment are expected. Big dif-
ferences in pour point may exist among different oils, a
maximum temperature of -40°C being specified in the
standards. Pour points and cloud points of modern
insulating oils should be carefully watched as
naphthenic oils are replaced by paraffinic oils (Myerset
al. 131, Duval et al. [381).Many utility companies use the
pour point test for the qualification of vendors but not
for routine acceptance purposes (Johnson [71).
Flash point is an indication of the flammabilityof oil.
Considering the elevated temperatures of modern
transformers, a change in the minimum acceptableflash
point temperature was made in ASTM D 3487 and
various specifications (TOPS).A level of 145"C, instead
of 140"C, was adopted. The flash point value is nor-
mally used as a qualification test and not for acceptance
purposes (Johnson 171, Griffin 1171).
Aniline point estimates the total aromatic content in
the oil. The aniline point test is used as a qualification
test, but not by all utility companies (Johnson [71). It is
related to the impulse strength, gassing characteristics
and oxidation stability of an oil. ASTM D 3487 specifi-
cation quotes a range of values, from 63°C to 84°C;
however, in the latest version of the TOPS of Doble, the
aniline point was set at 80°C maximum (Griffin [17]).
Interfacial tension is a parameter used for the qualifi-
cation of vendors. A high value of interfacial tension for
new oil, not less than 0.040 N/m, indicates the absence
of undesirable polar contaminants, which makes the
test a useful screening method for new oils exposed in
transport to soaps, acids, varnishes, and solvents. The
opinion has been expressed that the limit of accept-
ability could probably be raised to 0.045 N/m (Johnson
171, Pearce [SI).
Neutralization number (acidity) is a measure of the
trace amount of acidic or alkaline contaminants in the
oil. The test is normally accepted for both vendor quali-
achieve long life expectancy of oils in transformers,
neutralization numbers lower than 0.01 mg KOH/g are
required for new oils by many users (Johnson 171).
However, the acceptablelimit quoted by ASTM D 3487
is higher at 0.03 mg KOH/g. Alower value of 0.025 mg
KOH/g is given by TOPS (Myers et al. [31,Doble [201).
13
 Water content increases electric conductivity and dis-
sipation factor and worsens electric strength. However,
it may impede charge generation in the oil (Wilson 121,
Crofts 1391). The National Institute of Standards and
Technology (NIST)in the USA has prepared a water-in-
oil standard reference material (SRM) to enable the
detection of bias in automated test apparatus (NIST).
Oils with a moisture content below 10 ppm are consid-
ered to be dry and otherwise require drying before use.
The existing standards and specificationsset the accept-
able moisture levels in transformer oils at room tem-
perature at 25-35 ppm, and ASTM D 3487 gives a value
of 35 ppm. In general, the moisture level in oils is a
dynamic state strongly influenced by temperature and
any gas cushion or immersed paper. At ambient tem-
peratures the moisture transients between oil and air
are in the range of minutes (Griffin 1411).
Oxidation stability is one of the most important prop-
erties of insulating oils. In many cases a good oil oxida-
tion stability may be achieved by a suitable content of
the naturally occurring aromatics. However, a nitrogen
and sulphur compound-free oil is required (Clark [l],
Wilson [21). The evaluation of oxidation stability re-
quires acceleratedageing tests. ASTM D 2440 is used for
the qualification of oils and has two indicative limits
which, for the 72 hour test, are 0.1% of sludge by mass
and 0.3 mg KOH/g (for Type I oils) or 0.5 mg KOH/g
(for Type I1 oils).ASTM D 2112 (RotatingBomb Method)
is used for both qualification and acceptance testing of
inhibited oils and has a minimum limit of 195 minutes.
The Doble Power Factor Valued Oxidation Test (PFVO)
measures the power factor of an oil sample under accel-
erated ageing conditions. It measures oil quality up to
the point of sludge formation and measures the sludge-
free life (SFL) of the oil sample. The limit set by the
Doble procedure is 40+8 hours (Myers et al. 131, Griffin
[171). However, oxidation stability is not one of the
functional tests quoted by TOPS, although it is quoted
as the primary functional property by some other oil
users (Crine [151).
Inhibitor content is a parameter used for oil vendor
qualification, but the infrared (IR) absorption method
adopted by ASTM D 2668 is semi-quantitative and of
limited reliability. The ASTM D 3487 property require-
ments quote 0.08% of ditertiary-butyl-para-cresol
(DBPC) or 2.6-ditertiary-butyl phenol (DBP) inhibitors
by mass for Type I oils and 0.3% inhibitor by mass for
Type I1 oils. Alternatives to the most common (IR)
method are gas chromatography (GC), high perform-
ance liquid chromatography (HPLC) or differential cy-
clovoltametry (DCV) (Johnson 171, Crine 1151, Belanger
et al. [331).
14 January/February 1995-Vol.11,No.1
Gassing tendency is evaluated in new oils to satisfy
specification requirements, but it is not usually used as
a prime indicator of oil characteristics. Some standards,
such as AS 1883, recommend the measurement of the
total gas content of new oil. Adissolved gas analysis can
identify low energy discharges as well as high thermal
stresses and disruptive discharge conditions (Wilson
121).ASTM D 3487 sets upper limits of +15pL/min and
+30 pL/min (for Procedures A and B, respectively).
Some utilities prefer oils with slightly negative values,
(gas absorbing tendencies) but positive values are ac-
ceptable when price and availability are taken into ac-
count. General agreement does not exist on the most
desirable range of gassing values (Johnson 171).Gas-ab-
sorbing oils may become strongly gas evolving during
service. This suggests that the influence of the initial
aromatic content and thus the initial gassing tendency
value in the new oil is important for future gas forma-
tion (Duval and Lamarre [211).
AC electric strength, or the dielectric breakdown volt-
age at power frequency, is the most often controlled
parameter describing the oil's function as an insulant.
Electric strength is strongly dependent on the amount
of contamination in the oil and on the oil constituents.
It is sensitive to the amount of specific hydrocarbons
and increases considerably for oils with high aromatic
content (Angerer [421). As it is influenced by sampling
conditions, the preparation of the oil sample, especially
the need for rehomogenization, may greatly influence
the breakdown characteristics of oils. The breakdown
voltage value may give a totally misleading indication
of the real oil condition if it is performed days after
sampling, when particle settling has occurred (Crine
[15]). Dry and clean oils exhibit high breakdown volt-
ages, which can be reduced dramatically when solid
particles and dissolved water are present. Most of the
breakdown voltage specifications require a minimum
of 30 kV with a 2.5 mm gap (ASTM D877), when meas-
ured with disc electrodes. However, a high breakdown
voltage does not indicate that an oil is free of all con-
taminants (Miners [281, Bell [431).
Impulse strength is rarely considered in the various oil
test programs, but a limit of 145 kV is set by ASTM D
3487 for measurements with a one-inch gap and a nega-
tive needle. This property is sensitive to both polarity
and electrode geometry, but it also reflects the oil com-
position and can be lowered when the aromatic hydro-
carbon content is increased (Mathes 1441).Other factors
that adversely affect the impulse strength are the sul-
phur and nitrogen compound contents (Wilson [21).
Dissipation (power)factor andlor resistivity are impor-
tant parameters describing the oil's function as a dielec-
IEEE Electrical Insulation Magazine
tric. The dissipation factor of an oil at power frequency
(DDF) or power factor (PF) provide the same informa-
tion as the oil resistivity and are affected by the same
factors and test conditions. Useful information can be
obtained by measuring DDF, PF, or resistivity at both an
ambient and a higher temperature, such as 90°C (Bart-
nikas [451, Duval and Crine [461). A satisfactory result
at an elevated temperature coupled with an unsatisfac-
tory value at the lower temperature usually indicates
the presence of polar contaminants (e.g., water) precipi-
table in the cold, but generally at a tolerable level.
Unsatisfactory results at both temperatures indicate a
greater extent of contamination that can be difficult to
restore even by reconditioning the oil (AS 1883). The
dissipation factor limit values given by different speci-
fications vary. The ASTM D 3487 values are 0.05% and
0.3% when measured at 25°C and lOO"C, respectively.
However, 0.5%is set at 100°Cby TOPS (Griffin [17]).An
example of methodology using the power factor as an
oxidation indicator is given by the PFVO Doble Test
(Oliver [471).
More Recently Recognized Characteristics
Contaminant content may affect many oil properties;
however, no requirements, either on solid particle size
or particle content, have been imposed by international
standards. An IEC SClOA working group is currently
developing a methodology for the evaluation of con-
taminants in oils. As yet, no specific testing method has
been proposed by ASTM, although their standards
from the aerospace industry can be used (Crine [15]).
Particles can be counted in flowing oil using such meth-
ods as electron microprobing, ferrography, neutron ac-
tivation analysis and atomic absorption spectroscopy.
Using these methods, very low particle contents, down
to ppm levels, can be evaluated (Olivier et a1.[481,Samat
and Lacaze [49], Vincent and Crine [50]). The major
problem in reliable particle sizing and counting is inho-
mogeneity in the oil sample. This problem has led to
attempts at re-homogenization of the oil sample by
ultrasonic agitation (Vincent et a1.[511). Various novel
methods for the evaluation of the trace metal contami-
nant content in oils have been attempted. The sensitiv-
ity of these methods, such as neutron activation analysis
(NAA),can be of the order of 1 ppm, and copper, lead,
and iron contaminations of less than 5 pprn have been
detected by this method. Atomic absorption spectro-
photometry (AAS) can be used as an alternative for the
detection of copper (Crine [151.)
Another problem emerges from the sizing and
counting of non-metallic particles that are mainly fi-
bers. In transformers, most particles are long cellulose
fibers and very small carbon particles (below 2 pm in
size) that cannot be measured correctly by particle
IEEE Electrical Insulation Magazine January/February 1995-Vol.1 1, No.1
counters. For their identification, various microscopic
methods can be employed, including modified fer-
rographic methods (Olivier et al. 1481). The nature of
particles can be determined by an appropriate choice of
light filters and by electron microprobing and an image
analysis system. The advent of ion chromatography
makes possible the evaluation of the ionic and polar
contaminant content in oils (Crine [15]).
Moisture content is most often measured using the
Karl Fischer titration method, which is effective for
moisture contents down to 5 ppm. Various new meth-
ods, including capacitive moisture sensors based on
microdielectrometryprinciples, have been used (Zaret-
sky et a1.[52], Oommen 1531,von Guggenberg et a1.[541)
to extend the range of measurement down to much
lower values of 1 pprn and less.
Chemical composition analysis is receiving increased
attention from the oil users. Even slight changes in the
proportions of any of the oil compounds may affect oil
properties. In addition, problems have risen with the
shortage of the traditionally used naphthenic crudes.
Infrared (IR) spectroscopy has proved useful over
the years for the analysis of insulating oils (Kunzli [551,
Yasufuku [561).It can be used to determine the percent-
age of the aromatic content and the hydrocarbon com-
position proportions, as well as the presence of
inhibitors. However, IR methods do not give any data
on other important physical properties, such as the
boiling range and distribution, or on the blending of
oils. Moreover, this method is not able to distinguish
between closely similar insulating oils or identify their
sources (Hazelwood et al. [571).
Valuable information on the nature of hydrocarbons
and also various additives in an oil can be obtained from
modern instrumental techniques.High resolution mass
spectrometry provides a detailed analysis of hydrocar-
bons and detects low levels of oxygen and nitrogen
compounds. Trace amounts of ionic compounds (i.e.,
dibenzofuran) can also be detected by this method
(Hazelwood et al. 1571, Gallegos et al. [581). However,
for the overall chemical analysis of oil, the chroma-
tographic methods are the best (Kirkland [591, Hirsch et
al. [60]). Simple and rapid high-performance liquid
chromatography (HPLC) may provide "fingerprints"
of oils by giving data on the molecular size distribution,
the fraction of various hydrocarbons, the types of aro-
matic hydrocarbons, the mean degree of their alkyla-
tion, and the content of additives (Duval and Lamarre
[21]). Gel permeation chromatography (GPO may be
helpful in determining various additives (Duval et al.
[34]). Gas chromatography (GC) methods have been
identified as particularly useful for the comparison of
oils on the basis of the distribution of their aromatics
and were recommended for the control of the refining
15
process (Hazelwood et al. [571). GC has been stand-
ardized for the analysis of gases dissolved in oils (ASTM
D 3612) and the control of PCBs (ASTM D 4059).
Electrostatic Charging Tendency (ECT) describes the
property of an oil to become charged when in relative
motion against a solid surface. The degree of frictional
electrification determines whether or not this property
can lead to electrical discharges and dielectric break-
down in a transformer. Neither the measured quantity
nor the method of evaluation of ECT are standardized.
However, the Ministatic Charge Tester (MCT)has been
widely adopted as a de facto industrial standard (Oom-
men and Petrie [611). Other methods have been also
used, as summarized by Sierota and Rungis [621. The
spinning disc apparatus (SDA)was proposed as a meas-
uring device by CIGRE [63].Becausethe oil is the most
readily replaceable element in transformers, efforts
have been made to correlate electrostatic charging with
the long-term properties of insulating oils (Crofts [39]).
ECT values for new oils measured at room temperature
with the MCT range from one to hundreds of pC/m3
(Oommen [641, Griffin 1651).Streaming current values,
measured at room temperature with the SDA, can be in
the range of one to hundreds of picoamperes, depend-
ing on the rotational speed and the nature of the oil
(Kedzia [661, Sierota et al. [671). It is still an open ques-
tion if ECT can be used as a property characterizingnew
insulating oils.
Resistance to partial discharges is a term that has been
adopted worldwide for solid dielectrics (Kreuger [68])
but has not yet quite been accepted to describe quanti-
tatively the behavior of insulating oils. For insulating
liquids, the term "stability to electrical stress" has been
used to relate the gassing properties of oils under dis-
charge conditions (Wilson [2]). In general, the signifi-
cance of partial discharge parameters, such as inception
voltage, the magnitude of discharges and the dynamics
of discharge characteristics in insulating oils, still re-
main a matter of debate. There are no standard experi-
mental procedures, and a lack of agreement exists on
whether electric, optical, or acoustic characteristics of
partial discharge or only the effect of their activity
(gassing) should be considered. Data on the relation
between partial discharge parameters and most oil
characteristics are scarce, but the influence of moisture
has been investigated (Babula et al. [69], Borsi et al. [70]).
Electric strength of oil in motion is a new parameter
already being used in additional oil tests, although no
standard method is available for its evaluation. The
electric strength of oil flowing in electrically stressed
regions is a function of flow rate, electric field, tempera-
ture, moisture content and particulate contaminants
16 JanuaryFebruary 1995-Vol.1 1, No.1
(Johnson [71). In the oil velocity range of 5 cm/s to 200
cm/s, the mean breakdown strength may increase, but
it decreases at higher velocities (Ikeda et a1.[711).Theo-
dossiou et a1.[721 demonstrated that the breakdown
locations at the electrode are evenly distributed and
there is no preferential area in the gap where break-
downs occur, as would be provided by a stagnant liquid
region. The findings were confirmed and explained in
terms of hydraulic instabilities in flowing liquid (Nel-
son and Lee [731).The effect of oil composition and oil
impurities on the breakdown of oil in motion has not
yet been investigated. There is growing concern that the
electric strength of oil in motion is important in under-
standing the dielectric integrity of flowing oils (Ikeda et
al. [711, Nelson et al. [741).
Pre-treatment of New Oil by Users
In spite of the many precautions undertaken to en-
sure good oil quality as delivered from the manufac-
turer to the user for filling or retrofilling equipment,
some of the oil properties could be significantly
changed by an increase in moisture and contaminant
content. In order to ensure a suitable oil quality, various
pre-treatment procedures have to be used, either to
re-establish a previously achieved value or to intention-
ally improve the oil's characteristics.
Oil purification
This is a process that eliminates, by physical means
only, solid contaminants from the oil and decreases the
water content to an acceptable level. The techniques
used to remove water and solids from oil include differ-
ent types of filtration, centrifuging and vacuum dehy-
dration. During filtration, particles larger than a
nominal 10 pm should be removed. However, when
filtering is associated with precise particle counting,
filtering down to 5 pm may be required (Samat and
Lacaze [491). Filters deal efficiently with solid impuri-
ties but can remove only small quantities of water and
do not degas the oil. When a relatively large quantity of
water is present, most of it can be removed by centri-
fuging. Acentrifuge can handle a much greater concen-
tration of contaminants than can a conventional filter
but cannot remove some of the solid contaminants as
completely as a filter. Dissolved and suspended water
can be effectivelyreducedto very low values by treating
under vacuum (100 Pa and up to 80°C, Myers et al. [31).
Oil mixing
Insulating oils are balanced hydrocarbon mixtures,
and they can apparently be mixed successfully.The aim
is always to deliver a product with optimum or im-
IEEE Electrical Insulation Magazine
proved properties. Mixtures of different naphthenic-
based oils, as well as mixtures of these oils with straight-
chain aliphatic hydrocarbons and blends of commercial
mineral oils with organic and non-organic esters, alkyl-
benzene and perchloroethylene and with cottonseed
oil, castor oil and ethanol, have been used in different
proportions (Yasufuku [561, Kang [751, Narayana Rao et
al. [761).
The values of some oil properties in mixtures often,
but not always, lie between those of the individual
components, assuming no chemical interactions occur.
A large increase of viscosity, an increase in flash point,
and a lowering of the pour point have been found in
mixtures of naphthenic oils with alkylbenzene.Gassing
properties as well as resistivity, dissipation factor and
charging tendency have also been improved for these
mixtures (Narayana Rao et al. [76]). The dissipation
factor of various mixtures of naphthene-based oils with
aliphatic hydrocarbons of different viscosities was in-
creased (Kang [751).It has been found that the blending
of transformer oils with perchloroethylene produced
higher ECT levels than those of pure oil or perchlo-
roethylene (Oommen 1641).Changes in pour point may
occur in the topping-up of an oil with a different type.
Blended oils have a lower flash point than a "straight
cut" oil of the same viscosity (Wilson [2]).
Use of Additives
In most cases, the same rules apply to oil blending
with additives as to oil mixing, the difference being that
the highly active additives are only a small volume
fraction of the blend. In general, no blending proce-
dures are quoted in the literature. However, they are
known to particular users.
0 Oxidation inhibitors, passivators and metal deacti-
vators are added in different proportions to im-
prove the oxidation resistance of the oil. Except for
oxidation inhibitors, no limits on their content in
oils is given by the specifications.Apart from DBPC
and DBP, various amines and some aromatics are
also used. Metal deactivators used are hindered
polyphenols, alkyl phenyl amine, and triazole de-
rivatives. The depletion of anti-oxidant additives
corresponds to a drop in the interfacial tension
value (an indicator of polar contaminants), a rapid
increase in the acidity number, and sludge forma-
tion. There is concern that oxidation inhibitors,
when in excess, may negatively affect various oil
characteristics (dielectric properties, emulsifica-
tion, gassing,and others). However, adding a metal
deactivator to an oil may not only improve its ther-
mal resistance but also reduce ECT. Often the use
of both oxidation inhibitors and a metal deactivator
can be more beneficial than an inhibitor alone
IEEE Electrical Insulation Magazine January/February 1995-Vol.1 1, No. 1
(Stoker and Thompson 1771, Shroff and Wilson [781,
Frey and Gedemer [791).
Pour point depressants and flow improvers are
normally added to paraffinic crude oils. In many
cases where linear paraffins are below a critical
level, it is possible to reduce the pour point and
improve the flow to the same value as could be
obtained after an expensive de-waxing,by optimiz-
ing the additive. Temperatures down to -60°C can
be achieved with 0.45% as a typical value for the
additive. Although used worldwide, pour-point
depressants are not allowed in the American trans-
former industry (Geiman [6]).No standardized re-
quirements are imposed on the amount and use of
these additives.
0 Hydrogen acceptors, such as anthraquinone, ben-
zophenone and diphenyl affect mainly the gassing
properties but also other properties and the dielec-
tric strength in particular (Angerer [421, Zaky and
Megahed [231, Clarke and Reynolds [SO]). Also,
compounds such as naphthalene and dodecyl ben-
zene may modify gassing in oils (Wilson [21).They
can be effective in the bulk of the oil or in form
protective layers on the electrode surfaces
(Angerer [421). Small amounts of these additives
can optimize gas absorbing and/or gas evolving
properties and can increase dielectric strength.
However, as oils can be refined to retain a level of
aromatics that will impart gas absorbing qualities,
among other properties, the use of these inhibitors
is not essential.
Charge suppressants, such as benzotriazole
(BTA) and alkylbenzene (AB), have been used.
However, there is controversy between Japan
and the USA over the effectiveness of BTA (Ieda
et a1.[81], Griffin and Christie [82]). A concentra-
tion of BTA up to 10 ppm was claimed in Japanese
research to be beneficial in reducing ECT and did
not significantly reduce dielectric strength. This
was disputed in American research by Crofts
[39]. BTA, when present at the surface of paper,
can alter to some degree the physico-chemical
properties of insulation. Moreover, a concentra-
tion of BTA between 0-50 ppm did not signifi-
cantly affect the charge generation in oils.
Various static electrification, flashover and con-
ductivity modifiers have been employed in the
USA. It was found that Mobil DCA48 additive
with Refrigerant 113used as a coolant can be used
to eliminate electrification problems (Gasworth).
Blending AB with naphthenic oil may result in a
large increase in its viscosity and improvements in
its resistivity, dissipation factor and impulse
strength (Yasufuku [56],Griffin and Christie 1821).
17
Summary
Oil manufacturers use different refining processes
to produce the same nominal products, but even
under the same brand name, the properties of the
oils may significantly vary from one product or
batch to another. Manufacturers favor the specifi-
cation of well established and well understood
characteristics,such as the basic physical properties
and oxidation stability. Although manufacturers
provide certificates of oil quality, care has to be
taken that these have not become invalid during
shipment and storage.
The manufacturing process significantly affects the
properties of insulating oils. There is growing con-
cern that modern hydro-refined oils, which often
rely on the use of inhibitors, may have a long-term
stability inferior to that of acid-refined oils. A satis-
factory base oil should always be maintained while
balancing the manufacturing process for good oxi-
dation stability, gassing tendency, and impulse
strength of the oil.
Oil users prefer to develop their own specifications,
based on standards such as ASTM D 3487, to im-
prove oil characterization. The most important
physico-chemical characteristics for the users are
those that measure oil purity and thermal stability.
It is of fundamental importance that appropriate oil
purity be preserved for all applications in electrical
equipment. Oil purity can be maintained if good oil
handling and testing procedures are provided.
Trace contaminants and very small particle con-
tents have recently received more attention because
of improved measurement techniques.
As delivered, new oils require pre-treatment by the
users, but most often this is only drying and filter-
ing, although mixing and additive treatments are
also used. Care has to be taken, as problems with
the miscibility of the compounds can be experi-
enced.
A major problem with oxidation and other addi-
tives is that they are consumed with time; therefore,
the amount remaining has to be monitored peri-
odically, even in new oils. At present, infrared (IR)
spectroscopy seems to be the most accepted
method.
All the properties listed in the various specifica-
tions are important, but some have special merit for
the characterizationof an insulating oil. The impor-
tant ones are those that are likely to vary signifi-
cantly with oil purity and composition as well as
with external parameters, such as temperature and
electric field. Most important are high electric
strength and low viscosity, which are followed by
a low dissipation (power)factor, water content, and
18 January/February 1995-Vol.1 1,
neutralization number. Oxidation stability should
be evaluated to estimate service life.
The relatively new problems of electrostatic charg-
ing, partial discharges and gassing require more
attention. It is important that in the measurement
of the dielectric properties, and electric strength in
particular, the oil is re-homogenized in order to
avoid false test results. The problems associated
with micro-particlesare also emerging as new areas
of inquiry. There is confusion on the significance of
ECT measurements in new oils and many differing
opinions as to whether gas absorbing or gas evolv-
ing characteristics are the most desirable.
Infrared (IR)spectroscopyhas been widely used for
providing a ”fingerprint” of various oils, and liquid
chromatography (LC) and gas chromatography
(GC) can be used to identify the presence of polar
contaminants and additives as well as to establish
the hydrocarbon content. It would be useful to
correlate oil composition with various oil parame-
ters, such as the gassing tendency, impulse
strength, ECT, and electrical discharges.
In spite of existing specifications, the situation is far
from the ideal. Oil users should impose much
stricter and more explicit rules than are currently
used in purchase specifications. Many transformer
users are reluctant to implement new measurement
techniques for better diagnosis of new transformer
oils.
Acknowledgment
This article, and two to follow, were written at the
encouragement of the DEIS Liquid Dielectrics Commit-
tee.
Dr. Andrzej B. Sierota was graduated
from the Warsaw University of Technol-
ogy in 1964 where he also received in
1977his Ph.D. He worked with industry
and standardizing organizations in Po-
land. He also lectured and researched at
various universities in the UK, Italy and
Germany. For two years (1990-1991) he
held an appointment as a Visiting Professor at the EIRC
of the University of Connecticut. From March 1992
until1 June 1994 he worked at the Division of Applied
Physics of the CSIRO in Sydney, Australia. At present,
he is with the Institute of Power and High Voltage
Engineering of the Warsaw University of Technology In
Warsaw, Poland.
Dr. Sierota’s special research interests are modifica-
tion of dielectric materials properties, degradation of
dielectrics in hv electric fields, diagnostic of insulation,
electrical discharges, electrostatic charging, electrical
measurements, and testing of hv equipment. He is a
No.1 IEEE Electrical Insulation Magazine
member of IEE and IEEE and participates in work of
CIGRE WG 12/15.
Andrzej B. Sierota’saddress is Institute of Power and
High Voltage, Warsaw University of Technology, 00-662
Warszawa, UL, Koszykowa 75. Fax: 48-22-41 8652.
Juris Rungis graduated from the Australian Na-
tional University with BSc. and Sc. degrees in Physics
in 1963 and 1965and obtained a Ph.D. front the Univer-
sity of Western Australia in 1969. Since then he has
worked with the CSIRO Division of Applied Physics
and at present is the leader of the Electricity Supply
Technology Project. His research interests include high
voltage measurement and testing techniques and high
voltage insulation diagnostics.
Dr. Rungis is a member of CIGRE Study Committee
33 (Insulation Co-ordination) and participates in the
work of SC12 (Transformers) and SC15 (Insulating Ma-
terials) and also in the activities of IEC TC42 (High
Voltage Testing Techniques). He is a senior member of
IEEE and a Fellow of the Australian Institute of Physics.
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