annelie.lombard@eskom.co.

za



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Paper P507

Cigr 2009
6th Southern Africa
Regional Conference



QUALITY ASSURANCE OF INSULATING OIL FOR USE IN NEW
TRANSFORMERS


A. LOMBARD
Eskom Enterprises
(South Africa)
SUMMARY

Technical standards form the basis for insulating oil purchases. The procurement process commences
with the issuing of tenders which incorporates technical specifications. Within Eskom these technical
specifications are compiled by experts from the various line groups and supporting functions. The
specifications are compiled based on international standards, as well as the inclusion of specifics
derived from company experience and requirements.

In most cases, very limited testing are performed to establish conformation of oils to standards at point
of delivery and the end user are reliant upon the supplier information and documentation. These
practices put the end user at risk, especially when a number of role players are involved in the
handling and storage of the oil. Quality assurance testing becomes very necessary prior to oil
acceptance, not only to ensure that the correct product is delivered, but also to ensure that the oil was
not exposed to contaminants during the process of transportation, transfer and storage.

This paper discusses a number of case studies relating to problems that were experienced, as well as
new testing criteria that had to be established in order to ensure product conformance to the purchase
specification against which the oil was initially accepted.

The case studies cover particulate contamination, reduction of dissipation factor and interfacial tension
of the oil that were experienced as a result of exposure to unknown sources during transportation and
storage of oil. It also covers a case study where the presence of trace amounts of silicone oil
contamination was caused due to the usage of new flexible storage bags.

This paper attempts to make the end users aware of the risks that could be faced if a quality assurance
program to evaluate incoming oil is not in place, as well as the advantages of such a program to enable
the end user to affect the quality assurance process as agreed to during the tender is actually adhered to
by the supplier.

KEYWORDS
Transformer oil, quality assurance, QA, testing
2

INTRODUCTION

Utilities such as Eskom compile technical standards that form the basis for insulating oil purchases.
The procurement process commences with the issuing of tenders which incorporates technical
specifications. The tenders may be issued as a requirement for free oil - that is oil to be used for
topping up, maintenance etc. or the oil requirements may be included in the purchase documents of
power equipment such as a transformer. The specification forms the basis of a tender and suppliers
will offer products that they feel will meet the clients requirements. Within Eskom these technical
specifications are compiled by experts from the various line groups and supporting functions. The
specifications are compiled based on international standards, as well as the inclusion of specifics
derived from company experience and requirements. During the purchase of new equipment, the oil
will be as per manufacturers specification unless a client specifies a different requirement, subject to
the manufacturers approval.

The oil normally arrives in the country on a sea vessel from which it is pumped via pre-cleaned and
only in some cases, dedicated pipelines to a shore tank. The oil may be stored in the shore tank for
days or months, depending on the demand. From the shore tank the oil will be transferred via pipelines
to road tankers (not dedicated insulating oil tankers in most cases). The tankers will transport the oil to
site. At site the oil may be directly pumped into the transformer. The oil will only be pumped into
holding tanks or bags on site if the client specifies that a number of compliance tests need to be
performed prior to filling the transformer.

In most cases, very limited testing are performed to establish conformation of oils to standards at point
of delivery and the end user are reliant upon the supplier information and documentation. These
practices put the end user at risk, especially when a number of role players are involved in the
handling and storage of the oil. Quality assurance (QA) testing becomes very necessary prior to oil
acceptance, not only to ensure that the correct product is delivered, but also to ensure that the oil was
not exposed to contaminants during the process of transportation, transfer and storage.

SPECIFICATION AND REQUIREMENTS

A client may require oil that conforms to a specification such as indicated in Table 1 below. The
suppliers will offer a product that they feel meet the clients requirements. The oil would initially be
tested during batching at the refinery for most of the criteria listed on the clients specification. In most
cases it has been observed that the full test set is not performed by suppliers on batching of the oil.

From the refinery the oil will only be checked prior to loading onto the sea vessel, at point of off
loading into the shore tank, prior to loading and after loading into the road tanker. If the client insists
some checks specified may be performed prior to filling of equipment. In most cases the intermediate
checks only include checking of the dielectric strength, moisture, tan delta and appearance. On transfer
into the customers equipment, if the client does not specify a testing protocol, the oil may only be
checked for dielectric strength and moisture.

Based on some of the case studies discussed later, a testing protocol for prior to filling has been
compiled by Eskom that includes twelve of the tests listed in Table 1. The tests selected in Table 2
were decided upon due to merit of importance as well as characteristics that may be detrimentally
affected by contaminated pipelines, tanks and tankers. The list of tests as well as acceptance criteria is
given in Table 2 below.
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TABLE 1: Recommended limits for oil properties of new (virgin) inhibited oils (Type I).
Oil Unit Specification Reference and/or test
method

Oil type Naphthenic (Type I) Inhibited
Colour ISO units 0.5 max. ASTM D1500
Inhibitor % Inhibited
(see Anti-oxidant additives)
IEC 60666
Appearance Clear, free of sediment and
suspended matter
ASTM D1500/ISO 2049
Density @ 20 C kg/dm
3
0.895 max. ISO3675/ISO12185 or
ASTM D1298
Kinematic viscosity @ 40 C mm
2
/s 12 max. ASTM D445/ISO 3104
Flash point C 140 min. ASTM D93/ISO 2719 (closed cup)
Pour point C 21 max. ASTM D97
Aromatic content % 6 to 14 max. ASTM D2140/IEC 60590
Total fufural and furans mg/kg 0.1 IEC 61198
Polyaromatic hydrocarbons % 3.0 max. BS2000 / IP 346
Aniline point C 63 to 84 ASTM D611
Interfacial tension
@ 25 C
mN/m 40 min. ASTM D971
Neutralization value mg KOH/g 0.015 max. IEC 62021-1
Corrosive sulphur Non-corrosive IEC 62535
Moisture mg/kg 10 max.
(1)

20 max.
(2)
10 max.
(3)

IEC 60814 and ASTM D1533
Anti-oxidant additives % by mass 0.4 max IEC 60666
Oxidation stability RBOT minutes 220 min ASTM D2112 (RBOT)
Dielectric strength kV/2,5 mm 70 min.
(1)
60 min.
(2)
70 min.
(3)

IEC 60156
Dissipation factor @ 90 C 0.005 max. BS 5737 or IEC 60247
Gassing tendency mm
3
/min +5 IEC 60628 (Method A)/ASTM
D2300
Maximum particulate
contamination per 100 ml
Particule size
> 5 m
Particule size
> 15 m
2000 particles
250 particles
or 11/8 (ISO rating)
(3)

130 000 particles
16 000 particles
or 17/14 (ISO rating)
(2)

ISO 4406 (2000)/IEC 60970/IEC
60422
Silicon/silicone Content ppm Not detectable ASTM D6595
Polychlorinated biphenyl mg/kg Not detectable IEC 60619/EPA 600/ASTM D4059
NOTE 1: Prior to transportation
NOTE 2: On delivery
NOTE 3: Prior to filling

Table 2: Recommended limits for oil properties of new (virgin) inhibited oils

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Test criteria Acceptance criteria
1
FTIR ( oil type verification) Depends on oil ordered
2
Water content <10 ppm
3
Dielectric strength >70 kV
4
Dielectric dissipation factor (Tan
delta)
< 0.005
5
Interfacial tension > 40 mN/m
6
Test for PCB Non detectable
7
Acidity > 0.01 mg KOH/gram oil
8
Test for silicon (RDE) < 2 ppm
9
Corrosive sulphur A negative result
10
Sludge Non detectable
11
Appearance Clear from sediments and suspended matter
12
Particle analysis As per ISO 4406 (2000) - 17/14 ISO rating


TESTING

In general, the electrical characteristics of insulating fluids are influenced by the intrinsic properties of
the fluid, the presence of water and particles as well as the presence of dissolved polar compounds.
Moisture and particles mostly influence the dielectric breakdown voltage, whereas the power factor
and the resistivity are impacted upon more by dissolved polar compounds.

INTERFACIAL TENSION

New oil should have a high interfacial tension (IFT) value, which will decrease with the use of the oil.
The interfacial tension of a mineral insulating fluid is related to the deterioration or oxidation of the
oil. The oil is essentially a non-polar saturated hydrocarbon, however when the oil ages, oxygenated
species such as carboxylic acids, which are hydrophilic, are formed. Contamination of products that
are polar would thus also have an effect on the IFT. Prior to energising, the oil should have an IFT
value > 35 mN/m.

Tan Delta or Dielectric Dissipation Factor

The Tan Delta or Dielectric Dissipation Factor test measures the loss angle or percentage of current
that leaks through the oil under a high voltage stress in a test cell. This factor is dependant upon the
amount of ions, which are a by-product of oil degradation, present in the oil. New oil should have a
very low tan delta value. This value will, however, increase with the use of the oil. Water will not
directly affect this property, but might form stable complexes, which will give higher tan delta values.
As the oil ages, oxidation will cause the tan delta to increase.

Sludge and Sediment

Transformer oil consists of approximately 2900 hydrocarbons of which 2-35% is aromatic. The
greatest factor in the formation of sludge is the oxidation of the transformer oil. Sludge is a resinous
polymeric substance that becomes insoluble in transformer oil. It is partially conductive, hygroscopic
and is a heat insulator.

Sediment in transformers is normally made up of particulate contaminants that have precipitated out of
the oil. Sources of contamination are created during the manufacture, maintenance activities,
degradation of the cellulose insulation, or normal operation of the transformer. Other particles are
metal shavings from abrasions inside the unit, maintenance, repair work, or transformer construction,
shot-blast from cleaning, varnish chips, paint chips and carbon.
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MOISTURE CONTENT

Moisture is usually present in the oil as free moisture, in a soluble or dissolved form, or when
adsorbed by polar ageing products and is then called bound water. It has been found that as
temperature increases, some bound water can be converted into soluble water. Moisture is normally
attracted to very dry oil and any humidity in the air will affect the results. If tankers do not have
breathers, or the oil is not transported under vacuum, the moisture content will increase and the oil will
have to undergo filtration prior to filling.

Acidity or Neutralisation Value

The neutralisation value of the oil is a measure of the presence of acidic compounds in the oil. An
increase in the neutralisation number will normally indicate oxidation of the oil. The presence of acids
is negligible in new or virgin oil, however may be affected if contaminated.

Dielectric Strength

Dielectric strength can be defined as the ability of oil to withstand electrical stress. Moisture, particles
and in particular particles in the presence of dissolved moisture, may migrate to regions of high
electric stress. Fine particles may be dispersed or agglomerate and particle chains may develop.
Particles may even cause partial discharges to develop in the oil which will decrease the breakdown
voltage of the oil.

Particles can originate from various sources:

Cellulose fibres trapped in the transformer after manufacture or repair.
Metal particles from abrasion pump wear or manufacture and assembly.
Filter particles, originating from oil processing.
Silica gel dust from the breathers.
Small flakes from varnishes and other coating materials.

Acceptable values prior to energising the transformer should be as high as possible. Larger utilities tend to
prefer values of equal or above 70 kV.

Corrosive Sulphur

Some concern has been raised regarding the corrosiveness of sulphur in transformer oil and the impact
this has on the transformers insulation system. Sulphur in the oil reacts with the copper (conductors)
under high temperature conditions, forming copper sulphide. This formation is exacerbated by low
oxygen content in the oil such as when conservator bladders are installed on the transformer. Copper
sulphide is conductive, adheres to most surfaces (importantly, the paper insulation) and does not
dissolve in the oil. Deposits of this harmful compound may be responsible for several transformer
failures seen over the years.

Oil is not the only material that contains sulphur. Sulphur compounds are also present in the gaskets,
some water-based glues, copper and paper insulation used in the manufacture of transformers. Sulphur
can also be introduced into the transformer through accidental means such as through the use of
incompatible hoses.

PARTICLE CONTAMINATION

Insulation problems involve predominantly impairment of insulation conditions in service. A general
ageing problem is the accumulation of conductive and polar particles in oil, as well as the deposit of
these particles on the surface of the insulation material. Particles in oil decrease both the AC and DC
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breakdown voltages of the oil. The breakdown voltage is dependent on both the particle size and the
conductivity of the particles. With conducting metal or partially conductive particles such as carbon
and wet cellulose fibres, the decrease of the breakdown strength is significantly greater in the case of
direct voltage. Small particles can agglomerate to form larger particles. These larger agglomerates can
again break up under mechanical and electrical stresses to form smaller particles, resulting in
contradictory test results obtained in some laboratory analyses.

IEC 60422 has published the table below, which indicates acceptable levels of particles in insulating
fluid at various stages of the oil handling process.

ISO
CLASS
Maximum
counts per
100 cm
3

5m
15m
Conta
minati
on
level
Typical
occurrence
Dielectric
strength
Recommended action
Up to 8/5 250 32 Nil IEC requirement for
sample bottle filled with
solvent

9/6 10/7 1000 130 Low Excellent oil
cleanliness during
factory acceptance test

Good No further action 11/8
15/12
32000 4000 Normal Contamination level for
transformers in service
Poor Identify type of particles
Good Dirt or dry cellulose. Repeat
dielectric test with procedure
appropriate for particles.
16/13
17/14
130000 16000 Marginal Contamination level
found in transformers in
service
Marginal Identify type of particles.
Check moisture. Filtering
may be considered.
Good Recheck particle count.
Repeat dielectric test with
procedure appropriate for
particles. Investigate source
of particles
18/5 and
above
High Contamination level
rare and usually
indicative of abnormal
operating conditions
Marginal Filtration or replacement is
strongly recommended.


POLYCHLORINATED BIPHENYL (PCB)

PCB is the generic term for a broad class of fire-resistant synthetic insulating liquids composed of
polychlorinated biphenyls, sometimes with the addition of polychlorinated benzenes. PCB is a
synthetic substance not known to occur naturally. It was first described in technical literature in 1881
and commercial production commenced in the late 1920s. PCB is any one of a number of 209 possible
variations in which one to ten chlorine atoms are attached to a biphenyl group. PCB was produced
under a number of trade names by a number of manufacturers. PCB is soluble in most organic
solvents, but insoluble in water. It is denser than water and when added to water will sink to the
bottom. Most PCB mixtures are non-volatile at a temperature around 40 C, with a flash point at a
temperature exceeding 300 C. Overheating of electrical equipment can produce emissions of irritating
and toxic vapours. PCB is completely destroyed under extreme heat conditions, such as in
temperatures exceeding 1 100 C. PCB can only be found in equipment where it had been
intentionally placed or accidentally mixed in. The presence of PCB in mineral insulating oil is due to
contamination during top-ups, purification, filtration or oil replacement. PCB is listed on the United
Nations' Persistent Organic Pollutant (POP) list and is a banned substance.

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ANTI-OXIDANT (INHIBITOR) PRESENCE BY MEANS OF FOURIER TRANSFORM
INFRARED (FTIR) ANALYSIS

An inhibitor or antioxidant additive has the effect of slowing down the oxidation of oil and thus the
formation of byproducts such as sludge and acids. It is important to know whether and in what
proportion antioxidant additive has been added in order to monitor additive depletion rate during
service. 2,6-di-tertry-butyl-paracresol (DBPC) is the most commonly used antioxidant, but others may
also be used. DBPC also referred to as butylated hydroxytoluene (BHT), is used as an oxidation
inhibitor (antioxidant) in oils, plastics, food and other materials. The recommended addition of 0.3%
(by weight) to new and used insulating oils is recommended. The presence of inhibitor as well as any
obvious contaminants or oil property deviation may be checked by FTIR, which provides a quick scan
method for this purpose

SILICON/SILICONE

Silicon, a naturally occurring substance (sand/dust) often contaminates insulating oil, but is not
harmful to the unit. However, silicone oil contamination causes excessive foaming under the right
conditions. For large power transformers that use forced oil cooling this may be a problem with
cavitation on the forced oil cooling pumps. New oil or oil that was stored in rubber bags (especially
new bags) may be contaminated due to the presence of low level silicone based releasing agents used
in the manufacturing process of the bags. The presence of silicon may be checked with instruments
such as Ion Coupled Plasma (ICP) or Rotating Disc Emission Spectroscopy (RDE). The presence of
silicon does not automatically imply silicon oil contamination. This should be confirmed by means of
foaming analysis.

CASE STUDIES

As mentioned earlier Table 2 were compiled based on merit of importance as well as characteristics
that may be detrimentally affected by contaminated pipelines, tanks and tankers. Some of the tests
were incorporated based on past experience where problems in the field were

Case Study 1:

During the installation of a new generator transformer, filtration of a batch of new oil, totalling 100
000 litre that was stored in rubber bags, foamed excessively. The laboratory became involved in the
identification of the problem. Prior research as well as experience with foaming oil limited the cause
down to the presence of low levels of silicone oil. The laboratory confirmed the presence of silicone
oil as well as excessive foaming by means of elemental analysis and the foaming tendency test.
Following a lengthy investigation by means of elimination of every possible source in the oil process,
the rubber bags were found to be the root cause of the problem. This was established when the rubber
manufacturer confirmed the use of silicone oil as a releasing agent in the manufacturing process of the
rubber.
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Case Study 2:

A consignment of oil to one of the Transmission stations were tested and found to fail the IFT as well
as the tan delta test. It was suspected that this batch of oil was possibly contaminated with some
solvent during storage. This oil was stored in shore tanks previously not dedicated to oil. It was
decided to check the flash point of the oil as this would confirm this theory. The oil flash point was
established at approximately 20C lower than anticipated, which thus confirmed the hypothesis.

Case Study 3:

Oil was delivered to site for a new installation in Transmission. The oil failed both the dielectric
strength as well as the particulate analysis. In order to identify the source of contamination the supplier
submitted their retained samples prior to transportation. These samples passed both analyses. The
initial oil was filtered and particles were visible under the microscope. The particles could not be
identified in this manner and the filter paper containing the particulates was submitted for electron
microscope scanning. This analysis revealed that the particulates were amongst other, paint flakes,
iron ore, sea sand, fertiliser as well as bird feathers. The source was thus the utilisation of a visually,
but not chemical cleaned tanker.

Case Study 4:

In this particular case a consignment of new oil failed the tan delta test. The cause of failure was
eventually found to be the metal container used for sampling the tan delta. Glass containers are
normally used for new or regenerated oil analysis as the tan delta is normally much lower than tan
delta of in-service oil. Upon resampling in glass containers the oil was found to be conforming.

Case Study 5:

A new batch of oil was issued to a very remote Transmission site in the Northern Cape area. The oil in
this case did not, after several samples were submitted passed the particulate analysis. The on site
container was found to be contaminated and continues filtration of the oil back in the tank did not clear
the debris in the bottom of the tank. Filtration of the oil to specification directly into the transformer
was the only option to resolve this problem.

CONCLUSION

As can be seen from the case studies the quality assurance program that Eskom has instituted did on
many occasions safeguarded their new equipment against oil of inferior quality. It is thus
recommended that power equipment owners be vigilant on quality control of incoming oil in order to
ensure that their plant will reach and perform optimally.

REFERENCES

1. Lombard A, Fourie H, De Klerk P, Theory, design, maintenance and life management of
power transformers: Condition-based monitoring of oil/paper insulation systems, Eskom
Power Series Volume 5, Chapter 8, 2008.
2. Eskom Specification 32-406, Mineral insulating oils (uninhibited and inhibited) Part 1:
Purchase, Management, Maintenance and Testing.
3. Lombard A, Particle analysis Why has it been included in NRS 079-1: Mineral
insulating oils (uninhibited); purchase, management and test. Energize magazine,
September 2006.