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Edition 4.1
(2006-08)
Indian Standard
CODE OF PRACTICE FOR MAINTENANCE
AND SUPERVISION OF MINERAL INSULATING
OIL IN ELECTRICAL EQUIPMENT
( Third Revision )
(Incorporating Amendment No. 1)
© BIS 2007
Price Group 8
Fluids for Electrotechnical Applications Sectional Committee, ET 03
FOREWORD
This Indian Standard (Third Revision) was adopted by the Bureau of Indian Standards, after the
draft finalized by Fluids for Electrotechnical Applications Sectional Committee had been approved
by Electrotechnical Division Council.
This standard was first published in 1961 to cover the maintenance of insulating oil complying
with IS 335 : 1953 ‘Insulating oils for transformers and switchgear’. The first revision was
undertaken in 1978 to bring in line with the new oil requirements given in IS 335 : 1972
‘Specification for new transformers and switchgear’. The second revision was carried out to align
with the corresponding IEC 60422 (1973).
This third revision has been aligned with IEC 60422 (1989) ‘Supervision and maintenance guide
for mineral insulating oils in electrical equipment’ issued by International Electrotechnical
Commission. Values of permissible limits, relating to resistivity, dielectric dissipation factor (Tan
delta) and neutralization value of oil have been aligned with those in IEC 60422 (1989). The
following changes have been made in this revision:
a) Equipment has been categorized in order to take into account different user requirements.
The application and interpretation of tests are tabulated categorywise.
b) Classification of oils in service has been made based on the evaluation of significant
properties and/or their ability to be restored to the characteristics desired.
The requirements of new insulating oils at the time of delivery is covered by IS 335 : 1993 ‘New
insulating oils’. After receipt and storage, but prior to actual use there may be a change in the
properties of the oil particularly in the electrical characteristics due to ingress of moisture or
extraneous contamination. It is normal practice to filter/dehydrate this oil before filling in the
equipment. Moreover, monitoring and maintaining oil quality are essential in ensuring the
reliable operation of oil filled electrical equipment. No specific guidelines exists, as it is possible
that some characteristics may be lower than those specified in IS 335. However, the quality level is
expected to be better to the limiting values applicable for the case specified in the code. This code
helps to compare the value and significance of standardized oil tests and recommends uniform
criteria for evaluation of test data. This standard also indicates the type of treatment to which oil
should be subjected if considered necessary.
If oil deterioration exceeds a certain limit, there is some erosion on safety margins and therefore,
the question of the risk of premature failure of the equipment must be considered. While the
quantification of the risk may be very difficult, a first step involves the identification of potential
effects from the increased deterioration. The objective of this code of practice is to furnish the users
with as broad a base for understanding the oil quality deterioration as available so that they can
make informed decisions on maintenance practices.
The values of the various properties given in this standard should be considered only as indication
of the characteristics. In fact, for the proper interpretation of results, account has to be taken of
various factors, such as conditions of use, type of equipment and the general progression of the oil
characteristics. Sound engineering judgment will have to be exerted in seeking the best
compromise between the technical requirements and economic factors. In deciding the
standardized values of the oil properties, it is important to seek the advice of the equipment
manufacturer also.
In preparing this code, assistance has been derived from the following publications:
IEC 60422 (1989) ‘Supervision Maintenance and Guide for Mineral Insulating Oils in Electrical
Equipment issued by the International Electrotechnical Commission.
Technical Report No. 0037-INS-Oct. 1967 : A New Test for Quickly Determining the Acid Content
of Transformer Oils. Central Power Research Institute, Bangalore.
Technical Report No. 0050-TD (Chem)-March 1970 : The Interfacial Tension Test as Guide to the
Quality of Insulating Oils. Central Power Research Institute, Bangalore.
( Continued on third cover )
IS 1866 : 2000
Indian Standard
CODE OF PRACTICE FOR MAINTENANCE
AND SUPERVISION OF MINERAL INSULATING
OIL IN ELECTRICAL EQUIPMENT
( Third Revision )
1 SCOPE acetone and alcohol under prescribed
conditions.
1.1 This standard deals with maintenance and
supervision of mineral insulating oils 3.5 Neutralization Value (Total Acidity)
complying with the requirements of IS 335 and
IS 12463 in transformers, switchgears, and It is the measure of free organic and inorganic
similar electrical apparatus where oil sampling acids present together in the oil. It is expressed
is practicable and where the normal operating in terms of the number of milligrams of
conditions specified for the equipment are potassium hydroxide required to neutralize the
observed. total free acids in one gram of the oil.
NOTE — Recommendations for oil used in hermetically
sealed and low volume equipment are excluded from 3.6 Specific Resistance (Resistivity)
this code because such equipment is not designed for the
process of routine oil sampling. It is the ratio of the dc potential gradient in
2 REFERENCES volts per centimeter paralleling the current
flow within the specimens to the current
2.1 The Indian Standards given in Annex D are density in amperes per square centimeters at a
necessary adjuncts to this standard. given instant of time and under prescribed
conditions. This is numerically equal to the
3 TERMINOLOGY
resistance between opposite faces of a
For the purpose of this standard, the following centimeter cube of the liquid. It is expressed in
definitions shall apply. ohm-centimeter.
3.1 Electric Strength (Break Down 3.7 Dielectric Dissipation Factor (Tangent
Voltage) Delta)
The voltage at which the oil breaks down when It is the tangent of the angle (delta) by which
subjected to an ac electric field with a the phase difference between applied voltage
continuously increasing voltage contained in and resulting current deviates from π/2 radian
specified apparatus. The voltage is expressed in when the dielectric of the capacitor consists
kV. exclusively of the insulating oil.
3.2 Flash Point
3.8 Interfacial Tension
The temperature at which the oil gives off so
much of vapour that this vapour, when mixed It is a force necessary to detach a planar ring of
with air, forms a ignitable mixture and gives a platinum wire from the surface of the liquid of
momentary flash on application of pilot flame higher surface tension that is upward from the
under the prescribed conditions. water-oil surface. It is expressed in N/m.
3.3 Precipitable Sludge 3.9 Reconditioning
Oil deterioration products or contaminants or
This is a process to eliminate, by physical
both, which are insoluble after dilution of the
means only, solid particles from the oil and to
oil with n-heptane but are soluble in the solvent
decrease the water content to acceptable level.
mixture of equal parts of toluene, acetone and
alcohol under prescribed conditions. 3.10 Reclaiming
3.4 Sediment
This is a process to eliminate from the used oil,
Any substance which is insoluble after dilution all contaminants, insoluble and dissolved, to
of the oil with n-heptane and also insoluble in obtain an oil with characteristics similar to
the solvent mixture of equal parts of toluene, those of a new oil.
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IS 1866 : 2000
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IS 1866 : 2000
– Ensure that each container is filled to about are contemplated for the sample, crackle test or
95 percent of its capacity. any other test is not warranted.
– After sampling, carefully close the sampling NOTE — S D Myer et al have proposed determination of
quality index calculated as ratio of Interfacial tension in
valve. dynes to Neutralization value in mg KOH/g of oil. This
– Label the samples, including at least the index can also be employed in field by determining both
following details : the properties at field.
(Dark brown colour indicates dissolved asphal- The breakdown voltage is of importance as a
tenes and green colour indicates presence of measure of the suitability of an oil to withstand
copper compounds.) electric stress.
Dry and clean oil exhibits an inherently high
Inferences drawn from the above mentioned breakdown voltage. Free water and solid
visual inspection can be used as screening tests particles, the latter particularly in combination
at site and also at the laboratory after receipt of with high levels of dissolved water, tend to
samples for evaluation. The information shall
be noted for record purposes, as it is valuable to 1)
Only under special circumstances.
decide the periodicity of laboratory tests given 2)
Not essential, but can be used to establish type of oil.
in Table 2. However, when the laboratory tests 3)
Restricted to inhibited oils.
3
IS 1866 : 2000
migrate to regions of high electric stress and Its value, negligible in an unused oil, increases
reduce breakdown voltage dramatically. The as a result of oxidative ageing and is used as a
measurement of breakdown voltage, therefore general guide for determining when an oil
serves primarily to indicate the presence of should be replaced or reclaimed, provided
contaminants such as water or conducting suitable rejection limits have been established
particles, one or more of which can be present and confirmation is received from other tests.
when low breakdown voltage values are found
For quickly determining the total acidity of
by test. However, a high breakdown voltage insulating oils in service, a portable acidity
does not indicate the absence of contaminants. testing kit has also been devised with which
7.3 Water Content test for acidity of oils can be determined at site
with ease. The details of the portable kit is
Water may originate from the atmosphere or be given in Annex C.
produced by the deterioration insulating 7.5 Sediment and Sludge
materials. At comparatively low water content,
the water remains in solution and does not This test distinguishes between sediment and
alter the appearance of the oil. Dissolved water total sludge that is oil insoluble sludge plus
shall therefore be detected by chemical or sludge which is precipitated by adding
physical methods. heptane).
Solid matter comprises insoluble oxidation or
Dissolved water may or may not affect the elec- degradation products of insulating materials,
trical properties of the oil. The solubility of fibres of various origins, carbon, metallic
water in transformer oil increases with oxides, etc, arising from the conditions of
increasing temperature and neutralization service of the equipment. The presence of solid
value ( see Fig. 1 ). Above a certain water particles may reduce the electric strength of the
content (The saturation Water content), all the oil and, in addition, deposits may hinder heat
water cannot remain in solution and free water transfer, thus promoting further deterioration
may be seen in the form of cloudiness or water of insulation.
droplets; free water invariably results in
decreased dielectric strength and resistivity Sludge consists of products formed at an
and increased dielectric dissipation factor. advanced stage of oxidation and is forewarning
of sludge deposits in the equipment.
In a transformer, the total water content is 7.6 Dielectric Dissipation Factor (DDF)
distributed between the paper and the oil in a
and Resistivity
ratio that is predominantly in favour of the
paper. Small changes in temperature These characteristics are very sensitive to the
significantly modify the water content of the oil presence in the oil of soluble polar
but only slightly that of paper. contaminants, ageing products or colloids.
Changes may be motivated even when
Using graphs which may be found in the contamination is so slight as to be undetectable
literature, it is possible to obtain at a given by chemical methods.
temperature the water content of the paper
from the measured water content of the oil Acceptable limits for these characteristics
assuming equilibrium conditions. The limiting depend largely upon the type of apparatus and
values for water content which are application. However, high values of
recommended in Table 2 are intended to control dissipation factor may influence the power
the water content in cellulosic insulation within factor and/or the insulation resistance of
acceptable values and are related to normal transformer windings.
operating oil temperatures over 40 to 60ºC. There is generally a relationship between DDF
and resistivity at elevated temperature with
High water content accelerates the chemical resistivity decreasing as DDF increases. It is
deterioration of insulating paper and is normally not required to conduct both tests on
indicative of undesirable operating conditions the same oil.
or maintenance requiring correction. Crackle
test may be used as a field test for detecting Useful additional information can be obtained
free moisture. by measuring resistivity or DDF at both
ambient and at higher temperature such as
7.4 Neutralization Value 90ºC coupled with an unsatisfactory value at
lower temperature is an indication of the
The neutralization value of an oil is a measure presence of water or degradation products
of the acidic constituents or contaminants in precipitable in the cold but generally at a
the oil. tolerable level. Unsatisfactory results at both
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IS 1866 : 2000
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1 Separated selector tanks of on-load tap changers By way of a guide, a suggested frequency of
belong to the same category as the associated tests suitable for different types of equipment is
transformer. given in Table 2. However, oil preservation
2 Oil impregnated paper bushings and other
systems designed to control exposure of oil to
hermetically sealed equipment may be placed in atmosphere may permit less frequent testing.
category D if a routine monitoring programme is
desired. Any tests considered necessary would be Generally, check measurements can be carried
specialized in nature and require separate out on the basis of the following criteria, which
consideration. Refer to manufacturer’s instructions. apply particularly to transformer oils :
3 Small transformers up to 1 MVA and 36 kV are not – Check characteristics periodically, at
included in this classification. Routine monitoring
programme is considered uneconomical for this type of
intervals as suggested in Table 2, unless
equipment. Where a monitoring programme is required otherwise defined by the manufacturer.
for these transformers, the guidelines given for
Category C should be adequate.
– If possible, check at more frequent intervals
characteristics that are determinable at
9 EVALUATION OF NEW INSULATING site.
OIL IN NEW EQUIPMENT – Heavily loaded transformers may require
more frequent testing.
A substantial proportion of mineral oil is
supplied to the final user already filled into – Increase frequency of examination where
electrical apparatus and it is commonly any of the significant properties approaches
recognized that certain properties which reflect the limit recommended for continued
the presence of dissolved contaminants may service.
differ from those accepted for unused oil, that is
oil which has not been in contact with 10.2 Testing Procedures
insulation and construction materials. The The venue of testing and number and types of
extent of changes may vary with type of tests that can be carried out on a given sample
equipment due to the different types material of oil may vary depending on local
and ratios of liquid-to-solid insulation, and circumstances and economic consideration.
should be kept within acceptable limits through
proper oil processing techniques and careful Oil in service will vary widely in the extent of
selection of materials. degradation and the degree of contamination.
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IS 1866 : 2000
In general no one test can be used as the sole 10.3 Classification of Oils in Service
criterion of the condition of the oil sample.
It is virtually impossible to set hard and fast
Evaluation of condition should be preferably rules for the evaluation of oil in service or even
based on the composite evaluation of significant to recommend test limits for all possible
characteristics determined in properly applications of insulating oil in service.
equipped laboratories. However, some users
find it advantageous to make field screening According to current industrial experience, oils
test. in service can be placed in the following
classification based on the evaluation of
10.2.1 Field Screening Test significant properties and/or their ability to be
Field tests are usually limited to visual restored to the characteristics desired.
inspection (colour and appearance), breakdown Group 1 :
voltage and, with some approximation,
neutralization value. These tests can This group contains oils that are in satisfactory
sometimes be used classification of service-aged condition for continued use. Oils with property
oils in accordance with 10.3, though, more values laid in Table 2, for the appropriate
often, field tests are made to identify oil category of equipment, are considered to belong
samples requiring laboratory evaluation. this group. It should be understood that these
limits are indicative only. With the exception of
Experience has shown that breakdown voltage breakdown voltage, one or more properties
tests made on site often produce results that outside the limits indicated do not require
are more reliable than those obtained in the immediate action although, in the long run, the
laboratory following long-distance condition can result in accelerated
transportation and prolonged storage of oil deterioration and shortened equipment life. In
samples. Portable dielectric test sets have been interpreting the data, account has to be taken
available for a long time and have proved quite of various factors such as : conditions of use,
satisfactory. age of equipment and general progression of oil
10.2.2 Laboratory Tests characteristics.
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IS 1866 : 2000
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IS 1866 : 2000
The physical means that are used for removing 13.1.2 Reconditioning Equipment
water and solids from oil include several types
13.1.2.1 Filters
of filtration, centrifuging and vacuum
dehydration techniques. These are generally based on the principle of
forcing oil under pressure through absorbing
If vacuum treatment is not employed it is
material such as paper or other filter media.
advisable to limit the temperature to 60ºC.
Filters of this type are preferentially used in
Vacuum is employed a higher temperature may
removing contaminants in suspension (The
be advantageous. If vacuum is employed, the
filter medium should be capable of removing
initial boiling-point of that oil should not be
particles larger than a nominal 10 µm). These
exceeded, to avoid undue loss of lighter
devices do not de-gas the oil.
fractions. If this information is not available, it
is recommended that the oil should not be The water-removing ability of a filter is
vacuum treated at temperature over 70ºC dependent upon the dryness and quantity of
( see Note ). the filter medium. When filtering oil containing
If it is desired to reduce sludge or free water, water, the water content of the filter medium
cold treatment may be appropriate. rapidly comes into equilibrium with water
content of the oil. A continuous indication of the
Filters deal efficiently with solid impurities, water content of the out going oil is useful to
but are generally capable of removing small monitor the efficiency of the process.
quantities of water such as may be found in oil
from equipment housed in buildings. Where Care should be taken that paper filters are of
relatively large quantities of water are present, the correct grade to ensure that no fibres are
most of it can, and shall, be drained away shed by them.
before filtration of the oil. 13.1.2.2 Centrifuges
Centrifugal separators are, in general, In general, a centrifuge can handle a much
satisfactory for removing free water from oil greater concentration of contaminants than can
and can in any case deal also with any finely a conventional filter but cannot remove some of
divided solid impurities. the solid contaminants as completely as a filter.
If oil is purified hot, its viscosity is reduced and Consequently, the centrifuge is generally found
the throughput with certain types of purifiers is in use for rough bulk cleaning where large
greater. On the other hand, sludge and free amounts of contaminated oil are to be handled.
water are more soluble in hot oil than in cold,
therefore, more effectively removed by cold Frequently the output of the centrifuge is put
treatment. Dissolved and suspended water is through a filter for the final clean-up.
effectively removed by hot vacuum treatment. 13.1.2.3 Vacuum dehydrators
If the oil contains solid matter, it is advisable to The vacuum dehydrator is an efficient means of
pass through some kind of filter processing reducing the gas and water content of mineral
under vacuum. insulating oil to very low levels.
NOTE — Processing inhibited oil under vacuum and at
elevated temperatures may cause partial loss of
There are two types vacuum dehydrators; both
oxidation inhibitors; the common inhibitors, function at elevated temperature. In one
2,6-di-tertiary- butyl-paracresol and 2,6-di-tertiary- method the treatment is accomplished by
butyl-phenol, are more volatile than mineral insulating spraying the oil into a vacuum chamber; in the
oil. The selectivity for removal of water and air in other the oil flows in thin layers over a series of
preference to loss of inhibitor and oil is improved by use
of a low processing temperature. baffles inside a vacuum chamber. In both types
the objective is to expose maximum surface and
Conditions that have been found satisfactory minimum thickness of oil to the vacuum.
for most inhibited/uninhibited mineral oil
processing are : In addition to removing water, vacuum
dehydration will degas the oil and remove the
Temperature Pressure more volatile acids.
ºC Pa 13.1.3 Application to Electrical Equipment
40 5 13.1.3.1 Direct purification
50 10 The oil is passed through a purifier and then
60 20 stored in suitable clean containers. When the
electrical equipment is to be refilled the oil is
70 40 passed through the purifier again, and then
80 100 directly into the equipment. This method
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IS 1866 : 2000
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IS 1866 : 2000
<72.5 72.5 to 170 >170
Appearance Clear, free form sediment and suspended matter
Density at 29.5ºC (g/cm3), Max 0.89 0.89 0.89
Viscosity at 27ºC (cSt), Max 27 27 27
Flash point, (ºC), Min 140 140 140
Pour point, (ºC), Max –6 –6 –6
Neutralization value (mg KOH/g), Max 0.03 0.03 0.03
Water content (ppm), ( see Note 1 ), Max 20 15 10
Interfacial tension (mN/m), Min 35 35 35
Dielectric dissipation factor at 90ºC
and 40 Hz to 60 Hz ( see Note 2 ), Max 0.015 0.015 0.010
Resistivity (90ºC) × 1012 (ohm-cm), Min 6 6 6
Breakdown voltage (kV), Min 40 50 60
Oxidation stability of uninhibited oil
i) Neutralization value (mg KOH/g), Max 0.4 0.4 0.4
ii) Sludge (percent by mass), Max 0.1 0.1 0.1
Oxidation stability for inhibited oil
Induction period (hours) Similar values as before filling
NOTES
1 For use in transformers under 72.5 kV class; the maximum water content should be agreed between supplier and user
depending upon local circumstance.
2 Higher dielectric dissipation factor values may indicate excessive contamination or the misapplication of solid
materials used in manufacture and should be investigated.
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IS 1866 : 2000
Table 2 ( Concluded )
Property Test Venue Category of Frequency of Tests Recommended Action Notes
(Unit) F = field Equipment Action Limits
L = laboratory
(1) (2) (3) (4) (5) (6) (7)
Water L O,A,B,C,D,E O,A–After filling or O,A,D: ≤ 20 PPM Check source of 1 The given
content refilling prior to B: ≤ 40 PPM water and consider . values are
energizing–then E: ≤ 30 PPM reconditioning applicable only
after three and 12 C: ≤ 50 PPM where acidity
months, does not
subsequently in exceed
conjunction with 0.1 mg KOHg
dissolved gas 2 For
analysis . variation of
B,D,E–After filling water content
or refilling prior to of (IS 335)
energizing–then transformer
after 12 months, oil with oil
subsequently every temperature
one year or in and acid
conjunction with value.
dissolved gas See Fig. 1
analysis. Not a
routine test: only
when break down
voltage approaches
the rejection level
Neutrali- L O,A,B,C,D, Yearly O,A,B,C,D,E, Max Replace of Perform tests
zation E,F,G 0.3 mg KOH/g reclaim oil more frequently
value when
neutralization
value exceeds
0.2 mg KOH/g
Sediment L O,A,B,C,D,E Routine test-yearly No sediment or Where sediment is
and sludge precipitable sludge detected,
should be detected, recondition oil.
results below 0.02 Alternatively if
percent by mass more economic, or
may be neglected other tests dictate,
replace oil. Where
precipitable sludge
is detected consider
replacing or reclai-
ming existing oil
Resistivity L O,A,B,C,D,E After filling or At 27ºC, Min Investigate
C,E–Routine refilling prior to 1 × 1012 ohm-cm
test–yearly energizing–then 0.1 × 1012 ohm-cm
yearly At 90ºC, Min
Dielectric L O,A,B,C,D,E After filling or O,A,D, Max 0.2 Investigate Comply with
dissipation C,E–Routine refilling prior to B,C, Max 1.0 manufacturers
factor at test–yearly energizing–then E, Max 0.3 instructions if
90ºC and yearly other frequency
40 to 60 and limit are
Hz recommended
Interfacial L O,A,B,C,D,E O,A,B,C,D,E– O,A,B,C,D,E Investigate
tension After filling or Min.: 15 mN/m
refilling prior
to energizing–
then yearly
Gas L O,A,B,C,D,E – – – Comply with
content manufacturer
instructions
Flash point L O,A,B,C,D,E Yearly O,A,B,C,D,E Replace oil,
decrease in flash equipment may
point 15ºC (Max) of require inspection
the initial value,
minimum value
125ºC
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IS 1866 : 2000
ANNEX A
( Clause 4.3 )
DETERMINATION OF SEDIMENT AND SLUDGE
This method covers the determination of assistance of vacuum; rinse the flask with fresh
sediment and of precipitable sludge in used n-heptane to ensure complete transfer of the
insulating oils. precipitate to the crucible. Wash the crucible
and precipitate with n-heptane until free from
NOTES — For the purpose of this guide, sediment is
any substance which is insoluble after dilution of the oil
oil.
with n-heptane and which is insoluble in solvent Allow any n-heptane to evaporate and then dry
mixture mentioned in A-1. the crucible in an oven at 100 to 110ºC for 1 h.
Cool the crucible in a desiccator and then weigh
For the purpose of this guide, perceptible
it. Calculate the increase in mass of the
sludge is oil deterioration products or
crucible as a percentage of the mass of oil
contaminants, or both, which are insoluble
taken. Denote this value, representing the total
after dilution of the oil with n-heptane under
of insoluble material such as sediment and
prescribed conditions but which are soluble in
perceptible sludge, as A.
the solvent mixture mentioned in A-1.
Dissolve the sludge in the crucible by treatment
A-1 PROCEDURE with the minimum quantity of a mixture of
equal parts of toluene, acetone and alcohol
Thoroughly agitate the sample of used oil in the (either ethanol or iso-propanol may be used, 95
original container until any sediment is percent being satisfactory in either case), at
homogeneously suspended in the oil. approximately 50ºC, until no more will dissolve,
and collect the washings in an accurately tared
Weigh approximately 10 g of oil to the nearest flask. Distill off the solvent; visual examination
0.1 g into a stoppered conical flask and of the flask content at this stage will show
introduce a volume of n-heptane corresponding whether any precipitable sludge was present in
to 10 ml for each gram of oil taken. the oil.
If a quantitative value is required dry the flask
Thoroughly mix the sample and solvent and
in an oven at 100 to 110ºC for 1 h. Cool the flask
allow the mixture to stand in the glass flask, in
in a desiccator and then weigh it. Calculate the
the dark, for 18 to 24h.
mass of residue in the flask as a percentage of
If a solid deposit is observable filter the the mass of oil taken. Denote this value as B.
solution through a tared sintered glass crucible The difference A-B, if any, will represent
of Grade G-4 (5-15 microns) porosity with the sediment in the oil.
ANNEX B
( Clause 13.2 )
GENERAL GUIDANCE FOR OIL RECLAIMING
B-1 GENERAL CONSIDERATIONS steam-treated, or acid-treated. The processed
This is a process which eliminates, by chemical clays are more active but also more expensive.
and adsorbent means, the acidic and colloidal Activated alumina is an adsorbent for
contaminants and products of oil deterioration impurities found in oil. It is mechanically more
from the oil to obtain an oil with many stable, and may be reactivated.
characteristics similar to those of a new
product. In general, reclaiming is done in accordance
with one of two methods:
B-2 ADSORBENT PROCESS
Fuller’s earth, a naturally occurring clay with a a) Percolation through coarse clay using
fairly high surface activity, is the material most either gravity or pressure to force the oil
frequently used for reclaiming oils and is the through the clay, or
least expensive. It may be used in its original
state, except for drying, crushing, and sizing, or b) Contact at an elevated temperature with
it may be calcined, water-washed, finely divided clay.
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IS 1866 : 2000
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IS 1866 : 2000
oil reconditioning has been done in the past at a B-3.2 Reclaiming by Activated Carbon
central location, the gravity-percolation method Sodium Silicate
of reclaiming has many advantages in
requiring a minimum amount of new This method is capable of variation to meet the
equipment, attention and labour. requirements of different grades of service-aged
oil under favourable conditions, this process is
On a system where the oils requiring attention a continuous one. The method consists of the
are widely scattered in location, service outages following basic treatments:
are difficult to obtain, and spare equipment is
at a premium, some type of portable pressure – An activated carbon treatment in which 2
percolator may be preferred for reclaiming in percent by mass of activated carbon is used.
the field by recirculating the oil in the – A treatment involving 30 percent by volume
equipment. The possibility of recirculation with of a 2 percent by mass sodium silicate
the equipment alive may be considered in such solution.
cases, with due regard to safety measures.
– A clay treatment in which 2 percent by mass
Irrespective of the type of clay used, two of activated Fuller’s earth is used.
adjuncts should also be incorporated with the
treater: The oil is heated to 85ºC and is maintained at
a) The oil should be put through some this temperature until the final filtering
device for removing free water before it operation is reached.
contacts clay in order to prevent water The first step consists of a treatment by
from wetting the clay. agitation with activated carbon in cases where
b) Water will cause at least partial and the acid rating of the oil is 0.5 mg KOH/g or
possibly complete blocking of the clay, over. This step is necessary to prevent
thus making it necessary to discard that subsequent emulsification of acid oil with the
batch of clay. The oil coming out of the sodium silicate solution where the acid value is
clay treater should be put through some low, this process may be omitted.
kind of foolproof completely automatic The oil is next decanted through a filter to a
dehydrator equipped with positive means second tank where it is paddle-stirred with the
and safeguards for preventing any water sodium silicate solution. It is then run through
from being present in the finished a centrifuge and the silicate solution discarded.
product. This is particularly true when
recirculating the oil in a transformer and The oil is now run into a reaction tank with clay
absolutely essential if the reclaiming is added through a hopper. The resulting mixture
done when the transformer is energized. is agitated, allowed to settle and then cleaned
by passing through a second centrifuge. The oil
B-3 OTHER RECLAIMING METHODS is then run into a receiving tank and allowed to
B-3.1 Reclaiming by Trisodium Phosphate cool. Finally it is filtered and run into storage
tanks.
The trisodium phosphate/activated Fuller’s
earth method ( see Fig. B2 ) consists in When used without activated carbon, the
agitating a mixture of oil and trisodium process is continuous with an output of 570
phosphate solution maintained at 80ºC for 1 h litres per hour. When the activated-carbon
and then allowing the mixture to separate. treatment is necessary the process becomes a
Most of the spent phosphate solution is drained batch process with an output of 1 900 litres per
from the tank, the balance is washed from the day. As both clay and activated-carbon retain
oil with a water spray, and the oil is then about 60 percent of their weight of oil, the
decanted through a centrifuge and a heater to process should be run with a minimum of these
another tank, where 77 mesh/cm activated materials. Oil in fair condition shows
Fuller’s earth is added and the mixture satisfactory characteristics when treated with
agitated. This agitation with clay is allowed to activated carbon and clay; 1 percent of the oil
settle out overnight. The oil is again washed volume of either material is normally sufficient.
with hot water, decanted through a centrifuge,
and then dehydrated by passage through a B-3.3 Percolation by Thermo-Siphon
dehydrator or filter. Bypass on In-Service Transformer
The process is described as economical and Good oil which is deteriorating slowly may be
capable of yielding a uniform product by held in safe operating condition by applying a
varying the amounts of reclaiming agents as special bypass earth filter to the individual
determined by the analysis of the deteriorated transformer. The oil is forced through the filter
oil. The method may be more economical than by the action of the heat generated by the
reclaiming with clay alone for large quantities apparatus and the heat dissipated by the filter.
of badly deteriorated oil. As the actuating force is small, the filters must
16
IS 1866 : 2000
be loosely packed coarse activated alumina or is inoperative as the heat necessary to its
0.66 mesh/cm Fuller’s earth is employed, and operation is not constantly available. The
the apparatus operates without attention operation of bypass filters might also be termed
during the active life of the adsorbent. very ‘gentle’ as little force is available to drive
the oil through even a coarse filter bed. There is
The bypass method of maintaining oil in usable also the possibility that fine particles of the
condition has certain definite limitations. On earth may leak through the system into the
standby transformers or on circuit breakers it processed oil.
17
IS 1866 : 2000
ANNEX C
( Clause 7.4 )
PORTABLE KIT TEST METHOD
C-0 This is a simple, rapid and yet sensitive If the same amount of alkali is added to an oil
method for determining the total acidity of of total acidity greater than 0.5 the resulting
insulating oils. solution would be acidic or have a pH value
between 0 and 6 depending on the amount of
C-1 PRINCIPLE acid left un-neutralized.
Similarly, if the total acidity is less than 0.5 the
C-1.1 The total acidity of oil is expressed as resulting solution would be alkaline or have a
neutralization number which is defined in as pH value between 8 and 14, depending on the
the number of milligrams of potassium amount of alkali left behind.
hydroxide required to neutralize completely C-1.4 This change in pH values may be
acids present in one gram of the oil. sensitively determined by use of standard
indicators.
C-1.2 It is well known that all acids produced Thus, if the quantity of alkali is so adjusted
by oxidation of mineral oils are soluble in that it neutralizes 0.5 total acidity exactly oils
alcohol and can be extracted from the oil by it. having a total acidity of less than 0.5 would be
in the alkaline range and those with total
C-1.3 If these extracted acids are treated with a acidity above 0.5 in the acid range.
fixed quantity of suitable alkali, the resulting C-1.5 It has been found experimentally that
mixture would be acidic, neutral or alkaline sodium carbonate (anhydrous) is the most
depending upon the amount of acids present. suitable alkali, as its solutions do not change
concentration rapidly in contact with
For example, if the total acidity of an oil is 0.5 atmosphere, and universal indicator is a good
and to the extracted acids some alkali is added indicator, as this gives different colours at
which just neutralizes the acids, the resulting different pH values which may be easily
solution would be neutral or have pH value of 7. determined visually.
18
IS 1866 : 2000
C-1.6 Thus, with use of appropriate reagents the C-4 PREPARATION OF SODIUM
total acidity can be determined colorimetrically. CARBONATE SOLUTION
C-2 PROCEDURE This solution is prepared by dissolving 0.118 3 g
A 1.1 ml of portion of the insulating oil of anhydrous sodium carbonate in 250 ml of
(approximately 1 g) to be tested is accurately distilled water. 1.0 ml of this solution has just
pipetted into a clean dry test tube. To this enough alkali to neutralize the acids extracted
added 1 ml of rectified spirit (ethyl alcohol) and from an oil with an acid number of 0.5.
mixture is gently shaken. Sodium carbonate solution should be prepared
One millilitre of solution of 0.085 N sodium carefully taking the necessary precautions as
carbonate is then added. used in such procedures. This solution has a life
After shaking the test tube again, five drops of of three to four months after which it must be
universal indicator are added. discarded and fresh one shall be made.
The resulting mixture develops a colour C-5 PRECAUTIONS
depending on the pH value of the mixture. C-5.1 The test tubes and pipettes used for the
Oils having total acidity of 0.5 total acidity of 0 test should be absolutely clean and dry. It is
to 0.5 shall show transition colours from best to wash them with soap and hot water
prussian blue to yellow, whereas those having followed by a final rinse with distilled water.
total acidity 0.5 and above shall show a change The use of chromic acid for cleaning is also
from yellow to vermilion. recommended where possible, but traces of the
Plate 1 gives the colours obtained by using this acid must be completely washed off before
test on oils having neutralization value (total drying the glassware.
acidity) ranging from 0 to 10. C-5.2 Rectified spirit used shall be of good
C-3 PORTABLE TEST KIT quality conforming to IS 323. Commercial spirit
C-3.1 This kit consists of a box containing the (methylated) should not be used. Where
following: possible, the use of ethyl alcohol A R grade is
recommended.
a) Two polyethene bottles containing 100 ml
each alcohol and sodium carbonate C-5.3 While conducting the tests, the test tube
solution of 0.008 5 N concentration. should be gently shaken to mix the solutions
b) An indicator bottle containing universal and not closed with the thumb and vigorously
indicator; agitated. This may lead to contamination of the
c) Four clean glass test tubes; solution.
d) Three graduated droppers, with C-5.4 The same pipette can be used for a
neutralization number values; and number of oils provided it is thoroughly rinsed
e) Instructions booklet. with oil to be tested before pipetting it.
ANNEX D
( Clause 2.1 )
LIST OF REFERED INDIAN STANDARDS
IS No. Title IS No. Title
323 : 1959 Rectified spirits 6792 : 1992 Method for determination of
335 : 1993 New insulating oils ( fourth electric strength of
revision ) insulating oils ( first
1448 Methods of test for petroleum revision )
and its products: 9434 : 1992 Guide for sampling and
[P : 2] : 1967 Acidity analysis of free and dissolved
gases and oil from oil-filled
[P : 10] : 1970 Cloud point and pour point electric equipment ( first
[P : 16] : 1990 Density of crude petroleum revision )
and liquid petroleum 10593 : 1992 Method of evaluating the
products by hydrometer analysis of gases in oil-filled
method ( third revision ) electric equipment in service
[P : 21] : 1990 Flash point (closed) by ( first revision )
Pensky-Martens apparatus 12422 : 1988 Test method for oxidation
( third revision ) stability of inhibited mineral
[P : 25] : 1976 Determination of kinematic insulating oils
and dynamic viscosity ( first 12463 : 1988 Inhibited mineral insulating
revision ) oils
6103 : 1971 Methods of test for specific 13567 : 1992 Determination of water in
resistance (resistivity) of insulating liquids and in
electrical insulating liquids oil-impregnated paper and
6104 : 1971 Methods of test for interfacial press board by automatic
tension of oil against water coulometric Karl Fisher
by the ring method titration–Method of test
6262 : 1972 Methods of test for power 13631 : 1993 Method of test for detection
factor and dielectrical and determination of
constant of electrical antioxidant additives in
insulating liquids insulating oils
20
( Continued from second cover )
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