X WORKSPOT- 10th International Workshop on Power

Transformers, Transmission and Distribution Equipment,

Substations, Materials and Emerging Technologies

FOZ DO IGUAÇU, BR – NOVEMBER, 27 - 30, 2022

Study Committees A2/ D1

Preferential Subject number 3

Risk Assessment and Mitigation of Corrosive Sulphur Other Than DBDS

M. FOATA1)*), K. LINDL1), M. Da COSTA2)

J. LUKIC3), J. JANKOVIC3), D. MIHAJLOVIC3)
Maschinenfabrik Reinhausen 1) Germany, 2) Brazil
3) Institute Nikola Tesla, University of Belgrade, Serbia

ABSTRACT

Power transformer and reactors failures associated to the presence of corrosive sulphur have been
thoroughly investigated over the last couple of decades. Two CIGRE working groups (A2.32 “Copper
sulphide in transformer insulation” in 2005-2009 and A2.40 “Copper Sulphide Long Term Mitigation
and Risk Management” in 2009 -2015) shed considerable light on the copper sulphide formation due
to the presence of DBDS in oil, its risk assessment, and the long-term mitigation alternatives.

This paper will focus on corrosive sulphur species other than DBDS of which are prone to deposit
sulphides on silver which is particularly relevant for silver-plated tap-changers contacts. Different
reactive sulphur species, their origin and their relative corrosivity towards silver will be summarized
and the required tests methods or standards to detect their presence will be reviewed. In general, all
mineral transformer oils contain monosulphides, disulphides and tiophenes and the total sulphur
content in the oil depends on the origin of the crude oil and the following refining process. Elemental
Sulphur however, which was found to be most reactive corrosive sulphur compound to silver, can be
formed from pyrolysis of the oil at very high temperatures (from 600℃) and by catalytic cracking at
lower temperature (250 – 400°C) – for instance when in contact with the adsorbent during oil
reclamation.

The origin of the different corrosive sulphur species, their relative corrosivity to silver, the appropriate
tests to detect them will be presented. Failure scenarios that can occur in tap changers will be
described and the effectiveness of some field tests to detect the problem will be discussed. The risk
assessment for sulphur species other than DBDS will be discussed and the relative efficiency that can
be expected from different mitigation measures and more specifically passivation and oil reclamation
will be discussed in order to support operators of transformers in making the right decision. Indeed,
while the removal of DBDS is no longer a major problem, the removal of sulphur compounds reactive
to silver (such as elemental sulphur and reactive sulphur compounds other than DBDS) can be
challenging. Recent findings about the suitability of different methods for the removal of different
sulphur compounds will be described, together with the differences in their efficiency.

KEY WORDS

Power transformer, elemental sulphur, Disulphides, DBDS, corrosive sulphur, risk assessment,
mitigation, adsorbent, reclamation

* m.foata@reinhausen.com
1 INTRODUCTION

At about the same time that the problem of copper corrosion related to the use of DBDS was well
understood, documented, and being mitigated (2005-2015), failures associated to silver corrosion
seemed to emerge. All reported failures occurred at the On-Load Tap Changer (OLTC) and most were
found to coincide with a recent reclamation of the oil, in many cases to remove DBDS. In 2016,
Maschinenfabrik Reinhausen (MR) and Institute Nikola Tesla (INT) started a joint research program
to investigate the cause and possible mitigation methods related to silver corrosion. This paper
presents the most important findings of this joint project in the form of the most frequently asked
questions raised by power transformer operators.

2 WHERE DO THE DIFFERENT CORROSIVE SULPHURS COME FROM ?

Corrosive sulphur in transformer oil can originate from three sources essentially:

1- Crude oil origin and its refining process

2- Contamination
3- Improper oil reclamation process

2.1 Crude oil origin and refining process

Crude oil naturally contains thousands of different molecules with sulphur; all but a few classes of
sulphur compounds are non-corrosive. Some may actually have beneficial effects by providing
oxidation stability or acting as metal passivators [1]. Modern refining techniques will ensure that the
sulphur containing compounds that would survive the hydro-treatment process have very low
concentrations [1]., are stable, and are non-corrosive [2] per IEC 62535 [3], ASTM 1275-15 [4] and
DIN 51353 [5]. So nowadays, all new insulating oils from established suppliers can be expected to be
exempt of corrosive sulphur

However, experience shows that the presence of corrosive levels of reactive disulphides, originating
from base oil with a lower degree of refining, can still be found in some older transformers in service
[6]. An example of this so-called “old style corrosion” is illustrated in Figure 1.

Before cleaning After cleaning

Figure 1 : Tap selector contacts corrosion caused by insufficiently refined crude oil

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2.2 Contamination

DBDS is an additive that is used in applications other than transformer oil such as high-pressure
lubricants for its antioxidative properties. Its use in transformer oil started from the end of the eighties
and created, a few years later, a spate of failures mostly due to copper corrosion, but a few silver
corrosion failure cases have also been reported [7]. DBDS has been proscribed since 2012 for
dielectric insulation use [8], it is since considered as a contaminant. Nowadays all new oils must be
tested according to IEC 62697-1 and should reveal a non-detectable level of DBDS.

Oil can also be contaminated by contact with other sulphur containing materials. Among possible
others, at least the following have been identified to contribute to some corrosion cases:
• some cements used to fix the porcelains of the bushings to their flange,
• some gaskets materials,
• some damping materials used between the core and the tank bottom,
• some water-based glues used to secure the paper.

Finally, sulphur can also be inadvertently introduced into transformer oil, for example by the use of
incompatible hoses, by cross-contamination from another unit through the processing equipment or
simply by recycling oils retrieved from scrapped units.

2.3 Improper oil reclamation process

By far the most commonly reported silver corrosion cases over the last decade have been related to the
oil reclamation process. Dahlund et al. [9] first reported in 2009 about cases in Europe where oil
became more corrosive to silver following reclamation than before the treatment. The problem was
found to be related to certain design of reclaiming rigs (larger diameter columns) and the conversion
of certain sulphur-organics into elemental sulphur [10].

In the years that followed, similar situations were reported from all over the world in 2012 [11] [12],
2013 [13], 2015 [14] [15], and as late as 2018 [16] and 2019 [17]. Such a surge of cases may look
surprising considering that the high corrosivity of elemental sulphur to silver was well known for
decades [5] [18] and that oil reclamation had been applied without problems for many years. The
following few factors will provide an explanation:

1. Silver plating of OLTC contacts has only been commonly used starting in the early 80’s, these
transformers were not likely to go through an oil reclamation until 25-30 years later.
2. There has been an increase of oil reclamation over the last 15 years to handle the DBDS
copper corrosion issue.
3. Reclamation with reactivating adsorbents started to be applied extensively by late 90’s
4. Post-treatment testing for silver corrosion (DIN 51353 or ASTM D1275-15) was not
systematically applied until recently.

Formation of elemental sulphur is possible only at very high temperatures, from 250-400˚C upwards
in oil cracking reactions. Such conditions are met in the course of oil reclamation process during
reactivation of the adsorbent at high temperatures. Oil cracking can either be purely thermal at
temperatures above 600˚C, depending on the structure of sulphur molecule, or catalytic in the presence
of alumino-silicates (such as some reclamation clays) at temperatures at 250˚C [6]. Elemental sulphur
was also found to be created by the decomposition of DBDS from pure heating at about 275˚C for 12
hours [19]. Based on this information, the analysis of the reclamation process and some rig designs
identified up to four possible contamination sources and countermeasures:

1. By the re-introduction of oil exposed to high temperatures after the reactivation. In order to
avoid this, a proper flushing system of the spoiled oil must be included in the reclaiming rig
design [14].

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 2. An insufficient cool down of the clay after reactivation and before the oil filtering is restarted
[19]. This can be prevented by having proper monitoring of the columns. A maximum
temperature of 200 ˚C is recommended in [17].
3. When the oil storage tank is too close to the clay columns during the reactivation phase
allowing enough heat transfer during the reactivation phase to form elemental sulphur in the
oil [19].
4. From residual sulphur in the clay after reactivation. Prior to re-introducing oil from the bottom
of the columns into the transformer, some quantity of oil should be circulated through the
media to remove potential contaminants, and then be discarded [17].

The measures listed above should guarantee a safe reclamation process but, nevertheless, a proper
monitoring through laboratory testing and strict quality control are always essential.

3 WHICH SULPHUR SPECIES ARE RELEVANT FOR SILVER CORROSION ?

For silver corrosion in transformer oil, we can define essentially three sulphur categories as listed
below in order of their reactivity (most reactive to less reactive):

1. Elemental Sulphur (S8)

2. Some reactive disulphides other than Dibenzyldisulphide (DBDS)
3. Dibenzyldisulphide (DBDS)

Although DBDS at medium concentration (50 ppm) reacts to copper starting at 80°C, it does not
create corrosion to silver up to 150°C. On the other hand, a few ppm of elemental sulphur is sufficient
to create silver corrosion at temperature as low as 60 °C. At a 20 ppm concentration, elemental sulphur
will react to silver starting at ambient temperature while copper will remain clean at 80°C even after
72 hours, and minor depositions can be observed at 100°C as shown in Figure 2 [6].

Ag @ 40°C after 18h Ag and Cu @ 80°C after 72h Ag and Cu @ 100°C after 72h

Figure 2: Comparison of reactivity of elemental sulphur to silver (Ag) and Copper (Cu)

Similar tests were performed with DBDS at a typical concentration of 200 ppm. Silver sulphide
deposition did not occur even after 960h at 100°C but, at 150°C, sulphide deposits were formed on the
silver strip after 48-72h.

For the reactive disulphides other than DBDS, the corrosiveness will depend on the exact nature of the
sulphur compounds but it has been observed over numerous field cases to start at around 10 ppm, but
as low as 2.3 ppm in conjunction with a high concentration of DBDS. This is illustrated by the
selected samples of service oils shown in Table 1.

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 Table 1 : Results of corrosive sulphur testing on service oils to ASTM D1275-15

DBDS Other Disulphides Elemental Sulphur Silver strip test

(ppm) (ppm) (ppm) ASTM D 1275-15
178.0 0.2 n.d. Non-corrosive
37.2 1.0 / Non-corrosive
n.d. 1.9 / Non-corrosive
174.1 2.3 / Corrosive
n.d. 4.8 n.d. Non-corrosive
<5 9.4 <1 Borderline corrosive
n.d. 10.2 n.d. Non-corrosive
<5 25.1 n.d. Corrosive

4 WHAT ARE THE FAILURE MODES RELATED TO SILVER CORROSION ?

Contrary to copper sulphide which forms both on the copper surface and in oil with deposition on
paper, silver sulphide grows directly from the silver surface and can form multiple layers of different
thickness thus building a crust which tends to detach as shown in Figure 3.

Figure 3: Formation and flaking of a silver sulphide crust on OLTC tap selector contacts

Observations from the field identified two possible failure modes due to silver corrosion: dielectric
flashover and thermal hotspot.

When silver sulphide flakes detach from the surface of the contact, most often after a tap-changer
operation due to the sliding on the contacts, they become free to move into dielectric-stressed areas.
As silver sulphide is rather conductive, these flakes can create a weak insulation path, which can lead
to a sudden flashover. As illustrated in Figure 4, this is much more prone to occur in OLTC designs
where phases are stacked vertically (mostly in-tank type) so that, by gravity, flakes will travel down
from an upper phase and go across interphase insulation distances.

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 Figure 4: Example of flashover failure mode

The flashover failure mode is less likely in compartment-type OLTCs as phases are positioned
horizontally side by side (Figure 5a) and silver sulphide flakes normally travel downwards without
entering most critical insulation distances. On the other hand, compartment type OLTC, partly due to
their typically higher current ratings, are more prone to develop a hotspot (frequently at the change-
over switch) as a consequence of the formation of a silver sulphide layer on the contact surfaces
(Figure 5b).

a) Horizontal positioning of the phases b) Silver corrosion on the change-over contacts

Figure 5: Typical construction and failure mode of a compartment type OLTC

due to silver corrosion

5 WHAT ARE THE RECOMMENDED TESTS TO EVALUATE THE RISK ?

There have been ambivalent reports about the possibility to detect silver corrosion with conventional
winding resistance measurements and DGA. While some investigations confirmed the presence of
corroded contacts following an abnormal DGA or resistance test, in many other cases corrosion was
observed during an inspection or after a failure without any prior indication from the same tests [19].
This can be explained by the fact that the silver sulphide layer may be completely wiped out from the
surface area by the sliding action of the contacts as shown in Figure 6. In this condition, the copper-
copper contact surfaces will not cause any abnormal results while the risk of flakes detaching, and the
possible resulting flashover remains.

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 Figure 6: Silver plating completely removed by corrosion and action of the sliding contact

Abnormal DGA or winding resistance results should always trigger an investigation, however it must
not be concluded that normal results can be relied upon to exclude the possibility of silver corrosion.
Accordingly, oil tests are always indicated. There a two types of oil test that are available namely:
Qualitative (positive or negative result) to determine the corrosivity, and quantitative (ppm content) to
determine the concentration of the different corrosive sulphur species.

Qualitative methods are DIN 51353 (1985) or ASTM D1275-15. Whereas DIN 51353 is sensitive
essentially to elemental sulphur, ASTM D1275-15 (2015) will also detect elemental sulphur and be
sensitive to other reactive sulphur species as well. DIN 51353 test method is performed by heating of
100 ml of oil with silver strip in air-saturated condition, at 100 °C for 18 h. In ASTM D 1275-15 silver
strip test, 220 ml of degassed oil saturated with Nitrogen is heated with silver strip at 150 °C for 48 h.
Different testing conditions (higher temperature, longer test duration and higher oil/silver surface
ratio) can make the method sensitive to the presence of disulfide (DBDS), elemental sulphur (S8), and
other reactive sulphur compounds (disulfides and mercaptans):

• DIN 51353 is very selective for the presence of trace concentrations of elemental sulphur (S8),
down to 1 ppm.
• ASTM 1275-15 silver strip test is preferable to be used as an acceptance test for silver
corrosion, since it detects a variety of corrosive sulphur species.
• Since ASTM D 1275-15 is very severe test for the oil, it has some disadvantages, such as
potential problem with false positives results, due to possible interferences of silver oxides
deposits (Ag2O). In doubt, it is recommended to perform an Energy-dispersive X-ray
spectroscopy (EDX) of the silver plate.

It is evident that different results will be obtained by using ASTM D 1275-15 and DIN 51353 silver
corrosion test. If oil contains disulfides, usually DIN 51353 will not recognize their presence and will
be negative, while ASTM D1275-15 will be positive. In the case of elemental sulphur presence, both
tests will provide positive corrosion result.

If a qualitative test indicates that the oil is corrosive (including IEC 62535 which is very sensitive for
DBDS), it is then necessary to perform quantitative tests to identify the sulphur compounds present
and evaluate their concentration. Quantitative methods are prescribed in IEC 62697: “Test methods for
quantitative determination of corrosive sulphur compounds in unused and used insulating liquids” and
consist of 3 parts:

• Part 1: Test method for quantitative determination of dibenzyldisulphide (DBDS) (2012)

• Part 2: Test method for quantitative determination of total corrosive sulphur (TCS) (2018)
• Part 3: Test method for quantitative determination of elemental sulphur (2018)

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An alternative to “part 2” was established by the CIGRE Working Group A2.32 in 2009 “Method for
quantification of total reactive disulphides, mercaptans and elemental sulphur” [20]. For silver
corrosion analysis, CIGRE method is preferred as it is more sensitive to sulphur species that are
reactive to silver. It is presumed that IEC TR 62697 – Part 2 will have difficulty to obtain accurate
results due to partial conversion, therefore unrealistic low values may be expected (even in the oils
containing pure DBDS). On the other side CIGRE A2.32 TF 03 will quantify all reactive species,
which can be reduced by Zinc, and sometimes this may lead to overestimated values in the terms of
correlation to corrosive sulphur test parameters as set today. As a conclusion, aforementioned methods
for quantification of total corrosive or total reactive sulphur in the oil on the same sample, in some
cases, may provide significantly different results.

In cases where the insulating oil has been confirmed corrosive to silver after several years of service,
the only way to positively evaluate the presence of corrosion is through a visual inspection of all the
silver-plated contacts and an EDX measurement. It should not be assumed that silver corrosion is
uniform. Numerous field cases have shown that silver corrosion can be limited to a few specific
contacts. This is essentially due to the temperature effect. Contacts that are carrying current most often
(such as change-over selector contacts or current collector rings) may be highly corroded while all
other contacts may be corrosion-free.

Finally, it is worth noting that in some cases, silver corrosion was detected during an internal
inspection although all the oil tests above turned out negative. The situations arise from the fact that an
original content of a few ppm of elemental sulphur may have been fully consumed after a while in
service due to its high reactivity and would be sufficient to cause extensive corrosion of the silver-
plated contacts. In turn, this means that in cases where some sort of contamination to elemental
sulphur is suspected, by contamination or prior reclamation for example, only a visual inspection will
be able to confirm the exact condition of the silver-plated contacts.

6 CAN OIL PASSIVATION PROTECT AGAINST SILVER CORROSION ?

Special metal passivators (based on tolyltriazole) at the recommended concentrations of 100-200 ppm
cover copper surfaces effectively but service experiences [11] [10] and laboratory trials [21] showed
that they are not effective against silver sulphide formation. This is further demonstrated by the
following experiments conducted to simulate service conditions with passivated units and correlations
to the failure investigation findings and previous reports related to the protection of silver and copper
with metal passivator. In order to passivate silver and paper wrapped copper strip, 228 ppm of Irgamet
39 (IR39) was added to new mineral oil and extended ASTM1275-15 Ag and IEC 62535 test were
performed (at 150 °C for 72h). These strips were further used for experiment B. This was done to
simulate real situations in transformer, where the pre-passivated transformer is contaminated with
elemental sulphur.

Table 2 : Results of passivation tests according to ASTM D1275-15 and IEC 62535

Before (ppm) ASTM IEC 62535 S8 After (ppm) IR39 After (ppm)
Test S8 IR39 D1275-15 Ag ASTM IEC ASTM IEC
A 5.6 239 Corrosive Non-corrosive 0.60 0.29 85 35
B* 6.1 124 Corrosive Non-corrosive ND** 0.43 73 12
S8: Elemental sulphur
IR39: Irgamet 39 metal passivator
*- with previously passivated silver and paper wrapped copper strips
** Non-Detectable - limit of detection of S8=0.07 ppm; limit of quantification of S8=0.24 ppm

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 ASTM D1275-15 IEC 62535

Test A

Test B

Figure 7: Silver strip tests and paper-wrapped copper strip tests of Table 2

Results shown in Table 2 and Figure 7 confirmed previous findings that metal passivator is not
effective against silver sulphide formation (corrosive after ASTM D 1275-15), while it was effective
for the protection of paper wrapped copper strips (non-corrosive after IEC 62535). Metal passivator
consumption was higher in the presence of paper wrapped conductors, showing its protective function,
i.e. depletion in formation of protective 1-2 nm layer on the copper plate and adsorption the paper.

As shown in Figure 8, over-passivation at concentrations above 500 ppm seems to provide adequate
protection to silver surface against DBDS but not for low content of elemental sulphur even at 1000
ppm. Taking into account that passivator content will deplete over time and needs to be regularly
monitored / replenished, that passivation is known to cause stray gassing and that a 300 ppm may lead
to increased sludging [22], over-passivation is not considered an adequate measure against silver
corrosion.

Figure 8: Silver corrosivity of oil at different passivator concentrations [21]

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7 WHAT ARE THE APPROPRIATE MITIGATION METHODS ?

Choice and urgency of mitigation solutions to be applied must acknowledge the type of reactive
sulphur compounds in the oil. Solutions for silver corrosion mitigation are limited and available time
restricted, especially in the case of elemental sulphur when it can be very urgent to avoid a transformer
failure. In all cases where silver corrosion is suspected, an internal inspection and possibly cleaning of
the silver surfaces to remove any silver sulphide layer is required before any other measure can be
applied.

Oil change would typically be the most cost-effective option for smaller oil volumes (< 10.000 litres).
A proper oil change procedure requires a thorough draining and rinsing of the internal parts to ensure a
residual corrosive oil content of less than 3%. For larger transformers, oil reclamation with
reactivation of the adsorbent is often financially preferable but this is largely dependent on the
performance of the adsorbent. When performed on-line, the reclamation enables a more effective
removal of corrosive sulphur through a continuous rinsing of the solid insulation. Reactivable
adsorbents used in the industry are of varying composition (alumino-silicates such as Fuller’s earth or
aluminium oxides such as bauxite) and most have been found to have an adequate efficiency for the
removal of DBDS. However, their capability to remove elemental sulphur [19] in particular, but also
other reactive sulphurs [6] may range from totally inefficient to minimally adequate.

In order to evaluate the performance of different reclamation solutions and their applicability to silver
corrosion mitigation, a joint MR-INT project tested nine types of commercially available adsorbents in
addition to a new Highly Selective Adsorbent (HSA) [23] specially designed to mitigate problem of
corrosion of copper and silver induced by elemental sulphur and other disulphides. All tests were
performed using a percolation process by oil circulation through column in two different laboratory
setups (Figure 9) and, in the HSA case, the process was also tested full scale on a 35kV/2.5MVA
transformer at site.

Laboratory scale setup Pilot scale setup

Figure 9 : Laboratory setups used for the oil reclamation tests

Efficiency of the tested adsorbents in the removal of corrosive sulphur species from the oil was
determined by the measurements of oil properties, qualitative corrosion tests and quantification of
corrosive sulphur compounds in the oil, before and after treatments.

Test program had a focus on the removal of elemental sulphur, but a number of tests were also
performed with oils containing DBDS and other reactive sulphurs. Main findings from this
investigation are:

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 • The pilot scale setup simulated very well the performance of the full process performed in the
field, while the laboratory scale setup underestimated somewhat the efficiency of the
adsorbents and is used as fast screening test to evaluate whether the adsorbent is efficient or
not in the removal of particular sulphur compounds.
• All adsorbents showed adequate performance against DBDS but their efficiency is
considerably reduced against other reactive disulphides.
• Fuller’s earth was inefficient in reducing the content of elemental sulphur.
• Only two adsorbents (HSA and natural bauxite) could provide the necessary efficiency in the
treatment of elemental sulphur to make it viable for field application.

A comparison of some adsorbents’ relative efficiency (in oil cycles) for elemental sulphur removal is
exemplified in Figure 10 below.

Considering the high variability in the adsorbents’ performance and the different types of corrosive
sulphur and, also, to ensure the absence of oil contamination from an adsorbent which is releasing
elemental sulphur into the oil, the decision on an oil reclamation should be based on a prior laboratory
or pilot simulation with samples of the corrosive oil and proposed adsorbent. Such a simulation will
also support the cost analysis of the process by providing an estimate of the expected treatment time.

Figure 10: Decrease of elemental sulphur content in oil during treatment

8 CONCLUSIONS

Silver corrosion in transformers bears considerable differences with copper corrosion, namely:
• Much lower reactivity and therefore lower failure probability due to DBDS.
• Much higher sensitivity to elemental sulphur.
• Failures occur essentially at the OLTC (silver-plated contact).
• Addition of a metal passivator is not an effective solution.

Findings from a joint MR-INT research project provided a deeper understanding of silver corrosion
and proposed a series of recommendations on:
• the reactivity of silver to sulphur species other than DBDS and elemental sulphur,
• the required tests to evaluate the risk associated to silver corrosion,
• and the appropriate methods to mitigate the risk.

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