Transformer Life Extension by On-Line Continuous Oil Treatment and Monitoring

Transformer Life Extension by On-line
Continuous Oil Treatment and Monitoring
Field Test Report
Technical Report
Transformer Life Extension
by On-Line Continuous
Oil Treatment and Monitoring
Field Test Report
1001959
Final Report, December 2001
EPRI Project Manager

B. Ward
EPRI • 3412 Hillview Avenue, Palo Alto, California 94304 • PO Box 10412, Palo Alto, California 94303 • USA
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CITATIONS
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Surrey, B.C.
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Principal Investigator
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This report describes research sponsored by EPRI.
The report is a corporate document that should be cited in the literature in the following manner:
Transformer Life Extension by On-Line Continuous Oil Treatment and Monitoring: Field Test
Report, EPRI, Palo Alto, CA: 2001. 1001959.
iii
REPORT SUMMARY
Elevated temperature and the presence of moisture, oxygen, and degradation products accelerate
the decomposition of transformer insulation. On-line continuous removal of these compounds
will prevent their accumulation to levels where they may cause irreversible damage to the paper
in power transformers. This report describes the development of a unique on-line continuous oil
conditioning system, capable of keeping the transformer oil in an in-service transformer at near
new condition at all times.
Background
The insulation system of power transformers consists of oil, paper, and other cellulose-based
solids. Degradation of the insulation system is an ongoing process but is substantially accelerated
by elevated temperature and the presence of moisture, oxygen, and degradation products. In
order to extend the transformer life, it is essential to prevent the accumulation of compounds
primarily responsible for chemical changes in the oil—changes that culminate in deterioration of
the insulation system. It is generally accepted that the useful life of transformers is determined by
the residual strength of the cellulose insulation and not by its oil properties. Ideally, these
destructive compounds should be removed continuously so that accumulated levels do not reach
the point where they can cause irreversible damage to the paper. This report summarizes work to
date to develop technology for on-line, continuous oil treatment and monitoring of power
transformers.
Objective
To develop an efficient on-line continuous oil conditioning system capable of simultaneously
removing moisture, oil, and paper degradation products as well as dissolved oxygen from power
transformers.
Approach
The intent of the project was to build an on-line system that maintains oil in good condition,
rather than reclaims oil in poor condition. Using a plurality of selective adsorbents and
separation techniques, investigators attempted to efficiently remove moisture, acids, and
dissolved metals as well as oil and paper degradation products from transformer oil. They
executed the research in two phases. Phase 1 consisted of preliminary laboratory work to adapt
or develop technology suitable for on-line conditioning of transformer oil. Phase 2 involved
designing, building, and installing an on-line oil conditioning system on an in-service power
transformer and assessing its performance.
v
Results
Laboratory experiments demonstrated that acids, polar oxidation products, and moisture could be
removed with selective adsorbents. A hollow fiber module was used to remove oxygen and
moisture continuously from the oil. In the degassing mode, dissolved gases, moisture, and some
volatiles were removed by applying a vacuum on the shell side. In the dehydration mode,
moisture and other condensable products were removed by circulating the gases from the shell
side through a chiller. A laboratory prototype oil-conditioning unit applying these findings was
built and evaluated.
Based on results of the laboratory prototype, a full-scale, on-line, field-conditioning unit was
designed and built. The unit consisted of three adsorbent towers, a hollow fiber extractor unit, an
oil pump, a vacuum/circulation pump, particle filters and valves, gauges, sampling ports, and
safety devices. All components are housed in a NEMA 4 box. The unit was designed to operate
in three modes—adsorption, degassing, and dehydrating—concurrently or independently. Its
performance was first evaluated in the laboratory under controlled conditions, and later
following installation on both a de-energized and an energized 500-kV transformer in a high-
voltage lab. Results thus far have demonstrated that the full-scale prototype of the on-line
continuous oil conditioning system was capable of restoring the relevant transformer oil
characteristics to the level of new oil or better. Installation of this unit on an in-service
transformer is in progress, with publication of results slated for 2002.
EPRI Perspective
Increasingly, due to cost-reduction measures electric utilities need to employ transformer assets
to the fullest while maintaining system reliability. At the same time, the average age of power
transformers is now in excess of 25 years and many have already exceeded their design life. This
reality coupled with the high cost of transformer failure and/or replacement makes the extension
of useful life a key strategy in cost reduction. Transformer life span is determined primarily by
the life of the solid insulation (paper). Oil and paper degradation products accumulate in the
paper—since the paper preferably adsorbs these compounds—and accelerate aging. Therefore,
the most effective way to significantly extend the life of a transformer is to keep the transformer
oil clean at all times. An efficient on-line continuous oil conditioning system can significantly
prolong the life of the paper insulation, and consequently the life of the transformer, by
maintaining clean oil conditions. EPRI has already been awarded a patent for part of this
technology and will continue to work toward commercialization of the product.
Keywords
Oil conditioning
Oil degassing
Oil purification
Oil dehydration
Transformer insulation
Transformer
vi
ABSTRACT
The insulation system of high voltage power transformers consists of oil, paper and other
cellulose based solids. Degradation of the insulation system is an on going process but is
substantially accelerated by elevated temperature and the presence of moisture, oxygen and
degradation products. Thus in order to extend the transformer life we must prevent the
accumulation in oil of compounds primarily responsible for the chemical changes that
culminate in deterioration of the insulation system. It is generally accepted that the useful life
of transformers is determined by the residual strength of the cellulose insulation and not by its
oil properties. Ideally these materials should be removed continuously so that accumulated levels
do not reach the point where they can cause irreversible damage to the paper.
This report summarizes work to date to develop technology for on-line, continuous oil treatment
of power transformers. The intent was to build an on-line system to maintain oil good condition
rather than reclaim oil in poor condition. The anticipated benefits are reduced risk of dielectric
breakdown blamed for over 75% of extra high voltage (EHV) power transformer failures and
extended transformer life expectancy by retarding the cellulose aging processes.
The research was executed in two phases. Phase 1 consisted of preliminary laboratory work to
adapt or develop technology suitable for on-line conditioning of transformer oil.
Bench scale experiments were carried out using cartridges packed with candidate adsorbents.
Service-aged transformer oil was circulated through the cartridge and samples of oil collected
at the outlet side. These were examined by FT-IR for changes in the level of polar oxidation
products, aromatics and DBPC, and other properties. The results were used to select adsorbents
with optimum affinity towards specific contaminants. Three adsorbents were selected and
configured to optimize the system for the removal of acids, polar oxidation products and
moisture.
Of the several oxygen and moisture removal techniques considered, membranes seemed the
most suited for our application and were studied in detail. A hollow fiber extractor unit
consisting of a bundle of composite fibers cemented in a housing was used for continuous
degassing and dehydrating of the oil. In the degassing mode, with the oil circulating through
the hollow fibers, a vacuum was applied to the housing. Periodic analysis of the oil indicated
that all dissolved gases as well as moisture were removed. The operating parameters effecting
the efficiency of the hollow fiber module such as oil temperature, flow rate, pressure etc. were
studied in detail and used to design the laboratory prototype and field unit.
vii
In the dehydrating mode, the gases in the housing of the hollow fiber extractor were circulated
through a cold trap kept at -20oC. At these conditions, moisture and other volatile products from
the oil migrated through the fibers and were condensed in the trap.
A prototype laboratory scale system was built consisting of a 160L holding tank, variable flow
pump, vacuum pump, adsorbent cartridge holder, particulate filters, hollow fiber extraction filter
controls and valves. In the degassing mode, the system was tested at flow rates up to 330ml/min
and 27.5 mmHg. At these conditions, the system required 8 to 10 volume passes to reduce the
total gas-in-oil content from 11.3% to less than 2%.
Phase 2 consisted of designing, building and installing an on-line oil conditioning system on a
suitable in-service power transformer and assessing its performance. The unit consisted of three
adsorbent towers, a hollow fiber extractor unit an oil pump, a vacuum/circulation pump, particle
filters and valves, gauges, sampling ports and safety devices. All the components are housed in
a 3’x3.5’x8’ NEMA 4 box. The unit was designed to operate in three modes- adsorption,
degassing and dehydrating, concurrently or independently. Its performance was first evaluated
in the laboratory under controlled conditions then installed on a de energized transformer in our
high voltage lab. Its installation on an in-service transformer is in progress.
viii
CONTENTS
1 INTRODUCTION ................................................................................................................. 1-1
2 BACKGROUND................................................................................................................... 2-1
3 METHODOLOGY AND APPROACH................................................................................... 3-1
4 OBJECTIVES AND SCOPE ................................................................................................ 4-1

Phase 1.............................................................................................................................. 4-1
Phase 2.............................................................................................................................. 4-1
5 EXISTING TECHNOLOGIES............................................................................................... 5-1
6 PRELIMINARY LABORATORY WORK .............................................................................. 6-1

Evaluation of Adsorbents.................................................................................................... 6-1
Nature of Adsorbed Materials ........................................................................................ 6-6
Oxygen Removal Methods ................................................................................................. 6-7
Hollow Fiber Extractor Unit ............................................................................................ 6-8
Monitoring Mode ............................................................................................................ 6-9
Degassing Mode............................................................................................................ 6-9
Dehydrating Mode .............................................................................................................6-11
Laboratory Scale Prototype ...............................................................................................6-13
7 DETAILED LABORATORY WORK..................................................................................... 7-1

Identification and Evaluation of New Adsorbents ................................................................ 7-1
Moisture Removal.......................................................................................................... 7-2
Removal of Acids, Polar Compounds and Metals .......................................................... 7-4
Further Evaluation of Hollow Fiber Membrane...................................................................7-13
Identification of Oxygen Scavenging Methods ...................................................................7-13
ix
8 PROTOTYPE DESIGN ........................................................................................................ 8-1
Design Objectives .............................................................................................................. 8-1
Features and Approaches .................................................................................................. 8-1
Process .............................................................................................................................. 8-3
System Commissioning and Beta Testing .......................................................................... 8-4
9 FIELD TRIALS..................................................................................................................... 9-1
10 CONCLUSIONS AND RECOMMENDATIONS .................................................................10-1
A APPENDIX A ...................................................................................................................... A-1
B APPENDIX B ...................................................................................................................... B-1
x
LIST OF FIGURES
Figure 6-1 Bench-Scale Setup for Evaluation of Adsorbents ................................................... 6-2

Figure 6-2 Typical FT-IR (Transmission) Spectra Of New and Aged Naphthenic
Insulating Oils.................................................................................................................. 6-3
Figure 6-3 Typical FT-IR Spectra (Absorbance) Of New and Aged Mineral Oils Showing
the Carbonyl and Aromatic Regions ................................................................................ 6-4
Figure 6-4 Comparison of Adsorbent Capacity to Oil Oxidation Products................................ 6-5
Figure 6-5 GC/MS Chromatogram of Compounds Adsorbed on Adsorbent 9-1 ...................... 6-6
Figure 6-6 HPLC Chromatograms of Compounds Adsorbed on Selected Adsorbents ............ 6-7
Figure 6-7 Diagram of Hollow Fiber Extraction Unit................................................................. 6-8
Figure 6-8 Equilibrium Studies of the Hollow Fiber Extractor................................................... 6-9
Figure 6-9 Gas-In-Oil Content as a Function of Volume Passes Through HFE at 25-30
Mbar, 100 Ml/Min............................................................................................................6-10
Figure 6-10 Laboratory Evaluation of the HFE as a Function of Volume Passes....................6-11
Figure 6-11 Test Chamber Setup for Degassing/Dehydrating Removed by the HFE..............6-12
Figure 6-12 GC/MS Chromatogram of Volatiles from Chiller Trap Removed by HFE .............6-12
Figure 6-13 Schematic of Lab Prototype for On-Line Oil Conditioning....................................6-13
Figure 6-14 Photograph of the Lab Prototype Setup for On-line Oil Conditioning ...................6-14
Figure 6-15 Oil Degassing with Laboratory Prototype Test Setup ..........................................6-14
Figure 7-1 Bench-Scale Setup for Evaluation of Adsorbents ................................................... 7-2
Figure 7-2 The Desiccant Column at Different Stages of Adsorption....................................... 7-3
Figure 7-3 Desiccant testing for water adsorption ................................................................... 7-4
Figure 7-4 Adsorption of Carbonyl Compounds by Different Adsorbents Shown as FTIR
Absorbance Vs. Number of Bed Volumes of Oil Eluted ................................................... 7-6
Figure 7-5 Adsorbents’ Acid Adsorption Capacities Expressed as Neutralization Number
Vs. Number of Bed Volumes Eluted ................................................................................ 7-7
Figure 7-6 Acid Adsorption As Per Fig. 20, but with Expanded X Axis .................................... 7-7
Figure 7-7 IFT Values of Treated Oil Samples On Different Adsorbents ................................. 7-8
Figure 7-8 Adsorption of 2-Furaldehyde on Different Adsorbents............................................ 7-9
Figure 7-9 Adsorption of Bulk Polar Compounds on Different Absorbents..............................7-10
Figure 7-10 Adsorption of Dissolved Cu by Different Adsorbents ...........................................7-11
Figure 7-11 Adsorption of Dissolved Zn by Different Adsorbents ...........................................7-11
Figure 7-12 Oil Color Change Resulting From the Treatment of Different Adsorbents............7-12
Figure 8-1 Schematics of the On-Line Continuous Oil Conditioning System ........................... 8-2
xi
Figure 8-2 On-Line Continuous Oil Conditioning System Prototype ........................................ 8-5
Figure 9-1 Close-up of the On-Line Continuous Oil Conditioning System Connected to
the 500KV Power Transformer ........................................................................................ 9-2
Figure 9-2 On-Line Continuous Oil Conditioning System Prototype Connected in Line to
the 500KV Power Transformer ........................................................................................ 9-3
Figure A-1 HPLC Chromatograph of Polar Compounds in Oil after it was Treated with
Adsorbent 19 (after ~ 6 Volumes of Aged Oil were Passed) ........................................... A-1
Figure A-2 HPLC Chromatograph of Polar Compounds in Oil after it was Treated with
Adsorbent 19 (after ~ 60 Volumes of Aged Oil were Passed) ......................................... A-1
Figure B-1 Adsorption of 5-Hydrohyl -Methyl-Furfuralf on Different Adsorbents ...................... B-1
Figure B-2 Adsorption of Phenol on Different Adsorbents ....................................................... B-2
xii
LIST OF TABLES
Table 5-1 The Oil Conditioning Methods ................................................................................. 5-1

Table 6-1 Relative Capacities of Adsorbents........................................................................... 6-4
Table 6-2 Effect of Adsorbents on Oil Properties..................................................................... 6-5
Table 7-1 Amounts of Gas Removed From the Transformer Oil Per Pass Through the
Membrane Module .........................................................................................................7-13
Table 8-1 Characteristics of the New Voltesso 35 Oil Before and After Passing Through
the On-Line Continuous Oil Conditioning System Prototype............................................ 8-4
Table 9-1 Test Results of the On-Lline Continuous Oil Conditioning System Prototype
Installed in Line on the 500 KV Transformer.................................................................... 9-1
Table 9-2 HFM Efficiency When Employed in the Degassing Mode ........................................ 9-2
xiii
1
INTRODUCTION
The insulation system of high-voltage power transformers consists of oil, paper and other
cellulose based solids. Throughout its service life it is subjected to numerous stresses including
high temperatures, vibration, electric fields, exposure to moisture, oxygen, acids and other
chemical contaminants. It is designed to withstand these stresses for extended periods of time,
but there is a gradual loss in mechanical and dielectric properties that eventually compromises
the unit’s reliability. The degradation is primarily a chemical process that is substantially
accelerated by heat and the presence of oxygen and moisture. Moisture is particularly detrimental
to paper, as it will initiate hydrolysis and scission of the cellulose chain. Oxygen attacks both the
paper and the oil producing a range of acids and other polar materials. Over longer periods of
time, the degradation products accumulate in the insulation and become increasingly active in
promoting further degradation. A generalized degradation mechanism is shown below.
The maintenance of oil and paper insulation quality will significantly reduce the risk of dielectric
breakdown blamed for over 75% of extra high voltage (EHV) power transformer failures.
More importantly it will also extend transformer life expectancy by retarding the aging process
in paper and other cellulose solids.
1-1
Introduction
It is generally accepted that the useful life of transformers is determined by the residual
strength of the cellulose insulation and not by its oil properties. This is because the oil can be
reconditioned by conventional treatment with activated clay such as Fullers earth but the paper
degrades through an irreversible process of depolymerisation.
Unfortunately, while Fullers earth treatment is useful for restoring oil properties it is less
effective in removing degradation products from the paper. This is because moisture, and
many of the degradation products are strongly bound to the paper and are slow to migrate
into the bulk of the oil. It is found that substantial quantities of aging products are retained
by the solid insulation even if oil treatment and re circulation are continued for several days.
The paper and the oil aging processes also proceed at different rates and produce different
chemical by-products. This raises the following concerns: The timing of oil maintenance
procedures may not coincide with requirements to preserve the paper insulation. Fullers earth
may not be very effective in removing cellulose decomposition products, precursors to oxidation
products, including free radicals and peroxides, or catalysts such as dissolved metals. It is well
known that reclaimed oil does not have the same oxidation stability as new oil even though it
complies with the same industry standards. The poor oxidation stability has been attributed to
residual polar compounds that are precursors to acids.
Oxidation inhibitors are usually added to reclaimed oil to improve their oxidation stability
but there are currently no procedures for restoring the thermal resistance of paper insulation.
The thermal degradation of cellulose produces significant quantities of moisture that actively
promotes further decomposition. The moisture significantly increases the power factor, may
result in bubbling in the vicinity of hot-spots, and will increase the risk of electrical breakdown
if it appears as free water in highly stressed regions.
1-2
2
BACKGROUND
Over the last 15 years, Powertech Labs has conducted extensive research in the areas of oil
reclamation processes, oil aging and oil testing, paper decomposition and transformer life
extension.
Results of our research have led us to conclude the following:

· Transformer paper aged in oil subjected to periodic treatment with Fullers earth degraded
considerably less than paper aged in oil without any treatment.
· Oil reclaimed with Fullers earth does not have the same oxidation resistance as new oil.
This is because Fullers earth is not effective at removing some of the polar compounds
that are precursors to acids.
· In the presence of oxygen, paper degrades preferentially to oil.
· Free radicals, thought to be responsible for initiating most of the oil and paper degradation
processes, can be detected in oil subjected to various thermal and electrical stresses.
· Free radical concentration is related to partial discharge activity and indicative of poor
oil quality as suggested by its high power factor.
· Dissolved metal content correlates well with high power factor of the oil.
· The decomposition products of common oil oxidation inhibitors can be detrimental to
the insulation.
These results indicate that in order to extend the transformer life we must prevent the
accumulation in oil of compounds primarily responsible for the chemical changes that
culminate in deterioration of the insulation system. These detrimental impurities are:
· Free and dissolved water
· Free and dissolved oxygen
· Acids, polar compounds and colloids arising from oil and paper degradation
· Dissolved trace metals
· Free radicals and peroxides (oxidation precursors)
· Suspended particles: carbon, metals, cellulose fibers, dust etc.
Ideally these materials should be removed continuously so that accumulated levels do not reach
the point where they can cause irreversible damage to the paper. At the same time, effective
control of highly active but low-level residues would substantially, if not completely, reduce
requirements for Fullers earth treatment to remove much larger amounts of contamination at later
stages.
2-1
3
METHODOLOGY AND APPROACH
There are two approaches for protecting the oil/paper insulation. The traditional corrective
approach is based on periodic oil reclamation and the preventive approach is based on
continuous oil reclamation. Based on the previous arguments, it is apparent that a continuous
on-line insulation conditioning system could provide the following advantages over the
traditional periodic oil reclamation using Fullers earth:
· Oil and paper degradation products could be removed as they are formed. Overall
concentrations would be reduced along with any auto catalytic effects.
· Maintaining a low concentration of degradation products in the oil will also reduce their
concentration in the paper by assisting their transfer from paper to oil. This could also help
to remove residual sludge from the paper and core.
· The oil could be treated using selective filtration techniques.
· The oil and paper degradation processes would become segregated.
· Filters could be adapted to meet specific maintenance requirements.
In addition to the above, proper selection of a conditioning system will selectively trap and
concentrate degradation products from both oil and paper as well as byproducts formed under
abnormal operating conditions. Periodic removal of samples of filter material and laboratory
analysis of retained paper degradation products (e.g. furaldehydes) and other contaminants
would provide an insight on the operational history of the transformer. Specific products may
be indicative of maintenance needs or the presence of incipient faults.
The research work was executed in two phases.
Phase 1 consisted of laboratory work to adopt existing technology or develop new technology
suitable for on-line conditioning of transformer oil. The critical tasks identified as required to
achieve these goals were:
· Preliminary evaluation of promising adsorbents for the removal of chemically active oil and
paper degradation products.
· Identification and evaluation of technologies to remove or control levels of moisture, oxygen
and particles.
· Designing, building and testing of a prototype laboratory-scale system.
The intent was to build an on-line system to maintain oil in good condition not reclaim oil in
poor condition.
Phase 2 would proceed to design, build and test a system for in-service transformers. This was
contingent on successful results from Phase 1.
3-1
4
OBJECTIVES AND SCOPE
The specific objectives of the project were:
Phase 1
1. Assess existing technologies for on-line oil conditioning, (specifically to control levels of
moisture, oxygen, particles, and paper/oil degradation products) with a view to adapting an
existing product to meet project requirements.
2. Develop new technologies for on-line insulation conditioning; specifically to remove

chemically active oil and paper degradation products, organic acids, peroxides, free radicals,
trace metals, sulfur and nitrogenous compounds, colloids and trace metals.
Test prototype laboratory-scale on-line oil conditioning systems on model insulation systems.
Phase 2
1. Based on the laboratory test results, design and install full-scale on-line insulation
conditioning systems on suitable power transformers, and evaluate performance.
2. Evaluate the technical and economic viability of the new insulation conditioning systems for
industry-wide application, assess potential market and manufacturing resources, compile
final report.
4-1
5
EXISTING TECHNOLOGIES
Oil reclamation based on adsorbent beds has been around for quite some time. Typically this
is done off line using activated clay such as Fullers earth or activated alumina. There are also
systems suited for on-line applications. These units are designed to periodically treat the oil
from power transformers in a short time. While they are effective at oil reclamation, they are
too bulky and too expensive for permanent installation.
On-line dehydration of oil has been achieved using heat and vacuum. As with oil reclamation,
these units are intended for high throughput and are too expensive. More recently several
manufactures have offered small on-line units capable of reducing the moisture content of oils.
These are filtration type units packed with adsorbents. Their capacity is limited by the adsorbent
amount and must be replaced regularly.
Currently there are no commercially available technologies to selectively remove dissolved

oxygen from transformer oil. On-line degassing systems using vacuum techniques have been
proposed to remove dissolved oxygen. Utilities have been reluctant to adopt this technique
mainly for fear of creating gas bubbles in the transformer. Another suggested method to reduce
oxygen levels is by purging the conservator gas space with nitrogen. This requires a nitrogen
generator on site and may not be suitable for membrane type conservators.
The oil conditioning methods that were identified for further investigation are generically
classified below.
Table 5-1
The Oil Conditioning Methods
Process Contaminant Removed
Mechanical Filters Particulates
Adsorbent Filter Dissolved Water
Adsorption Media Acids, Oil & Paper Oxidation Products
Ion Exchange Media Ionic Species, Dissolved Metals
Scavenging Media Oxygen, Peroxides, Free Radicals
Membrane, Vacuum systems Oxygen, Gases, Moisture
5-1
6
PRELIMINARY LABORATORY WORK
The preliminary laboratory work consisted of the following tasks:

· Evaluation of adsorbents
· Identifications and evaluation of degassing methods
· Evaluation of dehydration methods
· Build and test a prototype lab-scale continuous oil conditioning system
Evaluation of Adsorbents
The conventional way to evaluate adsorbents is by their capacity to reduce the acid number of
the oil or alternatively to reduce its interfacial tension (IFT). These properties are a reflection of
acidic and polar contaminants in the oil. Previous research has indicated that reclaimed oils had
poorer oxidation stability than new oils with similar IFT and acid number. This was primarily
attributed to residual oil oxidation products or ‘acid precursors’ that are not completely removed
during the reclamation process. These are partially oxidized oil products chemically classified as
ketones , aldehydes and esters. It is our opinion that controlling the levels of acid precursors is
more effective at retarding the aging process than removing acidic products. For this reason we
selected the capacity to remove total ‘carbonyl’ content (sum of acids, and acid precursors) as the
primary criteria for adsorbent evaluation. The adsorbent effect on other critical oil properties was
also evaluated but not used for monitoring purposes. Infrared spectroscopy (IR) or Fourier
transform infrared spectroscopy (FT-IR) is well suited for this application and was used as the
method of choice.
Bench-scale experiments to evaluate several selected adsorbents consisted of a transparent

cylindrical column (approx. 1”id x 10’ long), packed with the test adsorbent. This was connected
to a variable flow pump, used oil reservoir, collection and sampling lines. Other test equipment
were connected as required. The oil used for this evaluation originated from in service
transformers to which 2-furaldehyde, soluble copper and iron compounds had been deliberately
added. The oil was pumped through the adsorbent bed and fractions collected for subsequent
analysis as it exited the outlet port. The bench-scale set-up is shown in Figure 6-1. All collected
samples were analyzed by FT-IR over the entire spectrum and compared to the untreated oil and
to new oil for observable changes. Notable changes occurred in the region of 1700 to 1740cm-1
(carbonyls), 1600 to 1620cm-1 (aromatics), and in the region of 3540cm-1 (DBPC antioxidant).
Typical FT-IR spectra of new and aged naphthenic mineral oils are shown in Figure 6-2.
6-1
Preliminary Laboratory Work
Figure 6-1
Bench-Scale Setup for Evaluation of Adsorbents
6-2
Figure 6-2
Typical FT-IR (Transmission) Spectra Of New and Aged Naphthenic Insulating Oils
In order to obtain relative capacities, the experimental conditions were kept similar as much as
possible. This included activation conditions, mesh size, and flow rate. The FT-IR absorbance at
1710 cm-1 was used to monitor the carbonyl content of the oil in each fraction collected. Changes
in the DBPC and aromatic concentrations were also monitored at the same time. The volume of
oil passed through each adsorbent required to give the same FT-IR absorption was used to
determine the relative capacity. The FT-IR spectra in the region for carbonyls and aromatics are
shown in Figure 6-3.
What is immediately apparent from Figure 6-3 is that under the test conditions used, adsorbent
7-1 has a significant higher capacity than all other adsorbents. The volume of the test aged oil
that adsorbent 7-1 can treat to a given level of oxidation products, as measured by FT-IR is 2 to
4 times greater than the other adsorbents.
In order to obtain relative capacities, the experimental conditions were kept similar as much as
possible. This included activation conditions, mesh size, and flow rate. The FT-IR absorbance
at 1710 cm-1 was used to monitor the carbonyl content of the oil in each fraction collected.
The volume of oil passed through each adsorbent required to give the same FT-IR absorption
was used to determine the relative capacity.
6-3
Figure 6-3
Typical FT-IR Spectra (Absorbance) Of New and Aged Mineral Oils Showing the Carbonyl
and Aromatic Regions
Details of the experimental parameters are given in Table 6-1and the results are shown in
Figure 6-4.
Table 6-1
Relative Capacities of Adsorbents
Adsorbent Mesh Amount Ave. Flow Oil Volume* (ml)

Type Size (g) (ml/min)
Adsorbent 7-1 35-70 46.1 6.8 400
Adsorbent 1 30-60 58.3 7.3 200
Adsorbent 9-1 30-60 64.0 6.3 100
Adsorbent 2 30-60 64.1 11.4 100
Adsorbent 12-1 30-60 64.8 6.7 100
Ion Ex. Resin N/A 81.4 6.2 N/A
*Single Pass Volume required to give 0.001 absorbance units (AU) at 1710 cm-1
6-4
Figure 6-4
Comparison of Adsorbent Capacity to Oil Oxidation Products
Whereas the primary role of the adsorbent was to remove oil oxidation products, the effect
on other oil properties was also determined. The oil properties measured and the results
obtained after 500 ml of aged oil was passed through each adsorbent are given in Table 6-2.
Again adsorbent 7-1 shows the greatest capacity towards polar compounds as shown by the
increase on the oil’s IFT. All adsorbents showed similar capacity towards reducing the acid
content and 2-furaldehyde to acceptable levels. All adsorbents removed some dissolved copper
and iron, but adsorbent 9-1 seemed most effective. This is also reflected in the reduction of the
power factor. These results indicate that a mixed bed adsorbent may be the most effective
combination for over all oil conditioning.
Table 6-2
Effect of Adsorbents on Oil Properties
Adsorbent IFT Neut. No PowerFactor 2-furald. Copper Iron

o
Type (nM/m) (mg/g oil) (%, 100 C) (ppm) (ppm) (ppm)
Adsorbent 7-1 34.8 0.01 4.36 <0.1 0.58 0.14
Adsorbent 1 33.4 <0.01 3.01 <0.1 0.4 <0.1
Adsorbent 9-1 32.6 0.01 2.54 <0.1 0.17 0.1
Adsorbent 2 28.4 0.02 6.60 <0.1 0.72 0.17
Adsorbent 12-1 31 0.01 4.19 N/A 0.67 0.15
Ion Ex. Resin - - 3.24 0.1 0.45 0.13
Initial Oil 26.7 0.05 4 0.4 0.77 0.14
New Oil VE35 38.6 0.01 0.20 0.0 N/A N/A
*Properties of oil after 500 ml – single pass through adsorbent
6-5
Nature of Adsorbed Materials
In order to elucidate the nature of compounds being adsorbed, equal amounts of spent adsorbent
media were analyzed for their chemical composition. The procedure consisted of washing the
adsorbent with hexane to remove residual oil followed by extraction with methanol. The extracts
were analyzed by gas chromatography/mass spectrometry (GC/MS) and high performance liquid
chromatography (HPLC). A typical GC/MS chromatogram is shown in Figure 6-5.
The chromatogram shows a broad band with a number of sharp superimposed peaks. The broad
band represents the multitude of hydrocarbon compounds typical of transformer oils. The sharp
peaks are additional compounds resulting from aging and contamination. The more significant
sharp peaks were tentatively identified by comparison of their mass spectrum with a library of
reference spectra from NIST. Most of these compounds were oxidation products of naphthenic,
aromatic and paraffinic origin. Some of these compounds were acids while others were
breakdown products from the DBPC antioxidant.
Figure 6-5
GC/MS Chromatogram of Compounds Adsorbed on Adsorbent 9-1
Figure 6-6 is a typical HPLC chromatogram of the extracts from various adsorbents along
with the extract from new oil for comparison purposes. The analysis were carried out using a
Hewlett Packard 1090 HPLC system with a photodiode array detector and a C18 reverse phase
column. At these conditions, the more polar compounds elute first. The detector was set to
monitor the signals at 220 and 270 nm in order to detect both polar and aromatic compounds.
6-6
In Figure 6-6, peaks eluting up to 20 min represent polar and oxidation products while peaks
eluting after 20 min represent aromatics and poly aromatics. We can see that all adsorbents
retained polar and oxidation products to varying degrees, however, adsorbent 2 also retained
considerable amounts of aromatics and poly aromatics, more specifically poly aromatic
hydrocarbons (PAHs).
Figure 6-6
HPLC Chromatograms of Compounds Adsorbed on Selected Adsorbents
Oxygen Removal Methods
Several oxygen removal techniques were considered, including:

· Conventional vacuum degassing
· Membrane degassing
· Chemical scrubbing
· Membrane separation combined with chemical scavenging
Of the above techniques, the use of membranes seemed the most promising for on-line
applications. Commercially available porous membranes for degassing liquids were available.
Their applications included de-oxygenating boiler water, aerating drinking water and
oxygenating blood. However, their application for non-aqueous liquids was unproven. One
6-7
advantage of membrane degassing is that unlike conventional vacuum techniques they do not
create bubbles. Many membranes are also available as hollow fibers, vastly increasing their
efficiency due to large surface area to volume ratio. High throughput is achieved by using
bundles of hollow fibers sized for the desired application.
Initial work consisted of evaluating a number of flat porous membranes to assess their
compatibility with oil, degassing properties and oil permeability. For this purpose, a membranes
type filtration apparatus was used. With the test membrane as the filter medium vacuum was
used to determine oil permeability. Membranes that did not swell and appeared impermeable
were further evaluated for degassing ability.
Based on this preliminary work and discussions with manufacturers of porous membranes, a
porous hollow fiber degassing unit was selected for detailed evaluation.
Hollow Fiber Extractor Unit
The unit consisted of a bundle of porous hollow fibers that had been cemented together at both
ends then sealed into a housing which contained two access ports. The inside of the hollow fibers
had been coated with a thin film of highly permeable polymer. A diagram of the unit is shown in
Figure 6-7.
In principle, as oil flows through the inside of the hollow fibers, dissolved gases permeate
through the wall and into the housing (shell side). This continues until equilibrium is achieved at
the operating conditions. If the gases and other products are continuously removed from the shell
side by applying a vacuum or a stripping gas, equilibrium will never be achieved and the oil can
be completely degassed. In order to determine its merits, the hollow fiber extractor (HFE) was
evaluated in the laboratory in various modes including, monitoring of dissolved gases, degassing
and dehydration of transformer oil.
A patent has been issued by the US Patent office for the use of the HFE for all three modes.
Figure 6-7
Diagram of Hollow Fiber Extraction Unit
6-8
Monitoring Mode
A set of bench scale laboratory tests designed to determine the rate of migration of dissolved
gases and equilibration times were carried out using the HFE described above. The equipment
set up consisted of an oil supply, a metering pump, the HFE unit, connecting tubing and valves.
The outlet ports on the shell side were sealed with rubber septa. The system was sealed from and
plumbed in a re circulating mode. The HFE was purged with argon until the air in shell side was
removed. The supply oil consisted of a four liter solution made up with known concentration of
gases. While the oil was circulated through the HFE samples of gas were removed periodically
with a syringe and analyzed by gas chromatography. Figure 6-8 shows the time dependence of
the concentration of gases in the shell side of the HFE. We can see that at the experimental
conditions, gas migration is relatively fast for all gases and equilibrium is reached in 30 to 40
minutes. Performance characteristics of the HFE as a function of flow rate, temperature and
pressure are the subject of another EPRI project.
Figure 6-8
Equilibrium Studies of the Hollow Fiber Extractor
Degassing Mode
The experimental set up was as described above but a vacuum was applied at the outlet of the
shell side of the HFE. The oil used for this test had been saturated with air, other gases were
added in the 50 to 700 ppm range. The gas extraction efficiency was studied at room temperature
as a function of applied vacuum and flow rate. Initial tests conducted in a single pass mode,
6-9
results indicated that degassing efficiency increased with increased applied vacuum.
For example, at an applied vacuum of 500-580 mbar and flow of 13.4 ml/min the gas-in-oil
content was reduced from 11.7% to 5.85%. When the vacuum was reduced to 25-30 mbar,
at a flow of 19.4 ml/min the gas-in-oil content was reduced from 10.96% to 1.17%. These results
confirmed that on line oil degassing was feasible. Subsequent experiments were carried out at
low vacuum (25-30 mbar) and flow rates at 50 and 100 ml/min. Also in order to better simulate
on line transformer conditions, the oil was degassed with the HFE in a re circulating mode.
The gas-in-oil content of the supply container was measured over time and plotted as a function
of the number of volume passes. One volume pass is the time required to pump the volume of oil
equal to that of the supply container. Figure 6-9 shows that the total gas-in-oil can be reduced to
approximately 1% after four volume passes
Figure 6-9
Gas-In-Oil Content as a Function of Volume Passes Through HFE at 25-30 Mbar,
100 Ml/Min
Removal of other dissolved gases tends to follow a similar trend. The results plotted as a
function of volume passes are shown in Figure 6-10.
6-10
Figure 6-10
Laboratory Evaluation of the HFE as a Function of Volume Passes
Dehydrating Mode
During the degassing experiments, it became clear that the HFE some moisture was also
removed from the oil. Further experiments were conducted with a transformer test chamber
set up for another research project was used. The test chamber contained an oil/paper insulation
system designed to simulate hot spots in power transformers. The HFE was connected in line
to the test chamber in a closed loop and oil was circulated through the hollow fibers. The shell
side of the HFE was connected in a closed loop to a chilled moisture trap and the gases circulated
using a small gas circulating pump. Alternatively, a vacuum pump may be connected in a
degassing/dehydrating mode. The experimental set up is shown in Figure 6-11. In one
experiment, the oil in the test chamber was heated to 90o C but was cooled to 70o C prior to
entering the HFE. The chiller trap was set at –20o C and both the oil and the shell side gas
were circulated. At these conditions, a condensate was collected in the chiller trap that consisted
mainly of water. However, detailed analysis by GC/MS revealed the presence of a multitude of
other volatile compounds some of which have been tentatively identified as low molecular
weight acids. The GC/MS chromatogram is shown in Figure 6-12.
6-11
Figure 6-11
Test Chamber Setup for Degassing/Dehydrating Removed by the HFE
Figure 6-12
GC/MS Chromatogram of Volatiles from Chiller Trap Removed by HFE
6-12
Laboratory Scale Prototype
These series of experiments were to test the effectiveness of the adsorption media and the
HFE at a larger scale and equipment configuration more closely resembling field conditions.
A schematic of the equipment setup is shown in Figure 6-13. It consisted of a holding tank
equipped with expansion tank, variable flow oil pump, adsorbent cartridge holders, a depth
and a membrane particulate filters, HFE module and vacuum pump. The system was
instrumented with pressure and temperature gauges and plumbed with by pass and diverting
valves to allow independent operation of in degassing or adsorption mode. An inline power
factor cell was installed for monitoring of oil condition but high background noise precluded
its use. A photograph of the laboratory set is shown in Figure 6-14.
In one experiment to measure the degassing efficiency, the supply tank was filled with aged oil.
Known amounts of gases were added with a syringe and the oil circulated until it was uniformly
mixed. The oil was then circulated through the HFE at 330ml/min while applying a vacuum of
27.5 mm Hg. At such conditions, one volume of the supply tank required 8.1 hours. Samples
of oil were periodically removed and analyzed for gas-in-oil. The results in Figure 6-15 show
that it requires about 9 to 10 volume passes to reduce the gas-in-oil content from 11.3% to less
than 2%. As expected, this is slower than the results from the bench scale test. The main factors
being a faster flow rate (330 vs 50ml/min) and a poorer vacuum. A second HFE from another
supplier was also evaluated, but oil seepage through the hollow fibers was too severe to continue
with the testing.
Figure 6-13
Schematic of Lab Prototype for On-Line Oil Conditioning
6-13
Figure 6-14
Photograph of the Lab Prototype Setup for On-line Oil Conditioning
Figure 6-15
Oil Degassing with Laboratory Prototype Test Setup
6-14
7
DETAILED LABORATORY WORK
The main objective of Phase 2 of this research, as mentioned earlier, was to design, build and
install a full scale on-line oil conditioning system on suitable in-service transformers and
evaluate its performance. When faced with the decision of scaling the prototype before finalizing
its design, it became clear that some unresolved issues remained. More specifically, what other
adsorbents are available with potential higher capacities or better selectivity, what are the effects
of operational parameters on the performance of the hollow fiber unit and what is the optimum
configuration of the adsorbents. To obtain the answers to these questions more detailed
laboratory work was undertaken.
The additional laboratory work consisted of the following tasks:

· Identification and evaluation of new adsorbents in regards to having specific enhanced
capabilities for the adsorption of moisture, acids, polar compounds and metals
· Further evaluation of hollow fiber membrane unit
· Identification of oxygen scavenging methods
Identification and Evaluation of New Adsorbents
The preliminary laboratory work indicated that the moisture in the transformer oil was the most
strongly adsorbed species on the four adsorbents tested. This means that moisture competed
favorably with the adsorption of all oil and paper decomposition products present in the oil, and
to a certain extent impairs the adsorbents’ adsorption capabilities for the decomposition products.
To distinguish the capacities of an adsorbent for oil and paper decomposition products from
adsorption capacities for moisture, two approaches were followed:
1. To find a combination of a potent desiccant, which will completely adsorb only water from
the oil, and a hydrophilic adsorbent or adsorbents, which will be capable of utilizing their full
adsorption capacities only for removing acids, polars, metals and other oil and paper
decomposition products from the moisture free oil.
2. To find hydrophobic adsorbent(s) which will have sufficient adsorbent capacities for oil and
paper degradation products and will not significantly adsorb water, if at all.
A total of 25 adsorbents and ion exchange resins were investigated including those that were
tested in Phase 1. All previously tested materials, after being exposed to different activation
procedures, were retested along with 15 new adsorbents and resins. Eleven of these were new
adsorbents, four of which were hydrophobic. Some of the new adsorbents, as well as Attapulgus
Clay, were tested after being reactivated according to established procedures or manufacturers
instructions.
7-1
Detailed Laboratory Work
Bench-scale experiments conducted to evaluate all selected adsorbents consisted of transparent

cylindrical columns (1.5 cm ID x 15 cm long) packed with the test adsorbent. In the case of
desiccant evaluation, the column used in Phase 1 was employed. The new bench-scale set up
is shown in Figure 7-1. Three columns in parallel were tested at the same time. The feed oil
supplied by a variable flow pump was passed through mechanical filters and then heated in an
oven before reaching the columns. The flow rate was regulated by metering valves mounted
at the inlet of each column. The oil temperature at the column inlet was continuously monitored.
Figure 7-1
Bench-Scale Setup for Evaluation of Adsorbents
Moisture Removal
Two approaches were investigated for the removal of moisture from transformer oil. The first
considered the use of a desiccant and was aimed at total H2O removal in order for the treated
oil to be virtually moisture-free (containing less than ~1 ppm of H2O). The second approach
was based on the use of the hollow fiber membrane already used for O2 removal. In this case,
the moisture removal from the transformer oil per pass would only be partial (up to 50%).
The application of both methods in series was considered a desirable option at this stage.
The reasoning behind this was to partially dry the incoming oil while degassing it by using
a suitable hollow fiber membrane module. Passing the oil through an adsorbent with high
7-2
affinity for water completed moisture removal. This way only moisture free oil would pass
through subsequent adsorption columns without degrading their affinity for oil and paper
degradation products. Since the water in the oil was completely removed, it was anticipated
that the optimum adsorption capacity for oil and paper degradation products would be achieved.
The emphasis was on finding an adsorbent that will selectively adsorb dissolved or dispersed
water from the oil. For that purpose, the aged transformed oil, which was in service and was
destined for reclamation, was used. Because in this particular test the oil had not been filtered
through mechanical filters, particulates (solid degradation products) progressively colored the
column as can be seen in Figure 7-2. Surprisingly, this did not noticeably influence the water
adsorption process,
The Neutralization Number of the untreated feed oil was 0.037mg KOH/g oil and an IFT of
24.4 dynes/cm. During the evaluation process, the oil temperature at the column inlet was
maintained at 60oC.
Figure 7-2
The Desiccant Column at Different Stages of Adsorption
7-3
The initial water content in the feed oil was 250ppm. Since the effective testing took almost 110
hours and most of it was done only during the daily working hours, with a few overnight runs,
the water content in the feed oil constantly dropped since the initial concentration was far above
the equilibrium value for its temperature. From Figure 7-3 it can also be seen that during the
duration of the test the amount of H2O in the treated oil was virtually zero (below the detection
limit of the Karl Fischer instrument -approximately within 1ppm).
Figure 7-3
Desiccant testing for water adsorption
The adsorbent used in this test, under the applied conditions, was extremely efficient. It is worth
mentioning that the test conditions were more stringent than the expected process conditions for
on-line continuous oil conditioning.
Removal of Acids, Polar Compounds and Metals
Most of the adsorbents and resins used for this study were conditioned (activated) prior to use.
Adsorbents were heated at temperatures ranging from 130oC to 265oC in a dry N2 stream,
depending on the nature of the adsorbents, while others were prepared according to the
manufacturers’ recommendations.
Following activation, the adsorbents were packed into the 15 cm long columns of 1.5 cm ID.
The first 12 cm of each column were filled with a particular adsorbent, while the remaining
3 cm at the top of the column were filled with a desiccant The feed was preheated to 55-66oC
7-4
before entering the adsorption columns. The interstitial velocity of the oil was ~10 cm/min.
After passing through the adsorbent columns, the oil was collected within pre selected time
intervals and analyzed. The processed oil was analyzed for Neut. No., IFT, color, FTIR,
Furans, inhibitor content (DBPC), total polar compounds, and metals (Cu, Zn)
Gas chromatography-mass spectrometry (GC-MS) analysis was carried out on samples extracted
from specific adsorbent. The objective was to try to identify the polar compounds, which are
most responsible for the deterioration of certain oil characteristics. The analyses did not reveal
any new information and was not pursued any further.
The feed used for this evaluation also originated from in-service transformers and had been
deliberately doped with propionic acid, 2-furaldehyde, soluble copper, and DBPC. Feed #4 used
for testing had the following characteristics:
H2O IFT Neut. No. FTIR DBPC 2-Fur Feed T
PF kV Col (o
(ppm) (Dynes/cm) (mgKOH/g) (1860-1670) (ppm) (ppm) C)
45 24.9 0.407 9.300 0.12 0.63 7.2 60 2.5 55-65
Polar Compound (ppm) (ppm)

5-Hydroxyl 0.56 0.487
Fur Alc 0.061 0.056
2-Fur 0.611 0.629
Acetyl Furan 0.255 0.258
5 Methyl Fur 0.305 0.313
Phenol 0.588 0.58
5-Meth2 furoate 0 0
m-cresol 1.79 1.268
o-cresol 0.389 0.458
2,3 Dimethyl 0.439 0.475
2,6 Dimethyl 1.254 1.398
Polar (bulk) 1741 1558
Metals (ppm) (ppm)

Cu 0.33 0.32
Zn 0.38 0.34
Since the feed barrel was exposed to atmospheric air at all times, even though the oil was
circulating in the barrel from which it was constantly pumped into the columns, some changes in
the oil composition over time were expected. The oil analysis done at different time intervals
confirmed this to some extent. However, most of the differences could be attributed to
experimental and analytical error.
In order to be able to appropriately compare the adsorbents’ capacities, the experimental

conditions were kept as similar as possible. This included feed flow rate, oil temperature,
adsorbent volume and mesh size.
7-5
The results of the analysis of the treated oil as monitored by FT-IR, neutralization number,
oxidation products, total polar compounds and metals are shown in Figures 7-4 to 7-12.
The FT-IR absorbance at 1674-1807 cm-1 was used to monitor the carbonyl content
(total acids, aldehydes and ketones) of the oil in each fraction collected (Figure 7-4)
Figure 7-4
Adsorption of Carbonyl Compounds by Different Adsorbents Shown as FTIR Absorbance
Vs. Number of Bed Volumes of Oil Eluted
Even though adsorbent 7 has the highest initial uptake, its total carbonyl uptake was much lower
than that of adsorbents 15 and adsorbent 12. Since adsorbent 15 was mostly an acid adsorbent it
may be concluded that for the removal of aldehydes, ketones, and esters in absence of acids, the
adsorbent 7 may be most advantageous.
The DBPC concentration was monitored at an absorbance of 3650 cm-1. Interestingly, none of
the adsorbents tested removed DBPC from the oil.
The Neutralization Number measure only the concentration of organic acids in the oil.
Non-acidic oxidation products (aldehydes, ketones, esters, etc.) are not included. Figure 7-5
shows the adsorption capacities of different adsorbents towards organic acids. From Figure 7-5
it is clear that adsorbent 15 has the highest acid adsorptions capacity followed by adsorbent 12.
The capacity of adsorbent 12, is generally considered high when compared with similar
adsorbents but is considerably lower when compared to adsorbent 15 as can be seen more
clearly in Figure 7-6
7-6
Figure 7-5
Adsorbents’ Acid Adsorption Capacities Expressed as Neutralization Number Vs. Number
of Bed Volumes Eluted
Figure 7-6
Acid Adsorption As Per Fig. 20, but with Expanded X Axis
7-7
Unsurpassed organic acid adsorption capacities of adsorbent 15 maintained the neutralization

number of treated oil at a very low level (<1/20th of incoming concentration) for a very long
time. Near saturation, the acid uptake slowed down, but remained high up to the elution of
450 bed volumes. Reducing the flow rate may further improve its capacity, but this was not
established.
The improvement of oil Interfacial Tension (IFT) after the oil treatment over certain adsorbents
is shown in Figure 7-7. For most adsorbents tested it was characteristic that the first samples of
treated oil had a higher IFT number than later ones. Adsorbents 9, 10 and 7 contributed the most
to the increase of IFT. On the other hand, adsorbents 15 and 8 had virtually no effect.
This test is intended to distinguish which adsorbents have the higher potential for IFT
improvement, but did not make a clear distinction among them. The high acid content present in
the oil, definitely competed with the adsorption of other polar components, and made it less clear
which adsorbent was the best for IFT improvement. It is important to note that IFT is a measure
of the total polar oxidation products including acids. It does not distinguish between acids and
other polar compounds. It is not surprising that adsorbents with a high capacity for either acid
or polar oxidation products will be effective at improving the IFT of the oil. The test oil used for
this study contained high levels of acids and may have obscured the effects of the polar oxidation
products. These are better measured by FT-IR.
Figure 7-7
IFT Values of Treated Oil Samples On Different Adsorbents
7-8
High performance liquid chromatography (HPLC) analysis of treated oil samples were designed
to monitor paper degradation products (furanic and phenolic ) by monitoring the detector signals
at 220 and 270 nm., and total amount of polar compounds eluted in 15 min (total polar) at 254
nm. A more detailed description of these analyses, with a sample chromatogram are shown in
Appendix 1.
Furans analysis was capable of determining the concentrations of the following paper
degradation products: 5-Hydroxyl methyl furfural, Furfuryl alcohol, 2-Furaldehyde, Acetyl
furan, 5-methyl furfural, Phenol, 5-methyl-2-furoate, m-cresol, o-cresol, 2,3 dimethyl, 2,6
dimethyl, and 2,3,5 trimethyl.
Figure 7-8 shows the adsorption capacities of different adsorbents towards to 2-Furaldehyde.
Adsorbents 12, 14 and 4 exhibited the highest adsorption capacities for 2-Furaldehyde.
The adsorption of some other oil and paper degradation products is given in Figures A3 and A4
in Appendix 2.
Figure 7-8
Adsorption of 2-Furaldehyde on Different Adsorbents
The total amount of polar compounds adsorbed by the different adsorbents is shown in
Figure 7-9. Adsorbents 7, 12 and 20 showed the highest capacities for the adsorption of bulk
polar compounds. Adsorbents 12 and 7 showed the highest initial capacities, while adsorbent
20 probably had the highest overall capacity. Relatively poor initial uptake is probably due to
7-9
kinetic restrains. Perhaps the smaller particle size of this adsorbent, or the lower linear oil
velocity may improve the initial uptake.
Figure 7-9
Adsorption of Bulk Polar Compounds on Different Absorbents.
The adsorption of dissolved metals, Cu and Zn, on different adsorbents is shown in Figures 7-10
and 7-11, respectively. Since the metals in the transformer oil are likely to be in the form of
complex metal compounds than in the simple form of salts of organic acids, the emphasis of
their removal from oil has to be more on some form of adsorption than on ion exchange.
From Figure 7-10 it can be seen that adsorbent 10 had the highest uptake for dissolved Cu
followed by adsorbent 9, and to a satisfactory degree with adsorbents 6, 7 and 12. A similar trend
for the two best adsorbents was found for the removal of dissolved Zn (Figure 7-11). In this case,
adsorbent 10 was the best performer followed distantly by adsorbent 9, which was closely
followed by adsorbents 12, 14 and 19.
In summary, for the removal of dissolved metals the best adsorbent is adsorbent 10, however it
cannot be easily regenerated. Therefore, in the case were adsorbent regeneration is of dominant
concern, adsorbent 9 certainly appears as the best alternative, although adsorbent 12 should not
be completely thrown out of the picture.
7-10
Figure 7-10
Adsorption of Dissolved Cu by Different Adsorbents
Figure 7-11
Adsorption of Dissolved Zn by Different Adsorbents
7-11
The color change of the treated oil on the different adsorbents is shown in Figure 7-12.
Even though the feed oil was at the reclamation stage, it contained all of the oil and paper
degradation products in high amounts which probably considerably impaired the adsorbents
capabilities for the removal of color compounds. From Figure 7-12 it is clear that adsorbents 7
and 9 (19) were better than the others, although adsorbents 10 and 12 were very close and should
be further examined.
Figure 7-12
Oil Color Change Resulting From the Treatment of Different Adsorbents
Four hydrophobic adsorbents, 5, 6, 8 and 14, that were tested and in general were not as good as
the best ones. However, some of them performed relatively well and in some aspects were even
better than the most widely used ones. In particular, adsorbent 5 was relatively good for the
removal of acids and the adsorption of carbonyl compounds. Adsorbent 14 was very good in
adsorption of 2-Furaldehude and relatively good for the adsorption of total polar compounds
and for the improvement of the IFT number, while adsorbent 6 was relatively good for dissolved
metal removal.
Even though some hydrophobic adsorbents showed comparable performances with respect to
acid and polar compounds, as did the better-performing hydrophilic adsorbents, they performed
purely in IFT improvement. However, the best acid, polar, and metal adsorptions capacities were
achieved by hydrophilic adsorbents. For some specific applications, where the removal of
moisture is not feasible, the use of hydrophobic adsorbents may be a reasonable option.
7-12
Further Evaluation of Hollow Fiber Membrane
Two additional tests at elevated oil temperature of approximately 50oC and at expected feed
flows were done on two the most promising hollow fiber membrane modules that were available
at this point. Module C-1 with approximately 4000 cm2 of effective membrane surface was
tested at the two flow rates, 0.0356 and 0.11ml/cm2*min. Module U-1 with 140 cm2 of effective
membrane surface was tested only at a higher flow rate of 0.1 ml/cm2*min. The test results are
summarized in Table 7-1.
Table 7-1
Amounts of Gas Removed From the Transformer Oil Per Pass Through the Membrane
Module
Membrane Flow rate Oil Temp. P. drop % Removed per pass

2 o
Type (ml/cm *min) C (psi) H2O O2 N2 CO2
C-1 0.036 45.8 2.5 33.3 52.5 45.8 39

C-1 0.036 50.4 2.5 37.5 54.2 48.8 41.5
C-1 0.110 35.1 14.5 18.2 21.1 18.3 15.2
U-1 0.103 48.2 7.5 46.9 12.2 4.1 5.2
U-1 0.102 46.8 2.5 50 5.8 2.5 9.6
The C-1 module, at the expected prototype flow rate of 0.1 ml/cm2*min was able to remove
21% of the O2 per pass, while moisture removal was around 18%. Unfortunately this module
was permeable to oil to some extent. In addition to being permeable to oil, the pressure drop
through the membrane at that flow rate was relatively high, 14.5psi. The U-1 membrane
exhibited extremely good permeability to moisture, capable of removing half of the dissolved
moisture from oil in one pass. Unfortunately, oxygen removal was relatively low. Exact oxygen
removal capacities were difficult to determine due to the small size of the test module. With a
bigger membrane module it may be clearer which of the two values that are shown in Table 7-2
is more accurate. If the higher number of 12% oxygen removal rate per pass can be confirmed,
by using twice the size of the membrane area than as employed in the C-1 module, U-1
membrane would slightly exceed the capabilities of C-1 module with respect to oxygen.
However, moisture removal in this case would probably exceed 75%. Since the price of U-1
hollow fiber membrane per cm2 is about 3 times lower than that of the C-1 this would be a
preferred option not only because of price, but also because the U-1 membrane is impermeable to
oil. Slight improvements in O2 permeation of the U-1 type membranes would be the best option.
We are currently cooperating with the manufacturer of the gas membrane to proceed in this
direction.
Identification of Oxygen Scavenging Methods
Four potential oxygen scavenging methods were identified. They are based on oxygen
chemisorptions, electro-catalytic, electrolytic or catalytic consumption of oxygen. A brief
description is shown below.
7-13
· Catalytic O2 dissipation (has been tested)

– Catalytically removes O2 from ~ 0.5% O2 in the gas stream to less than 10 ppm of O2
per pass.
– It works efficiently at all gas flows tested
– Requires a constant supply of H2 or CO
– In the case of H2, the minimum operating temperature is 70oC while in the case of
CO, the minimum operating temperature is 30oC
· Electro-catalytic O2 removal
– Removes O2 through the electrode reaction of a fuel cell
– Continuous O2 removal (if feasible due to the depleted amount of O2 in the catholic
feed)
· Electrolytic O2 removal
– Removes O2 through the electrode reaction of a metal/air cell
– Works until the metal electrode is used up
– Continuous removal of O2 for as long as the electrode material lasts
– Easy to renew/replace the electrode
– A depleted amount of O2 in the feed gas may not be sufficient to drive the electrode
reaction or to sufficiently deplete the amount of O2 per pass due to mass transfer
restrains.
· Chemisorption
– Limited capacity; initially will require more often changes of media
– Would require a bigger column to satisfy the requirements
– Has to be properly sealed to prevent any leakage of atmospheric air/O2 that could
come in contact with the media.
Further evaluation of electro-catalytic, electrolytic and chemisorption O2 dissipation methods is

under way.
7-14
8
PROTOTYPE DESIGN
Design Objectives
The desirable design objectives for the full-scale on-line continuous oil conditioning system
prototype were:
· To be capable of continuously purifying relatively clean transformer oil and maintaining its
characteristics at near new conditions: More specifically,
– To remove dissolved moisture from the oil in order to achieve less than 2ppm H2O
– To maintain the Neutralization Number at less than 0.01 mgKOH/g oil
– To improve the oil IFT number to a value of 35 dynes/cm or higher
– To minimize or eliminate dissolved metals in the oil (especially Cu)
– To maintain PF at less than 0.2% (measured @ 100oC)
– To improve and maintain the oil breakdown voltage at 50KV or higher
– To reduce the amount of relevant polar oil and paper by-products that are responsible
for negatively affecting the PF and IFT number
– To reduce or eliminate the paper degradation products from the treated transformer
oil
· To operate in a fail safe mode
· To fit in a NEMA 4 box approximately 3’x3’x1’
· To have capabilities for oil degassing and oxygen scavenging
· To operate on an in-service transformer in multiple modes (adsorption, degassing and
dehydrating)
· To be reliable and relatively easy to maintain
Features and Approaches

The laboratory tests conducted on more than 25 adsorbents clearly suggested a need for a multi-
adsorbent approach. A combination of five different adsorbents was found to be the most
efficient in improving and maintaining the oil quality at near new conditions. They were
contained in three different adsorbent beds connected in series. The important part of the system
is the membrane hollow fiber module, which precedes the adsorbent columns. It was designed to
operate in three possible modes:
8-1
Prototype Design
1. Vacuum mode - oil degassing mode

2. Pressure-vacuum mode in conjunction with a chiller – oil partial dehydration mode
3. Pressure-vacuum mode in conjunction with a chiller and O2 scavenging system – O2
scavenging and partial dehydration mode
Figure 8-1 depicts the schematics of the on-line continuous oil conditioning system prototype.
In addition to the above mentioned features, the prototype system was equipped with two
particulate filters, one at the inlet and the other at the system’s outlet, a fixed flow oil pump,
a vacuum-pressure pump, a chiller powered by a compressor, oil collecting vessels with a level
switch which triggers the small oil re-circulating pump which then returns the collected oil
(that may have seeped through the hollow fiber module) into the feed stream.
The system was instrumented with pressure and temperature gauges, thermocouples,
temperature and pressure switches and plumbed with bypass and diverting valves to allow the
system to operate in the degassing/adsorption or only in the adsorption mode. Also the system
was designed and equipped with fail-safe features and sample ports to allow periodic sampling
from various locations.
Figure 8-1
Schematics of the On-Line Continuous Oil Conditioning System
8-2
Prototype Design
Process
From Figure 8-1 it can be seen that the incoming transformer oil enters the system through a
solenoid valve, SV, and after that goes through the oil pump which transports it further through
a 2µ particle filter, F1. Afterwards, depending on the desired mode, by opening or closing the
appropriate valves, the oil can go through the hollow fiber module or through a bypass valve.
If the oil goes through the hollow fiber module, depending on how the vacuum-pressure pump
and the chillers are engaged, three modes (mentioned in Section 8.2) of extracting dissolved
gases and moisture from the oil are possible.
After passing through the hollow fiber membrane or the bypass loop, the oil enters three columns
filled with five adsorbents where it is stripped of all dissolved water, organic acids, and oil and
paper degradation products.
Before leaving the system, the oil passes through a second particle filter, F2, and returns to the
transformer.
Pump 2, a vacuum/pressure pump, may act as a vacuum pump or as vacuum/pressure

re-circulating pump. It acts as a vacuum pump when it maintains a vacuum in the HFM housing
while it effectively purges it and basically maintains the oil degassing capabilities of the HFM.
In this case, the pump outlet is open to the atmosphere, while the lower HFM housing port has
to be closed.
As shown in Figure 8-1, pump 2 acts as a re-circulating vacuum/pressure pump which takes
gasses from the HFM housing and directs them through the de-oiling vessels where the oil that
leaked through the hollow fibers (due to its imperfections) is separated from the gas stream.
The oil free gas stream then enters the chiller where the moisture, which was extracted from
the oil through the hollow fiber membrane, is condensed. The dried gas stream goes back to
the HFM housing through its lower port. Due to the H2O partial pressure difference in the oil
and the dry gas stream, when the dry gas passes around the hollow fibers it will become enriched
with moisture. The moisture will then be condensed in the chiller in the next cycle, as already
described.
When the collected oil level in the oil collecting vessels reaches a certain value, the level switch,
LS, will trigger small oil pump 3, which returns the oil to the oil feed stream.
In the third mode (see Section 8.2) after the chiller, the re-circulating gas stream would go
through an O2 scavenging device, where O2 would be removed. The O2 depleted gas stream will
then enter the HFM housing where it will pick up an additional amount of O2 from the oil, due to
the O2 partial pressure difference in the oil and the O2 depleted gas stream. After that, the cycle
will repeat itself.
As mentioned earlier, the system is equipped with self-regulating fail-safe features. Mainly it
consists of two pressure switches (PS) and one thermal switch (TS) as well as suitable electrical
relays and connections.
8-3
Prototype Design
The low-pressure switch shuts off the main oil pump and the solenoid valve (SV) at the inlet
when the system pressure drops below the preset value (~7 psig). It is anticipated that system
pressure can go below this value only if there is an oil leak somewhere in the system.
The high-pressure switch also shuts off the main oil pump and the inlet solenoid valve when
the system pressure exceeds 30 psig, since the present HFM cannot tolerate a higher pressure.
The high temperature switch shuts off the main oil pump and the solenoid valve when the
incoming oil temperature reaches 60oC to protect some of the adsorbents and minimize oil
seepage.
Shut off caused by any of these three switches isolates the prototype system from the
transformer, so that it cannot in any way interfere with the transformer operation.
System Commissioning and Beta Testing
After assembling the on-line continuous oil conditioning system prototype as shown in
Figure 8-2, functionality tests on all the components as well as on the system as a whole
were performed.
After all performed tests are successfully passed, the beta-test, with new transformer oil, was
conducted in order to prove that the system does not negatively influence the new transformer
oil’s characteristics in any way. As can be seen from Table 8-1, the on-line continuous oil
conditioning system prototype actually slightly improved all the relevant transformer oil
properties.
Table 8-1
Characteristics of the New Voltesso 35 Oil Before and After Passing Through the On-Line
Continuous Oil Conditioning System Prototype
H2O IFT NN PF KV Col DBPC

ppm dyn/cm mg/kg % KV %
At inlet 23 42.6 - 0.288 36.1 - -
Outlet <1 45.2 - 0.03 65 - -
8-4
Prototype Design
Figure 8-2
On-Line Continuous Oil Conditioning System Prototype
8-5
9
FIELD TRIALS
The field trial is anticipated as an evaluation of the continuous oil conditioning system prototype,
which is put in line on a power transformer. The prototype was installed in line on a 500 KV
power transformer in our High Voltage Lab. At first the test was performed on the non-energized
transformer, and later on the energized transformer.
The unit of the on-line continuous oil conditioning system prototype was connected at the bottom
of the transformer. The incoming oil was preheated to 50-60oC. Samples of oil were taken from
the inlet and outlet of the unit and analyzed for property changes.
The on line continuous oil conditioning system prototype connected in line on the energized
transformer is shown in Figures 9-1 and 9-2.
The field trial results show that the on-line continuous oil conditioning system prototype is
very efficient in purifying the transformer oil, regardless of whether the transformer is energized
or not. Its operation does not in any way interfere with the transformer operation, except it
conditions the transformer oil to specifications equal to or better than those for new oil. The
properties of the oil at the outlet of the conditioning unit, as a function of treated oil volume,
are shown in Table 9-1.
Table 9-1
Test Results of the On-Lline Continuous Oil Conditioning System Prototype Installed in
Line on the 500 KV Transformer
Volume treated H 2O IFT NN PF Breakdown Col DBPC Cu T in

o
L ppm dyn/cm mg/kg % KV % ppm C
Incoming oil 3 36.8 0.014 0.935 32 1 0.22 0.07 51.9
110.7 <1 43.2 <.01 0.042 57 1 0.23 0.001 51.9
575 <1 41.5 <.01 0.079 62 1 0.23 0.010 41.5
799 <1 42.1 <.01 0.051 60.9 1 - 0.009 55.5
1018 <1 41.6 - 0.06 - 1 - - 47.2
In addition, the HFM was tested in the degassing mode by simple valve switching, without
stopping or disturbing the system’s continuous operation. In this mode, the HFM basically
extracts all dissolved gasses from the oil to a certain extent, and releases them to the atmosp
here. To determine the efficacy of the HFM, the amount of gasses in the oil was measured before
and after it was passed through the HFM. The test results of the HFM’s efficacy are shown in
Table 9-2.
9-1
Field Trials
Table 9-2
HFM Efficiency When Employed in the Degassing Mode
Oil System
Membrane Flow rate Temp. Vacuum Pressure % Removed per pass
o
Type (L/min) C (inHg) (psig) H2 O2 N2 CO2 CO CH4
CMC 0.450 57 -23.5 20.7 26.3 24.1 28.1 11 28 28.6
Evaluation of the HFM in the dehydration mode was not possible since the moisture level of
the transformer oil after it was being treated through the system prototype for a certain period of
time had dropped from 3ppm to ~ 2, which was too close to the detection limit of the Karl Fisher
instrument. However, the operational functionality of the system prototype in the dehydration
mode, which involves the chiller and a vacuum/pressure pump connected as depicted in
Figures 9-1 and 9-2, was successfully tested and it appears to be working according to the
design requirements. The quantifiable test will be performed on the field transformer with
higher moisture content in the oil.
Figure 9-1
Close-up of the On-Line Continuous Oil Conditioning System Connected to the 500KV
Power Transformer
9-2
Field Trials
Figure 9-2
On-Line Continuous Oil Conditioning System Prototype Connected in Line to the 500KV
Power Transformer
9-3
10
CONCLUSIONS AND RECOMMENDATIONS
The on-line continuous oil conditioning system prototype was tested in line on a 500 kV
power transformer. Despite the short testing time, it met all the designed parameters, and in
some instances exceeded them. This limited test indicates that it is capable of restoring and
maintaining the transformer oil characteristics of an in service transformer at near new
conditions at all times. In particular, it dries the transformer oil to less than 1 ppm of H2O per
pass, regardless of the concentration of dissolved moisture in the incoming oil. At the same time,
it removes most of the oil and paper degradation products from the oil. This creates and
maintains conditions that should significantly prolong the life of the solid insulation and
consequently the transformer life. The capacity and long-term performance on in service
transformers has not yet been determined.
In order to fully establish the on line continuous oil conditioning system prototype’s
performance, as well as its reliability and economics, a prolonged test on in service power
and/or distribution transformers is recommended.
10-1
A
APPENDIX A
Figures A-1 and A-2 show an example of the amounts of polar compounds in the oil after it has
been treated with adsorbent 19. Due to the high concentration of acids and other oil and paper
degradation products in the treated sample, as well as the nature of this particular adsorbent, a
relatively fast saturation of the adsorbent can be observed.
Figure A-1
HPLC Chromatograph of Polar Compounds in Oil after it was Treated with Adsorbent
19 (after ~ 6 Volumes of Aged Oil were Passed)
Figure A-2
HPLC Chromatograph of Polar Compounds in Oil after it was Treated with Adsorbent
19 (after ~ 60 Volumes of Aged Oil were Passed)
A-1
B
APPENDIX B
The adsorption of selected paper degradation products from the aged oil on different adsorbents
is shown in Figures B-1 and B-2.
Figure B-1
Adsorption of 5-Hydrohyl -Methyl-Furfuralf on Different Adsorbents
B-1
Target: About EPRI
Substation Operation and Maintenance EPRI creates science and technology solutions for
the global energy and energy services industry. U.S.
electric utilities established the Electric Power
Research Institute in 1973 as a nonprofit research
consortium for the benefit of utility members, their
customers, and society. Now known simply as EPRI,
the company provides a wide range of innovative
products and services to more than 1000 energy-
related organizations in 40 countries. EPRI’s
multidisciplinary team of scientists and engineers
draws on a worldwide network of technical and
business expertise to help solve today’s toughest
energy and environmental problems.
EPRI. Electrify the World
© 2001 Electric Power Research Institute (EPRI), Inc. All rights

reserved. Electric Power Research Institute and EPRI are registered
service marks of the Electric Power Research Institute, Inc.
EPRI. ELECTRIFY THE WORLD is a service mark of the Electric
Power Research Institute, Inc.
Printed on recycled paper in the United States of America
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EPRI • 3412 Hillview Avenue, Palo Alto, California 94304 • PO Box 10412, Palo Alto, California 94303 • USA
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Appendix B
Figure B-2
Adsorption of Phenol on Different Adsorbents
B-2

Transformer Life Extension by On-Line Continuous Oil Treatment and Monitoring

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Transformer Life Extension by On-line

Continuous Oil Treatment and Monitoring

Field Test Report

Final Report, December 2001

EPRI Project Manager

(A) MAKES ANY WARRANTY OR REPRESENTATION WHATSOEVER, EXPRESS OR IMPLIED, (I)

(B) ASSUMES RESPONSIBILITY FOR ANY DAMAGES OR OTHER LIABILITY WHATSOEVER

ORGANIZATION(S) THAT PREPARED THIS DOCUMENT

Powertech Labs Inc.

This report was prepared by

Powertech Labs Inc.

This report describes research sponsored by EPRI.

1 INTRODUCTION ................................................................................................................. 1-1

3 METHODOLOGY AND APPROACH................................................................................... 3-1

4 OBJECTIVES AND SCOPE ................................................................................................ 4-1

5 EXISTING TECHNOLOGIES............................................................................................... 5-1

6 PRELIMINARY LABORATORY WORK .............................................................................. 6-1

7 DETAILED LABORATORY WORK..................................................................................... 7-1

9 FIELD TRIALS..................................................................................................................... 9-1

10 CONCLUSIONS AND RECOMMENDATIONS .................................................................10-1

A APPENDIX A ...................................................................................................................... A-1

B APPENDIX B ...................................................................................................................... B-1

Figure 6-1 Bench-Scale Setup for Evaluation of Adsorbents ................................................... 6-2

Table 5-1 The Oil Conditioning Methods ................................................................................. 5-1

Results of our research have led us to conclude the following:

The specific objectives of the project were:

2. Develop new technologies for on-line insulation conditioning; specifically to remove

Currently there are no commercially available technologies to selectively remove dissolved

Process Contaminant Removed

Mechanical Filters Particulates

Adsorbent Filter Dissolved Water

Adsorption Media Acids, Oil & Paper Oxidation Products

Ion Exchange Media Ionic Species, Dissolved Metals

Scavenging Media Oxygen, Peroxides, Free Radicals

Membrane, Vacuum systems Oxygen, Gases, Moisture

The preliminary laboratory work consisted of the following tasks:

Bench-scale experiments to evaluate several selected adsorbents consisted of a transparent

Adsorbent Mesh Amount Ave. Flow Oil Volume* (ml)

Adsorbent IFT Neut. No PowerFactor 2-furald. Copper Iron

*Properties of oil after 500 ml – single pass through adsorbent

Nature of Adsorbed Materials

Oxygen Removal Methods

Several oxygen removal techniques were considered, including:

Hollow Fiber Extractor Unit

Laboratory Scale Prototype

The additional laboratory work consisted of the following tasks:

Identification and Evaluation of New Adsorbents

Bench-scale experiments conducted to evaluate all selected adsorbents consisted of transparent

Removal of Acids, Polar Compounds and Metals

Polar Compound (ppm) (ppm)

Metals (ppm) (ppm)

In order to be able to appropriately compare the adsorbents’ capacities, the experimental

Unsurpassed organic acid adsorption capacities of adsorbent 15 maintained the neutralization

Further Evaluation of Hollow Fiber Membrane

Membrane Flow rate Oil Temp. P. drop % Removed per pass

C-1 0.036 45.8 2.5 33.3 52.5 45.8 39

Identification of Oxygen Scavenging Methods

· Catalytic O2 dissipation (has been tested)

Further evaluation of electro-catalytic, electrolytic and chemisorption O2 dissipation methods is

Features and Approaches

1. Vacuum mode - oil degassing mode

Pump 2, a vacuum/pressure pump, may act as a vacuum pump or as vacuum/pressure

System Commissioning and Beta Testing