Chemists Perspective

Metals Analysis in Transformers,

Load Tap-Changers
and Oil Circuit Breakers

by Lance Lewand
Doble Engineering Company

Introduction the absolute quantity in identifying

the location of an incipient fault.
Laboratory testing is of increasing importance today as new and better tests be- Usually, these tests are better suited
come available on a routine basis. This is especially true in an environment where as investigative analyses to help aid
in determining the cause of certain
testing of out of service apparatus is not possible under some conditions and often incipient-fault conditions such as
performed less frequently. The testing, primarily performed on easily-sampled high temperature overheating of
electrical insulating liquids, can help to assess the condition of the insulating the oil.
materials and more importantly serve as diagnostic procedures to detect and
Dissolved Metals-In-Oil
identify incipient faults in apparatus. In addition, some of these same tests can This analysis is performed
be used to verify that a failure has occurred and then to aid in the identification through the use of atomic emission
of the cause. Finally, some tests can be performed to help decide which remedial spectroscopy (AE) such as induc-
tively-coupled plasma (ICP). This
actions might be most effective. type of metals analysis is the test
Metals testing in oil is not a new test but one that is being used more frequently most frequently used for electrical
to diagnosis conditions in electrical apparatus. One thing that the user should be apparatus oil as it is a quick test
very aware of, however, is that there is not one test for metals in oil but actually a to perform, can analyze for a wide
variety of tests. The goal of this article is to define the different tests and provide variety of elements, and can deter-
information on where and when they should be used. The three tests that this mine the concentrations of these
article will focus on are: elements over a very large range.
There are two major drawbacks. The
Dissolved metals-in-oil first one is that the dissolved metals
Particulate metals-in-oil, and or free particles in the oil have to
SEM/EDX analysis be less than about 10-20 microns
in order to be detected (depending
Analysis for metals in oil is most appropriate as a diagnostic or investigative on the analytical equipment itself ).
tool when other symptoms indicate an incipient-fault condition. The analysis This is a function of the way the
can be performed to identify and quantify either dissolved or particulate met- sample is introduced into the ana-
als in the oil of which particulate metals are an order of magnitude less. When lytical equipment for detection. The
looking for bearing wear in pumps, a quantitative analysis for particulate copper, other drawback is that the lower
lead, zinc, and iron is performed [1]. Since new oil in transformers should not level of detection is about 0.5 to
have significant quantities of any dissolved or particulate metals, any appreciable 1.0 mg/kg (ppm) depending on the
increase in the oil could be an indicator that a problem may exist. A baseline test element and using older instrumen-
for dissolved metals in oil is important as the trend can be more important than tation. Newer instrumentation may

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have detection limits as low as 0.01-0.10 ppm. This type of
analysis is satisfactory for certain incipient-fault conditions
where the metal is sublimed (change of a solid material into
vapor through heat) into the oil to form an organo-metallic
complex or where the particles are smaller than 10 microns.
This method, ASTM D 7151, is most commonly used to
determine if heating within the transformer has caused
metals to sublime and become entrained in or to the oil
molecules. It is also used in the analysis of LTC and OCB
oils where there is usually an overabundance of metals and
the idea is to find a quick and inexpensive way to determine
concentration of a wide variety of metals.
Follow-up testing for dissolved metals in oil is not usu-
ally necessary unless dissolved gas-in-oil tests indicate an
incipient-fault condition. The most common metals dis-
solved in the oil would be iron and copper or aluminum,
depending on coil construction. Lead is usually indicative of
brazes, solders, and paints, and zinc is indicative of brazes,
solders, and plated parts. Unusual metals such as titanium
in high concentrations could come from the degradation
of titanium based paints used by some manufacturers on
the interior walls of the transformer. Silicon contamina-
tion usually indicates either outside contamination (i.e.,
silicone fluids, caulks, or greases) or overheating of the iron
components such as the core metal or degradation of certain
components such as gaskets. Contamination with silicone
fluids can present a serious impediment during vacuum
processing because it can result in uncontrollable foaming
[2] of the insulating oil.
Particulate Metals-In-Oil (Bearing Wear)
For transformers cooled by pumps, the test for bearing
wear metals should be performed every few years. The most
common metals tested for are copper, lead, iron, zinc, alumi-
num, and silver. Some of these metals are produced in the
particulate state when the bearings of the transformer pump,
the pump shaft, and/or the impeller start to degrade in some
manner. The small pieces of metals are jettisoned into the
oil where, if small enough, they can remain suspended and
thus be sampled and analyzed. This type of analysis incor-
porates the use of a graphite furnace coupled with an atomic
absorption spectrometer. In addition, metal particulates are
concentrated by passing a certain volume of oil through a
0.45 micron filter to capture them. The filter is then treated
in a manner to leave only the metals in a solution of acid
and water. The analysis has the ability to detect elements at
extremely low levels, <1 g/kg (ppb), which is necessary as
problems with pumps are usually detected where the con-
centrations of certain metals are around 20 ppb. Although
not an ASTM test method, Doble performs this analysis
on a very routine basis, and it has the capability of being
expanded to perform metals analysis on solid materials such
as paper, pressboard, and other materials.
Like ICP and AE, there are advantages and disadvan-
tages. For one, it uses a much larger volume of oil for analysis,
500 mL (0.5 quarts) whereas the ICP only requires 2-10
mL. There is also a significant amount of sample prepara-
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tion involved, and the analysis time is lengthy. However,
there is really no limit on the metal particle size that can
be analyzed.
Sampling
The analysis of dissolved or particulate metals is very sen-
sitive to sampling methodology. The sample valve has to be
prepared in such a manner as to not introduce contaminant
metals or elements from that area into the sample. Depend-
ing on the type of valve, contamination from copper, tin,
and zinc (brass, bronze) as well as iron is not uncommon.
Zinc from such items as galvanized pipe nipples and drain
plugs is also a very common contaminant. In addition, copi-
ous amounts of oil should be flushed through the valve to
not only clean out the valve but to clean the area near the
valve inside the transformer. For transformers with pumps,
it is preferable that at least one bank of pumps be operat-
ing at the time of sampling so that the particulates are in
a homogenous solution inside the unit. The table below
illustrates the effect of cleaning and flushing..
Metal Results before and after Cleaning the Drain Valve
Metal 1st Sample 2nd Sample, after cleaning and flushing
Copper 63 ppb 6 ppb
Lead 10 ppb 1 ppb
Iron 33 ppb 4 ppb
Zinc 6 ppb 14 ppb
As shown in the table, there is a significant decrease in
the concentration of most metals once the cleaning and
flushing were performed. The importance of the sampling
efforts cannot be overemphasized, as incorrect results can
lead to the wrong conclusion.
SEM/EDX Analysis
Scanning electron microscopy (SEM) and energy disper-
sive X-ray (EDX) analysis are two separate tests conducted
at the same time. SEM is an analysis in which a beam of
electrons, a few hundred angstroms in diameter, systemati-
cally sweeps over the specimen in an evacuated chamber.
The intensity of secondary electrons generated at the point
of impact on the specimen surface is measured, and the
resulting signal fed into a cathode-ray tube display which is
scanned in synchronism with the scanning of the specimen
to produce a picture. All prepared samples stubs are coated
with evaporated graphite before analysis which improves
imaging resolution and stability.
EDX is when an electron beam of the scanning electron
microscope enters the bulk of a sample producing an x-ray
emittance. The x-ray peak positions along the energy scale
identify the elements present in the sample and can provide
the percentage concentrations of each of these elements
thus providing an elemental breakdown of the material or
particles.
 Obviously, this is no ordinary test. This powerful tool
can be used in investigative type analysis such as corro-
sive sulfur issues on paper or copper samples and other
contaminants from a transformer, LTC, OCB, bushing,
etc. This type of analysis is not performed on the oil itself
but on filtered materials from the oil or from components
or contamination inside the transformer that needs to be
identified. Although this analysis tool has many advantages,
like most analytical techniques there are disadvantages as
well. The foremost is cost of the instrumentation itself and
the significant operating expenses associated with it. Other
drawbacks include the amount of time necessary to prepare
the sample for analysis, the length of time for analysis and
the very high level of detection (0.5%, 5000 ppm) when
compared to other analysis techniques.
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Conclusion
The three main types of metals analysis that can be
performed are dissolved metals-in-oil, particulate metals-
in-oil, and SEM/EDX analysis. The goal of the article is to
explain the differences between each test and to list certain
advantages and disadvantages to help the user in determin-
ing which test to request.
References:
1. Oommen, T.V. and Petrie, E.M. Particle Contamination
Levels in Oil-Filled Large Power Transformers, IEEE
Transactions on Power Apparatus and Systems, May 1983,
Vol. PAS-102, No. 5, pp. 1459-1465.
2. Griffin, P.J. A Cup Full Of Trouble, Report on the
Minutes of the Doble Oil Committee Meeting, April
1989, pp. 8-14.
Lance Lewand received his Bachelor of Science degree from St.
Marys College of Maryland in 1980. He has been employed by the
Doble Engineering Company since 1992 and is currently the Laboratory
Manager for the Doble Materials Laboratory and Product Manager for
the DOMINO product line. Prior to his present position at Doble, he
was Manager of the Transformer Fluid Test Laboratory and PCB and
Oil Services at MET Electrical Testing in Baltimore, MD. Mr. Lewand
is a member of ASTM Committee D 27.