1/12/2021 Elemental Analysis Explained and Illustrated

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Elemental Analysis Explained and

Illustrated
Noria Corporation

For those just getting started in the oil analysis game, the learning curve can initially seem steep and
daunting. Technical jargon such as elemental analysis, Fourier Transform Infrared Spectroscopy
(FTIR), absolute and kinematic viscosity, ISO particle count, wear debris analysis and Karl Fischer
moisture can easily intimidate those who haven’t taken a chemistry class in many years.

So, for our oil analysis freshmen, POA will be running a series of articles throughout 2002 on all of
these fundamental oil analysis tools to explain how they work, what they are designed to tell you and
what all those numbers that come back from the lab actually mean. The rst article in the Oil Analysis
101 seriesWewill focus on Elemental
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Elemental analysis is probably the most fundamental test in the oil analysis toolbox. Its history goes
back to the 1940s and 1950s when it was used in the railroad industry to determine the presence of
wear metals in diesel engine oils. However, elemental analysis, sometimes referred to as elemental
spectroscopy, atomic emission spectroscopy (AES) or simply wear metal analysis is about more than
just measuring the concentrations of wear metals such as iron, lead and copper.

In its present form, elemental analysis is used to determine the concentrations of 15 to 25 different
elements ranging from wear metals and contaminants to oil additives. Table 1 gives an overview of
some common elements that are measured and their usual source.

Elemental analysis works on the principle of atomic emission spectroscopy (AES). In AES, individual
atoms within the sample, for example iron atoms from wear debris, zinc atoms from a ZDDP additive
molecule, or silicon from silica (dirt) contamination, are excited using a high-energy source.

The atoms absorb energy from the excitation source and are transformed to a high-energy electronic
state. Due to the laws of quantum physics, atoms do not like being in these excited states and rapidly
lose the energy they have gained, mainly by emitting light energy.

The energy of light emitted, which is inversely proportional to the wavelength, is dependent on the
electronic structure of the atom, and is thus different for each type of atom. So, by measuring the
amount of light emitted at the characteristic emission wavelength for atoms such as iron, copper, zinc
and sodium, the concentration of each atom can be determined.

In uence of Particle Size

The major limitation with AES is that because the method requires excitation of individual atoms, the
sample must be fully vaporized to allow all atoms present to be measured. While this is not a problem
for small particles and dissolved metals, the probability that a particle can be vaporized and analyzed
using AES drops very rapidly above 5 microns. In fact an AES spectrometer is all but blind to particles
in excess of 10 microns.

Unfortunately, depending on the wear mechanism and the severity of the problem, active machine
wear may generate particles that are greater than 10 microns in size, and will thus be invisible to the
AES instrument. For this reason, it is important in any oil analysis program to not rely solely on AES
data to determine active wear, but to include tests such as particle counting, ferrous density analysis
and patch microscopy to measure larger particles.

Units of Measure
So, what exactly is a ppm? On an oil analysis report, the numbers typically seen, depending on
component type, oil type, application, etc., may range from a few parts per million (ppm) or several
hundred ppm for wear metals and contaminants, to several thousand ppm for certain additive
elements.

As the name implies, a ppm is simply the number of parts of the element in question, per million parts
of the sample. Put another way, a reading of 1 ppm of a particular element is equivalent to 1 µg of the
element per g of sample, which is the same as 1 mg per Kg, or approximately one ounce per 6500
gallons of oil!

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How does the lab go from measuring light intensity to reporting a concentration in ppm? I would use
the original form. To do this, each AES instrument is calibrated using standard calibration solutions.
These solutions contain known concentrations of certain elements of interest. Metal sulfonates are
commonly used for this purpose.

By analyzing the calibration standards, the amount of light at a speci c wavelength can be determined
for the elements in question, which can then be related to the known concentration in the standard
solution.

In this way, a calibration curve can be generated which allows the unknown concentration of the same
element in a test sample to be determined by measuring the amount of light emitted at a speci c
wavelength, and using the calibration curve to convert this light intensity into a concentration or ppm.

Trending the Data

When analyzing elemental analysis data, it is important to look not at the absolute value of each
element, but rather the trend line, that is, the change in elemental concentrations over consecutive
samples.

This is important because wear rates will be different for different machines, depending on
component types, manufacturer and model, oil type, age, usage, etc. This type of rate-of-change
analysis can be invaluable in nding early signs of wear and contamination related problems.1

In analyzing AES data, it is important to know both the machine metallurgy, and the chemical
composition of common contaminants that may be present so the data can be related back to active
wear of a speci c component, or to ingress of speci c contaminants.

It is also important to know the expected concentrations of the different metal-containing additives in
the oil. To do this, new oils should be baselined on an annual basis, or whenever a change in oil type or
formulation is suspected. By comparing the elemental ngerprint of the new oil baseline to the used
oil sample, problems such as additive depletion or the addition of wrong oil can be quickly and easily
diagnosed.

Care should be exercised however, when looking at elemental additive elements because additive
depletion does not necessarily cause a drop in additive element concentration, as measured by AES.2

Due to its ability to determine unusual wear, contaminants and additive elements, AES is an invaluable
tool in any oil analysis program. Used correctly, it can determine everything from corrosive wear, to a
coolant leak, to sea water ingression to additive stripping and should be considered the cornerstone of
a well-engineered oil analysis program.

Anatomy of an Atomic Emission Spectrometer

Nearly all oil analysis labs use one of two types of atomic emission spectrometer, either an inductively
coupled plasma (ICP) instrument, or a rotating disc electrode (RDE) instrument. The basic difference
between the two lies mainly in the way in which the sample is vaporized and the atoms excited by the
high-energy source.

In an ICP instrument, the oil is injected into a high-temperature argon plasma, where the atoms are
vaporized, excited and subsequently emit light. In an RDE spectrometer, also sometimes referred to as
We instrument,
an “Arc-Spark” encourage you
the oil to read and
is vaporized ourexcited
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The rest of the instrument, whether it be an ICP or RDE spectrometer, is basically the same. The light
emitted by the excited atoms is collected and focused onto the slits of the spectrometer. The
spectrometer contains a diffraction grating, which is similar to a prism in that it splits light of different
wavelength or colors into discrete wavelength, based on their angle of diffraction.

The light intensity at each angle, typically referred to as a channel, is measured using a light-sensitive
photodiode and the resultant voltage signal converted to a concentration in ppm based on a simple
calibration procedure.

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In practice, provided the two instruments are calibrated properly, there is very little difference between
the accuracy of data from both types of instrument. However, there is one very important difference
between ICP and RDE instruments. Both ICP and RDE instruments suffer from size limitation effects.

This effect limits the size of particle that can be measured using conventional AES. For ICP, only
particles smaller than approximately 3 microns can be measured. For RDE instruments, the limit is
slightly higher, around 8 to 10 microns. The implication is that if an oil sample is analyzed rst by ICP,
then by RDE, the concentrations of certain elements, particularly wear metals and contaminants,
which may be present as 3- to 10-micron particles will potentially be different.

While this is of little concern when trending data from different samples analyzed by the same
instruments, data from samples analyzed by RDE and ICP instruments typically will not correlate.

References
1. Sowers, J. (2001). “Use Statistical Analysis to Create Wear Debris Alarm Limits.” Practicing Oil
Analysis. November-December, p. 38-41.

2. Gustavsen, A.J. (2001). “Assessing Additive Health Using Elemental

Spectroscopy and the Stoke’s Procedure.” Practicing Oil Analysis. May-June, p. 14-16.

Further Reading
1. “Source Book For Used Oil Elements,” by James C. Fitch (available in the Bookstore at
www.practicingoilanalysis.com).

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Practicing Oil Analysis (1/2002)

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