COE-110.10, Methodology of Laboratory Failure Analysis

Engineering Encyclopedia
Saudi Aramco DeskTop Standards
METHODOLOGY OF
LABORATORY FAILURE ANALYSIS
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Engineering Development Program (PEDP) of Engineering Services.
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of the Vice President, Engineering Services, Saudi Aramco.
Chapter : Corrosion For additional information on this subject, contact

File Reference: COE-110.10 PEDD Coordinator on 874-6556
Engineering Encyclopedia Materials Selection and Failure Analysis
Methodology of
Laboratory Failure Analysis
Content Page
INTRODUCTION............................................................................................................ 4
LABORATORY FAILURE ANALYSIS PROCEDURES USED

IN SAUDI ARAMCO CONSULTING SERVICES LABORATORY .................................. 5
Preliminary Examination/Measurements ............................................................. 6
Dimensional Measurements ..................................................................... 7
Preliminary Alloy Identification Tests ........................................................ 7
Specimen Selection and Preparation .................................................................. 9
Failure Location ........................................................................................ 9
Sample Cutting ....................................................................................... 11
Metallographic Specimens...................................................................... 13
Mechanical Test Specimens ................................................................... 18
Analytical Test Specimens...................................................................... 20
Specimen and Archive Material Preservation ......................................... 20
Optical Metallography and SEM Analysis .......................................................... 20
Optical Metallography ............................................................................. 20
Scanning Electron Microscopy Analysis ................................................. 25
Fractography........................................................................................... 29
Material Characterization................................................................................... 33
Mechanical Testing ................................................................................. 33
Chemical Analysis................................................................................... 40
Corrosion Tests ...................................................................................... 41
VALUE OF LABORATORY SIMULATION

FOR CONFIRMATION OF FAILURE MODE ............................................................... 42
THE STEPS BY WHICH LABORATORY INFORMATION IS OBTAINED ................... 44
SUMMARY................................................................................................................... 47
Saudi Aramco DeskTop Standards i

Methodology of
GLOSSARY ................................................................................................................. 48
REFERENCES............................................................................................................. 50
FORM A ....................................................................................................................... 51
FORM B ....................................................................................................................... 52
FORM C ....................................................................................................................... 53
FORM D ....................................................................................................................... 54
FORM E ....................................................................................................................... 55
FORM F ....................................................................................................................... 56
List of Figures
Figure 1. Procedure Outline for a Laboratory Analysis.................................................. 5
Figure 2. The Origins of Characteristic X-Rays Used in EDS Analysis ......................... 8
Figure 3. Relation Between Atomic Number and Characteristic X-Ray Lines ............... 9
Figure 4. Important Metallurgical Directions in an As-Rolled Plate.............................. 12
Figure 5. Flow Chart for the Preparation of Metallographic Samples (Reference 4) ... 14
Figure 6. Mounted Metallographic Sample.................................................................. 15
Figure 7. The Effect of Eching on a Polished Metal Surface ....................................... 16
Figure 8. Standard Round Tensile Test Specimen...................................................... 18
Figure 9. Standard Flat Tensile Test Specimen for a Transverse Weld ...................... 19
Figure 10. ASTM Requirements for Charpy V Notch Sample ..................................... 19
Figure 11. Principles of the Optical Metallograph ........................................................ 21
Figure 12. Lightly Sensitized Stainless Sample........................................................... 22
Figure 13. Sensitized Stainless Steel Sample (Photo) ................................................ 23
Saudi Aramco DeskTop Standards ii

Methodology of
Figure 14. Grain Size Measurement............................................................................ 24
Figure 15. Operational Characteristics of Light and Electron Microscopes ................. 26
Figure 16. Comparison of Optical and Electron Microscopes...................................... 27
Figure 17. Methods of Cleaning Fracture Surfaces ..................................................... 30
Figure 18. Typical Charpy Testing Machine ................................................................ 34
Figure 19. Shift in Transition Curve Caused By Temper Embrittlement ...................... 36
Figure 20. Fractured Charpy V-Notch Specimens

With Varying Amounts of Shear Deformation ............................................. 37
Figure 21. Basic Parameters in Brinell Hardness Test ................................................ 38
Figure 22. (a) Sigma Phase Appearance Before Annealing,

(b) After Annealing, and (c) After Simulated Heat Treatment...................... 43
Figure 23. Laboratory Failure Analysis Flow Chart...................................................... 45
Figure 24. Failure Analysis Work Flow ........................................................................ 46
Saudi Aramco DeskTop Standards iii

Methodology of
INTRODUCTION
Proper diagnosis of equipment failure often results in a wealth of

information about the factors that contribute to the failure. This
knowledge assists in eliminating the causes of possible future
failures. In order to effectively carry out all stages of a failure
analysis, it is necessary to have a good understanding of the
various procedures that are used during a metallurgical
laboratory examination.
Saudi Aramco DeskTop Standards 4

Methodology of
LABORATORY FAILURE ANALYSIS PROCEDURES USED IN SAUDI ARAMCO

CONSULTING SERVICES LABORATORY
Failure analysts usually follow a prescribed procedure during an

investigation. An example of this type of procedure is outlined
in Figure 1.
1. Preliminary Examination/Measurements
- visual (macroscopic)
- photographic record
- dimensional
2. Preliminary Alloy Tests

- pH, magnetic, chemical spot, EDS
3. Nondestructive Testing
- liquid penetrant, radiography
4. Selection, Identification, Preservation,

and Cleaning of Surfaces
5. Microscopic Examination
- metallography
- SEM fracture surface
- SEM /EDS
6. Quantitative Chemical Analysis
7. Mechanical Testing
- hardness, tensile, impact
8. Simulated Service Testing
Figure 1. Procedure Outline for a Laboratory Analysis

Methodology of
Preliminary Examination/Measurements
The laboratory failure analysis begins with several of the

techniques used in the field failure analysis. Preliminary
observations include thorough visual examination supplemented
by sketches and photography. In addition to general
photographs of the failed part, macrophotographs are obtained
using a macrocamera. A low-power binocular microscope or
“stereomicroscope” can be used for closer examination of
surface cracks, corrosion, or defects. Macrophotographs should
include a ruler or other maker to indicate relative size.
In the majority of cases, the steps in Figure 1 are followed until

the problem is solved; however, in many cases, the sequence of
steps is altered in order to suit the particular situation. Visual
examination sometimes leads directly to an important next step;
for example, chemical analysis may be suggested when a
particular type of corrosion is observed or suspected. Three
examples where visual examination led directly to key laboratory
tests are cited below:
• A failed boiler tube was cut open and thick deposits were
found. In order to determine if improper water treatment
was the cause of failure, a sample of the deposits was
chemically analyzed by x-ray diffraction. (This method of
analysis will be described later in this module.)
• A cast heater tube with radial cracks was submitted for a

failure analysis. In this instance, visual examination led to
microscopic examination in order to determine the
operating temperatures and condition of the microstructure.
• A fatigue failure from a compressor disk was submitted for

examination. Visual examination indicated beach marks
that emanated from a weld region and propagated along
planes of high stress. The sample was then submitted for
subsequent laboratory examination, which included
metallography and both scanning and transmission
electron microscopy. Subsequent fracture surface
examination with the electron microscope determined that
surge loading had caused the failure, and it provided
information on the remaining life of the component.

Methodology of
Dimensional Measurements
It is important to mechanically measure dimensions of the failed

part in many failures. For example, diametrial measurements of
bulged tubes, as well as thickness measurements of deformed
or corroded parts may be required to confirm the root cause of
failure. Measuring tools include rulers, tape measures, calipers,
and micrometers. Such measurements must be performed
before cutting.
Preliminary Alloy Identification Tests
Just as in the field failure analysis, a very important starting

point in the laboratory examination of failures is preliminary
identification of sample composition, both base metal and
deposits/scale/corrosion products.
Chemical Spot Testing - Chemical spot testing is one method

for determining material composition. A wider variety of spot
tests can be performed more conveniently in the laboratory than
in the field. A good discussion on chemical spot testing is given
in Reference 2.
Energy Dispersive Chemical Analysis (Texas Nuclear) -

Chemical spot tests tend to be time consuming, and the
required techniques can take considerable time if several spot
tests need to be performed. An alternative method of analysis
utilizes the portable nuclear analyzer. Today this method is one
of the most frequently used methods for conducting in-situ alloy
identification or chemical analysis of a material. Portable
nuclear analyzers, such as the Texas Nuclear Alloy Analyzer,
have been utilized since the late 1970s.
A quantitative analysis can be performed by evaluating the

amount of x-rays that are emitted at each characteristic energy
level. This device utilizes energy dispersive analysis to
determine the elemental composition of a sample. It uses a
radioactive isotope, such as Fe-55, as its primary energy
source.

Methodology of
N
M
L
K Kα
Nucleus
Kβ
Lα
Mα
Figure 2. The Origins of Characteristic X-Rays Used in EDS Analysis
The basic principle of energy dispersive x-ray spectroscopy

(EDS) can be illustrated using Figure 2. Electrons that are
scattered within the volume of a specimen deposit energy into
atoms of the specimen. In order to return to the ground state,
the atom releases a distinct quantum of energy. If the excited
atom ejects an inner shell electron, the outer shell electron fills
that vacancy and emits an x-ray that has an energy that is equal
to the difference between the two electron shells. This filing of
the inner shell with an outer shell electron is called a K
transition. Other transitions are also possible, as shown in
Figure 2. These transitions give rise to different emissions, and
an energy spectrum is developed that relates directly to a given
element. These energy values can then be related to a special
element as shown in Figure 3, which relates atomic number and
energy levels for various characteristic x-rays.

Methodology of
100 Lβ
Mα
Ly
90 Lα
80
70
Atomic Number
60
50
Kα Kβ
40
30
20
10
0 5.0 10.0 15.0 20.0 25.0 30.0
Energy, keV
Figure 3. Relation Between Atomic Number and Characteristic X-Ray Lines
Specimen Selection and Preparation
Failure Location
Careful visual examination is always required at the start of

every failure investigation. In some cases, further examination
is required to determine the failure location, and nondestructive
examination (NDE) methods are used. Several types of NDE
tests, including liquid penetrant (LP) testing and radiography
(RT), can be used. These methods have been described in
COE 106.06.

Methodology of
Example: How NDE plays a role in a laboratory examination
Leaks were experienced in a 2 inch - 600 lb gate valve almost

immediately following installation. The valve was in acid
service. Liquid penetrant (LP) examination revealed what
appeared to be external surface irregularities on the valve body
in the vicinity of the leakage. A radiograph was required to
demonstrate that internal casting defects were responsible for
this leakage. Although some of these defects were identified
directly through RT examination, a subsequent metallurgical
examination was required. In this case, it was learned that the
valve manufacturer was having difficulties with two supplier
foundries. Special steps were taken to identify all castings, that
were made by these foundries for future inspections. Many
other casting defects were found.
Prior to destructive sampling, the failure analyst should make a

photographic record of key observations. This photographic
record is referred to as macrophotography. Macrophotography
usually requires magnifications of 1 to about 50x. Most
metallurgical laboratories have the necessary equipment, which
includes cameras, proper light sources, and, in some cases,
stereomicroscopes with photographic attachments. The
photographic record should include major areas of damage. In
the case of a corrosion failure, the nature of a deposit should be
recorded. For fractures, the orientation of key features will be
important because subsequent higher magnification
examinations will take place.
At this stage of the examination, a plan of attack must be

developed to determine what laboratory tests will be required.
Some of the key steps in a laboratory investigation include:
metallographic examination, fractography, hardness, chemical,
and mechanical tests such as tensile and impact testing. Most
of these tests require destructive sampling.

Methodology of
Sample Cutting
In a large number of cases, failure samples that are received in

a metallographic laboratory for microscopic examination are too
big to handle conveniently; therefore, large samples require the
use of sectioning equipment. In many cases, samples of
associated deposits/scale/corrosion deposits should be
removed and preserved before sectioning.
Sectioning is the first step in the process of specimen

preparation, and it is one step that should be considered
carefully. A sketch that shows the orientation of the cut section
relative to the specimen should be prepared. The section is
then outlined with an appropriate marker. Too often, more
attention is paid to getting the sample cut instead of how it
should be sectioned. The result can be a severely damaged
specimen that can not be replaced.
In some cases, important metallurgical properties and

microstructural features are dependent on the orientation of the
sample; for example, it may be necessary to keep track of the
rolling direction of a plate for subsequent metallographic
examination. In an as-rolled plate, the grains will take on a
preferred orientation as shown in Figure 4. The other directions
in the plate are referred to as the long and short transverse
directions.

Methodology of
Long
Transverse Longitudinal
Direction
of Rolling
Short
Transverse
Figure 4. Important Metallurgical Directions in an As-Rolled Plate
Several methods are available to the metallographer for

reducing sample size. These methods include: fracturing,
sawing, or abrasive wheel cutting. The alternatives should be
considered carefully; for example, a piece may be simply
fractured to reduce it to a manageable size. In the case of
brittle metals and alloys, such as cast irons, the piece may be
fractured by hammer to obtain a fragment; however, this method
is not often recommended because of potential damage to the
sample. The preferred methods include sawing, abrasive wheel
cutting, and sometimes torch cutting. Each of these techniques
is described below.

Methodology of
Sawing - A commonly used method of sectioning in

metallographic laboratories. If the section that is to be cut is
relatively soft, it may be removed by either manual or power
hacksawing. Sawing is usually accomplished with a handheld
hacksaw or a band saw. Handheld hacksaws or band saws do
not generate enough frictional heat to alter the microstructure;
consequently, coolants are not usually required. Ideally, the
methods that produce surfaces that are suitable for immediate
fine grinding or polishing (as required for metallographic
examination) are preferred; however, this type of surface can
not always be achieved because saw-cut surfaces are rough.
Coarse grinding can be required to obtain a flat surface prior to
fine grinding.
Abrasive Wheel Sectioning - Specimens of hard materials that

cannot be easily sawed, such as fully hardened steel, must be
cut with an abrasive cut-off wheel. The cut-off wheel’s abrasive
material that does the cutting is usually either silicon carbide or
aluminum oxide, but diamond rimmed cut-off wheels are used in
special applications. Each abrasive particle that is contained in
an abrasive cut-off wheel acts as a miniature cutting tool that
removes a very definite chip of material.
Torch Cutting - Occasionally, the sample is too large to be

handled by saw cutting or other mechanical means. In these
cases, torch cutting will be required. Special care is necessary
to avoid overheating of the sample material and causing
metallurgical changes. For this reason, there must be enough
space between the cut region and the actual location that is to
be examined in the laboratory.
Metallographic Specimens
A key step in all examinations is the choice of a representative

sample for metallographic examination. The examination can
include inspection of the sample with the scanning electron
microscope as well as with the optical microscope. Specimens
that are selected should be characteristic of the material; for
example, if a sample has seen mechanical damage, a specimen
should be taken from a region where this damage has occurred.
A sample from an undamaged area is sometimes removed for
comparative purposes.

Methodology of
Metallographic Preparation - The outline in Figure 5 lists the

basic steps that are required in a metallographic examination.
These steps must be followed carefully to ensure that the
metallurgical nature of the sample is not altered prior to
examination. Incorrect preparation techniques could change the
metallurgical structure and lead to faulty conclusions as to the
cause of failure.
CUTTING
MOUNTING
Compression Molding
Cold Mounting
FINE GRINDING
Coarse (120 µm - - - Fine 600 µm)
grit silicon carbide grinding
ROUGH POLISHING
Diamond Abrasive (6µm)
CLEANING
Solvents
ETCHING (a) LIGHT MICROSCOPE (b)
LIGHT MICROSCOPE SEM/EDS
Figure 5. Flow Chart for the Preparation of Metallographic Samples

(Reference 4)

Methodology of
To a large extent, metallographic sample preparation is an art.

The procedures will vary somewhat from one laboratory to
another. Usually, the first step after cutting involves sample
mounting, which involves compression molding or cold molding,
as shown in Figure 6. Coarse and fine grinding are the initial
steps in producing a polished specimen for detailed examination
with the optical microscope (and in some cases with the
scanning electron microscope). Together with polishing,
grinding serves to smooth the surface and to reveal the true
structure of the material.

Metal Specimen

Plastic Disc
Figure 6. Mounted Metallographic Sample
Polishing - The purpose of polishing is to remove the grinding

scratches and the heavily deformed layer that is caused by
grinding. Polishing is the last step in the overall preparation of
metallographic specimens for microscopic examination.
Diamond abrasives are used for rough polishing, but final
polishing usually employs aluminum abrasives. The specimen
is ready after polishing for microscopic examination prior to
etching.

Methodology of
Etching - Preferential attack of a metal surface is called

etching. When a metallographic sample is etched for the first
time after polishing, the true structure may not be revealed
because of the presence of disturbed metal. Even when the
greatest care is taken in polishing and grinding, distortions will
occur. In order to reveal the true structure, the metallographer
must alternately polish and etch several times. Microscopic
examination is required to determine that the disturbed region
has been removed.
Prior to final etching, microscopic examination of an as-polished

specimen can reveal certain features of interest, such as
inclusions, oxidation layers, and cracking. These features can
be best observed in the as-polished condition. Although certain
information may be obtained from as-polished specimens, the
microstructure is usually only visible after etching. Features that
exhibit a significant difference in reflectivity are the only ones
that can be viewed without etching. Microstructural features
with heavy contrast or with large differences in surface relief will
exhibit a significant difference in reflectivity. The effect of
etching on the polished surface of a metal is illustrated in Figure
7.
Reflected
Incident
light
light

Microstructure
(a) (b)

(c)
Figure 7. The Effect of Eching on a Polished Metal Surface

Methodology of
As shown in Figure 7a, no microstructural features are present

in the as-polished condition. When chemically etched, the grain
boundaries appear (Figure 7b), and, when more heavily etched,
the internal structure is revealed (Figure 7c). Other etching
methods can also be used such as optical, electrochemical, and
physical etching.
Chemical etching is the most commonly used etching method.

It is achieved by the use of acidic or basic chemicals in an
aqueous or alcoholic solution. The metallographer must decide
which etchant is to be used for a particular alloy. A metal or
alloy that is to be satisfactorily etched requires the use of a
reagent that has been specifically formulated for the
composition of the specimen of interest; for example, an etchant
that is composed of ammonium hydroxide and hydrogen
peroxide is ideally suited for copper and brass. It is totally
unsuitable for iron and steel.
Carbon and alloy steels are most commonly prepared with an

etchant for steel called nital. Nital is a solution of methanol and
nitric acid (usually about 4 or 5 % nitric acid). Ferrite grain
boundaries can be etched by using nital in most carbon steels
because of their simple microstructure.
A wide range of constituents is encountered in carbon and low-

alloy steels such as ferrite, austenite, and cementite. Each of
these constituents has been described previously. A weld is
one of the more common examples where several of these
constituents can be observed near one another. Ferrite,
pearlite, and martensite can be seen in adjacent regions of the
same weld.
On some occasions it is necessary to reveal larger scale

features in forgings and castings by macroetching. These
features can include segregation, grain flow, porosity, and
nonmetallic inclusions. In such cases, macroetchants are used.
A typical macroetchant for steel is a solution of hydrochloric acid
and water.

Methodology of
Mechanical Test Specimens
Sometimes it is necessary to determine whether the material

from a failed component meets the specified mechanical
properties. In such cases, it will be necessary to machine test
samples. The two most commonly used mechanical tests are
the tensile test and the impact test. The test sample dimensions
for these tests are available in the American Society for Testing
Materials (ASTM) standards. It should be noted that, in some
cases, the dimensions of a failed component may be too small
to permit removal of a standard-sized test sample. In such
cases, subsized samples may be removed.
Tensile samples can be either flat or round. The standard round

tensile test sample is shown in Figure 8. ASTM E8 provides
dimensions for round samples. Tensile tests are also
conducted on weld samples as shown in Figure 9.
4-1/4"
3/4" 2-1/4" 3/4"
2" ± 0.005" gage length
3/4"
0.500 ± 0.01"
R =3/8 min
Shouldered or square ends may be used if desired;
dimensions shown are for threaded ends.
Figure 8. Standard Round Tensile Test Specimen

Methodology of
A standard flat sample that was taken across a weld is shown in

Figure 9.
These edges may Weld reinforcement

be flame-cut shall be machined
flush with base metal
1/4"
10" approx
†
2"R
1/4"
Edge of
widest face
W = 1-1/2" ± 0.01", if t of weld
1/4"
does not exceed 1".
W = 1" ± 0.01", if t
exceeds 1"
This section machined,
preferably by miling
Figure 9. Standard Flat Tensile Test Specimen for a Transverse Weld
The most commonly used test for impact testing is the Charpy V
notch test. The keyhole test was previously used. Standard
test samples are shown in Figure 10. The actual sample
dimensions are specified in ASTM E23.
Figure 10. ASTM Requirements for Charpy V Notch Sample

Methodology of
Analytical Test Specimens
In the majority of cases, only semiquantitative chemical

analyses are required. A scanning electron microscope that is
equipped with an energy dispersive analyzer can be used. In
most of these cases, the test specimen will be the previously
described metallographic sample. At other times, it is desirable
to remove test material for more accurate analytical tests, such
as bulk chemical analysis or analysis of deposits and scale. For
bulk chemical analysis, either filings or small coupons are
usually removed. The typical methods of analysis are x-ray
fluorescence, emission spectroscopy, and wet chemical
analysis.
Specimen and Archive

Material Preservation
Large pieces of the failed sample often are archived for possible
additional testing in the future. The prepared surface of a
metallographic specimen, in either the etched or unetched
condition, may be temporarily preserved in a desiccator, which
usually contains solid desiccants such as magnesium chloride.
Etched surfaces that are to be preserved for very long periods
of time may be coated thinly with a lacquer such as Krylon.
Optical Metallography and SEM Analysis
Optical Metallography
The metallurgical microscope, also called an optical

metallograph, has one basic function: magnification. The
metallograph differs from the ordinary optical microscope in that
the light is reflected from the metal surface, while ordinary
microscopes generally use transmitted light. A camera that is
attached to the metallograph permits photomicrographs (optical
micrographs) to be taken.

Methodology of
The basic principle of the metallurgical microscope is illustrated

in Figure 11.
To eyepiece
or camera
Partially silvered mirror
From light source
Specimen
Figure 11. Principles of the Optical Metallograph
The metallurgical microscope contains two separate optical

systems: the objective and the eye piece as shown in Figure 11.
As illustrated in Figure 11, a beam of light from a source is
diverted by a mirror downward through the microscope objective
onto the surface of the specimen. Some of this incidental light
is reflected from the surface of the specimen. The reflected light
that again passes through the objective will form an enlarged
image.

Methodology of
Since metals are opaque, only the surface can be examined by

metallograph. Metal specimens are carefully ground and
polished before examination by means of the methods that were
previously described. Observation of the polished surface
reveals considerable information about the general
characteristics of the metal; for example, a feature that often
helps distinguish grains in a metal is their different orientations.
Figure 7, in the previous section on etching, illustrated this effect
schematically.
In many cases, it is necessary to observe grain boundaries.

Figure 12 shows a slightly sensitized, stainless steel
microstructure.
Figure 12. Lightly Sensitized Stainless Sample

Methodology of
When a Type 300 series stainless steel is heated in the 450-815

°C (850-1500 °F) temperature range, a secondary phase
(chromium carbide) precipitates along the grain boundaries and
certain crystallographic planes. This secondary phase is
delineated by an etchant that attacks grain boundaries and
stains the carbide precipitate, as shown in Figure 13.
Figure 13. Sensitized Stainless Steel Sample (Photo)

Methodology of
On some occasions, the metallographer may need to measure

grain size. Size is important because the amount of grain
boundary surface has a significant effect on many properties of
metals, especially strength. One method of measuring grain
size is the ASTM method, in which the grain size number “n” is
defined by:
N = 2n-1 (1)
where “N” is the number of grains per square inch on a polished

and etched surface at a magnification of 100X, and “n” is an
integer referred to as ASTM grain size number. The grain size
number is illustrated in Figure 14.
In the laboratory, grain size measurements are made with

reference charts. These charts are often in the form of
templates that can be placed over a photomicrograph and
compared to the grains whose average size is to be measured.
Nominal number
of grains
Grain Per sq Per sq

Size mm at in at
no. 1X 100X
1 15.5 1.0
2 31.0 2.0
3 62.0 4.0
4 124.0 8.0
5 248.0 16.0
6 496.0 32.0
7 992.0 64.0
8 1980.0 128.0
9 3970.0 256.0
10 7940.0 512.0
Figure 14. Grain Size Measurement

Methodology of
Scanning Electron
Microscopy Analysis
The scanning electron microscope (SEM) is the major

diagnostic tool in a failure analysis. The SEM has often been
referred to as a “universal” microscope because it can
accomplish many of the important tasks in the characterization
of metal structure and composition. The SEM plays an
especially important role in the examination of fracture surfaces.
In a typical failure analysis where a fracture has occurred, the

fracture is first observed with a light microscope at low
magnifications (up to 30X) to determine, among other things,
the region of crack initiation and direction of crack propagation.
When a more definitive examination is required, however, it
should be noted that the light microscope has the following two
serious limitations:
• The useful magnification is limited to about 2,000X.
• The very limited depth of field makes it extremely difficult to

view objects with rough surfaces.
To a great extent, the above limitations are eliminated through

use of the electron microscope. There are two basic types of
electron microscopes: the transmission electron microscope
(TEM) and the scanning electron microscope (SEM). The TEM
is an instrument with outstanding capability. It can resolve
structures almost as small as individual atomic planes in metallic
crystals, and it can provide photographic magnifications of about
a million times. The TEM is most often found in metallurgical
research laboratories. On the other hand, the SEM, due to its
unique feature, is found in most modern failure analysis
laboratories.
Figure 15 shows a schematic comparison of the light, the

transmission, and the scanning microscopes. This Figure
indicates the similarity between the light and transmission
microscopes. In both instruments, the image is formed by
focusing a beam of light or electrons through the specimen and
then magnifying this beam to produce a final image. Of course,
with the optical metallograph, the light is reflected back from the
surface of the specimen instead of through it to form a final
image.

Methodology of
Figure 15. Operational Characteristics of Light and Electron Microscopes

Methodology of
The scanning electron microscope, or SEM, has properties that

place it between the optical metallograph and the transmission
electron microscope (TEM). Although both the SEM and the
TEM use focused beams of electrons, their operations are
based on two different concepts. With the SEM, magnetic
lenses focus the electron beam before it strikes the specimen,
and no focusing is done afterward. As the sharply focused
beam [about 100 Angstroms (A) in diameter], strikes the
specimen, a signal is generated from this area of the surface.
This signal is amplified and displayed on a cathode ray tube.
The strength of the signal at any given point on the surface of
the specimen is a function of the surface topography at that
point. Magnifications of up to 100,000 times are obtainable on
an SEM; however, the normal working magnification is generally
a lot less, for example, in the range of 1-10,000X.
Figure 16 shows a comparison of optical and electron

microscopes in terms of various performance capabilities.
Optical SEM TEM
Usable 10-2,000 10-100,000 1,000-500,000

Magnification
Resolving Power 2,000 50-100 2-4

(Angstroms)
Depth of Field Very Low High High
Signal Used for Transmitted or Surface Transmitted

Image Formation Reflected Generated
Type of Illumination Visible Light Electrons Electrons

(1-50 kV) (50-1,000 kV)
Specimen Polished and None Surface Replicas

Requirements Etched Mounting Shadowed or
Ultrathin Foils
Figure 16. Comparison of Optical and Electron Microscopes

Methodology of
Note that with the optical microscope, usable magnification is

limited to about 2,000 times, whereas the SEM can be used at
up to 100,000 times magnification, and the transmission
electron microscope can be used at much higher
magnifications. An important factor relating to the quality of
images that are obtainable at any given magnification is the
resolving power. Resolving power refers to the ability to identify
two closely spaced features as being two rather than one. The
limit of the optical microscope is about 2,000 A, whereas the
scanning electron microscope is considerably better, and the
transmission microscope is even better than the SEM.
An important feature of the scanning electron microscope as

compared to the optical instrument is its high depth of field.
When an optical microscope is used at a magnification other
then the very lowest magnification, it is difficult to bring rough
surfaces into focus. By contrast, the scanning electron
microscope has a very high depth of field, and it is possible to
see extremely rough surfaces at high magnifications with the
entire surface in focus. This feature makes the SEM a very
powerful tool for the study of fracture surfaces.
Usually, the SEM is equipped with an energy dispersive x-ray

analyzer or EDS. EDS can analyze all of the x-rays that are
emitted from a single region (selected area) on the specimen or
the entire area of a specimen being scanned. These x-rays
carry a characteristic energy and wavelength, which when
measured will reveal the elemental composition of the
specimen. With this method, we are able to obtain in a matter
of a few seconds a qualitative indication of most elements that
are present on the surface of a sample.
The basic principles of the EDS system are the same as the
Texas Nuclear Analyzer, which was described previously
(Figure 2).
EDS analysis can be performed on a wide variety of sample

types that contain elements that encompass a large portion of
the periodic table. A polished sample represents the ideal
sample configuration. It is analytically the most accurate when
a quantitative analysis is required. Because the specimen
mounting media are poor conductors, a ground connection is
required between the specimen and the specimen holder. A
loose powder may be analyzed with EDS by mounting it on a
proper substrate.

Methodology of
EDS is an extremely important tool for analysis of fracture

surfaces where environmental factors are involved.
Magnifications from 2,000X to 10,000X are usually employed in
the analysis of service failures, and the high resolution and
depth of field of the SEM make it a very valuable tool for such
work.
Previously, because of inherent limitations, it was not possible

to detect elements with atomic numbers lower than sodium
(Number 11). Today, light elements, including C, O, and F, can
be analyzed by specially equipped EDS systems. As an
example, with this system one may analyze rust as an iron-
based oxide; however, the specific compound, for example,
ferritic or ferrous, cannot be identified because specific
compounds cannot be identified.
Fractography
Fracture surfaces must be handled carefully because they may

contain tiny microscopic features that may help explain the
cause of failure. Very often, a fracture surface will be coated
with a lacquer to preserve it until it is ready for examination.
Particular care must always be taken not to rub the two surfaces
of a fracture together. Care should also be taken so as not to
contaminate the fracture surface through handling because the
surface is often examined chemically with the EDS system. If
there is evidence of debris and deposits on the fracture surface,
the fracture is initially examined with EDS in the SEM, then the
sample may be cleaned.
The fracture surface must often be cleaned in order to examine

the surface for microfeatures. Figure 17 lists the various
cleaning methods according to their degree of aggressiveness.
Typically, replica stripping is used to obtain a clean surface;
however, on some occasions, corrosion inhibiting acids are
required to remove oxides. Cleaning by the various techniques
is often facilitated using an ultrasonic bath.

Methodology of
Method Removal Of
Organic Solvent Oil/Grease
Acetate Replica Stripping Debris/Oxides
Detergents Corrosion Products/Oxides
Corrosion Inhibited Acids Sulfides/Oxides
Figure 17. Methods of Cleaning Fracture Surfaces
Very often, the experienced fractographer can identify by

thorough examination the failure origin, mode of failure, and
even the stress system that produced the failure. Ductile and
brittle fractures can be distinguished fractographically,
depending on the degree of plastic deformation.
Brittle failures can be classified as intergranular or transgranular

fracture mechanisms. Intergranular mechanisms include: stress
corrosion cracking, liquid metal embrittlement, hydrogen
embrittlement, creep, and grain boundary embrittlement.
Transgranular mechanisms include: brittle cleavage, stress
corrosion, and usually fatigue. Ductile failure can be subdivided
into tensile overload, transverse shear, torsional shear, and
bending overload.
A failure can occur by one or more of the listed mechanisms.

Fortunately, each mechanism usually results in a characteristic
appearance of the fracture surface, which distinguishes it from
the other types of fracture. Each of the characteristic
“fingerprints” was shown previously in the module on
mechanical failures.

Methodology of
In the case of fatigue failures, the SEM can be used to confirm

the failure mode; for example, many fatigue failures exhibit
clamshell markings. Fatigue can sometimes be confirmed by
the presence of fatigue striations revealed by SEM.
Case histories, where the scanning electron microscope

assisted in the diagnosis of a failure, are presented in the
following sections:
Example: Control Valve Stud Failure
Samples of fractured studs from a three-inch flow-control valve

were submitted for laboratory examination. The studs failed in
hydrogen service, and this failure caused the valve bonnet to
separate from the body of the valve.
Visual examination of the stud surfaces revealed many cracks

and a dark, carbonaceous residue that was located one or two
threads away from the fracture surface. There were no cracks,
nor was there residue, on the lower half of the studs that were
located in the valve body. All fracture surfaces were also
covered with a dark deposit. These deposits were removed
before fractographic examination using the scanning electron
microscope.
SEM analysis provided the opportunity to distinguish between

ductile and brittle fracture of the studs. It also provided
information regarding the environmental factors that were
involved. In this case, the fracture surface was over 75 %
intergranular of a type that is associated with a brittle failure
mode.
The lower halves of the failed studs, which were stressed to

failure in a laboratory test, showed the typically dimpled rupture
features of a ductile overload fracture. Further microscopic
examination revealed that the studs had been plated. Follow-up
surface examination by energy dispersive analysis showed that
the plating was zinc. Furthermore, subsequent analysis by EDS
of the intergranular cracks identified the residue in the cracks as
zinc.

Methodology of
The studs failed in a brittle manner with no sign of ductile

behavior. Liquid zinc is a known embrittling agent for materials
such as those materials that are used in B-7 bolting. The
intergranular failure mode with zinc at the grain boundaries
provided confirming evidence that the failure mechanism was
liquid metal embrittlement. Subsequent discussion with valve
manufacturing personnel indicated they were aware of the
potential for liquid metal embrittlement for some time. Based on
the above analysis, steps were taken to avoid future failures.
The most important step was immediate replacement of all
plated, low-alloy steel bolting (studs and nuts) in control valves
that are operating at elevated temperature and pressure. These
studs and nuts were replaced with high-strength stainless
material.
Example: Pump Shaft Failure
A failed pump shaft was submitted for laboratory examination.

The fracture surface ran perpendicular to the axis of the shaft.
Final, fast fracture was the result of torsional load. Closer
examination showed the presence of numerous creases that are
typical of fatigue. After the surface was cleaned, a crack that
was extending along the corner of the keyway was detected by
visual examination.
Examination with the scanning electron microscope revealed the

presence of fatigue striations, which are classic fatigue features.
High resolution SEM fractography revealed traces of fatigue-like
indications at the origin that is located at the corner of the
keyway. There was no evidence of other features that would
have suggested other causes of initiation of the failure, such as
intergranular stress corrosion cracking.
It was concluded that failure of the pump shaft resulted from

mechanical fatigue which initiated at the sharp key corner.
Corrective measures included machining a larger radius on the
keyway corner to minimize the potential for fatigue.

Methodology of
Material Characterization
Mechanical Testing
Mechanical test apparatus is used to supplement microscopy

and confirm its results in the investigation of metal failures.
Some of the more commonly used tests are Tensile, Impact,

Hardness, Bend, and Compression.
Tensile Test - The tensile test machine is a device in which one

end of a metal specimen (Figure 8) is gripped in a stationary
crosshead while the other end gripped in a movable crosshead.
The specimen is broken by pulling from the ends. The tensile
test provides a measure of ductility and strength. Because of
the uniformity of strain (elongation) before necking-down begins,
measurements of the relationship between stress (load) and
strain can be obtained.
The tensile test machine consists of the following two essential

members:
1. A device for straining the specimen (load frame)
2. A device for measuring the resistance of the specimen to

this straining (load cell).
A strain gauge (extensometer) is used to measure the extent of

the strain (elongation). The significant measurements that are
made with the tensile test machine include: yield strength,
tensile strength, and final elongation. These parameters were
described in COE 106.03.
Impact Test - The impact test determines the energy that is

absorbed in fracturing a test bar at high velocity. The impact
test is a simple evaluation of notch toughness of a metal. The
test that is most commonly used is the Charpy V notch test,
which employs a swinging pendulum to fracture a notched
specimen as illustrated in Figure 10. The conventional size
Charpy machine (Figure 18) has a total available striking energy
of 220 ft/lb.

Methodology of
Figure 18. Typical Charpy Testing Machine
The specimen, which is supported at both ends as a beam, is

broken by a single blow of the pendulum, which is applied at the
middle of the span. Ordinarily, the specimen breaks at the
notch, the two halves fly away, and the pendulum then passes
between the two parts of the anvil. The height of the fall minus
the height of the rise equals the amount of energy absorption in
deforming and breaking the specimen plus friction losses. The
instrument has a scale with moving pointer, which is calibrated
in terms of energy, to indicate the “impact value” of the test
specimen.

Methodology of
Temperature has the pronounced effect of changing the energy

absorption and fracture behavior of steel in a notched condition.
This change in behavior occurs over a relatively narrow range
and at approximately atmospheric temperatures for most ferritic
steels that have not been heat treated. The sharpness of the
change or transition from tough to brittle depends on the
material and also on the notch geometry. (See Figure 5 in COE
106.03 for an example of a ductile-rittle transition curve.)
The impact test is the primary evaluation tool that is used to

determine the serviceability of steels and the necessity for heat
treatment. For pressure vessel applications, very specific
conditions must be met as specified in the ASME Pressure
Vessel Code. Although impact values of steel are a necessary
criteria for design, this test also is generally used for the
evaluation of material that is involved in metal failures.
Service failures corroborate the test results by pointing to the

increased hazards of subnormal temperatures, and
determinations of transition temperatures have come to be
useful criteria of steel “quality” or applicability to the part in
question. An application of transition temperature curves is the
determination of susceptibility to temper embrittlement. Results
of refinery impact tests on hydrocracker plate material are
presented in Figure 19. Quenched and tempered 2-1/4 Cr-1 Mo
plate metal was subjected to various heat treatments to induce
temper embrittlement. The curves show that there has been a
temperature shift that was caused by temper embrittlement.

Methodology of
Figure 19. Shift in Transition Curve Caused By Temper Embrittlement

Methodology of
Other information can be obtained from Charpy V notch

samples as shown in Figure 20. The fracture appearance
changes considerably as we move down the transition curve.
The fracture surface becomes flat, brittle, and loses all evidence
of shear. The percent shear can be obtained from the Charpy
test.
Figure 20. Fractured Charpy V-Notch Specimens With

Varying Amounts of Shear Deformation
Hardness Tests - Hardness testing is one of the simplest and

most inexpensive tests used in the metallurgical laboratory.
Hardness is a measure of the resistance of a material to
indentation. Several types of hardness test equipment are
available. The two most commonly used hardness machines
are as follows:
• Brinell
• Rockwell

Methodology of
Brinell Hardness Test - The Brinell hardness test machine

usually consists of a hand-operated, vertical hydraulic press that
is designed to force a ball indenter into the test specimen. The
surface on which the impression is made must be reasonably
smooth and free of surface defects. The load that is applied by
the instrument can be varied over a considerable range. The
Brinell hardness number (BHN) is expressed in units of
kilograms per square millimeter. It is expressed, as shown in
Figure 21, by the load P divided by the surface area of
indentation.
P
where: Brinell hardness number = and
A

πD D – D2 Š D12 
 
A= (2)
2

D1
Figure 21. Basic Parameters in Brinell Hardness Test

Methodology of
Rockwell Hardness Tests - The most widely used laboratory

test is the Rockwell hardness test. A Rockwell test is made by
slowly elevating a specimen against the indenter until a minor
load has been applied, as indicated by an index hand on a dial
gauge. The Rockwell hardness number is based primarily on
the resulting depth of indentation. A diamond cone indenter or
1.6 to 3.2 mm (1/16 to 1/8 in) diameter indenters are generally
used. Major loads are 60, 100, and 150 kg. The Rockwell
hardness number is dependent on the load and indenter;
consequently, a letter is used for each of these combinations.
As an example, for hardened steels, the letter C, which
represents a diamond indenter with a 150 kg major load, is
used. The useful range for this scale is about Rc20 to Rc70. A
“B” scale, which requires a 1.6 mm (1/16 in) diameter indenter
with a 100 kg major load, is used for softer materials. An “A”
scale, which covers the widest range of hardness, can also be
used. The “A” scale requires a diamond indenter with a 60 kg
major load.
For convenience, hardness conversion charts have been

prepared to permit hardness numbers to be converted from one
Rockwell hardness scale to another. Rockwell readings can
also be converted to Brinell by the use of conversions.
Hardness tests are used to determine the heat treated condition

or the amount of cold work; for example, it has been established
that B7 exchanger bolting is subject to hydrogen embrittlement if
the hardness of the bolt exceeds 22 Rockwell C. Therefore,
hardness measurements are performed to assure that the bolts
are heat treated (tempered) to hardnesses below this level.
Microhardness Test - The purpose of a microhardness test is

to determine material hardness in very localized areas; for
example, the hardness across a weld is sometimes important
when it is suspected that parts of it are hard and susceptible to
hydrogen embrittlement. A Rockwell hardness indentation,
however, often covers too much area in the weld, and, as a
result, the resultant hardness averaged over this area.
Microhardness readings that are taken in the same region would
delineate between local hard spots and the surrounding area.

Methodology of
The principle of the microhardness measurements is much the

same as it is for Rockwell testing. An indenter is forced into the
material by known weights on a level system. The depth of
penetration is then a measure of the hardness of the material.
Bend and Compression Tests - The bend test is one of the

simplest and least expensive of the mechanical tests that are
used in evaluating metals. The simplest bend test may be
performed by clamping one end of the specimen in a vise and
bending the other end by hammering. After the initial bend is
made, both ends are clamped in a vise and compressed. The
end point of the test is reached when the required angle of bend
has been accomplished without rupture of the outer fibers.
Various types of bend tests are used in the evaluation of welded
joints. Bend samples may be longitudinal or transverse to the
weld axis.
Compression testing is conducted on the tension test machine

by pushing on the specimen instead of by pulling on it. This test
is used in the laboratory primarily for measuring the ductility of
pipe and tube, somewhat as a modified bend test. This test has
been used to illustrate the brittleness of carburized heater tubes.
Chemical Analysis
In some cases, the SEM-EDS system can be supplemented by

other types of chemical analyses. Some of these methods are
described below:
Wet Chemical Analysis - One of the oldest, yet most accurate

techniques for determining the compositions of metal alloys is
wet chemical analysis whereby a number of chemical laboratory
bench-type analytical techniques are used primarily to identify
elements in a sample.
Emission Spectroscopy - All elements have specific

characteristic wavelengths that are as individual as fingerprints.
Emission spectrographic analysis of a material results in a
characteristic wavelength spectrum that can be used to identify
the elements that are present in the sample being analyzed. In
situations where approximate metal composition is required, this
technique is faster and more economical than wet chemical
analysis.

Methodology of
X-ray Diffraction - When a beam of X-rays is directed at a

material, the beam is diffracted by the crystal structure of the
material in much the same way as an optical grating diffracts a
light beam. This diffraction pattern is specific for each material
and can be used to identify metals and metal compounds in
very much the same manner as emission spectroscopy. This
technique is particularly suited for analysis of thin surface
corrosion films and very small samples. The unique advantage
of X-ray diffraction (XRD) over most other analytical techniques
is that this technique identifies the crystal structure and specific
compounds analyzed, not just the elements contained in the
compound. Information concerning the composition of these
corrosion products frequently reveals the source and nature of
the corroding agent.
X-ray Fluorescence - This analytical technique is used to

identify elements in a sample by exciting inner-shell electrons
using x-rays. X-rays are emitted in spectra characteristic of the
target elements. This technique has several similarities to the
previously discussed EDS/Texas Nuclear technique.
Corrosion Tests
Various types of corrosion tests can be used as part of the

failure investigation. Quite often, the test is accelerated by an
increase in temperature or by use of a more aggressive
environment. Extreme care is required in the interpretation of
accelerated corrosion tests.
One such test is the NACE test for wet H2S cracking. This test
is designed to test metals for resistance to cracking in aqueous
environments that contain hydrogen sulfide. Sulfide stress
corrosion cracking (SSC) has been a long-term problem in both
oil field and refinery environments. Although this test focuses
primarily on SSC failures, other failure modes, including
blistering and stepwise cracking, can be observed when
conducting this test. These failure modes have been covered in
COE 106.02. Details of this test can be found in NACE
Standard TM-01-77.

Methodology of
VALUE OF LABORATORY SIMULATION FOR CONFIRMATION OF FAILURE MODE
Laboratory simulation tests are often used in the analysis of

failures. In such tests, the actual part is often tested; for
example, if a stress corrosion environment is to be simulated, it
may be of importance to use the actual part with its locked in or
residual stresses.
Laboratory failure simulation is often extremely useful in

confirming a theory regarding the cause of failure. Examples
are provided to illustrate the two methods of failure reproduction
that are described below.
Example: Use of simulated heat treatments in laboratory failure

analyses
A flange fire occurred in a major vessel. The flange was overlaid

with Type 347 stainless steel. Cracking was found in the ring
groove region. It was suspected that cracking of stainless steel
was caused by sigma phase embrittlement. It was speculated
that sigma phase had formed during postweld heat treatment
(PWHT) of the pressure vessel. Evidence of what appeared to
be sigma phase was observed through metallographic
examination (Figure 22a). In order to determine whether PWHT
was responsible for sigma formation, pieces of the stainless
overlay were annealed to remove any sigma phase (Figure 22b)
and exposed to a simulated PWHT. Metallographic examination
again showed the sigma phase formation (Figure 22c).
Subsized Charpy V-notch tests were also conducted on sample
material before and after heat treatment. These tests confirmed
that embrittlement had occurred as a result of PWHT. Thus,
sigma phase embrittlement was determined as the cause of
failure.

Methodology of
(a) (b) (c)
400x 400x 400x
As-received microstructure. Microstructure after Microstructure after

Note light grain boundary solution annealing. Only reembrittlement. Note
constituent-ferrite. Dark austenite and carbides reappearance of sigma
areas represent sigma are present. phase (dark grain
phase locations. Some boundary constituent)
carbides also present in along grain boundaries.
grain boundaries. Similar to (a).
Figure 22. (a) Sigma Phase Appearance Before Annealing,

(b) After Annealing, and (c) After Simulated Heat Treatment
Example: Use of synthesized environments in laboratory failure

analyses
Failures of floating roof tank seals were experienced when a

new gasoline product additive, MTBE, was used. Deterioration
of the standard nonmetallic materials, such as Viton, occurred
after only very short time periods.
A program was set up to reproduce the conditions that led to

deterioration, including volumetric swelling and loss of tensile
elongation. A simulated test environment was developed for
laboratory testing. A slightly elevated test temperature was
selected to accelerate deterioration.
Exposure tests reproduced the form of deterioration that had

occurred in the field. The test program was then continued to
evaluate alternate materials. Based on a ranking system that
was developed as part of the test program, materials were
found that were compatible with the MTBE additive.

Methodology of
THE STEPS BY WHICH LABORATORY INFORMATION IS OBTAINED
Figure 23 is a general flow chart for procedures conducted in a

failure analysis laboratory. Figure 24 shows the typical work
flow path through Consulting Services Laboratory. The work
request forms (A though F) are provided in the Addendum. Key
steps that take place during a laboratory examination are
indicated below:
• Work arrives at Materials Laboratory Unit (MEU) with a

form that requests services. This form contains a job
description as well as important background information
that is provided by the operating plant.
• Work is assigned at MEU to an engineer who then

establishes a work plan for laboratory testing. A technician
will follow laboratory work to conclusion.
• A report is written and issued to the operating plant, and

the sample is tagged and stored short term.
• After 3-6 months, a decision is made to scrap or long-term

store the sample.

Methodology of
Sample arrives in
laboratory
Background
Information
Stereographic Visual Photography/

Examination Examination Macrophotography
Dimensional
Measurements
Spot Tests/NDE
Tests
Deposit, Scale and

Archive Archive
Sample Cutting Corrosion Product
Material Material
Removal
Specimen SEM Metallographic SEM Analytical Chemistry

Machining Fractography Preparation Examination Analyses
Mechanical EDS
Metallography
Testing Analysis
Laboratory Experimental Specimen

Simulation Results Storage
Analysis of Results
Failure Analysis
Report
Figure 23. Laboratory Failure Analysis Flow Chart

Methodology of
Start Lab supervisor completes 'A'.

Keeps updated copy of
allocated job numbers.
Work arrives in MEU Lab. OR
Engineer (rare occurrence)
MEU completes job log, allocates OR

next number, and informs
supervisor to update his copy. Proponent on arrival at MEU
with job
OR
Sheet 'A' submitted to supervisor if
RQD. MEU completes 'A' and
interrogates for information.
MEU marks work with allocated job

number.
Sheet 'F' completed and

accompanies work piece until
scrapped.
Sheet 'A' returned to MEU with

assigned engineer. Filed.
Engineer completes sheet 'B' or

technician completes 'B' under
instruction from engineer or lab
supervisor.
To MEU and on to Engineer

Technician allocated to follow job
through to conclusion.
Technician or engineer completes Chemical Yes

Results
instructions updating 'B' as RQD or Analysis
new 'B' until job complete. Form
'E'
No
XRF Yes
XRD Results
SEM
Form
MEU lab awaits issue of report and
'C'
then places job in short term store.
No
Storage section of 'F' completed.
HIC Test Yes

Results
3-6 months - Decision to scrap or
END Form
long term store. Sheet 'F' updated
'D'
and filed if scrapped.
No
Figure 24. Failure Analysis Work Flow

Methodology of
SUMMARY
This module identified the laboratory failure analysis procedures

that are used in Saudi Aramco Consulting Laboratories. It is
important for the field engineer to know these procedures so he
can answer questions that might arise. An understanding of the
general flow path through the failure analysis laboratory is also
important. Figure 23 summarizes laboratory failure analysis
procedures in a flow chart.

Methodology of
GLOSSARY
characteristic x-rays Specific energy emissions that are emitted by chemical

elements.
Charpy V notch test A mechanical test that measures the resistance to impact.
energy dispersive A method of chemical analysis that identifies and

analysis measures elements by their characteristic radiation.
fractography The examination of fracture surfaces by means of optical

or electron microscopes.
grain Most metals are composed of many tiny crystals that are
called grains.
long and short The directions that are perpendicular to rolling directions in
transverse sheet or plate.
macroetchant A chemical solution (usually an acid) that is used to reveal

grain flow or other directional features.
metallograph An optical microscope that examines microstructure of

metals.
metallographic Microscopic examination of a metal to determine its

examination microstructure.
microstructure Unique microscopic features that are representative of a

given metal or alloy.
optical microscope A microscope that uses optical lenses for analysis (see
metallographic above) of materials.
rolling direction The direction of rolling that is found in metal sheet and
plate.
scanning electron A microscope that uses a scanning electron beam for

microscope analysis on materials surfaces.
stereomicroscope A low-power binocular optical microscope.
tensile test A mechanical test that measures strength.

Methodology of
transition curve The Charpy energy curve that shows how energy varies
with temperature.
transmission electron A microscope that uses an electron beam to examine the

microscope internal structure of metals.

Methodology of
REFERENCES
1. American Society for Metals (ASM). “Failure Analysis and

Prevention,” Metals Handbook, Eighth Ed., Vol. 10, Metals
Park, OH, USA, 1975.
2. American Society for Metals (ASM), “Nondestructive

Inspection and Quality Control,” Metals Handbook, Eighth
Ed., Vol. 11, Metals Park, OH, USA, 1975.
3. J. L. McCall and W. M. Mueller, Metallographic Specimen

Preparation: Optical and Electron Microscopy, Plenum
Press, New York, NY, USA, 1976.
4. G. Petzow, Metallographic Etching, American Society for

Metals (ASM), Metals Park, OH, USA 1978.
5. M. A. Meyers and K. K. Chawla, Mechanical Metallurgy,

Prentice Hall, Englewood Cliffs, NJ, USA, 1984.
6. B. L. Gabriel, SEM: A User’s Manual for Materials Science,

American Society for Metals (ASM), Metals Park, OH,
USA, 1985.

Methodology of
FORM A

Methodology of
FORM B

Methodology of
FORM C

Methodology of
FORM D

Methodology of
FORM E

Methodology of
FORM F

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Saudi Aramco DeskTop Standards

Chapter : Corrosion For additional information on this subject, contact

LABORATORY FAILURE ANALYSIS PROCEDURES USED

VALUE OF LABORATORY SIMULATION

THE STEPS BY WHICH LABORATORY INFORMATION IS OBTAINED ................... 44

Saudi Aramco DeskTop Standards i

Figure 1. Procedure Outline for a Laboratory Analysis.................................................. 5

Figure 2. The Origins of Characteristic X-Rays Used in EDS Analysis ......................... 8

Figure 4. Important Metallurgical Directions in an As-Rolled Plate.............................. 12

Figure 6. Mounted Metallographic Sample.................................................................. 15

Figure 7. The Effect of Eching on a Polished Metal Surface ....................................... 16

Figure 8. Standard Round Tensile Test Specimen...................................................... 18

Figure 10. ASTM Requirements for Charpy V Notch Sample ..................................... 19

Figure 11. Principles of the Optical Metallograph ........................................................ 21

Figure 12. Lightly Sensitized Stainless Sample........................................................... 22

Figure 13. Sensitized Stainless Steel Sample (Photo) ................................................ 23

Saudi Aramco DeskTop Standards ii

Figure 14. Grain Size Measurement............................................................................ 24

Figure 15. Operational Characteristics of Light and Electron Microscopes ................. 26

Figure 16. Comparison of Optical and Electron Microscopes...................................... 27

Figure 17. Methods of Cleaning Fracture Surfaces ..................................................... 30

Figure 18. Typical Charpy Testing Machine ................................................................ 34

Figure 19. Shift in Transition Curve Caused By Temper Embrittlement ...................... 36

Figure 20. Fractured Charpy V-Notch Specimens

Figure 21. Basic Parameters in Brinell Hardness Test ................................................ 38

Figure 22. (a) Sigma Phase Appearance Before Annealing,

Figure 23. Laboratory Failure Analysis Flow Chart...................................................... 45

Figure 24. Failure Analysis Work Flow ........................................................................ 46

Saudi Aramco DeskTop Standards iii

Proper diagnosis of equipment failure often results in a wealth of

Saudi Aramco DeskTop Standards 4

LABORATORY FAILURE ANALYSIS PROCEDURES USED IN SAUDI ARAMCO

Failure analysts usually follow a prescribed procedure during an

2. Preliminary Alloy Tests

4. Selection, Identification, Preservation,

6. Quantitative Chemical Analysis

8. Simulated Service Testing

Figure 1. Procedure Outline for a Laboratory Analysis

Saudi Aramco DeskTop Standards 5

The laboratory failure analysis begins with several of the

In the majority of cases, the steps in Figure 1 are followed until

• A cast heater tube with radial cracks was submitted for a

• A fatigue failure from a compressor disk was submitted for

Saudi Aramco DeskTop Standards 6

It is important to mechanically measure dimensions of the failed

Preliminary Alloy Identification Tests

Just as in the field failure analysis, a very important starting

Chemical Spot Testing - Chemical spot testing is one method

Energy Dispersive Chemical Analysis (Texas Nuclear) -

A quantitative analysis can be performed by evaluating the

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Figure 2. The Origins of Characteristic X-Rays Used in EDS Analysis

The basic principle of energy dispersive x-ray spectroscopy

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Figure 3. Relation Between Atomic Number and Characteristic X-Ray Lines

Specimen Selection and Preparation

Careful visual examination is always required at the start of

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Example: How NDE plays a role in a laboratory examination

Leaks were experienced in a 2 inch - 600 lb gate valve almost

Prior to destructive sampling, the failure analyst should make a

At this stage of the examination, a plan of attack must be