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Engineering Encyclopedia

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Field Failure Analysis Procedures

Note: The source of the technical material in this volume is the Professional
Engineering Development Program (PEDP) of Engineering Services.
Warning: The material contained in this document was developed for Saudi
Aramco and is intended for the exclusive use of Saudi Aramco’s
employees. Any material contained in this document which is not
already in the public domain may not be copied, reproduced, sold, given,
or disclosed to third parties, or otherwise used in whole, or in part,
without the written permission of the Vice President, Engineering
Services, Saudi Aramco.

Chapter : Materials & Corrosion Control For additional information on this subject, contact
File Reference: COE10606 S.B. Jones on 874-1969 or S.P. Cox on 874-2488
Engineering Encyclopedia Materials & Corrosion Control
Field Failure Analysis Procedures

CONTENTS PAGES

LOCATIONS OF PRIMARY..................................................................................... 4
Initial Observations ......................................................................................... 4
Field Examination ........................................................................................... 6
Failures Involving Fires ....................................................................... 6
Determining Primary Failures............................................................ 10

PRESERVATION OF FAILED COMPONENTS.................................................... 11


Sampling Techniques .................................................................................... 11
Failed Equipment ............................................................................... 11
Corrosion Products, Scales, Deposits ................................................ 13
Samples of Process Environments ..................................................... 15
Sample Preservation/Handling ...................................................................... 15

REMOVAL OF FAILED SAMPLES AND ASSOCIATED DEPOSITS ................ 16


Boat Samples................................................................................................. 17
Microbiological Samples............................................................................... 18
Sample Identity Control ................................................................................ 18

NONDESTRUCTIVE EVALUATION (NDE) TECHNIQUES USED


TO SUPPLEMENT VISUAL FIELD EXAMINATION .......................................... 19
Inspection Techniques................................................................................... 19
Leak/Pressure Testing........................................................................ 19
Liquid Penetrant Testing (PT)............................................................ 20
Magnetic Particle Testing (MT)......................................................... 21
Eddy Current Testing......................................................................... 21
Ultrasonic Testing (UT) ..................................................................... 22
Boroscope Examination ..................................................................... 22
Radiography....................................................................................... 24
Field Microscopy ............................................................................... 24

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Replication ......................................................................................... 25
Field Chemical Analyses ................................................................... 27
Portable Hardness Tests..................................................................... 30

FLOW PATH FOR FIELD FAILURE ANALYSIS PROCEDURES ...................... 32

COMPLETING A FAILURE ANALYSIS INFORMATION FORM ...................... 34


Key Information ............................................................................................ 37
Background Information ............................................................................... 37
Equipment Specifications .................................................................. 38
Operating Conditions/History ............................................................ 38
Eye Witness Accounts ....................................................................... 38

GLOSSARY ............................................................................................................. 39

REFERENCES.......................................................................................................... 41

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LOCATIONS OF PRIMARY

Initial Observations

Field failures often result in disruption of operations. In the worst cases, explosions and/or
fires occur after the root failures and cause additional damage. When rotating equipment
such as turbines fail, projectiles can destroy every blade in the flow path. One can
understand how difficult it is to find the initially failed turbine blade in a turbine where all of
the blades have been bent or fractured by impact.

When a failure occurs, it is important to obtain as much information as possible that pertains
to events that led up to the failure as well as what happened after the failure. Some of the
questions to answer are listed in the following paragraphs.

The questions that might be asked regarding the events that led up to the failure are as
follows:

• What were normal operating conditions for the equipment (temperature,


pressure, stream composition)?

• Has there been a history of problems? Obtain as much information on the


operating history for the equipment as possible.

• What were design parameters for the equipment?

• What were the materials of construction?

• What were operating conditions just prior to the failure?

• Were there any unusual circumstances?

• Have there been any process upsets? What were the conditions during these
upsets?

• Has equipment been shut-down due to extended turnarounds or for a lay-up?


If so, what, if any, precautionary steps have been taken to protect the
equipment?

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The questions that might be asked that pertain to the failure and subsequent events are as
follows:

• What was the time of failure?

• Were there accompanying explosions or other noises?

• Did the failure result in a fire?

• What was the fuel source?

• How long did the fire last?

• Did the fire spread?

• What methods were used to fight the fire (firewater, nitrogen purge)?

• Did secondary fires ensue?

• What is the source/quality of the water used near the equipment?

• Was equipment thermally insulated?

Information may be obtained from operators, firefighters, and eyewitnesses as well as from
records such as logbooks. Photographs that were taken during the event are helpful. With
prolonged fires, remote temperature measurement may be possible.

As soon as possible after the failure, the degree (and types) of assistance from Saudi Aramco
Consulting Services Department personnel should be assessed. Consultants from the
following units may be helpful in assessing damage and cause of failure:

• Materials Engineering

• Piping, Valves, and Vessels

• Civil and Structural

• Electrical

• Instrumentation

• Pumps, Compressors, and Turbines.

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Field Examination

Once the equipment is completely shutdown and fires are fully extinguished, access to the
failure site will be possible pending safety clearance. High temperatures that remain in some
areas, as well as the presence of combustibles or explosive gases, asbestos or other
hazardous chemicals, and structural instability can create dangerous zones that must be
evaluated by safety experts. Subsequent access to such areas may be possible only with
respirators and/or protective clothing.

Failures Involving Fires

In some cases, when there has been severe damage caused by a fire, it will be necessary to
determine whether the affected equipment is suitable for reuse. Materials Technology
Institute Publication No. 30, “Guidelines for Assessing Fire and Explosion Damage”
(Reference 1), provides detailed information on damage assessment. Photographic
documentation of the area is essential. The locations of the primary and secondary fires
should be located, and zones of varying heat exposure should be mapped. Six zones
corresponding to heat exposure typically are used:

• Zone 1: Ambient; no fire effects

• Zone 2: Ambient to 66 °C (150 °F); smoke and water damage

• Zone 3: 66 °C (150 °F) to 204 °C (400 °F); light heat exposure

• Zone 4: 204 °C (400 °F) to 427 °C (800 °F); moderate heat exposure

• Zone 5: 427 °C (800 °F) to 732 °C (1350 °F); heavy heat exposure

• Zone 6: Above 732 °C (1350 °F); severe heat exposure.

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Figure 1 lists some of the temperature indicators that are used in determining heat exposure
zones. Several of the indicators are more accurately determined under laboratory conditions
that require sampling; for example, while oxidation may be visually apparent,
metallographic cross sectioning would be necessary for more information on
time/temperature effects.

Temperature Approximate
Indicators Temperatures

† Varying for different


Melting, charring, ignition
materials

† > 540 °C for carbon steel


Oxidation of metals
> 816 °C for stainless steel
††
Tempering of steels > 205 °C

* Grain growth in copper alloys > 205 °C


††
Softening of aluminum alloys > 150 °C

* Spheroidization of carbon steel > 649 °C

Stress relief of stainless steels


> 490 °C
and nickel alloys

* Sensitization of stainless steels > 490 °C


* Grain growth of carbon steel > 927 °C

Distortion of structural steel > 760 °C

Can often be determined visually in the field
††
May be evaluated by portable hardness testing in the field
* Requires portable metallographic techniques for preliminary answers

Figure 1. Temperature Indicators (Approximate Temperatures)

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Temperature Material Effect

93 °C (200 °F) Vinyls and Alkyd Coatings Blistering, charring

127 °C (260 °F) Polyethylene Pipe Melts

182 °C (360 °F) Lead/tin Solder Melts

190 °C (375 °F) Baked phenolics Turns black

260 °C (500 °F) Steel Develops blue


temper color

271 °C (520 °F) Babbit Bearings Melts

388 °C (730 °F) Zinc/aluminum Die Castings Melts

421 °C (790 °F) Galvanized Layer on Steel Melts

593 °C (1100 °F) Steel Vessels and Piping Thermal distortion

649 °C (1200 °F) Steel Vessels and Piping Black oxide forms

657 °C (1215 °F) Aluminum Melts

695 °C (1285 °F) Glass Windows Melt

904 °C (1660 °F) Galvanize Oxidizes to white


powder or vaporizes

1093 °C (2000 °F) Copper Melts

1516 °C (2760 °F) Steel Melts

Figure 2. Effects of Temperature for Various Materials

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Temperatures at which damage occurs for selected materials are given in Figure 2. Heat
exposure zones are plotted as shown in Figure 3.

Figure 3. Heat Exposure Zones for a Rupture and Fire (Reference No.1)

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Determining Primary Failures

To locate the primary failure requires thorough on-site examination and often includes
mapping procedures for fires and explosions. Secondary failures usually can be attributed to
either impact, concussion, or fire damage. When doubts exist, secondary failures will require
failure analyses to prove that they were not the cause of the problem, but rather the effect.
With rotating equipment, primary failures usually occur on the upstream side, but secondary
failures usually occur on the downstream side. In heavily damaged pumps and compressors,
internals may require reassembly and examination by specialists to locate the possible failed
parts.

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PRESERVATION OF FAILED COMPONENTS

Sampling Techniques

Failed Equipment

Primary equipment that has failed and, in some cases, secondary equipment failures must be
carefully preserved to ensure that the maximum amount of information is available to
complete the failure analysis. The failed regions may have been exposed to the environment,
fire, and firewater; however, any additional contamination or damage will make the failure
analysis even more difficult.

All parts of the failed equipment should be located, mapped, and identified. Before the failed
region(s) is disturbed in any way, visual observations should be recorded with sketches, and
photographs (overall and closeups) should be taken. The observations should be made by a
trained observer, who should be assisted, if necessary, by a Consulting Services Department
failure analyst. In some cases, mechanical measurement of components may be required
before cutting. Changes during cutting, such as springback, also should be recorded.

A magnifying glass or low power microscope can be helpful for the initial examination.
Boroscopes and fiberoptic equipment (fiberscopes) are also useful. Nondestructive
Examination (NDE), which is covered in a separate section, may be necessary at this stage.

Specific guidelines must be followed during the examination and subsequent sampling
operations as follows:

• Do not sandblast, wirebrush, or clean (acid or otherwise) failed parts.

• Do not touch fracture regions or fit fractures back together.

Samples that are selected for removal should be large enough to allow for test specimens.
When samples such as failed heater tubes are removed, it is wise to remove samples from
undamaged regions for comparison. Such samples and resulting specimens are referred to as
control samples and control specimens. Prior to cutting, a sketch of the pieces that result
should be prepared, and each piece should be identified with a code. Pieces should be
identified by code on a well-secured tag, indelible marker, or scribing (vibrograving) in a
noncritical area. Code marking should be performed before or immediately after cutting.
Precautions during cutting are as follows:

• When possible, cut samples dry (without cutting fluids) to avoid the
possibility of contamination.

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• If necessary, use flame cutting; however, do not use flame cutting if cuts
cannot be made far enough away from the failure location to avoid
overheating of the region that is to be examined.

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Corrosion Products, Scales, Deposits

Before cutting failed parts, samples of corrosion products, oxide scales, and/or deposits
should be obtained in sufficient quantities to provide specimens for numerous laboratory
tests.

Colors and smells of samples should be recorded during the field examination. Some
samples are hygroscopic or volatile, and subtle changes in the chemical nature may occur
before the samples reach the laboratory. For these reasons, field observations are important.
It also is important to obtain the samples quickly, and seal off the container or bag. Two
quick field tests that can aid the investigation are as follows:

• Check for magnetic attraction as a quick check on whether or not the sample
contains iron.

• To test for pH, use pH paper. This test will serve to indicate if the sample is
corrosive, particularly to the sample container.

Since some samples are corrosive to certain sample container materials, judgment in
container selection must be exercised. For example, samples that contain hydrofluoric acid
may attack glass. For this reason and because it is less likely that the container will break in
transit, polyethylene often is preferred. Conversely, solvents may attack plastics. One of the
best sample containers for solids is the Whirlpak bag. These plastic bags are free of
contaminants, seal reasonably well, and come in an assortment of sizes.

Some samples are soft or flocculent and can easily be scrapped into a sample container by
means of a clean spatula or similar tool. Tweesers come in handy for small particles. Harder
particles may be more difficult to pry loose and are often better left on the failed part.

When layers of deposits are observed, segregating each layer should be attempted. The
locations of each layer (from the outer surface to the surface of the base metal), as well as
each side (OD or ID) of each layer should be recorded. Compositional variations of the
layers, as determined in the laboratory, may provide information on operating history and
exposure to corrodants. Sometimes, oxide thickness measurement can provide useful
information as indicated below.

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Various laboratory studies have shown that in steam or other oxide forming environments
the growth of oxide scale is a function of temperature and time of exposure. Based on these
studies, experimental curves have been developed that relate oxide thickness and time of
service at different temperatures; for example, the curves in Figure 4 were developed for
boiler tubes with the commonly used 2 1/4 Cr - 1 Mo steel alloy.

Figure 4. Oxide Thickness as a Function of Time of Exposure


for Various Temperatures (2 1/4 Cr-1 Mo Steel in Steam)

With the proper method of measurement, an estimate of tube metal temperature can be
made. This method could involve direct measurements of oxide removed, removal of a
minisample cone sample (which will be described later in this module), or by special
ultrasonic measurements. It is important to note that the steam side oxide layer thickness can
be used to estimate only an “equivalent” exterior tube metal temperature. Despite this
limitation, the oxide scale measurement has become a standard tool in life prediction in the
electric power industry. On some occasions, this method can also provide useful information
in failure analysis of heater tubes.

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Example: Heater Tube Failure - A boiler was experiencing several failures by tube
splitting. The boiler tube material was 2 1/4 Cr - 1 Mo. The design temperature was 538 °C
(1000 °F). The boiler had been in service for 6 years with the original tubes. Minisamples
were removed from the failed boiler tubes, and the scale depth was measured. The average
scale depth was measured as 35 mils. According to Figure 4, a temperature of 593 °C (1100
°F) corresponds to this scale thickness. This infomation provided evidence that the boiler
tubes had been operated at temperatures that were above their design limits.

Samples of Process Environments

Occasionally, samples of process streams may be required for analysis to aid in determining
the cause of failure, especially for cases of corrosion and stress corrosion cracking. Samples
should be obtained from regions as close to the failures as possible. Metal sample bombs,
glass, or polyethylene containers are usually used. The samples are analyzed for
composition and contaminants in the analytical chemistry laboratory.

Sample Preservation/Handling

Failed parts that have been removed should be sealed in Whirlpak bags, in bags that are
similar to Whirlpak, or in appropriate containers, and they should be stored indoors, if at all
possible. When multiple fracture surfaces are available, such as in the case of a fractured
shaft, one of the two matching faces may be coated with a acrylic or oil-based preservative.
The coating can be removed at the laboratory to expose uncorroded surfaces for
fractographic examination.

Shipment to the failure analysis laboratory should be arranged as soon as possible for the
following two reasons:

• To minimize corrosion or deterioration.

• To allow adequate time to obtain additional field samples if the first samples
do not provide enough information to complete the failure analysis.

Parts should be shipped in weatherproof containers, and they should be handled as the
fragile items that they indeed are. Where necessary, shipping instructions should include
precautions such as transit by vehicles that are equipped with air suspension.

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REMOVAL OF FAILED SAMPLES AND ASSOCIATED DEPOSITS

The removal of a failed sample for shipment to the Consulting Services Laboratory requires
serious attention, and, if uncertainties exist, an experienced failure analyst should be
consulted. Each failure is unique in some way. Sometimes an entire piece of equipment may
be taken out of service and sent for analysis. Examples might be valves, small pumps, or the
rotor from a small compressor. In other cases, the failed region may be disassembled from,
or cut out of the equipment or system. Figure 5 offers some helpful rules on the removal and
handling of failures.

• DO NOT sandblast, wirebrush or acid clean failed parts.


• DO NOT handle fracture surfaces.
• DO NOT flame-cut within six inches of a fracture or failure.
• DO NOT store failed items out of doors or in warehouses for
long periods of time.
• DO send a trained observer to the scene of the incident as
soon as possible to document the position of any fragments
and the surface condition of the failed parts and to collect
eyewitness accounts.
• DO contact an experienced failure analyst as soon as
possible concerning preserving, handling and shipping the
failed items.
• DO collect a complete history of the failed item including
purchase specifications, drawings, installation date and
service conditions.

Figure 5. Proper Handling of Failure Samples

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Boat Samples

Sometimes large samples cannot be cut out of the system or disassembled from equipment.
Also, some failure analyses require small samples of "good" material for comparison with
the failed region. Various types of small samples can be removed from equipment. The best
known is called a boat sample. Boat samples are taken from the wall of vessels or piping by
making congruent cuts with a cutoff wheel. The resulting sample exhibits the appearance of
a hull of a boat or canoe, and it can be machined into an impact or tensile specimen for
mechanical testing. Since repairs (and often subsequent heat treatment) to the vessel or
piping usually are required, boat sampling is not always an NDE test; however, for some
failure analyses, boat samples may be required, especially for determining impact or tensile
properties. One important consideration regarding removal of boat samples is that Saudi
Aramco Consulting Services is to be contacted before removal of the sample, especially if
the sample is to be removed from a pressure vessel.

To allow an assessment of the through thickness microstructure from a vessel, another type
sample, which is called a core sample, can be removed. Core samples up to 60mm (2.35 in.)
in diameter may be removed by means of a portable trepanning tool. The tool consists of a
hollow cylindrical saw cutter that is mounted on a drilling stand that can be strapped to the
component by adjustable chains. The cutting tool is lowered by hand and rotated up to 100
rpm by a compressed air supply mechanism. Selection of the location for sampling must be
done with utmost care so that the integrity of the component is not compromised. After the
plug has been removed, the component can be weld repaired by welding onto it a dummy
oversize stub. The above sample types are illustrated in Figure 6.

An example of where this method is used is in the examination of pressurized equipment in


wet H2S service. In some cases after internal surface inspection, crack-like indications are
found. It becomes necessary to determine whether these indications are stress corrosion
cracks, weld fabrication defects or some other form of wet H2S damage. The technique will
permit removal for laboratory examination and categorization.

Smaller surface samples, which are called “cone” samples, can also be removed. These
samples are most useful in optical metallography and fracture examinations with the
scanning electron microscope. It has been determined that a conical sample of
approximately 5mm (0.2 in) in both base diameter and height is adequate for these purposes.
Sample cutting is usually achieved by a compressed air motor driven cutter. Following
sample removal, the defect that is left in the component may be machined to a hemispherical
hole to minimize any stress concentration.

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10 20 30 40 50 60 70 80 90 100
mm

Left: Boat sample.


Right: Core-plug samples.

Figure 6. Typical Sample Shapes That are Removed


From Pressurized Field Equipment

Microbiological Samples

When microbiologically induced corrosion (MIC) is suspected, special techniques for


obtaining and handling deposit specimens may be required. Some of the more common
types of bacteria can be routinely identified microscopically. Special cases may require
identification while the bacteria are alive. In this case, special handling may involve factors
such as maintaining moisture in the sample, and shielding the sample from sunlight. Rapid
transit to a qualified laboratory may also be essential.

Sample Identity Control

Depending on the type of sample that is to be forwarded for laboratory analysis, various
types of identity control will be required; for example, in the case of heater tubes and boiler
tubes, the specific identity of the tube and the tube pass from which it was removed should
be marked on the sample at the failure site. Important locations such as tube orientation
relative to burners or height from the floor should also be indicated. Similar procedures
should be followed for other components such as rotating equipment. The orientation and
location of piping and pressure vessel parts relative to the particular piece of equipment from
which they have been removed should be maintained.

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NONDESTRUCTIVE EVALUATION (NDE) TECHNIQUES USED TO


SUPPLEMENT VISUAL FIELD EXAMINATION

Visual examination, magnetic attraction testing, and pH measurement are types of


nondestructive examination (NDE) tests. Additional, specialized NDE tests often are
employed in the field or laboratory to aid in locating failures. When a failure occurs, it is
usually necessary to inspect similar components throughout the equipment to determine if
additional, incipient failures or significantly damaged areas exist. Since complete failures are
often badly damaged due to fires or erosion that is caused by leakage, imminent failures are
often included in the failure analysis. Some of the more common NDE techniques that are
used to locate leaks, corroded regions, and cracks are discussed below. Also included are
NDE techniques that are used for materials characterization in the field. Most NDE
techniques require specially trained technicians.

Inspection Techniques

Leak/Pressure Testing

Pressure tests reveal leaks by the flow of gas or liquid through the damaged area.
Hydrostatic testing is most commonly used; however, water will seep only through relatively
large flaws, and important contaminants that are associated with the failure may be lost.
Pneumatic testing is more effective than hydrotesting, but, with pneumatic testing, there is a
greater risk of catastrophic rupture due to stored energy if failure were to occur; therefore,
pneumatic testing is more of a concern from a safety viewpoint. Helium leak detection,
where sensitive detectors can locate leaks at relatively low internal pressures, is sometimes
preferred for locating failures such as tight cracks.

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Liquid Penetrant Testing (PT)

Liquid or dye penetrant testing is a relatively simple technique that is used to locate surface
defects. Liquid penetrant spread on the sample seeps into small cracks or defects. After the
excess penetrant is wiped or washed from the surface, a developer, which draws the
penetrant to the surface to reveal small defects, is applied. See Figure 7. The penetrant either
contains a bright visible dye or fluorescent particles that are visible under ultraviolet (black)
light. Liquid penetrant tests can be used for magnetic or nonmagnetic materials. The main
disadvantage of PT in failure analyses is contamination of the failed region. Figure 7
displays the steps in the liquid penetrant procedure.

Figure 7. General Steps for Water-Washable PT Technique

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Magnetic Particle Testing (MT)

Magnetic particle testing can be used to detect defects at or near a surface of ferromagnetic
materials. Two steps in the technique are as follows:

• Magnetization of the test piece by means of alternating current for surface


defects or direct current for subsurface defects.

• Application of finely divided magnetic particles in either a dry powder or


suspended in a liquid. The magnetic particles, in forming visible indications,
are attracted to the leakage flux that is created by the magnetic field.

Magnetic particle inspection is most effective when it is used to detect small cracks. As with
PT, contamination of the failed region is a concern in failure analysis. In recent years, wet
flourescent magnetic particle testing has served as a useful method for detection of various
types of wet H2S cracking in refinery vessels.

Eddy Current Testing

When a coil that is conducting alternating current is placed in proximity to a sample, eddy
currents are set up in the sample by magnetic induction. Defects within the material cause, in
the current, distortions that can be metered, usually by oscilloscope. Materials to be tested
must be electrically conductive, and reference standards are required. The advantage of this
NDE technique is that the sample is not contaminated by liquids. This technique is
particularly useful for inspecting exchanger tube bundles by probing from the ID.

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Ultrasonic Testing (UT)

The ultrasonic inspection technique (Figure 8) uses low energy, high frequency sound waves
to measure wall thickness or to detect defects in materials. Sound waves are beamed into the
test material and reflected from surfaces or discontinuities. Based on the time for return of
the echoes, metal thickness can be determined or defects located, usually by calibration with
reference standards.

Figure 8. Principles of Ultrasonic Testing

The UT technique is especially useful in failures that involves corrosion and wall thinning.
Unique properties of this technique are useful for finding cracks. For example, cracks in
studbolts can be found by contacting the bolt ends while the equipment is bolted together.
Except for the possible contamination from liquid or gel couplant that is used between the
probe and sample, the UT technique does not present problems in the failure analysis.

Boroscope Examination

A boroscope is a tool which is used to access and visually inspect areas of a part or piece of
equipment. Boroscopes come in various sizes (lengths and diameters) and may contain
glass, fiber, or electronic (camera) optics. boroscopes are especially useful for inspecting the
ID surfaces of heat exchanger tubes.

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Figure 9. Advantages and Limitations of Inspection Methods

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Radiography

Radiography is one of the most widely used NDE techniques. Radiation is directed through
the material of interest, and a photographic image is recorded on film that is located on the
opposite side. The X-rays are often used for laboratory radiography. Field testing more often
employs a gamma ray source. Radiography can be useful in locating failures, and it presents
no problems in the subsequent failure analysis.

In general, the following facts cover all NDE techniques:

• Each failure can be unique and result in unique test procedures and results.

• Nondestructive tests are often qualitative, and they should be followed by


destructive tests.

• Skill and experience are needed to select the best test method and to establish
the best test procedure for a specific case.

• Interpretation of test results usually requires the use of highly trained experts.

Figure 9 describes some of the advantages and limitations of the above inspection methods.

Field Microscopy

Portable microscopes are available for in situ metallographic examination in the field when
samples cannot be removed for laboratory analysis. Some of the applications include
determination of microstructure (including sensitization of stainless steels), examination for
creep fissures and hydrogen attack, and the study of crack morphologies.

The procedure that is used to prepare the specimen surface in the field involves polishing
and etching that is similar to the procedure that is performed in the laboratory (COE 106.07).
Before polishing, surface scale must be thoroughly removed with a portable grinding wheel
(typically attached to a drill). Successively finer grit disks are then used to produce a smooth
finish that finally is polished with alumina, diamond paste, or electrolytically.

Portable microscopes do not have the optical quality of laboratory optical metallographs.
Furthermore, the polishing process is complicated by dirty field conditions as well as by
curved or irregular sample surfaces. It is for these reasons that in situ metallography is best
suited for qualitative observation by skilled personnel; for example, in cases where
overheating of austenitic stainless steel equipment may have caused undesirable
sensitization, in situ metallography may be used to identify regions where replacement is
necessary.

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Replication

An alternative to in situ metallographic examination is surface replication of the field


sample. The polished surface of the selected specimen is prepared according to routine
procedures for field metallography. A replica of the surface then is obtained by means of
one of several possible replication materials such as acetate or silicon rubber (RTV). The
commonly used acetate technique involves pressing acetate tape that is wetted with acetone
on the specimen surface. When the surface has dried, the tape is removed as a negative
replica as demonstrated in Figure 10. The replica can then be taken back to the laboratory
where it can be shadowed to improve contrast and where it can be examined by optical or
electron microscopy.

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Figure 10. Surface Replication Using Acetate Tape

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The acetate replication technique offers several advantages over silicon rubber. This
technique is capable of achieving high quality metallographs in the laboratory. It is also
totally nondestructive, and it can be used for periodic monitoring. The replicas provide a
permanent record of observations, and they can be stored. Because the replicas can be
examined at high magnification in the scanning electron microscope, a very high degree of
resolution can be achieved. This technique is capable of detecting damage in highly
localized regions, but acetate replication also has some limitations as follows:

• Replicas can only be taken at accessible locations.

• The replicas give no information regarding volumetric changes.


Indiscriminate replication can be expensive and counterproductive.

• Because there is some variability in interpretation of replicas, evaluations can


sometimes differ.

At present, the acetate replication technique is used principally for reproducing surface
features such as small cracks, fissures, creep cavities and gross microstructural features. The
RTV technique, which involves covering the area to be replicated with RTV and allowing to
cure before peeling away the replica, is useful for macroscopic investigation of larger cracks
and defects.

The first requirement for field applications of metallographic methods to components is


identification of the locations to be sampled or replicated. Although preinspection stress
analysis is helpful, location selection still requires judgement that comes only with
experience. Some typical sites for field metallography include:

• Known hot spots on high temperature equipment.

• Welds that are associated with known stress concentrations.

• Locations with prior history of failure.

• Locations with flaw indications, as determined by NDE techniques.

After the locations that require inspection have been identified, the exact sampling position
must be selected. Positions that are likely to represent the most damaged parts of the
component are the positions that should be chosen.

Field Chemical Analyses

A simple test used in the field is the pH test to determine acid or basic conditions. If the
sample is moist, direct contact with pH paper can indicate the pH. If the sample is dry, use

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distilled or deionized (DI) water of known pH. (Test the water with the pH paper.) Then, wet
the sample with the water using as little water as possible to avoid dilution, and measure the
pH.

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There are various instruments and techniques for alloy identification in the field. The
simplest tool is the hand-held magnet for distinguishing iron alloys. Chemical spot tests are
also used to sort alloys. Portable spot testing kits are available for field use in the
identification of various steels, aluminum alloys, copper alloys, and silver alloys.

Most chemical spot tests involve the addition of drops of a test chemical to the unknown
material. Reactions such as color changes or bubbling indicate the alloy or specific elements
within the alloy; for example, to test for carbon steel, one drop of 50 % nitric acid to a clean
metal surface for five minutes will cause a brown spot to appear after flushing with water.
Some additional spot test techniques are included in Figure 11, and more test technique
details are available in Reference 6.

Magnetic Test Since the Type 300 series stainless steels are nonmagnetic
under most conditions, they are easily distinguished from the
magnetic steels by this test.
Copper Chloride Test A drop of 20 % copper chloride solution in admiralty brass
leaves a black spot if the brass is inhibited. This test is a
simple test for inhibited brass.
Chromium Spot Test The chromium content of alloy steels may be estimated by
the reaction rates with various concentrations of nitric acid.
Nitric Acid Spot Test Monel and other copper bearing white metals may be
distinguished from steel by the reaction rate in nitric acid.

Figure 11. Commonly Used Alloy Identification Tests

Today, portable nuclear analysis is the preferred method of in situ chemical analysis. This
method is an energy dispersive X-ray spectroscopic (EDS) analysis technique whereby the
elements in the sample give off characteristic X-rays after being excited by electrons or
gamma rays. The laboratory scanning electron microscope (SEM) utilizes its high voltage
electron beam as the excitation source. The portable analyzer has a gamma ray source. A
detailed description of EDS principles is given in COE 106.07.

The portable nuclear analyzer is accurate enough for most alloy identifications; however,
laboratory SEM-EDS is more accurate, and it offers the additional option of analyzing
lighter elements such as carbon and oxygen when the system is equipped with a light
element spectrometer.

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Portable Hardness Tests

Metal hardness is a characteristic that frequently can be indicative of prior heat treatment,
method of fabrication, degree of cold work or even, in some cases, alloy type. A primary
interest in hardness measurements has been the determination of whether heat treatment of
hardenable grades has been adequate. The following discussion describes one of the most
frequently used portable hardness testing methods: the Telebrinneler.

The Telebrinneler uses a hardened and accurately ground steel ball as an indenter. This ball
is placed between a calibrated bar of known hardness and the work piece. When a force is
applied to the bar, the ball makes an indentation in both pieces of the material. The ratio of
the depth of the impression in the bar and the depth of the impression in the work piece is
proportional to the ratio of the hardness of the bar and the work piece, and it is independent
of the force that is applied. Since the impressions are spherical, depths, which can be
determined by direct measurement of the impression diameters, are proportional to the
square of their diameters.

Recently, several electronic portable hardness devices have appeared on the market. An
advantage of the new devices is that the impression left on the workpiece is very small and
less of a stress riser. Also, the devices are quick and easy to operate. Disadvantages involve
accuracy, which is questionable for certain devices. Inexperienced operators also can misuse
these devices, and obtain inaccurate results.

Figure 12 indicates some of the important features of the Telebrinneller.

Accuracy Spec +- 3%; actual +- 5%

Range 100-500 BHN

Safety No unsafe aspects

Size of Ball 10.0 mm (0.3937 inch)

Number of Balls 1

Manufacturer Teleweld, Inc.


416 North Park St.
Streator, IL 61364

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Figure 12. Significant Features of the Telebrinneller

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FLOW PATH FOR FIELD FAILURE ANALYSIS PROCEDURES

An example of a typical flow path for field failure analysis procedures is illustrated in Figure
13.

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Figure 13. Field Failure Analysis Procedure Flow Chart

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COMPLETING A FAILURE ANALYSIS INFORMATION FORM

Use of a well-documented systematic procedure to gather field information is a major step in


the determination of the cause of a failure; therefore, one of the most important parts of a
failure analysis is the information report form. This form is usually the way information is
forwarded to the laboratory failure analyst. A typical failure analysis information form is
shown in Figure 14.

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Failure Analysis Information Form

Location ____________________________________________________Date _________________________

Local Contact ______________________________________________________________________________

Unit_______________________________________________________________________________________

Type of Equipment _____________________________________Manufacturer _________________________

Component ________________________________________________________________________________

Size ______________________________________________________________________________________

Date of Failure _____________________________________ Length of Service_________________________

Material of Construction_______________________________________________________________________

Temperature _____________________________________________Pressure _________________________

Environment________________________________________________________________________________

Corrosives Present (including concentration)______________________________________________________

__________________________________________________________________________________________

Location of Failure___________________________________________________________________________

__________________________________________________________________________________________

Nature of Failure ____________________________________________________________________________

__________________________________________________________________________________________

Unusual Circumstances Related to Failure________________________________________________________

__________________________________________________________________________________________

__________________________________________________________________________________________

Previous Failures____________________________________________________________________________

Tentative Cause_____________________________________________________________________________

Sample Taken ______________________________________________________________________________

Comments _________________________________________________________________________________

__________________________________________________________________________________________

__________________________________________________________________________________________

Investigator ________________________________________________________________________________

(Use reverse side of this sheet for sketches of other additional information)

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Figure 14. Typical Failure Analysis Information Form

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Key Information

Key information is provided by the field engineer in the failure analysis information form.
After identification of location and the field contact engineer, the form is used to identify the
following: unit, type of equipment, manufacturer of equipment, and component. For
example, if a production unit fire occurred in a pump, the failure analysis form would be
used to indicate the type of pump, the manufacturer, and, if possible, the exact component
that failed, e.g., the pump shaft.

Other information may or may not be available, but every effort should be made to supply as
much information as possible on the form. The actual operating temperature or pressure at
the time of failure may not have been recorded. In such a case, operating conditions as close
to the time of failure as possible should be listed and so indicated. A review of prior
inspection results may further supplement the above information by identifying previous
problems. Such a review could, for example, reveal that a previous repair may have taken
place that has a direct bearing on the cause of failure.

The failure analysis information form also provides space for the field engineer to describe
the nature of the failure (for example, visual appearance) and report any other unusual
circumstances which could be related to the failure. Space also is provided to speculate on
tentative causes of failure. Such speculation about possible causes of failure is optional, but
could aid in the laboratory failure analysis. Lastly, the samples taken should be identified
along with the field investigator, if different from the local contact. Sketches, can be made
on the back of the form.

Background Information

Since the failure analyst can not always be present when the preliminary diagnosis of a
failure is made, it is important for the engineer who is responsible for the equipment to
recognize the type of information that may be required. The various types of information
that are required include the following:

• Design conditions. This information can be obtained from equipment data


sheets and specifications.

• Operating conditions/history including upset and lay-up conditions.

• Eye witness accounts.

Often all of the background information may not fit on the failure analysis information form.
In such cases, the additional information can be attached to the form.

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Equipment Specifications

The equipment specifications can offer useful information on design conditions that should
be compared with operating conditions; for example, in the case of exchanger tubing, and
depending on the type of alloy that is used, certain velocity limitations must be followed to
prevent high rates of corrosion. In the case of heater tubes, maximum tube metal
temperatures must be maintained. In the case of rotating equipment such as pumps, certain
operating conditions must be maintained. Very often, in the case of rotating equipment,
manufacturer’s specifications can be supplemented by direct discussions with the equipment
supplier. For example, the operating parameters of the failed component may have been
provided by another supplier, and the original equipment manufacturer can supply additional
requirements that may be of importance to the investigation. In one case, the equipment
supplier was able to provide important information on fabrication of a gear. It was learned
that the gear was induction hardened; however, the hardening method, as shown in the
laboratory examination, was not properly performed.

Operating Conditions/History

An excellent source that is used to determine failure modes and failure causes for many
components and structures is operating experience and data. Operating conditions must be
obtained from records and recorded data; for example, temperatures may be recorded
periodically with thermocouples or optical pyrometers. Pressure gage measurements are also
recorded, and, in some cases, feed stream composition is available. This information should
be compared with design limits. This information is pertinent to defining functional
requirements and expected as well as unexpected loadings for components and structures.
Insight on failure modes and potential causes can be gained from these data. For instance,
locations in piping systems that are susceptible to fatigue or erosion can be determined by
noting those locations where frequent thermal transients or high flow rates occur.

Eye Witness Accounts

Sometimes, eye witness accounts may be of importance. In the case of a reactor, observation
of hot spots may be of importance, and they should be noted. Sometimes, unusual noises
that were heard prior to failure may be of importance. A bearing failure in a pump may have
created a sound that should be noted. Photographs that have been taken at the failure site are
also very important. If photos cannot be taken, a sketch can be made. Also, history of
previous failures should be recorded. The expert opinion of the personnel who have first-
hand experience from operating and maintaining the equipment of interest is another
valuable source of information. These people may know of prior failures, malfunctions,
degradation, and human errors that are not documented but are extremely important to the
investigation.

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GLOSSARY

Acoustic Emission NDE technique for measuring stress waves that are emitted
Testing (AE) from discontinuities in materials under stress.

chemical spot testing Identification of alloy by way of surface reaction.

control sample/control Undamaged material that is used to compare with failed


specimen material in failure analyses.

Eddy Current Testing NDE technique whereby eddy currents are set up by
(ET) electromagnetic induction and used to reveal defects in
conductive materials.

energy dispersive X-ray Chemical analysis by characteristic x-radiation.


spectroscopy

explosion Sudden bursting of an enclosure such as a vessel due to


overpressurization.

flocculent Fluffy; resembling wool.

hydrotesting Pressurizing with water for leak detection.

hygroscopic Readily taking up and retaining moisture.

in situ metallography Microscopic examination that is conducted in the field.

incipient failure A failure that is beginning to become apparent. For example, a


tube that has thinned by corrosion beyond the calculated
minimum wall thickness where failure is imminent.

Liquid Penetrant Testing NDE technique for detecting surface flaws by means of a liquid
(PT) penetrant and developer.

Magnetic Particle Testing NDE technique that uses magnetic particles for detecting
(MT) surface or subsurface defects in ferromagnetic materials.

Nondestructive Examination by methods that do not destroy or impair the


Examination (NDE) serviceability of the part.

pneumatic testing Gas (usually air) pressure testing for leak detection. For use
with low pressure testing only.

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portable nuclear analysis Field chemical analysis with x-rays.

sample (test sample) Generally a large quantity of material (failed or control) or


associated deposits, scale, or corrosion product that is obtained
in the field. Specimens for specific chemical or physical tests
that are subsequently obtained from the sample.

specimen Portion of a sample that is designated or fabricated (for


example, a tensile bar) for a specific chemical or physical test.

surface replication Removal of surface characteristics by way of plastic replica.

Ultrasonic Testing (UT) NDE technique that uses ultrasonic waves to determine defects
or remaining thickness.

vapor cloud Flammable fuel that is dispersed in the air. When ignited, high
pressures can result in a “vapor cloud explosion.”

volatile Readily vaporizable at low temperatures.

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REFERENCES

1. D. R. McIntyre and W. G. Ashbaugh, MTI Publication No. 30, “Guidelines


for Assessing Fire and Explosion Damage,” Materials Technology Institute of
the Chemical Process Industries, Inc., published by National Association of
Corrosion Engineers, Houston, TX, USA, 1990.

2. R. D. Merrick and M. L. Bullen, “Prevention of Cracking in Wet H2S


Environments”, NACE Corrosion ’89 , Paper No. 269, National Association
of Corrosion Engineers, Houston, TX, USA, 1989.

3. American Society for Metals (ASM), “Failure Analysis and Prevention,”


Metals Handbook, Ninth Ed., Vol. 11, Metals Park, OH, USA, 1986.

4. American Society for Metals (ASM), "Nondestructive Evaluation and Quality


Control," Metals Handbook, Ninth Ed., Vol. 17, Metals Park, OH, USA,
1989.

5. American Society for Metals (ASM), “Nondestructive Inspection and Quality


Control," Metals Handbook, Eighth Ed., Vol. 11, Metals Park, OH, USA,
1976.

6. American Petroleum Institute (API), Guide to Refinery Inspections, Ch. 4,


Washington, DC, USA, 1972.

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