CHAPTER

Modern analytical
techniques in failure analysis
of aerospace, chemical, and
oil and gas industries
2
Seifollah Nasrazadani*, Shokrollah Hassani†
Engineering Technology Department, University of North Texas, Denton, TX, USA*
BP America Inc., Houston, TX, USA†

CHAPTER OUTLINE
1 Microscopy Techniques ...................................................................................... 39
1.1 Optical Microscopy ............................................................................. 39
1.2 Scanning Electron Microscopy ............................................................. 40
1.3 Focused Ion Beam ............................................................................. 41
2 Chemical and Radiographic Analysis ................................................................... 42
2.1 Energy Dispersive Spectroscopy .......................................................... 42
2.2 X-Ray Fluorescence ............................................................................ 44
2.3 X-Ray Diffraction ................................................................................ 45
2.4 Fourier Transform Infrared Spectrophotometry ...................................... 46
2.5 X-Ray Photoelectron Spectroscopy ....................................................... 47
2.6 Radiography ...................................................................................... 49
2.7 Neutron Radiography .......................................................................... 50
2.8 X-Ray Radiography ............................................................................. 51
2.9 Gamma-Ray Radiography .................................................................... 52
2.10 Fluoroscopic Radiography ................................................................. 53
3 Conclusion and Future Outlook ............................................................................ 53
References .............................................................................................................. 53

1 MICROSCOPY TECHNIQUES
1.1 OPTICAL MICROSCOPY
Human curiosity about the shapes and appearance of objects at both macro and micro
scales has helped us develop microscopes with higher resolving powers. Human eyes
with resolution power of 0.1 mm are not sufficient to observe features smaller than
0.1 mm. Therefore, microscopes with higher resolution are needed to examine mate-
rials’ features at micro, nano, or angstrom size. By definition, optical resolution is
Handbook of Materials Failure Analysis With Case Studies from the Oil and Gas Industry.
http://dx.doi.org/10.1016/B978-0-08-100117-2.00010-8
Copyright © 2016 Elsevier Ltd. All rights reserved.
39
40 CHAPTER 2 Modern analytical techniques in failure analysis

defined as the shortest distance between two points that can be differentiated. Optical
microscopes can resolve features approximately 0.2 mm apart. The resolving power
of optical microscopes represents three orders of magnitude improvement over that
of human eyes. Applications of optical microscopes in the oil and gas industry
includes but not limited to geoscience studies, mineral identification, microfossils
and biostratification, geochronology as well as porosity analysis. Among the men-
tioned applications, porosity analysis appears to be more popular due to the fact that
the presence of interconnected pores affects permeability of oil and gas in sandstones
and this facilitates oil and gas extraction from a reservoir.

1.2 SCANNING ELECTRON MICROSCOPY

Scanning electron microscopy (SEM) is the most popular technique in the analysis of
failed components in the oil and gas industry. The popularity of SEM is due to the
fact that failure mode(s) can be easily identified through morphological features
obtained from analysis of the fracture surfaces. Specifically one can look for forma-
tion of dimples in a fracture surface of a highly ductile alloy such as low carbon steels
as well as all nonferrous alloys, such as aluminum and copper, indicating severe plas-
tic deformation prior to failure. High carbon steels hardened through heat treatment
processes can undergo brittle fracture when exposed to subzero temperatures or a
sudden blow, exhibiting cleavage fracture morphology that is indicative of fast frac-
ture without any demonstration of plastic deformation. Ferrous and nonferrous alloys
experiencing fatigue typically exhibit striation marks indicating application of a cyclic
load prior to failure. Oftentimes alloys experiencing fatigue failure demonstrate stri-
ation marks but absence of striation marks does not eliminate the possibility of fatigue
failure. Figure 2.1a–c show examples of ductile failure (a), brittle failure (b), and
fatigue failure (c).
One of the issues in the oil and gas industry is flow-accelerated corrosion (FAC).
SEM has been effectively used in identification of the flow regime based on mor-
phology of the damaged steel surfaces. Steel pipes used in the oil and gas industry
where highly energetic fluids such as steam passing through elbows (Figure 2.2a)
cause severe FAC in carbon steels and even alloy steels showing scalloped formation

15 kV 700X 20 µm 20.0k V 500 10 μm 1k 10 μm

(a) (b) (c)
FIGURE 2.1
SEM micrographs showing morphologies of ductile failure (a), brittle failure (b), and
fatigue failure (c).
 1 Microscopy Techniques 41

FIGURE 2.2
Elbow section of a small bore pipe used to transfer single-phase steam (a) and corresponding
SEM micrograph (b). Basic principle of SEM.

shown in a single-phase flow regime (Figure 2.2b) whereas two-phase flow regime
results in the formation of tiger bands.
A SEM image is formed in an electron gun through a shower of electrons
(
100 nA) produced by either thermionic or field emission mechanisms. Primary
electrons bombard surface of the sample under investigation to produce secondary
electrons through the inelastic collision of primary electrons and valence electrons
orbiting the nucleus of the samples’ atoms. A set of electromagnetic lenses guide the
shower of electrons to raster sample surface where as a scanning coil controls the
spot size of the electron shower. A secondary electron detector is used to collect them
and be utilized in image formation. Backscattered electrons are also produced
through elastic collision between primary electrons and the nucleus of the sample
atoms that can be collected using a backscattered electron detector to produce an
image with differentiable contrast in regions with concentration of high atomic num-
ber as compared to those of low atomic number elements. X-ray signals are also pro-
duced and utilized for chemical identification of materials on the surface of atoms.
This aspect will be discussed in detail in the following sections.
Samples used in SEM analysis must be vacuum (106 torr) compatible though
recent developments in new designs of SEMs (called environmental SEM) capable
of operating at pressure of 13 torr that is much closer to atmospheric pressure
(760 torr). Exposure of nonconductive samples to an electron shower results in elec-
trical charging of the sample producing a useless image with glaring spots. Deposi-
tion of
100 Å gold or carbon coating eliminates the charging issue.

1.3 FOCUSED ION BEAM

Focused ion beam (FIB) technique is analogous to SEM with the exception of using
Ga ions in place of electrons (used in SEM) to form an image. FIB has a highly
enhanced resolution that allows observation of much finer features such as porosity
42 CHAPTER 2 Modern analytical techniques in failure analysis

FIGURE 2.3
FIB image showing cross-section of a mineral containing porosity. Mineral is coated
in a Ag coating protecting the metal from milling process.

in core samples cut and drilled in the geological analysis for oil and gas industry used
in oil exploration efforts. Application of FIB in core sample analysis reduces oil and
gas explorations’ risks. Pore analysis can provide quantitative chemical analysis of
minerals that contain pores at nanometer scale. Organic matters also contain pores at
the nanometer scale that require highly resolved images to be observed. Simulta-
neous observations on pore size and chemical quantification can be achieved through
transmission electron microscopy (TEM). FIB can be used to prepare samples for
TEM analysis saving sample preparation time and cost.
Sample preparation to the nanometer thickness has been a challenge in the past
but the advent of FIB has reduced time and cost needed for sample preparations for
TEM significantly. Figure 2.3 shows a FIB image of a mineral sample containing
pores. Measured thickness shows the mineral oxide formed on a metallic pipe that
is covered with silver coating (top layer) which is normally deposited on the mineral
surface for mineral protection. The cut sample is welded to a probe to be transported
to a TEM microscope for further analysis.

2 CHEMICAL AND RADIOGRAPHIC ANALYSIS

2.1 ENERGY DISPERSIVE SPECTROSCOPY
The energy dispersive spectroscopy (EDS) technique is mostly used for qualitative
analysis of materials but is capable of providing semi-quantitative results as well.
Typically, SEM instrumentation is equipped with an EDS system to allow for the
chemical analysis of features being observed in SEM monitor. Simultaneous SEM
 2 Chemical and Radiographic Analysis 43

and EDS analysis is advantageous in failure analysis cases where spot analysis
becomes extremely crucial in arriving at a valid conclusion. Signals produced in
an SEM/EDS system includes secondary and backscattered electrons that are
used in image forming for morphological analysis as well as X-rays that are
used for identification and quantification of chemicals present at detectable con-
centrations. The detection limit in EDS depends on sample surface conditions,
smoother the surface the lower the detection limit. EDS can detect major and
minor elements with concentrations higher than 10 wt% (major) and minor
concentrations (concentrations between 1 and 10 wt%). The detection limit for
bulk materials is 0.1 wt% therefore EDS cannot detect trace elements (concentra-
tions below 0.01 wt%) [1]. A typical EDS spectrum is shown in Figure 2.4 produced
from spring housing failure of tubing retrievable safety valve assembly used in
oxygenated water in field location testing for the oil and gas industry. Spectrum
shows expected major elements such as Fe and O due to corrosion products of
ferrous base alloy along with minor elements such as Cl, Ca, and Si which were
due to contamination.
EDS technique is capable of producing elemental distribution maps, an example
of which is shown in Figure 2.5. SEM image on the left corner shows patches of salt
particles that correspond to Na and Cl maps indicated in the dot map images.

FIGURE 2.4
EDS spectrum of a field samples used in oil and gas exploration project.
44 CHAPTER 2 Modern analytical techniques in failure analysis

SEM O Na Si

Cl Cr Fe

FIGURE 2.5
Dot map of a failed component used in oil and gas exploration component showing patchy salt
on surface and corresponding Na and Cl distribution.

2.2 X-RAY FLUORESCENCE

X-ray fluorescence (XRF) is an elemental analysis technique that provides quantita-
tive chemical information. The detection limit of XRF is better than that of EDS and
the concentration of trace elements can be detected using XRF. The major difference
between EDS and XRF is in the signal collection mechanism. Whereas EDS uses a Si
(Li) detector, XRF uses an analytical crystal to differentiate X-rays coming off of the
sample surface. This makes XRF peak resolution better than that of EDS. An ana-
lytical crystal of known composition provides fixed interplanar spacing between
planes of atoms within the crystal that facilitates differentiation of X-rays emitted
from a sample under investigation. Figure 2.6 shows schematic diagram of a typical
XRF detection system.
Elemental identification for qualitative and quantitative analysis in XRF tech-
nique is based on Bragg’s law of diffraction given as:

nl ¼ 2dhkl siny

where n represents order of diffraction, l is the X-ray’s wavelength, dhkl is the inter-
planar spacing, and y represents incident and diffraction angle. Various materials
used as analytical crystals offering a wide range of interplanar spacing along with
a wide range of diffraction angle allows for detection and quantification of most
materials of technological importance. Therefore, dispersion of wavelength in a
multi-element containing sample can be easily utilized for its chemistry with high
degree of precision and accuracy. XRF is preferred over EDS due to the fact that
XRF provides quantitative information as compared to the semi-quantitative nature
of data produced using the EDS technique.
 2 Chemical and Radiographic Analysis 45

Sample
X-ray source

Detector

Analytical
crystal

FIGURE 2.6
Schematic diagram of X-ray detection system used in XRF technique.

2.3 X-RAY DIFFRACTION

X-ray diffraction (XRD) is a highly versatile technique that provides chemical informa-
tion for elemental analysis as well as for phase analysis. Besides chemical characteri-
zation, XRD is extremely useful for stress measurements as well as for texture
analysis. Samples to be analyzed using XRD must be crystalline however the technique
can provide the degree of crystallinity in polymers. XRD has traditionally been used for
bulk sample’s analysis but with the advent of new optical systems thin film analysis can
also be carried out using XRD. The technique uses Bragg’s law of diffraction as was
discussed earlier. Typical output of an XRD experiment is shown in Figure 2.7.

FIGURE 2.7
XRD pattern of carbon steel sheet showing major peaks of body-centered cubic structure.
46 CHAPTER 2 Modern analytical techniques in failure analysis

3000 (3 1 1)

d=2.5352/2θ=35.377
2500 (4 4 0)

d=1.4844/2θ=62.520
(2 2 0) (5 1 1)
(4 0 0) (5 3 3)

d=1.6168/2θ=56.904
d=2.9759/2θ=30.003
(4 2 2)

d=2.1001/2θ=43.035
(2 2 2)

d=1.2806/2θ=73.956
d=1.7148/2θ=53.386
Intensity (Counts)

2000

d=2.4290/2θ=36.978
1500

1000

500

0
10 20 30 40 50 60 70 80 90
Theta (deg)
FIGURE 2.8
XRD pattern of a corroded low carbon steel pipe damaged through flow-accelerated
corrosion.

The XRD technique is mainly used for phase identification of corrosion products
in the oil and gas industry. For example, XRD effectively differentiates between
iron oxides (FeO, Fe2O3, and Fe3O4) and oxyhydroxides (a-FeOOH, b-FeOOH,
g-FeOOH). Since the XRD technique identified phases based on their crystal struc-
tures, the technique cannot separate Fe2O3 and Fe3O4 due to the fact that both these
phases have a similar crystal structure and very close lattice parameter. The author
has shown the application of Fourier transform infrared spectrophotometry (FTIR) in
successful identification of all iron oxides (including Fe2O3 and Fe3O4) and oxyhydr-
oxides. Calcite and other Ca containing phase formation on ferrous alloys used in oil
exploration projects can be identified using XRD. In addition, XRD can be used in
crystalline phase analysis of concrete and related materials. Typical XRD pattern of
iron oxide is shown in Figure 2.8. The peaks in the XRD spectrum belong to Fe3O4
phase for different crystallographic planes identified as (hkl) with their correspond-
ing d-spacing (d) values in Å.

2.4 FOURIER TRANSFORM INFRARED SPECTROPHOTOMETRY

FTIR utilizes infrared light as the probing beam and enjoys the advantages of being a
fast, reliable, and safer technique (as compared to XRD and XRF that utilize X-rays
as probe beam). FTIR was originally developed for characterization of organic
 2 Chemical and Radiographic Analysis 47

matters but now a great deal of inorganic materials analysis is being done with FTIR.
As indicated earlier, the author has used FTIR extensively for the characterization of
iron oxides and hydroxides. FTIR has been shown to be capable of even quantitative
analysis of iron oxides [2–5]. Spectra of a large number of phases are available
through commercial libraries and have been published in literature by many inves-
tigators around the world. All three phases of matter (solids, liquids, and gases) can
be analyzed using FTIR and analysis of thin film materials is also possible using
reflectance mode. Sample preparation and data interpretation through comparison
of fingerprint spectra comparison can easily be done. Recently, hand-held FTIR
spectrometers have been made commercially available, making the technique highly
appealing for quick field sample analysis where immediate decisions have to be
made. Capital cost of the FTIR instruments and analysis of cost per sample are less
expensive by far as compared to other techniques that provide nearly the same type of
information.
The FTIR technique is based on infrared light absorption in the wavelength
range of 2.5-25 mm by the material under investigation, resulting in the occur-
rence of a mechanical motion of different forms with the molecule or compound
atoms. Light energy absorption is not haphazard but follows a highly precise pat-
tern. Atoms within molecules and compounds can undergo mechanical motions
such as stretching and bending. Electronic transition may also occur due to
absorption of light in the IR range. Small energy differences resulting from vibra-
tional and rotational states in different compounds are the basis of FTIR analysis
for organic matter analysis. In inorganic materials such as oxides bonds between
constituents of oxides (Fe and O in iron oxides) results in the appearance of
absorption bands in their FTIR. Therefore, fingerprint FTIR spectra of different
oxides can be easily compared for their identifications. Figure 2.9 shows a typical
FTIR spectrum of an iron oxide containing magnetite (Fe3O4) as indicated by
absorption band at wavenumber 570 cm1. The vertical axis of FTIR spectra rep-
resents the number of photons absorbed in an arbitrary unit of intensity and the
horizontal axis for mid-IR region represents 2.5-25 mm. In terms of corresponding
wavenumber, 2.5 mm corresponds to wavenumber 4000 cm1 and 25 mm corre-
sponds to 400 cm1 wavenumber.
The aerospace industry extensively uses aluminum alloys for structural purposes.
Corrosion products of aluminum can be either Al2O3 or oxyhydroxides of aluminum
and FTIR can be used to identify these compounds. Figure 2.10 shows FTIR spectrum
of aluminum compounds.
FTIR is used in analysis of paint systems, epoxies, cement constituents, etc.

2.5 X-RAY PHOTOELECTRON SPECTROSCOPY

Also known as electron spectroscopy for chemical analysis, ESCA is a surface-
sensitive technique that is extremely useful for the identification of oxidation states
in multivalent elements such as oxides of iron and chromium. Corrosion products
and constituents of thin films deposited for protection of engineering alloys used
48 CHAPTER 2 Modern analytical techniques in failure analysis

20 4340 flakes
19
18
17

865.83
16
15

575.71
453.12
14
% Transmittance

13
12
11

1629.97
10
9
8
7
6
5
3448.35

4000 3500 3000 2500 2000 1500 1000 500

Wavenumbers (cm–1)

FIGURE 2.9
FTIR spectra of iron oxides.

8.5 Tue Aug 12 15:20:23 2014 (GMT-05:00)

8.0
7.5
7.0
6.5
6.0
5.5
% Transmittance

5.0
4.5
1408.70

4.0
1633.48

3.5
3.0
848.78
955.04

2.5
2.0
1.5
1.0
58.60

0.5
3500 3000 2500 2000 1500 1000 500
Wavenumbers (cm–1)

FIGURE 2.10
FTIR spectra of aluminum oxides.
 2 Chemical and Radiographic Analysis 49

Fe-2p
Sputtering 10 min (21 min) O-1s
Cr-2p
C-1s

Sputtering 5 min (11 min)

Intensity (a.u.)

Sputtering 5 min (6 min)

Sputtering 1 min

Surface

1200 1000 800 600 400 200 0

Binding energy (ev)
FIGURE 2.11
XPS spectra of Cr3+-substituted Fe3O4 films on carbon steel.

in the oil and gas industry are analyzed using X-ray photoelectron spectroscopy
(XPS). Typically, the top few monolayers are analyzed and the technique has etching
provisions that allows layer-by-layer removal of materials to facilitate depth profil-
ing for qualitative and quantitative elemental analysis.
Chromium conversion coatings are proven to be effective in reducing corrosion of
engineering alloys used in the oil and gas industry. However, Cr (VI) is known as a
potentially health hazardous material and human exposure to materials containing
Cr (VI) should be avoided. XPS has successfully been applied in identification and quan-
tification of Cr (VI) [6,7]. The first author has deposited Cr substituted magnetite
(Fe3O4) on carbon steel substrates and applied XPS to detect the presence of chromium
containing iron oxide as shown in Figure 2.11. XPS spectra of a chromium-substituted
magnetite that was sputtered for a 21 min duration and reduction in the intensity of
Cr-2p and C-1s peaks along with increase in intensity of O-1s and Fe-2p peaks were
observed. The changes in XPS spectra indicate relative depth at which Cr3+ substituted
for Fe3+. When photoelectrons from a certain depth of the oxide were detected, the
presence of a Cr-free oxide was verified as only the oxygen and iron peaks were
detected.

2.6 RADIOGRAPHY
Radiography is a nondestructive inspection technique used for materials failure anal-
ysis investigation in different industries including oil, gas, and aerospace. This tech-
nique is an internal examination of materials using X-ray, gamma-ray, or neutron
50 CHAPTER 2 Modern analytical techniques in failure analysis

Source of
radiation

Small discontinuities: Material

1. Inclusions under investigation
2. Flacks
3. Micro fissures Void
Surface
delamination
Cracks

Darkened area Radiography film Darkened area

After processing
FIGURE 2.12
Radiography ability for detecting different types of defects and discontinuities in materials.

radiation. Radiography is based on the differential adsorption of the penetrating radi-

ation into the target material. Radiation is directed through the sample to a photog-
raphy film. Path length of radiation and density of sample are the two main
parameters determining the intensity of light passing through the sample and creating
contrast on the photographic film. Internal discontinuities such as porosity and
cracks can be detected using this technique. However, smaller discontinuities such
as small inclusions, flacks, and micro fissures are hard or impossible to detect using
this technique. The direction of the crack is also an important determining factor
using radiography technique. Cracks perpendicular to the radiation are less likely
to be detected since they are similar to small discontinuities in terms of radiation path
length. Therefore, laminar flaws on the surface are hard to detect using this technique
(Figure 2.12). The radiography technique can be used for most of the materials while
needing low surface preparation. Safety precautions are some of the important lim-
itations of this technique [8–11]. All sources of radiation are potentially dangerous
and personal protection is required for using these techniques [12].

2.7 NEUTRON RADIOGRAPHY

Neutron radiography is a nondestructive technique for radiographic imaging, mainly
used for inspection [13]. Neutron radiography uses neutron radiation instead of X-ray
or gamma-ray [10] and it is considered as a complimentary technique to X-ray radi-
ography [14]. It is suitable for components that are not X-ray opaque such as organic
materials, hydrogen atoms in water [15], and hydrogenous materials surrounded by
metal [16]. In general, neutron radiography can be used for materials with a very high
atomic number (very heavy materials) and a very low atomic number (very light
 2 Chemical and Radiographic Analysis 51

Failed valve Good valve

Failed "O" Ring

FIGURE 2.13
Neutron radiography for detecting O-ring failure in a valve [16].

materials) which X-ray and gamma-ray are not able to inspect [13]. Metals are not
neutron opaque and therefore can be distinguished from organic compounds using
this technique. Figure 2.13 shows an example of neutron radiography used for detect-
ing O-ring failure in a valve.

2.8 X-RAY RADIOGRAPHY

X-rays are emitted as a result of the interaction between a rapid moving stream of
electrons and atoms in a solid target material. X-ray radiography is suitable for com-
plex geometries which are difficult to inspect with ultrasonic techniques [17]. The
principle component of an X-ray unit is shown in Figure 2.14. X-ray radiation
can be recorded on film which is black/white/gray, fluorescent screen which is

Cathode structure High-voltage

power supply

Low-voltage Filament Electron

power beam
supply
Target

Anode
Focal structure
Focusing cup
spot

Tube
X-ray beam envelope
FIGURE 2.14
Schematic of the principle components of an X-ray unit [13].
52 CHAPTER 2 Modern analytical techniques in failure analysis

colorful or by a radiation monitor [14]. Materials with very high atomic number (very
heavy materials) or very low atomic number (very light materials) are hard to inspect
using X-ray or gamma-ray radiography techniques. In this case, neutron radiography
can be used [13]. X-rays are generally attenuated more by materials of high density
than by materials of low density.

2.9 GAMMA-RAY RADIOGRAPHY

Gamma rays are electromagnetic radiation emitted from decay of an unstable source
such as radioactive isotope (e.g., Co 60, Ir 192, Cs 139, Tm 70) [13,17]. Each isotope
has specific characteristics which makes it suitable for certain applications. Gamma
ray energy levels are constant and its energy intensity decays with time [13]. Gamma
rays are similar to X-rays and are suitable for detection of nonplanar defects [13].
X-rays and gamma-rays are capable of penetrating into opaque materials and detect
because of their relatively short wavelength (high energy) [13]. Table 2.1 shows a
comparison of suitability of three different radiographic methods for the inspection
of light and heavy metals.

Table 2.1 Comparison of suitability of three radiographic methods for the

inspection of light and heavy metals [13]
Suitability of light metals Suitability of heavy metals

Film Film Film Film

Inspection with Real-time with with Real-time with
application X-ray radiography Y-ray X-ray radiography Y-ray

General
Surface cracks F(C) F F(C) F(C) F F(C)
Internal cracks F(C) F F(C) F(C) F F(C)
Voids G G F F G G
Thickness F G F F G F
Metallurgical F F F F F F
variations
Service
Fatigue and heat F(C) F P(C) P P P
cracks
Stress corrosion F F P F F P
Blistering P P P P P P
Thinning F F F F F F
Corrosion pits F F P G G P
Note: G, good; F, fair; P, poor; (c) radiation beam must be parallel to the cracks, laps, or flakes. In real
time radiography, the testpiece can be manipulated for proper orientation.
 References 53

2.10 FLUOROSCOPIC RADIOGRAPHY

Fluoroscopic radiography is similar to X-ray radiography but it has the option for
real-time viewing of X-ray radiography. Fluoroscopic radiography can be used
for composite materials and also for molded plastic [17].

3 CONCLUSION AND FUTURE OUTLOOK

Analytical techniques applicable to failure analysis in different industrial sectors have
evolved in past few decades and enhancement of such techniques has been taking place
and even intensified in recent years. New analytical procedures and data analysis
based on existing techniques and instrumentation are being developed constantly.
It is anticipated that modern characterization tools based on enabling technolo-
gies be developed in future to facilitate better characterization of failed components
used in oil and gas industry. Optical and energy resolution of research instruments
are being improved continuously and it is expected that practitioners will have
resources available to them that make analysis of corroded and/or failed components
faster, easier, and less costly.

REFERENCES
[1] Goldstein J, Newbury D, Joy D, Lyman C, Echlin P, Lifshin E, et al. Scanning electron
microscopy and x-ray microanalysis. 3rd ed. New York: Springer; 2003.
[2] Namduri H, Nasrazadani S. Quantitative analysis of iron oxides using Fourier transform
infrared spectroscopy. Corros Sci 2008;50:2493–7.
[3] Nasrazadani S. Application of IR spectroscopy for study of phosphoric and tannic acids
interactions with magnetite, goethite, and lepidocrocite. Corros Sci 1997;39(10–
11):1845–59.
[4] Nasrazadani S, Raman A. The application of infrared spectroscopy to the study of rust
systems. Corros Sci 1993;34(8):1355–65.
[5] Nasrazadani S, Namduri H. Study of phase transformation in iron oxides using laser
induced breakdown spectroscopy (LIBS). Spectrochim Acta B 2006;61:565–71.
[6] Murphy V, Tofail SAM, Hughes H, McLoughlin P. A novel study of hexavalent chro-
mium detoxification by selected seaweed species using SEM-EDX and XPS analysis.
Chem Eng J 2009;148:425–33.
[7] Zhanga X, van den Bosa C, Sloofa WG, Hovestadb A, Terrync H, de Wit JHW.
Comparison of the morphology and corrosion performance of Cr(VI)- and Cr(III)-based
conversion coatings on zinc. Surf Coat Technol 2005;199:92–104.
[8] Heidersbach R. Metallurgy and corrosion control in oil and gas production; John Wiley
& Son; 2011. ISBN 978-0-470-24848-5.
[9] Becker WT, Shipley RJ. ASM handbook: volume 11: failure analysis and prevention;
John Wiley & Son; 2011 2002.
[10] ASM International Handbook Committee. ASM handbook, volume 17 – nondestructive
evaluation and quality control, ASM International; 1989. http://www.asminternational.
org/materials-resources/results/-/journal_content/56/10192/06070G/PUBLICATION.
54 CHAPTER 2 Modern analytical techniques in failure analysis

[11] Raj B, Venkataraman B. Practical radiography; 2004. http://app.knovel.com/web/toc.v/

cid:kpMHMILH04/viewerType:toc/root_slug:military-handbook-mil-6/b-off-set:0/b-cat-
name:Nondestructive%20Testing%20%26%20Evaluation/b-cat-slug:nondestructive-
testing-evaluation/b-cat-id:679/b-off-set:0/b-order-by:name/b-sort-by:ascending/b-filter-
by:all-content.
[12] Smith P. Piping materials guide – selection and applications. Burlington, MA USA:
Elsevier; 2005.
[13] Bray DE, Stanley RK. Nondestructive evaluation: a tool in design, manufacturing and
service; 1996. http://app.knovel.com/web/toc.v/cid:kpMHMILH04/viewerType:toc/
root_slug:military-handbook-mil-6/b-off-set:0/b-cat-name:Nondestructive%20Testing
%20%26%20Evaluation/b-cat-slug:nondestructive-testing-evaluation/b-cat-id:679/b-
off-set:0/b-order-by:name/b-sort-by:ascending/b-filter-by:all-content.
[14] Aircraft Inspection and Repair by Federal Aviation Administration Federal Aviation
Administration. http://app.knovel.com/web/toc.v/cid:kpMHMILH04/viewerType:toc/
root_slug:military-handbook-mil-6/b-off-set:0/b-cat-name:Nondestructive%20Testing
%20%26%20Evaluation/b-cat-slug:nondestructive-testing-evaluation/b-cat-id:679/b-
off-set:0/b-order-by:name/b-sort-by:ascending/b-filter-by:all-content.
[15] Dance WE, Middlebrook JB. Neutron radio-graphic nondestructive inspection for
bonded composite structures, nondestructive evaluation and flaw criticality for compos-
ite materials. In: Pipes RB, editor. ASTMSTP 696. Philadelphia, PA: American Society
for Testing and Materials; 1979. p. 57–71.
[16] Berger H. In: Symposium on practical applications of neutron radiography and gaging.
ASTM International, American Society for Testing and Materials; 1976, Committee E-7

on nondestructive testing, american society for testing and materials, Etats-Unis.
National Bureau of Standards.
[17] Military handbook – MIL-HDBK-793(AR): nondestructive active testing techniques for
structural composites. U.S. Department of Defense. http://app.knovel.com/web/toc.v/
cid:kpMHMILH04/viewerType:toc/root_slug:military-handbook-mil-6/b-off-set:0/b-
cat-name:Nondestructive%20Testing%20%26%20Evaluation/b-cat-slug:nondestruc
tive-testing-evaluation/b-cat-id:679/b-off-set:0/b-order-by:name/b-sort-by:ascending/b-
filter-by:all-content.