Identification of alloys using quantitative chemical analysis is an essential step during a metallurgical failure analysis process. There are several methods available for quantitative analysis of metal alloys, and the analyst should carefully approach selection of the method used. The choice of appropriate analytical techniques is determined by the specific chemical information required, the condition of the sample, and any limitations imposed by interested parties. This article discusses some of the commonly used quantitative chemical analysis techniques for metals. The discussion covers the operating principles, applications, advantages, and disadvantages of optical emission spectroscopy (OES), inductively coupled plasma optical emission spectroscopy (ICP-OES), X-ray spectroscopy, and ion chromatography (IC). In addition, information on combustion analysis and inert gas fusion analysis is provided.

X-ray spectroscopy is generally accepted as the most useful ancillary technique that can be added to any scanning electron microscope (SEM), even to the point of being considered a necessity by most operators. While “stand-alone” x-ray detection systems are used less frequently in failure analysis than the more exact instrumentation employed in SEMs, the technology is advancing and is worthy of note due to its capability for nondestructive analysis and application in the field. This article begins with information on the basis of the x-ray signal. This is followed by information on the operating principles and applications of detectors for x-ray spectroscopy, namely energy-dispersive spectrometers, wavelength-dispersive spectrometers, and handheld x-ray fluorescence systems. The processes involved in x-ray analysis in the SEM and handheld x-ray fluorescence analysis are then covered. The article ends with a discussion on the applications of x-ray spectroscopy in failure analysis.

A coil made of a nickel-chromium alloy (Material No. 2.4869) with approx. 80Ni and 20Cr had burned through after a brief period of operation as a heating element in a brazing furnace. The protective atmosphere consisted of an incompletely combusted coal gas. Furnace temperature reached 1150 deg C. This type of selective oxidation at which the easily oxidized chromium burns, while the nickel is not attacked, is caused by mildly oxidizing gases and is sometimes designated as green rot. Under these conditions, chromium-containing steels and alloys whose oxidation resistance is based upon formation of tight oxide layers are not stable.

Chemical analysis is a critical part of any failure investigation. With the right planning and proper analytical equipment, a myriad of information can be obtained from a sample. This article presents a high-level introduction to techniques often used for chemical analysis during failure analysis. It describes the general considerations for bulk and microscale chemical analysis in failure analysis, the most effective techniques to use for organic or inorganic materials, and examples of using these techniques. The article discusses the processes involved in the chemical analysis of nonmetallics. Advances in chemical analysis methods for failure analysis are also covered.

Work rolls made of indefinite chill double-poured (ICDP) iron are commonly used in the finishing trains of hot-strip mills (HSMs). In actual service, spalling, apart from other surface degeneration modes, constitutes a major mechanism of premature roll failures. Although spalling can be a culmination of roll material quality and/or mill abuse, the microstructure of a broken roll can often unveil intrinsic inadequacies in roll material quality that possibly accentuate failure. This is particularly relevant in circumstances when rolls, despite operation under similar mill environment, exhibit variations in roll life. The paper provides an insight into the microstructural characteristics of spalled ICED HSM work rolls, which underwent failure under similar mill operating environment in an integrated steel plant under the Steel Authority of India Limited. Microstructural features influencing ICDP roll quality, viz. characteristics of graphite, carbides, martensite, etc., have been extensively studied through optical microscopy, quantitative image analysis (QIA), and electron-probe microanalysis (EPMA). These are discussed in the context of spalling propensity and roll life.

Penetration by molten copper occurred in the economizer of a large water-tube boiler. A cross section through a weld and the crack in the tube revealed a crack was an intergranular fissure. Small fissures of the same type also extended from its flanks. The main fissure was filled with an oxide scale in which were embedded particles having the appearance of metallic copper. It was concluded that the cracking that occurred at the time of re-welding was due to intergranular penetration by copper present in the deposit within the tubes, which had not been completely removed prior to welding. Subsequently, it was ascertained that trouble had been experienced with the centrifugal feed pumps, resulting in scuffing of some bronze rings. The presumption is that bronze particles had been carried in mechanical suspension in the feed water and deposited in the economizer tubes.

The quantitative characterization of fracture surface geometry, that is, quantitative fractography, can provide useful information regarding the microstructural features and failure mechanisms that govern material fracture. This article is devoted to the fractographic techniques that are based on fracture profilometry. This is followed by a section describing the methods based on scanning electron microscope fractography. The article also addresses procedures for three-dimensional fracture surface reconstruction. In each case, sufficient methodological details, governing equations, and practical examples are provided.

Nineteen out of 26 bolts in a multistage water pump corroded and cracked after a short time in a severe working environment containing saline water, CO 2 , and H 2 S. The failed bolts and intact nuts were to be made from a special type of stainless steel as per ASTM A 193 B8S and A 194. However, the investigation (which included visual, macroscopic, metallographic, SEM, and chemical analysis) showed that austenitic stainless steel and a nickel-base alloy were used instead. The unspecified materials are more prone to corrosion, particularly galvanic corrosion, which proved to be the primary failure mechanism in the areas of the bolts directly exposed to the working environment. Corrosion damage on surfaces facing away from the work environment was caused primarily by chloride stress-corrosion cracking, aided by loose fitting threads. Thread gaps constitute a crevice where an aggressive chemistry is allowed to develop and attack local surfaces.

Admiralty brass (Alloy C44300) cooling tubes which were part of a heat exchanger in a turbogenerator that provided electricity to a manufacturing plant failed. A mixture of non-recirculating city and “spring pit” water flowed through bundles of tubes to cool the oil in which they are immersed. However, a problem developed when several of the brass tubes cracked transversely, allowing cooling water to mix with the oil. The presence of a tensile stress, intergranular cracks, and a corrosion product suggested the tube failures resulted from stress-corrosion cracking. The main corrosion product was cupric hydroxychloride. In addition to switching to a more corrosion-resistant alloy, extreme care should be taken in the manufacturing of the replacement tube bundles to avoid imparting any residual tensile stresses in the tubing. Analyses of city and spring-pit water were recommended also, to determine which contained the least-harmful corrosive chemicals.

After a quick-release fitting of an ejection seat broke, an investigation was performed to determine the manner and cause of crack propagation. Most fractography-based investigations aim to characterize only qualitative characteristics, such as the fracture orientation and origin position, topology, and details of interactions with microstructural features. The aim of this investigation was to use quantitative fractography as a tool to extract information, including striation spacing and size of the stretched zone, in order to make a direct correlation with fracture mechanic concepts. As the crack propagated, striations were created on the fracture surface as a result of service-induced load changes. The size of the striations were measured to estimate crack propagation rate. Remaining lifetime estimates were also made. The dimensions of plastically stretched zones found at the tips of the cracks were evaluated using electron micrograph stereo image pairs to characterize local fracture toughness. To complete the failure analysis, nondestructive evaluation, metallographic examination, and chemical investigations were carried out. No secondary cracks could be found. Most of the broken parts showed that the microstructure, the hardness, and the chemical composition of the Al-alloy were within the specification, but some of the cracked parts were manufactured using a different material than that specified.

A fracture mechanics based failure analysis and life prediction of a large centrifugal fan made from low-carbon, medium-strength steel was undertaken following shortcomings in attempts to explain its fatigue life from start stop cycles alone. Measurements of the fracture toughness and flaw size at failure, coupled with quantitative SEM fractography using striation spacing methods, revealed that the cyclic stress amplitudes just prior to failure were much larger than expected, in this particular case. Subsequent improvements in fan design and fabrication have effectively alleviated the problem of slow, high cycle fatigue crack growth, at normal operating stresses in similar fans.

A masonry type drill bit, designed for impact drilling in rock, fractured after a short time in service. Samples of the failed bit were analyzed using optical and scanning electron microscopy, quantitative metallography, and chemical analysis. The composition was found to be that of 18CrNi3Mo steel. Investigators also found evidence of inclusions and prior austenite grain size, although it was determined that neither played a role in the failure. Rather, according to test data, the failure occurred because of stress concentration (due to geometric discontinuities along the tooth profiles) and the cumulative effect of torque and force loading (the byproduct of continuous twisting and axial impact). Cracks readily initiate under these conditions then propagate quickly through what was found to be networks of tempered martensite, thus resulting in premature failure.

Cracking was discovered in an in-service, second-stage turbine impeller during a downtime inspection. The fabricated 4300 series low-alloy steel impeller was used in a compressor in an industrial petrochemical plant. It was also reported that a process upset had allowed a 10% NaOH solution to be ingested by the unit. Routine magnetic particle inspection revealed numerous cracks in the hub area and vane tips of the second-stage impeller Additionally, the outside surface of the backing plate showed a cyclic pattern of cracks. An overview of a conventional, systematic metallurgical approach to failure analysis to confirm that the cracking was caused by a caustic stress-corrosion cracking mechanism is presented.

Although a precise understanding of roll failure genesis is complex, the microstructure of a broken roll can often unravel intrinsic deficiencies in material quality responsible for its failure. This is especially relevant in circumstances when, even under a similar mill-operating environment, the failure involves a particular roll or a specific batch of rolls. This paper provides a microstructural insight into the cause of premature breakage of a second-intermediate Sendzimir mill drive roll used at a stainless steel sheet rolling plant under the Steel Authority of India Limited. Microstructural issues influencing roll quality, such as characteristics of carbides, tempered martensite, retained austenite, etc., have been extensively studied through optical and scanning electron microscopy, electron-probe microanalysis, image analysis, and x-ray diffractometry. These are discussed to elucidate specific microstructural inadequacies that accentuated the failure. The study reveals that even through retained austenite content is low (6.29 vol%) and martensite is non-acicular, the roll breakage is a consequence of intergranular cracking caused by improper carbide morphology and distribution.

An investigation was conducted to determine the cause of numerous cracks and other defects on the surface of a cast ASTM A743 grade CA-15 stainless steel main boiler feed pump impeller. The surface was examined using a stereomicroscope, and macrofractography was conducted on several cross sections removed from the impeller body. Areas that appeared to have the most severe surface damage were sectioned, fractured open, and examined using SEM. The chemistry of the impeller and an apparent repair weld were also analyzed. The examination indicated that the cracks were shrinkage voids from the original casting process. Surface repair welds had been used to fill in or cover over larger shrinkage cavities. It was recommended that more stringent visual and nondestructive examination criteria be established for the castings.

The intermediate pressure (IP) turbine of a thermal generating station is driven by steam from the boiler's reheater. On one particular IP turbine, a thick deposit was found on the insides of the rotor blade shrouds in two instances two years apart. The source of the deposits was not known; bulk chemical analysis had simply shown that iron was a major component. Optical microscopy and electron microprobe analysis were used to identify the deposits. In the first instance, the deposit was found to be debris that was left in the reheater tubes during boiler modification and swept to the turbine by the steam. There were still some of these debris particles present when the incident two years later was investigated but generally the second deposit was found to be of two layer oxide particles which were shown to have spalled from 2-14% chromium reheater tube surfaces.

Several compressor disks in military fighter and trainer aircraft gas turbine engines cracked prematurely in the bolt hole regions. The disks were made of precipitation-hardened AM355 martensitic stainless steel. Experimental and analytical work was performed on specimens from the fifth-stage compressor disk (judged to be the most crack-prone disk in the compressor) to determine the cause of the failures. Failure was attributed to high-strain low-cycle fatigue during service. It was also determined that the cyclic engine usage assumed in the original life calculations had been under estimated, which led to low-cycle fatigue cracking earlier than expected. Fracture mechanics analysis of the disks was carried out to assess their damage tolerance and to predict safe inspection intervals.

A type 430Ti stainless steel flue gas expansion joint cracked because of caustic-induced stress-corrosion cracking. Energy-dispersive X-ray spectroscope analysis of the fracture surface deposits revealed the presence of sodium and potassium—caustics in hydroxide form. Primary fracture surfaces were all similar in appearance, and a primary crack origin could not be identified. A secondary crack brought to fracture in the laboratory showed brittle, cleavage features rather than classic, tensile overload features. This suggested that the material was embrittled.